Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'M. Mazzanti' _publ_contact_author_address ; Departement de Recherche Fondamentale sur la Matiere Condensee Laboratoire de Reconnaissance Ionique CEA - Grenoble 17 rue des Martyrs Grenoble F-38054 FRANCE ; _publ_contact_author_email MAZZANTI@DRFMC.CENG.CEA.FR _publ_section_title ; Fixation of atmospheric CO2 by a dimeric lanthanum hydroxide complex; Assembly of an unusual hexameric carbonate. ; loop_ _publ_author_name 'M. Mazzanti' 'Louise Natrajan' 'Jacques Pecaut' # Attachment 'cifstruc1.doc.pdf' data_struc[La(tpen)(Otf)3].CH3CN,_1 _database_code_depnum_ccdc_archive 'CCDC 285413' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (La(tpen)(Otf)3).CH3CN _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H31 F9 La N7 O9 S3' _chemical_formula_weight 1051.72 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.733(6) _cell_length_b 16.032(7) _cell_length_c 17.135(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.697(7) _cell_angle_gamma 90.00 _cell_volume 4020(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 1.320 _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 293(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 17176 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 23.47 _reflns_number_total 5841 _reflns_number_gt 5246 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0738P)^2^+1.5126P] 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 5841 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La La 0.915393(12) 0.298721(11) 0.750573(10) 0.02059(11) Uani 1 1 d . . . N1 N 1.0198(2) 0.30041(16) 0.88960(18) 0.0271(7) Uani 1 1 d . . . N2 N 0.93153(19) 0.45402(18) 0.81478(16) 0.0273(6) Uani 1 1 d . . . N3 N 1.02920(19) 0.16373(18) 0.78264(16) 0.0285(7) Uani 1 1 d . . . N4 N 0.8710(2) 0.18341(18) 0.85377(18) 0.0283(7) Uani 1 1 d . . . N5 N 0.78301(19) 0.36052(19) 0.84657(16) 0.0311(7) Uani 1 1 d . . . N6 N 0.90731(19) 0.43158(17) 0.65608(17) 0.0283(7) Uani 1 1 d . . . C1 C 1.1045(2) 0.2502(2) 0.8883(2) 0.0303(8) Uani 1 1 d . . . H1A H 1.1308 0.2401 0.9420 0.036 Uiso 1 1 calc R . . H1B H 1.1482 0.2826 0.8629 0.036 Uiso 1 1 calc R . . C2 C 1.0906(2) 0.1680(2) 0.8468(2) 0.0287(8) Uani 1 1 d . . . C3 C 1.1444(3) 0.0997(3) 0.8728(3) 0.0413(10) Uani 1 1 d . . . H3 H 1.1867 0.1042 0.9173 0.050 Uiso 1 1 calc R . . C4 C 1.1343(3) 0.0258(3) 0.8324(3) 0.0479(11) Uani 1 1 d . . . H4 H 1.1702 -0.0201 0.8487 0.058 Uiso 1 1 calc R . . C5 C 1.0699(3) 0.0208(3) 0.7670(3) 0.0452(10) Uani 1 1 d . . . H5 H 1.0609 -0.0287 0.7388 0.054 Uiso 1 1 calc R . . C6 C 1.0197(3) 0.0907(2) 0.7446(2) 0.0358(9) Uani 1 1 d . . . H6 H 0.9765 0.0872 0.7006 0.043 Uiso 1 1 calc R . . C7 C 0.9657(2) 0.2660(2) 0.9500(2) 0.0305(8) Uani 1 1 d . . . H7A H 0.9202 0.3067 0.9609 0.037 Uiso 1 1 calc R . . H7B H 1.0061 0.2571 0.9982 0.037 Uiso 1 1 calc R . . C8 C 0.9184(2) 0.1849(2) 0.9259(2) 0.0280(8) Uani 1 1 d . . . C9 C 0.9211(3) 0.1167(3) 0.9744(2) 0.0456(10) Uani 1 1 d . . . H9 H 0.9528 0.1194 1.0245 0.055 Uiso 1 1 calc R . . C10 C 0.8767(3) 0.0443(3) 0.9489(3) 0.0539(12) Uani 1 1 d . . . H10 H 0.8799 -0.0027 0.9810 0.065 Uiso 1 1 calc R . . C11 C 0.8276(3) 0.0423(3) 0.8753(3) 0.0442(10) Uani 1 1 d . . . H11 H 0.7963 -0.0055 0.8568 0.053 Uiso 1 1 calc R . . C12 C 0.8265(2) 0.1133(2) 0.8302(2) 0.0347(9) Uani 1 1 d . . . H12 H 0.7931 0.1127 0.7807 0.042 Uiso 1 1 calc R . . C13 C 0.8407(3) 0.4949(2) 0.8126(2) 0.0353(9) Uani 1 1 d . . . H13A H 0.8176 0.5068 0.7584 0.042 Uiso 1 1 calc R . . H13B H 0.8481 0.5477 0.8404 0.042 Uiso 1 1 calc R . . C14 C 0.7724(2) 0.4433(2) 0.8485(2) 0.0312(8) Uani 1 1 d . . . C15 C 0.7002(3) 0.4816(3) 0.8804(2) 0.0429(10) Uani 1 1 d . . . H15 H 0.6948 0.5394 0.8803 0.051 Uiso 1 1 calc R . . C16 C 0.6374(3) 0.4331(3) 0.9119(2) 0.0475(11) Uani 1 1 d . . . H16 H 0.5882 0.4575 0.9326 0.057 Uiso 1 1 calc R . . C17 C 0.6480(3) 0.3481(3) 0.9128(2) 0.0460(11) Uani 1 1 d . . . H17 H 0.6070 0.3140 0.9352 0.055 Uiso 1 1 calc R . . C18 C 0.7205(3) 0.3142(3) 0.8796(2) 0.0380(9) Uani 1 1 d . . . H18 H 0.7270 0.2565 0.8799 0.046 Uiso 1 1 calc R . . C19 C 0.9870(3) 0.5063(2) 0.7668(2) 0.0321(8) Uani 1 1 d . . . H19A H 1.0497 0.4867 0.7732 0.038 Uiso 1 1 calc R . . H19B H 0.9867 0.5636 0.7850 0.038 Uiso 1 1 calc R . . C20 C 0.9495(2) 0.5027(2) 0.6810(2) 0.0302(8) Uani 1 1 d . . . C21 C 0.9578(3) 0.5689(2) 0.6312(2) 0.0396(9) Uani 1 1 d . . . H21 H 0.9870 0.6176 0.6499 0.048 Uiso 1 1 calc R . . C22 C 0.9223(3) 0.5624(3) 0.5532(2) 0.0437(10) Uani 1 1 d . . . H22 H 0.9276 0.6065 0.5188 0.052 Uiso 1 1 calc R . . C23 C 0.8791(3) 0.4899(2) 0.5270(2) 0.0391(9) Uani 1 1 d . . . H23 H 0.8547 0.4840 0.4748 0.047 Uiso 1 1 calc R . . C24 C 0.8729(2) 0.4264(2) 0.5798(2) 0.0318(8) Uani 1 1 d . . . H24 H 0.8434 0.3774 0.5621 0.038 Uiso 1 1 calc R . . C25 C 1.0495(2) 0.3874(2) 0.9114(2) 0.0303(8) Uani 1 1 d . . . H25A H 1.0979 0.4035 0.8807 0.036 Uiso 1 1 calc R . . H25B H 1.0743 0.3884 0.9664 0.036 Uiso 1 1 calc R . . C26 C 0.9731(2) 0.4502(2) 0.8983(2) 0.0313(8) Uani 1 1 d . . . H26A H 0.9261 0.4359 0.9312 0.038 Uiso 1 1 calc R . . H26B H 0.9966 0.5049 0.9143 0.038 Uiso 1 1 calc R . . S1 S 0.95441(6) 0.20062(5) 0.55086(6) 0.0305(2) Uani 1 1 d . . . F1S1 F 0.79800(18) 0.13818(19) 0.48799(16) 0.0669(8) Uani 1 1 d . . . F2S1 F 0.89176(19) 0.1692(2) 0.40632(14) 0.0648(7) Uani 1 1 d . . . F3S1 F 0.81887(19) 0.26586(19) 0.45821(16) 0.0674(8) Uani 1 1 d . . . O1S1 O 0.90957(17) 0.22418(17) 0.61950(15) 0.0348(6) Uani 1 1 d . . . O2S1 O 1.00978(19) 0.26444(19) 0.52373(18) 0.0502(7) Uani 1 1 d . . . O3S1 O 0.9905(2) 0.11825(18) 0.55489(16) 0.0480(7) Uani 1 1 d . . . C1S C 0.8605(3) 0.1932(3) 0.4716(3) 0.0416(10) Uani 1 1 d . . . S2 S 0.67504(6) 0.26741(6) 0.63613(5) 0.0301(2) Uani 1 1 d . . . F1S2 F 0.58056(18) 0.2303(3) 0.75076(15) 0.0685(9) Uani 1 1 d . . . F2S2 F 0.5838(2) 0.3606(2) 0.72458(17) 0.0698(8) Uani 1 1 d . . . F3S2 F 0.50158(18) 0.2782(3) 0.64714(18) 0.0925(12) Uani 1 1 d . . . O1S2 O 0.75261(18) 0.2749(2) 0.69522(17) 0.0519(8) Uani 1 1 d . . . O2S2 O 0.6599(2) 0.18553(18) 0.60556(19) 0.0527(8) Uani 1 1 d . . . O3S2 O 0.6670(2) 0.33328(18) 0.58001(16) 0.0486(7) Uani 1 1 d . . . C2S C 0.5800(3) 0.2854(3) 0.6932(3) 0.0478(11) Uani 1 1 d . . . S3 S 1.15873(6) 0.36957(6) 0.70433(5) 0.0322(2) Uani 1 1 d . . . F1S3 F 1.31166(19) 0.31130(19) 0.6670(2) 0.0837(11) Uani 1 1 d . . . F2S3 F 1.2386(2) 0.2254(2) 0.7317(2) 0.0829(10) Uani 1 1 d . . . F3S3 F 1.1937(2) 0.2478(2) 0.6107(2) 0.0909(11) Uani 1 1 d . . . O1S3 O 1.07347(15) 0.32926(16) 0.71797(15) 0.0322(6) Uani 1 1 d . . . O2S3 O 1.1511(2) 0.42392(19) 0.63852(17) 0.0508(8) Uani 1 1 d . . . O3S3 O 1.20820(19) 0.4001(2) 0.77499(18) 0.0527(8) Uani 1 1 d . . . C3S C 1.2289(3) 0.2829(3) 0.6765(3) 0.0548(13) Uani 1 1 d . . . N7 N 0.8527(3) 0.4077(3) 0.0599(3) 0.0705(12) Uani 1 1 d . . . C31 C 0.7883(3) 0.4268(3) 0.0850(3) 0.0502(11) Uani 1 1 d . . . C32 C 0.7060(3) 0.4531(3) 0.1176(3) 0.0589(12) Uani 1 1 d . . . H32A H 0.7134 0.4436 0.1733 0.088 Uiso 1 1 calc R . . H32B H 0.6547 0.4216 0.0937 0.088 Uiso 1 1 calc R . . H32C H 0.6956 0.5114 0.1074 0.088 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 0.01338(15) 0.02570(17) 0.02298(16) 0.00137(7) 0.00339(10) -0.00042(6) N1 0.0187(16) 0.0308(17) 0.0323(17) 0.0011(12) 0.0054(13) -0.0022(11) N2 0.0227(15) 0.0315(16) 0.0281(15) -0.0026(12) 0.0044(12) 0.0002(12) N3 0.0209(15) 0.0324(17) 0.0331(16) 0.0058(13) 0.0063(13) 0.0010(12) N4 0.0209(16) 0.0322(16) 0.0329(17) 0.0020(13) 0.0083(13) -0.0033(13) N5 0.0209(15) 0.0429(19) 0.0300(16) -0.0033(13) 0.0051(13) 0.0020(13) N6 0.0232(15) 0.0290(16) 0.0337(17) 0.0043(13) 0.0070(13) 0.0013(12) C1 0.0184(18) 0.037(2) 0.034(2) 0.0036(16) -0.0036(15) 0.0011(15) C2 0.0163(17) 0.035(2) 0.037(2) 0.0077(16) 0.0102(15) 0.0015(15) C3 0.029(2) 0.042(2) 0.053(2) 0.0115(19) 0.0034(18) 0.0079(17) C4 0.040(2) 0.039(2) 0.067(3) 0.011(2) 0.016(2) 0.0154(19) C5 0.053(3) 0.034(2) 0.053(3) -0.0021(19) 0.024(2) 0.0050(19) C6 0.036(2) 0.035(2) 0.038(2) -0.0028(17) 0.0098(17) -0.0022(17) C7 0.0286(19) 0.037(2) 0.0263(19) 0.0015(15) 0.0040(15) -0.0037(16) C8 0.0162(18) 0.038(2) 0.030(2) 0.0029(16) 0.0048(15) -0.0018(15) C9 0.045(2) 0.052(3) 0.038(2) 0.0125(19) -0.0019(19) -0.010(2) C10 0.061(3) 0.044(3) 0.055(3) 0.018(2) 0.000(2) -0.014(2) C11 0.037(2) 0.040(2) 0.056(3) 0.0037(19) 0.006(2) -0.0155(18) C12 0.0243(19) 0.040(2) 0.040(2) 0.0003(18) 0.0061(16) -0.0065(16) C13 0.035(2) 0.037(2) 0.034(2) -0.0020(16) 0.0073(17) 0.0115(17) C14 0.0224(18) 0.044(2) 0.0278(19) -0.0017(15) 0.0049(15) 0.0076(16) C15 0.037(2) 0.054(3) 0.038(2) -0.0051(19) 0.0067(18) 0.016(2) C16 0.031(2) 0.072(3) 0.042(2) -0.006(2) 0.0149(19) 0.014(2) C17 0.028(2) 0.072(3) 0.040(2) -0.003(2) 0.0138(18) -0.004(2) C18 0.025(2) 0.050(2) 0.040(2) 0.0007(18) 0.0079(18) -0.0053(17) C19 0.030(2) 0.0266(19) 0.041(2) -0.0012(15) 0.0079(16) -0.0016(15) C20 0.0228(18) 0.031(2) 0.038(2) 0.0011(16) 0.0088(16) 0.0026(15) C21 0.040(2) 0.034(2) 0.047(2) 0.0053(18) 0.0165(19) -0.0033(17) C22 0.049(2) 0.041(2) 0.044(2) 0.0167(19) 0.018(2) 0.0036(19) C23 0.039(2) 0.046(2) 0.034(2) 0.0083(18) 0.0122(17) 0.0038(18) C24 0.0267(19) 0.037(2) 0.032(2) 0.0039(16) 0.0045(16) 0.0014(15) C25 0.0248(18) 0.033(2) 0.0317(19) -0.0009(15) -0.0001(15) -0.0067(15) C26 0.032(2) 0.033(2) 0.0295(19) -0.0048(15) 0.0034(15) -0.0053(16) S1 0.0221(5) 0.0387(6) 0.0315(5) -0.0035(4) 0.0071(4) 0.0017(3) F1S1 0.0444(15) 0.090(2) 0.0648(17) -0.0103(15) 0.0005(13) -0.0288(15) F2S1 0.0649(18) 0.098(2) 0.0323(13) -0.0146(14) 0.0082(12) 0.0004(16) F3S1 0.0587(18) 0.0738(19) 0.0636(18) -0.0039(15) -0.0194(14) 0.0227(15) O1S1 0.0261(14) 0.0466(15) 0.0326(14) -0.0066(12) 0.0076(11) 0.0020(12) O2S1 0.0384(17) 0.0615(19) 0.0536(18) -0.0025(15) 0.0179(14) -0.0148(14) O3S1 0.0500(18) 0.0488(17) 0.0460(16) -0.0036(13) 0.0089(14) 0.0186(14) C1S 0.038(3) 0.049(3) 0.038(2) -0.0062(18) 0.0034(19) 0.0013(19) S2 0.0178(4) 0.0414(5) 0.0311(5) -0.0027(4) 0.0035(4) -0.0011(4) F1S2 0.0567(19) 0.101(2) 0.0511(18) 0.0117(15) 0.0187(15) -0.0278(15) F2S2 0.0666(19) 0.084(2) 0.0610(16) -0.0096(17) 0.0173(14) 0.0352(16) F3S2 0.0174(14) 0.204(4) 0.0554(19) -0.013(2) 0.0017(13) 0.0018(18) O1S2 0.0170(14) 0.098(2) 0.0404(17) -0.0175(16) 0.0018(12) -0.0002(14) O2S2 0.058(2) 0.0434(17) 0.0561(19) -0.0098(14) 0.0053(16) -0.0020(14) O3S2 0.0571(19) 0.0471(17) 0.0437(16) 0.0048(13) 0.0147(14) -0.0034(14) C2S 0.021(2) 0.083(3) 0.040(2) 0.000(2) 0.0039(18) -0.001(2) S3 0.0210(5) 0.0373(5) 0.0397(5) 0.0039(4) 0.0092(4) -0.0036(4) F1S3 0.0264(15) 0.084(2) 0.148(3) 0.001(2) 0.0410(18) 0.0007(13) F2S3 0.063(2) 0.0654(18) 0.125(3) 0.033(2) 0.0280(19) 0.0235(16) F3S3 0.073(2) 0.092(2) 0.107(3) -0.048(2) 0.0103(19) 0.0181(18) O1S3 0.0160(12) 0.0395(14) 0.0423(15) 0.0038(12) 0.0091(10) -0.0050(11) O2S3 0.0414(17) 0.0573(18) 0.0570(18) 0.0233(15) 0.0196(14) 0.0003(14) O3S3 0.0320(16) 0.074(2) 0.0521(18) -0.0105(15) 0.0022(13) -0.0164(15) C3S 0.030(2) 0.058(3) 0.079(4) 0.002(3) 0.018(2) 0.002(2) N7 0.049(3) 0.093(3) 0.074(3) -0.021(2) 0.027(2) -0.021(2) C31 0.048(3) 0.062(3) 0.042(2) -0.007(2) 0.011(2) -0.025(2) C32 0.048(3) 0.061(3) 0.071(3) -0.016(2) 0.023(2) -0.009(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 O1S2 2.503(3) . ? La O1S3 2.506(2) . ? La O1S1 2.537(3) . ? La N6 2.670(3) . ? La N1 2.681(3) . ? La N4 2.691(3) . ? La N2 2.721(3) . ? La N3 2.754(3) . ? La N5 2.870(3) . ? N1 C1 1.487(4) . ? N1 C7 1.484(5) . ? N1 C25 1.496(4) . ? N2 C19 1.484(5) . ? N2 C13 1.487(5) . ? N2 C26 1.491(5) . ? N3 C6 1.339(5) . ? N3 C2 1.341(5) . ? N4 C12 1.339(5) . ? N4 C8 1.346(5) . ? N5 C14 1.337(5) . ? N5 C18 1.357(5) . ? N6 C20 1.344(5) . ? N6 C24 1.348(5) . ? C1 C2 1.500(5) . ? C2 C3 1.394(5) . ? C3 C4 1.370(6) . ? C4 C5 1.384(6) . ? C5 C6 1.373(6) . ? C7 C8 1.509(5) . ? C8 C9 1.371(5) . ? C9 C10 1.379(6) . ? C10 C11 1.380(6) . ? C11 C12 1.375(6) . ? C13 C14 1.490(5) . ? C14 C15 1.394(5) . ? C15 C16 1.366(6) . ? C16 C17 1.372(6) . ? C17 C18 1.380(6) . ? C19 C20 1.510(5) . ? C20 C21 1.377(5) . ? C21 C22 1.381(6) . ? C22 C23 1.375(6) . ? C23 C24 1.372(5) . ? C25 C26 1.507(5) . ? S1 O2S1 1.420(3) . ? S1 O3S1 1.422(3) . ? S1 O1S1 1.464(3) . ? S1 C1S 1.827(4) . ? F1S1 C1S 1.328(5) . ? F2S1 C1S 1.316(5) . ? F3S1 C1S 1.324(5) . ? S2 O2S2 1.421(3) . ? S2 O3S2 1.424(3) . ? S2 O1S2 1.441(3) . ? S2 C2S 1.822(4) . ? F1S2 C2S 1.323(6) . ? F2S2 C2S 1.318(6) . ? F3S2 C2S 1.326(5) . ? S3 O2S3 1.419(3) . ? S3 O3S3 1.425(3) . ? S3 O1S3 1.456(2) . ? S3 C3S 1.828(5) . ? F1S3 C3S 1.329(5) . ? F2S3 C3S 1.316(6) . ? F3S3 C3S 1.312(6) . ? N7 C31 1.128(6) . ? C31 C32 1.456(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 O1S2 La O1S3 145.05(9) . . ? O1S2 La O1S1 70.16(9) . . ? O1S3 La O1S1 80.27(8) . . ? O1S2 La N6 85.36(10) . . ? O1S3 La N6 71.69(8) . . ? O1S1 La N6 81.05(9) . . ? O1S2 La N1 139.75(9) . . ? O1S3 La N1 75.19(9) . . ? O1S1 La N1 138.44(9) . . ? N6 La N1 120.75(9) . . ? O1S2 La N4 81.30(10) . . ? O1S3 La N4 125.73(9) . . ? O1S1 La N4 105.81(9) . . ? N6 La N4 161.72(9) . . ? N1 La N4 65.24(9) . . ? O1S2 La N2 109.12(10) . . ? O1S3 La N2 82.63(8) . . ? O1S1 La N2 141.38(9) . . ? N6 La N2 60.71(9) . . ? N1 La N2 67.51(8) . . ? N4 La N2 112.29(9) . . ? O1S2 La N3 119.33(10) . . ? O1S3 La N3 68.77(9) . . ? O1S1 La N3 76.31(9) . . ? N6 La N3 136.98(8) . . ? N1 La N3 63.75(8) . . ? N4 La N3 61.17(9) . . ? N2 La N3 128.02(9) . . ? O1S2 La N5 65.47(9) . . ? O1S3 La N5 140.50(9) . . ? O1S1 La N5 135.63(8) . . ? N6 La N5 94.99(9) . . ? N1 La N5 81.09(9) . . ? N4 La N5 68.11(9) . . ? N2 La N5 59.05(8) . . ? N3 La N5 126.55(8) . . ? C1 N1 C7 109.2(3) . . ? C1 N1 C25 106.7(3) . . ? C7 N1 C25 109.7(3) . . ? C1 N1 La 112.1(2) . . ? C7 N1 La 108.5(2) . . ? C25 N1 La 110.6(2) . . ? C19 N2 C13 106.8(3) . . ? C19 N2 C26 111.3(3) . . ? C13 N2 C26 108.0(3) . . ? C19 N2 La 108.7(2) . . ? C13 N2 La 111.0(2) . . ? C26 N2 La 110.9(2) . . ? C6 N3 C2 117.8(3) . . ? C6 N3 La 124.3(2) . . ? C2 N3 La 117.4(2) . . ? C12 N4 C8 118.4(3) . . ? C12 N4 La 121.8(2) . . ? C8 N4 La 116.8(2) . . ? C14 N5 C18 116.5(3) . . ? C14 N5 La 116.5(2) . . ? C18 N5 La 126.1(2) . . ? C20 N6 C24 118.0(3) . . ? C20 N6 La 119.8(2) . . ? C24 N6 La 121.6(2) . . ? N1 C1 C2 114.5(3) . . ? N3 C2 C3 121.7(4) . . ? N3 C2 C1 118.4(3) . . ? C3 C2 C1 119.9(3) . . ? C4 C3 C2 119.6(4) . . ? C3 C4 C5 118.9(4) . . ? C6 C5 C4 118.3(4) . . ? N3 C6 C5 123.8(4) . . ? N1 C7 C8 113.4(3) . . ? N4 C8 C9 121.1(3) . . ? N4 C8 C7 116.2(3) . . ? C9 C8 C7 122.7(3) . . ? C8 C9 C10 120.1(4) . . ? C11 C10 C9 119.2(4) . . ? C10 C11 C12 117.7(4) . . ? N4 C12 C11 123.6(4) . . ? N2 C13 C14 113.2(3) . . ? N5 C14 C15 122.9(4) . . ? N5 C14 C13 117.0(3) . . ? C15 C14 C13 120.0(4) . . ? C16 C15 C14 119.2(4) . . ? C15 C16 C17 119.2(4) . . ? C16 C17 C18 118.6(4) . . ? N5 C18 C17 123.5(4) . . ? N2 C19 C20 110.8(3) . . ? N6 C20 C21 121.9(3) . . ? N6 C20 C19 116.4(3) . . ? C21 C20 C19 121.7(3) . . ? C22 C21 C20 119.4(4) . . ? C23 C22 C21 119.2(4) . . ? C24 C23 C22 118.5(4) . . ? N6 C24 C23 123.1(4) . . ? N1 C25 C26 113.2(3) . . ? N2 C26 C25 112.7(3) . . ? O2S1 S1 O3S1 117.35(19) . . ? O2S1 S1 O1S1 114.03(17) . . ? O3S1 S1 O1S1 113.68(17) . . ? O2S1 S1 C1S 102.6(2) . . ? O3S1 S1 C1S 102.81(18) . . ? O1S1 S1 C1S 103.90(18) . . ? S1 O1S1 La 149.42(16) . . ? F2S1 C1S F3S1 108.1(4) . . ? F2S1 C1S F1S1 107.8(3) . . ? F3S1 C1S F1S1 107.6(4) . . ? F2S1 C1S S1 109.9(3) . . ? F3S1 C1S S1 111.5(3) . . ? F1S1 C1S S1 111.7(3) . . ? O2S2 S2 O3S2 116.03(19) . . ? O2S2 S2 O1S2 114.4(2) . . ? O3S2 S2 O1S2 114.2(2) . . ? O2S2 S2 C2S 104.3(2) . . ? O3S2 S2 C2S 103.7(2) . . ? O1S2 S2 C2S 101.88(18) . . ? S2 O1S2 La 157.72(18) . . ? F2S2 C2S F1S2 108.1(4) . . ? F2S2 C2S F3S2 108.4(4) . . ? F1S2 C2S F3S2 108.3(4) . . ? F2S2 C2S S2 111.4(3) . . ? F1S2 C2S S2 110.9(3) . . ? F3S2 C2S S2 109.7(3) . . ? O2S3 S3 O3S3 116.7(2) . . ? O2S3 S3 O1S3 114.25(17) . . ? O3S3 S3 O1S3 112.43(17) . . ? O2S3 S3 C3S 104.7(2) . . ? O3S3 S3 C3S 103.5(2) . . ? O1S3 S3 C3S 103.26(19) . . ? S3 O1S3 La 164.68(16) . . ? F3S3 C3S F2S3 108.5(4) . . ? F3S3 C3S F1S3 108.5(4) . . ? F2S3 C3S F1S3 107.7(4) . . ? F3S3 C3S S3 111.8(3) . . ? F2S3 C3S S3 111.2(4) . . ? F1S3 C3S S3 109.1(3) . . ? N7 C31 C32 178.9(5) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 23.47 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.578 _refine_diff_density_min -2.022 _refine_diff_density_rms 0.127 # Attachment 'cifstruc2.doc.pdf' data_struc_2,_[La(tpen)(OH)]2(Otf)4.3CH3CN _database_code_depnum_ccdc_archive 'CCDC 285414' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (La(tpen)(OH))2(Otf)4.3CH3CN _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H67 F12 La2 N15 O14 S4' _chemical_formula_weight 1880.37 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.056(3) _cell_length_b 15.309(3) _cell_length_c 18.514(4) _cell_angle_alpha 78.59(3) _cell_angle_beta 84.49(3) _cell_angle_gamma 81.36(3) _cell_volume 3852.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1884 _exptl_absorpt_coefficient_mu 1.301 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22899 _diffrn_reflns_av_R_equivalents 0.0112 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 28.68 _reflns_number_total 16895 _reflns_number_gt 13832 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0357P)^2^+2.7510P] 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 16895 _refine_ls_number_parameters 1128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.087 _refine_ls_shift/su_mean 0.002 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 La1 La 0.363385(10) 0.868233(9) 0.776516(8) 0.03036(4) Uani 1 1 d . . . La2 La 0.260735(11) 0.678940(10) 0.698147(8) 0.03132(4) Uani 1 1 d . . . O1 O 0.25107(16) 0.75889(13) 0.79846(11) 0.0357(4) Uani 1 1 d . . . H1O H 0.210(2) 0.767(2) 0.8157(18) 0.038(10) Uiso 1 1 d . . . O2 O 0.38484(15) 0.77523(13) 0.68340(11) 0.0345(4) Uani 1 1 d . . . H2O H 0.427(3) 0.763(2) 0.667(2) 0.049(12) Uiso 1 1 d . . . N1 N 0.49249(17) 0.93486(15) 0.84993(12) 0.0378(5) Uani 1 1 d . . . N2 N 0.34410(17) 0.82328(16) 0.92892(12) 0.0387(5) Uani 1 1 d . . . N3 N 0.53088(18) 0.90839(16) 0.69877(13) 0.0413(5) Uani 1 1 d . . . N4 N 0.38664(19) 1.05266(16) 0.73319(15) 0.0492(6) Uani 1 1 d . . . N5 N 0.21961(18) 0.96487(17) 0.84789(15) 0.0496(6) Uani 1 1 d . . . N6 N 0.48316(17) 0.72891(15) 0.84148(12) 0.0374(5) Uani 1 1 d . . . N31 N 0.25837(18) 0.51083(15) 0.65779(12) 0.0394(5) Uani 1 1 d . . . N32 N 0.23315(17) 0.54250(15) 0.81435(12) 0.0381(5) Uani 1 1 d . . . N33 N 0.35957(17) 0.65163(15) 0.57060(12) 0.0388(5) Uani 1 1 d . . . N34 N 0.14841(19) 0.67107(17) 0.57707(13) 0.0460(6) Uani 1 1 d . . . N35 N 0.42024(17) 0.56486(15) 0.74554(12) 0.0369(5) Uani 1 1 d . . . N36 N 0.07559(18) 0.66001(18) 0.75564(14) 0.0466(6) Uani 1 1 d . . . C1 C 0.5914(2) 0.9234(2) 0.81360(16) 0.0456(7) Uani 1 1 d . . . H1A H 0.6214 0.8615 0.8300 0.055 Uiso 1 1 calc R . . H1B H 0.6298 0.9635 0.8297 0.055 Uiso 1 1 calc R . . C2 C 0.5942(2) 0.94285(19) 0.73072(16) 0.0396(6) Uani 1 1 d . . . C3 C 0.6633(3) 0.9918(2) 0.68987(19) 0.0573(8) Uani 1 1 d . . . H3 H 0.7064 1.0161 0.7136 0.069 Uiso 1 1 calc R . . C4 C 0.6675(3) 1.0040(3) 0.6141(2) 0.0658(10) Uani 1 1 d . . . H4 H 0.7142 1.0363 0.5854 0.079 Uiso 1 1 calc R . . C5 C 0.6034(3) 0.9689(3) 0.58094(19) 0.0633(9) Uani 1 1 d . . . H5 H 0.6052 0.9765 0.5292 0.076 Uiso 1 1 calc R . . C6 C 0.5362(3) 0.9224(2) 0.62455(17) 0.0522(8) Uani 1 1 d . . . H6 H 0.4915 0.8991 0.6014 0.063 Uiso 1 1 calc R . . C7 C 0.4593(3) 1.0324(2) 0.85059(19) 0.0550(8) Uani 1 1 d . . . H7A H 0.5100 1.0575 0.8695 0.066 Uiso 1 1 calc R . . H7B H 0.4021 1.0374 0.8849 0.066 Uiso 1 1 calc R . . C8 C 0.4354(2) 1.0879(2) 0.77676(19) 0.0497(7) Uani 1 1 d . . . C9 C 0.4592(3) 1.1749(2) 0.7579(2) 0.0623(9) Uani 1 1 d . . . H9 H 0.4935 1.1975 0.7898 0.075 Uiso 1 1 calc R . . C10 C 0.4320(3) 1.2270(2) 0.6923(3) 0.0697(11) Uani 1 1 d . . . H10 H 0.4462 1.2864 0.6790 0.084 Uiso 1 1 calc R . . C11 C 0.3841(3) 1.1920(2) 0.6464(3) 0.0730(11) Uani 1 1 d . . . H11 H 0.3660 1.2265 0.6007 0.088 Uiso 1 1 calc R . . C12 C 0.3624(3) 1.1048(2) 0.6683(2) 0.0625(9) Uani 1 1 d . . . H12 H 0.3294 1.0811 0.6365 0.075 Uiso 1 1 calc R . . C13 C 0.2406(2) 0.8423(2) 0.95300(17) 0.0496(7) Uani 1 1 d . . . H13A H 0.2340 0.8358 1.0069 0.060 Uiso 1 1 calc R . . H13B H 0.2055 0.7980 0.9394 0.060 Uiso 1 1 calc R . . C14 C 0.1963(2) 0.9346(2) 0.9194(2) 0.0574(9) Uani 1 1 d . . . C15 C 0.1296(4) 0.9851(4) 0.9602(3) 0.1061(18) Uani 1 1 d . . . H15 H 0.1163 0.9646 1.0109 0.127 Uiso 1 1 calc R . . C16 C 0.0836(5) 1.0652(4) 0.9252(4) 0.154(3) Uani 1 1 d . . . H16 H 0.0380 1.1002 0.9520 0.184 Uiso 1 1 calc R . . C17 C 0.1036(4) 1.0946(3) 0.8518(3) 0.117(2) Uani 1 1 d . . . H17 H 0.0705 1.1484 0.8269 0.140 Uiso 1 1 calc R . . C18 C 0.1732(3) 1.0437(2) 0.8151(2) 0.0673(10) Uani 1 1 d . . . H18 H 0.1890 1.0649 0.7648 0.081 Uiso 1 1 calc R . . C19 C 0.3733(2) 0.7254(2) 0.95128(16) 0.0467(7) Uani 1 1 d . . . H19A H 0.3211 0.6938 0.9424 0.056 Uiso 1 1 calc R . . H19B H 0.3816 0.7117 1.0045 0.056 Uiso 1 1 calc R . . C20 C 0.4644(2) 0.68970(19) 0.91175(15) 0.0409(6) Uani 1 1 d . . . C21 C 0.5240(3) 0.6155(2) 0.94594(18) 0.0536(8) Uani 1 1 d . . . H21 H 0.5093 0.5890 0.9953 0.064 Uiso 1 1 calc R . . C22 C 0.6049(3) 0.5806(2) 0.9073(2) 0.0604(9) Uani 1 1 d . . . H22 H 0.6458 0.5302 0.9296 0.072 Uiso 1 1 calc R . . C23 C 0.6239(2) 0.6210(2) 0.8358(2) 0.0520(8) Uani 1 1 d . . . H23 H 0.6786 0.5989 0.8081 0.062 Uiso 1 1 calc R . . C24 C 0.5622(2) 0.69447(19) 0.80475(17) 0.0420(6) Uani 1 1 d . . . H24 H 0.5762 0.7217 0.7555 0.050 Uiso 1 1 calc R . . C25 C 0.4979(2) 0.8872(2) 0.92811(15) 0.0439(7) Uani 1 1 d . . . H25A H 0.5306 0.9215 0.9552 0.053 Uiso 1 1 calc R . . H25B H 0.5363 0.8280 0.9294 0.053 Uiso 1 1 calc R . . C26 C 0.3995(2) 0.8753(2) 0.96576(16) 0.0465(7) Uani 1 1 d . . . H26A H 0.4070 0.8444 1.0170 0.056 Uiso 1 1 calc R . . H26B H 0.3626 0.9347 0.9669 0.056 Uiso 1 1 calc R . . C31 C 0.3381(2) 0.49366(19) 0.60158(16) 0.0446(7) Uani 1 1 d . . . H31A H 0.3232 0.4476 0.5761 0.054 Uiso 1 1 calc R . . H31B H 0.3975 0.4699 0.6266 0.054 Uiso 1 1 calc R . . C32 C 0.3555(2) 0.57646(19) 0.54501(16) 0.0411(6) Uani 1 1 d . . . C33 C 0.3693(3) 0.5731(2) 0.47068(18) 0.0572(9) Uani 1 1 d . . . H33 H 0.3674 0.5193 0.4540 0.069 Uiso 1 1 calc R . . C34 C 0.3857(3) 0.6503(3) 0.42165(19) 0.0683(11) Uani 1 1 d . . . H34 H 0.3937 0.6501 0.3707 0.082 Uiso 1 1 calc R . . C35 C 0.3905(3) 0.7279(2) 0.44744(18) 0.0581(9) Uani 1 1 d . . . H35 H 0.4023 0.7811 0.4148 0.070 Uiso 1 1 calc R . . C36 C 0.3775(2) 0.7253(2) 0.52191(16) 0.0456(7) Uani 1 1 d . . . H36 H 0.3814 0.7779 0.5398 0.055 Uiso 1 1 calc R . . C37 C 0.1649(2) 0.5102(2) 0.62743(18) 0.0500(7) Uani 1 1 d . . . H37A H 0.1141 0.5103 0.6675 0.060 Uiso 1 1 calc R . . H37B H 0.1673 0.4544 0.6086 0.060 Uiso 1 1 calc R . . C38 C 0.1384(2) 0.5887(2) 0.56634(16) 0.0446(7) Uani 1 1 d . . . C39 C 0.1013(3) 0.5751(3) 0.50327(19) 0.0591(9) Uani 1 1 d . . . H39 H 0.0964 0.5166 0.4969 0.071 Uiso 1 1 calc R . . C40 C 0.0720(3) 0.6479(3) 0.4503(2) 0.0675(10) Uani 1 1 d . . . H40 H 0.0455 0.6401 0.4077 0.081 Uiso 1 1 calc R . . C41 C 0.0818(3) 0.7322(3) 0.46056(19) 0.0626(9) Uani 1 1 d . . . H41 H 0.0625 0.7832 0.4250 0.075 Uiso 1 1 calc R . . C42 C 0.1206(3) 0.7407(2) 0.52397(17) 0.0547(8) Uani 1 1 d . . . H42 H 0.1280 0.7987 0.5303 0.066 Uiso 1 1 calc R . . C43 C 0.3212(2) 0.5210(2) 0.85667(16) 0.0458(7) Uani 1 1 d . . . H43A H 0.3152 0.4674 0.8949 0.055 Uiso 1 1 calc R . . H43B H 0.3258 0.5710 0.8814 0.055 Uiso 1 1 calc R . . C44 C 0.4115(2) 0.50466(18) 0.80871(15) 0.0406(6) Uani 1 1 d . . . C45 C 0.4821(2) 0.4324(2) 0.82891(18) 0.0500(7) Uani 1 1 d . . . H45 H 0.4732 0.3907 0.8728 0.060 Uiso 1 1 calc R . . C46 C 0.5647(3) 0.4224(2) 0.7843(2) 0.0555(8) Uani 1 1 d . . . H46 H 0.6132 0.3737 0.7968 0.067 Uiso 1 1 calc R . . C47 C 0.5756(2) 0.4853(2) 0.72062(18) 0.0487(7) Uani 1 1 d . . . H47 H 0.6322 0.4809 0.6894 0.058 Uiso 1 1 calc R . . C48 C 0.5021(2) 0.55480(19) 0.70351(16) 0.0416(6) Uani 1 1 d . . . H48 H 0.5101 0.5973 0.6599 0.050 Uiso 1 1 calc R . . C49 C 0.1529(2) 0.5741(2) 0.86434(16) 0.0454(7) Uani 1 1 d . . . H49A H 0.1730 0.6196 0.8880 0.055 Uiso 1 1 calc R . . H49B H 0.1380 0.5236 0.9032 0.055 Uiso 1 1 calc R . . C50 C 0.0635(2) 0.6138(2) 0.82477(17) 0.0464(7) Uani 1 1 d . . . C51 C -0.0271(3) 0.6062(3) 0.8605(2) 0.0608(9) Uani 1 1 d . . . H51 H -0.0335 0.5725 0.9086 0.073 Uiso 1 1 calc R . . C52 C -0.1070(3) 0.6484(3) 0.8246(2) 0.0740(12) Uani 1 1 d . . . H52 H -0.1689 0.6451 0.8483 0.089 Uiso 1 1 calc R . . C53 C -0.0963(3) 0.6957(3) 0.7536(2) 0.0746(12) Uani 1 1 d . . . H53 H -0.1504 0.7245 0.7280 0.090 Uiso 1 1 calc R . . C54 C -0.0040(2) 0.6998(3) 0.7208(2) 0.0606(9) Uani 1 1 d . . . H54 H 0.0035 0.7317 0.6722 0.073 Uiso 1 1 calc R . . C55 C 0.2679(2) 0.43691(19) 0.72362(16) 0.0447(7) Uani 1 1 d . . . H55A H 0.3360 0.4223 0.7346 0.054 Uiso 1 1 calc R . . H55B H 0.2474 0.3831 0.7120 0.054 Uiso 1 1 calc R . . C56 C 0.2089(2) 0.46089(19) 0.79124(16) 0.0465(7) Uani 1 1 d . . . H56A H 0.1405 0.4707 0.7814 0.056 Uiso 1 1 calc R . . H56B H 0.2185 0.4098 0.8323 0.056 Uiso 1 1 calc R . . S1 S 0.19552(6) 0.92307(5) 0.62377(4) 0.04332(16) Uani 1 1 d . . . F1S1 F 0.03351(19) 0.9760(2) 0.69113(18) 0.1086(10) Uani 1 1 d . . . F2S1 F 0.0242(2) 0.9759(2) 0.5773(2) 0.1292(12) Uani 1 1 d . . . F3S1 F 0.0888(2) 1.07802(16) 0.6113(2) 0.1198(11) Uani 1 1 d . . . O1S1 O 0.24322(15) 0.94918(13) 0.68026(12) 0.0471(5) Uani 1 1 d . . . O2S1 O 0.17019(15) 0.83282(13) 0.64354(12) 0.0477(5) Uani 1 1 d . . . O3S1 O 0.2364(2) 0.9462(2) 0.55090(14) 0.0818(8) Uani 1 1 d . . . C1S C 0.0780(3) 0.9921(3) 0.6261(3) 0.0711(11) Uani 1 1 d . . . S2A S 0.75999(18) 0.16552(16) 0.83392(18) 0.0494(5) Uani 0.657(8) 1 d P A -1 C2SA C 0.8026(9) 0.1890(5) 0.7374(4) 0.081(3) Uani 0.657(8) 1 d P A -1 F3S2 F 0.7346(9) 0.2163(7) 0.6969(4) 0.235(6) Uani 0.657(8) 1 d P A -1 O3S2 O 0.8461(4) 0.1372(5) 0.8684(3) 0.114(2) Uani 0.657(8) 1 d P A -1 S2B S 0.7338(5) 0.1836(3) 0.8083(3) 0.0615(11) Uani 0.343(8) 1 d P A -2 C2SB C 0.8531(17) 0.1663(13) 0.7581(13) 0.110(7) Uani 0.343(8) 1 d P A -2 F4S2 F 0.9136(9) 0.1279(12) 0.8066(12) 0.216(9) Uani 0.343(8) 1 d P A -2 O4S2 O 0.6699(9) 0.2169(9) 0.7491(11) 0.137(6) Uani 0.343(8) 1 d P A -2 F1S2 F 0.8654(5) 0.2434(4) 0.7238(2) 0.237(3) Uani 1 1 d . . . F2S2 F 0.8453(3) 0.1161(2) 0.71299(17) 0.1180(11) Uani 1 1 d . . . O1S2 O 0.7123(3) 0.0947(3) 0.8414(2) 0.1298(15) Uani 1 1 d . . . O2S2 O 0.7247(4) 0.2476(2) 0.8513(2) 0.154(2) Uani 1 1 d . . . S3A S 0.2379(3) 0.27474(19) 1.00689(16) 0.0636(8) Uani 0.575(6) 1 d P B -1 F3S3 F 0.3980(4) 0.2471(5) 0.9375(4) 0.098(2) Uani 0.575(6) 1 d P B -1 O3S3 O 0.1430(3) 0.2383(6) 1.0079(3) 0.089(2) Uani 0.575(6) 1 d P B -1 C3SA C 0.3106(3) 0.2227(3) 0.9401(2) 0.0287(11) Uani 0.575(6) 1 d P B -1 S3B S 0.2814(3) 0.2819(2) 0.99517(19) 0.0473(7) Uani 0.425(6) 1 d P B -2 F4S3 F 0.1435(4) 0.1815(4) 0.9893(4) 0.0706(18) Uani 0.425(6) 1 d P B -2 O4S3 O 0.3663(6) 0.2907(6) 0.9574(4) 0.065(2) Uani 0.425(6) 1 d P B -2 C3SB C 0.2303(6) 0.1980(5) 0.9596(4) 0.048(2) Uani 0.425(6) 1 d P B -2 F1S3 F 0.3016(2) 0.12516(17) 0.96641(17) 0.1122(10) Uani 1 1 d . . . F2S3 F 0.2492(4) 0.2325(3) 0.87989(18) 0.175(2) Uani 1 1 d . . . O1S3 O 0.28064(17) 0.24246(15) 1.07423(12) 0.0547(6) Uani 1 1 d . . . O2S3 O 0.2166(3) 0.36270(17) 0.98107(16) 0.0917(10) Uani 1 1 d . . . S4 S 0.69228(9) 0.67615(7) 0.58339(6) 0.0709(3) Uani 1 1 d . . . C4SA C 0.7987(13) 0.7242(10) 0.5359(8) 0.085(4) Uani 0.580(7) 1 d P C -1 F1S4 F 0.8708(10) 0.7151(12) 0.5650(6) 0.151(7) Uani 0.580(7) 1 d P C -1 F2S4 F 0.7746(12) 0.8131(10) 0.5286(11) 0.235(11) Uani 0.580(7) 1 d P C -1 F3S4 F 0.8159(5) 0.7085(5) 0.4689(3) 0.129(3) Uani 0.580(7) 1 d P C -1 O1S4 O 0.6184(6) 0.7146(10) 0.5491(6) 0.175(6) Uani 0.580(7) 1 d P C -1 O2S4 O 0.7267(8) 0.5841(6) 0.5784(7) 0.151(4) Uani 0.580(7) 1 d P C -1 O3S4 O 0.7002(5) 0.6887(6) 0.6571(3) 0.106(3) Uani 0.580(7) 1 d P C -1 C4SB C 0.7706(15) 0.7563(11) 0.5505(16) 0.097(8) Uani 0.420(7) 1 d P C -2 F4S4 F 0.7433(12) 0.8154(9) 0.4958(5) 0.110(5) Uani 0.420(7) 1 d P C -2 F5S4 F 0.8588(16) 0.700(2) 0.5400(17) 0.248(17) Uani 0.420(7) 1 d P C -2 F6S4 F 0.7778(8) 0.8053(6) 0.6037(7) 0.139(5) Uani 0.420(7) 1 d P C -2 O4S4 O 0.6721(12) 0.6468(7) 0.5186(6) 0.130(5) Uani 0.420(7) 1 d P C -2 O5S4 O 0.7240(8) 0.6163(9) 0.6376(9) 0.149(7) Uani 0.420(7) 1 d P C -2 O6S4 O 0.5962(6) 0.7344(5) 0.6013(6) 0.093(3) Uani 0.420(7) 1 d P C -2 N101 N 0.8006(4) 0.4199(3) 0.9473(3) 0.1119(15) Uani 1 1 d . . . C101 C 0.8661(3) 0.3714(3) 0.9416(2) 0.0720(11) Uani 1 1 d . . . C102 C 0.9504(4) 0.3071(4) 0.9369(3) 0.1048(18) Uani 1 1 d . . . H10A H 0.9660 0.2761 0.9861 0.157 Uiso 1 1 calc R . . H10B H 1.0040 0.3377 0.9131 0.157 Uiso 1 1 calc R . . H10C H 0.9384 0.2638 0.9081 0.157 Uiso 1 1 calc R . . N102 N 1.0113(3) 0.3875(4) 0.7420(3) 0.1149(17) Uani 1 1 d . . . C103 C 0.9338(4) 0.4179(3) 0.7408(3) 0.0803(13) Uani 1 1 d . . . C104 C 0.8343(5) 0.4537(4) 0.7397(4) 0.125(2) Uani 1 1 d . . . H10D H 0.7966 0.4066 0.7365 0.187 Uiso 1 1 calc R . . H10E H 0.8246 0.5019 0.6973 0.187 Uiso 1 1 calc R . . H10F H 0.8138 0.4769 0.7846 0.187 Uiso 1 1 calc R . . N103 N 1.0486(2) 0.8152(2) 0.8656(2) 0.0714(9) Uani 1 1 d . . . C105 C 0.9757(3) 0.8540(2) 0.8537(2) 0.0590(9) Uani 1 1 d . . . C106 C 0.8804(3) 0.9031(3) 0.8368(3) 0.0892(15) Uani 1 1 d . . . H10G H 0.8778 0.9217 0.7837 0.134 Uiso 1 1 calc R . . H10H H 0.8688 0.9557 0.8599 0.134 Uiso 1 1 calc R . . H10I H 0.8315 0.8644 0.8556 0.134 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 La1 0.03033(8) 0.03059(8) 0.03009(8) -0.00629(6) -0.00192(6) -0.00310(6) La2 0.03325(8) 0.03332(8) 0.02812(8) -0.00565(6) -0.00266(6) -0.00654(6) O1 0.0337(11) 0.0416(11) 0.0331(10) -0.0102(8) 0.0022(9) -0.0079(9) O2 0.0324(11) 0.0384(10) 0.0337(10) -0.0105(8) 0.0032(8) -0.0064(8) N1 0.0412(13) 0.0409(12) 0.0340(12) -0.0113(10) -0.0011(10) -0.0094(10) N2 0.0397(13) 0.0459(13) 0.0326(12) -0.0131(10) 0.0032(9) -0.0080(10) N3 0.0447(14) 0.0437(13) 0.0368(12) -0.0080(10) 0.0011(10) -0.0118(11) N4 0.0501(15) 0.0354(13) 0.0600(17) -0.0031(12) -0.0049(12) -0.0059(11) N5 0.0403(14) 0.0500(15) 0.0594(17) -0.0196(13) -0.0011(12) 0.0023(11) N6 0.0385(13) 0.0407(12) 0.0335(12) -0.0092(9) -0.0064(9) -0.0010(10) N31 0.0472(14) 0.0390(12) 0.0349(12) -0.0075(10) -0.0051(10) -0.0129(10) N32 0.0422(13) 0.0410(12) 0.0335(12) -0.0067(10) -0.0020(10) -0.0141(10) N33 0.0443(13) 0.0413(13) 0.0327(12) -0.0108(10) 0.0006(10) -0.0091(10) N34 0.0491(15) 0.0533(15) 0.0367(13) -0.0083(11) -0.0089(11) -0.0067(12) N35 0.0392(13) 0.0343(11) 0.0380(12) -0.0052(9) -0.0058(10) -0.0070(9) N36 0.0373(13) 0.0577(15) 0.0470(14) -0.0125(12) -0.0023(11) -0.0108(11) C1 0.0374(15) 0.0590(18) 0.0437(16) -0.0092(14) -0.0042(12) -0.0165(13) C2 0.0374(15) 0.0407(15) 0.0413(15) -0.0082(12) 0.0010(12) -0.0089(12) C3 0.054(2) 0.066(2) 0.057(2) -0.0120(17) 0.0047(16) -0.0265(17) C4 0.067(2) 0.075(2) 0.057(2) -0.0069(18) 0.0163(18) -0.034(2) C5 0.075(3) 0.076(2) 0.0399(18) -0.0077(16) 0.0100(16) -0.025(2) C6 0.059(2) 0.061(2) 0.0385(16) -0.0062(14) -0.0004(14) -0.0214(16) C7 0.067(2) 0.0473(18) 0.0544(19) -0.0193(15) -0.0028(16) -0.0085(16) C8 0.0541(19) 0.0357(15) 0.0589(19) -0.0127(14) 0.0036(15) -0.0048(13) C9 0.065(2) 0.0434(18) 0.081(3) -0.0186(18) 0.0093(19) -0.0144(16) C10 0.068(2) 0.0367(17) 0.098(3) -0.0050(19) 0.016(2) -0.0109(16) C11 0.070(3) 0.048(2) 0.089(3) 0.0155(19) -0.004(2) -0.0061(18) C12 0.061(2) 0.0490(19) 0.073(2) 0.0092(17) -0.0172(18) -0.0137(16) C13 0.0450(17) 0.065(2) 0.0423(16) -0.0200(15) 0.0108(13) -0.0130(15) C14 0.0461(19) 0.063(2) 0.064(2) -0.0254(17) 0.0133(16) -0.0034(15) C15 0.108(4) 0.103(4) 0.090(3) -0.028(3) 0.038(3) 0.026(3) C16 0.165(6) 0.114(5) 0.134(5) -0.015(4) 0.065(5) 0.076(4) C17 0.111(4) 0.083(3) 0.128(5) -0.016(3) 0.019(4) 0.053(3) C18 0.057(2) 0.058(2) 0.085(3) -0.0211(19) -0.0046(19) 0.0103(17) C19 0.0579(19) 0.0483(17) 0.0322(14) -0.0031(12) 0.0023(13) -0.0104(14) C20 0.0501(17) 0.0394(15) 0.0354(14) -0.0074(12) -0.0100(12) -0.0077(12) C21 0.071(2) 0.0445(17) 0.0456(17) -0.0015(14) -0.0225(16) -0.0053(15) C22 0.064(2) 0.0413(17) 0.078(3) -0.0120(17) -0.0319(19) 0.0070(15) C23 0.0393(16) 0.0492(18) 0.073(2) -0.0273(16) -0.0140(15) 0.0027(13) C24 0.0364(15) 0.0456(16) 0.0477(16) -0.0180(13) -0.0071(12) -0.0017(12) C25 0.0483(17) 0.0526(17) 0.0357(15) -0.0125(13) -0.0061(12) -0.0142(13) C26 0.0529(18) 0.0576(18) 0.0340(15) -0.0178(13) 0.0021(13) -0.0139(14) C31 0.0536(18) 0.0401(15) 0.0436(16) -0.0146(13) -0.0019(13) -0.0096(13) C32 0.0428(16) 0.0450(16) 0.0390(15) -0.0146(12) -0.0003(12) -0.0094(12) C33 0.079(2) 0.058(2) 0.0429(17) -0.0242(15) 0.0088(16) -0.0233(18) C34 0.103(3) 0.071(2) 0.0373(17) -0.0198(16) 0.0149(18) -0.033(2) C35 0.080(3) 0.057(2) 0.0391(17) -0.0090(14) 0.0098(16) -0.0227(18) C36 0.0512(18) 0.0472(16) 0.0417(16) -0.0142(13) 0.0028(13) -0.0133(13) C37 0.0505(18) 0.0543(18) 0.0489(18) -0.0063(14) -0.0105(14) -0.0182(15) C38 0.0387(16) 0.0590(18) 0.0403(16) -0.0125(13) -0.0049(12) -0.0138(13) C39 0.059(2) 0.075(2) 0.0519(19) -0.0210(17) -0.0138(16) -0.0156(18) C40 0.066(2) 0.094(3) 0.047(2) -0.0215(19) -0.0197(17) -0.006(2) C41 0.067(2) 0.076(2) 0.0426(18) -0.0077(17) -0.0180(16) 0.0045(19) C42 0.062(2) 0.058(2) 0.0434(17) -0.0085(15) -0.0136(15) 0.0005(16) C43 0.0517(18) 0.0503(17) 0.0353(15) -0.0011(13) -0.0075(13) -0.0126(14) C44 0.0483(17) 0.0364(14) 0.0388(15) -0.0048(11) -0.0098(12) -0.0096(12) C45 0.062(2) 0.0381(15) 0.0489(18) -0.0004(13) -0.0168(15) -0.0048(14) C46 0.059(2) 0.0416(17) 0.066(2) -0.0150(15) -0.0188(17) 0.0068(14) C47 0.0455(17) 0.0512(18) 0.0533(18) -0.0220(15) -0.0073(14) 0.0006(13) C48 0.0413(16) 0.0411(15) 0.0445(16) -0.0104(12) -0.0063(12) -0.0068(12) C49 0.0489(17) 0.0510(17) 0.0379(15) -0.0080(13) 0.0065(13) -0.0177(14) C50 0.0445(17) 0.0540(18) 0.0461(17) -0.0170(14) 0.0054(13) -0.0193(14) C51 0.049(2) 0.079(2) 0.062(2) -0.0261(19) 0.0138(16) -0.0290(18) C52 0.042(2) 0.106(3) 0.085(3) -0.044(3) 0.0130(19) -0.023(2) C53 0.0405(19) 0.109(3) 0.085(3) -0.044(3) -0.0113(19) -0.005(2) C54 0.0466(19) 0.081(2) 0.057(2) -0.0208(18) -0.0085(16) -0.0023(17) C55 0.0612(19) 0.0344(14) 0.0413(16) -0.0064(12) -0.0071(14) -0.0139(13) C56 0.061(2) 0.0380(15) 0.0423(16) -0.0030(12) -0.0017(14) -0.0196(14) S1 0.0487(4) 0.0420(4) 0.0354(4) 0.0004(3) -0.0071(3) -0.0014(3) F1S1 0.0607(16) 0.124(2) 0.127(2) -0.0237(19) 0.0187(16) 0.0160(15) F2S1 0.102(2) 0.137(3) 0.152(3) -0.029(2) -0.089(2) 0.0259(19) F3S1 0.111(2) 0.0513(14) 0.180(3) 0.0099(16) -0.041(2) 0.0222(14) O1S1 0.0510(12) 0.0371(10) 0.0530(12) -0.0054(9) -0.0169(10) -0.0001(9) O2S1 0.0507(13) 0.0397(11) 0.0526(12) -0.0032(9) -0.0188(10) -0.0032(9) O3S1 0.109(2) 0.088(2) 0.0429(14) 0.0004(13) 0.0118(14) -0.0216(17) C1S 0.063(2) 0.059(2) 0.085(3) -0.001(2) -0.031(2) 0.0129(18) S2A 0.0586(11) 0.0471(9) 0.0428(12) -0.0107(8) -0.0106(8) -0.0002(7) C2SA 0.153(9) 0.057(4) 0.039(3) 0.002(3) -0.023(4) -0.037(5) F3S2 0.246(11) 0.323(11) 0.076(4) 0.009(5) -0.061(5) 0.120(9) O3S2 0.082(4) 0.200(6) 0.055(3) -0.025(3) -0.024(3) 0.017(4) S2B 0.089(3) 0.0499(19) 0.046(2) -0.0101(16) -0.018(2) -0.0024(18) C2SB 0.139(19) 0.076(11) 0.124(17) 0.005(11) -0.069(14) -0.038(11) F4S2 0.076(8) 0.284(19) 0.31(2) -0.086(17) -0.055(12) -0.033(10) O4S2 0.074(8) 0.144(11) 0.192(16) -0.041(10) -0.061(9) 0.032(7) F1S2 0.437(9) 0.191(4) 0.130(3) -0.051(3) 0.096(5) -0.236(6) F2S2 0.143(3) 0.120(2) 0.099(2) -0.0472(19) 0.048(2) -0.046(2) O1S2 0.168(4) 0.128(3) 0.110(3) -0.040(2) 0.052(3) -0.084(3) O2S2 0.280(6) 0.082(2) 0.078(2) -0.0242(19) -0.021(3) 0.065(3) S3A 0.085(2) 0.0513(12) 0.0508(12) -0.0105(9) -0.0091(13) 0.0056(13) F3S3 0.076(4) 0.126(5) 0.085(4) 0.000(3) 0.015(3) -0.030(3) O3S3 0.040(3) 0.129(6) 0.092(4) -0.015(4) -0.005(2) -0.003(3) C3SA 0.038(3) 0.025(2) 0.021(2) -0.0046(15) -0.0012(17) 0.0011(17) S3B 0.0542(18) 0.0467(11) 0.0422(13) -0.0023(9) -0.0026(12) -0.0188(13) F4S3 0.052(3) 0.076(4) 0.100(4) -0.048(3) 0.004(3) -0.022(3) O4S3 0.065(5) 0.082(5) 0.056(4) -0.017(3) 0.014(3) -0.039(4) C3SB 0.050(5) 0.048(4) 0.051(4) -0.021(3) 0.001(3) -0.007(3) F1S3 0.150(3) 0.0681(16) 0.123(2) -0.0492(16) -0.030(2) 0.0270(16) F2S3 0.291(6) 0.154(3) 0.078(2) -0.057(2) -0.074(3) 0.059(3) O1S3 0.0648(15) 0.0566(13) 0.0410(12) -0.0025(10) -0.0069(10) -0.0090(11) O2S3 0.151(3) 0.0408(14) 0.0705(18) -0.0016(12) -0.0073(18) 0.0158(16) S4 0.0881(8) 0.0618(6) 0.0638(6) -0.0054(5) 0.0062(5) -0.0292(5) C4SA 0.101(11) 0.066(8) 0.086(7) -0.010(7) 0.015(7) -0.021(7) F1S4 0.093(7) 0.285(18) 0.098(5) -0.041(7) -0.005(4) -0.096(9) F2S4 0.25(2) 0.130(11) 0.34(2) -0.123(14) 0.185(18) -0.118(13) F3S4 0.127(5) 0.199(7) 0.062(3) -0.024(4) 0.029(3) -0.047(5) O1S4 0.069(5) 0.296(15) 0.137(9) 0.050(9) -0.042(6) -0.052(7) O2S4 0.224(10) 0.088(5) 0.152(9) -0.050(6) 0.049(8) -0.060(6) O3S4 0.101(5) 0.165(7) 0.065(4) -0.045(4) 0.037(3) -0.056(5) C4SB 0.077(11) 0.034(8) 0.18(2) 0.005(10) -0.025(12) -0.017(7) F4S4 0.176(10) 0.086(7) 0.064(4) 0.036(5) -0.016(5) -0.067(6) F5S4 0.116(18) 0.36(3) 0.33(4) -0.21(3) 0.13(2) -0.110(19) F6S4 0.145(9) 0.105(6) 0.197(11) -0.049(7) -0.092(8) -0.030(6) O4S4 0.233(14) 0.076(6) 0.104(8) -0.048(6) 0.002(8) -0.062(7) O5S4 0.132(9) 0.123(10) 0.146(12) 0.100(9) -0.033(9) -0.020(8) O6S4 0.078(5) 0.054(4) 0.133(8) -0.008(5) 0.033(6) -0.005(3) N101 0.099(3) 0.094(3) 0.139(4) -0.036(3) -0.016(3) 0.022(3) C101 0.076(3) 0.066(2) 0.071(3) -0.009(2) -0.007(2) -0.002(2) C102 0.082(3) 0.110(4) 0.100(4) 0.002(3) 0.008(3) 0.021(3) N102 0.070(3) 0.172(5) 0.115(4) -0.027(3) -0.001(3) -0.059(3) C103 0.083(3) 0.093(3) 0.078(3) -0.021(2) -0.003(3) -0.046(3) C104 0.119(5) 0.099(4) 0.158(6) -0.040(4) -0.025(4) 0.013(4) N103 0.0491(19) 0.080(2) 0.088(2) -0.0228(19) -0.0046(17) -0.0104(16) C105 0.052(2) 0.052(2) 0.070(2) -0.0078(17) 0.0063(17) -0.0099(16) C106 0.062(3) 0.073(3) 0.111(4) 0.015(2) 0.005(2) 0.012(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 La1 O2 2.415(2) . ? La1 O1 2.421(2) . ? La1 O1S1 2.577(2) . ? La1 N6 2.669(2) . ? La1 N5 2.717(3) . ? La1 N3 2.725(3) . ? La1 N2 2.766(2) . ? La1 N1 2.786(2) . ? La1 N4 2.838(3) . ? La1 La2 3.9884(10) . ? La2 O1 2.401(2) . ? La2 O2 2.411(2) . ? La2 O2S1 2.568(2) . ? La2 N33 2.696(2) . ? La2 N35 2.728(2) . ? La2 N32 2.729(2) . ? La2 N36 2.750(3) . ? La2 N31 2.824(2) . ? La2 N34 2.894(3) . ? N1 C1 1.486(4) . ? N1 C25 1.490(4) . ? N1 C7 1.498(4) . ? N2 C19 1.480(4) . ? N2 C13 1.483(4) . ? N2 C26 1.487(4) . ? N3 C2 1.337(4) . ? N3 C6 1.345(4) . ? N4 C8 1.342(4) . ? N4 C12 1.347(4) . ? N5 C14 1.339(4) . ? N5 C18 1.342(4) . ? N6 C20 1.340(4) . ? N6 C24 1.340(4) . ? N31 C37 1.480(4) . ? N31 C31 1.484(4) . ? N31 C55 1.491(4) . ? N32 C49 1.475(4) . ? N32 C43 1.488(4) . ? N32 C56 1.492(3) . ? N33 C36 1.337(4) . ? N33 C32 1.339(3) . ? N34 C42 1.338(4) . ? N34 C38 1.344(4) . ? N35 C48 1.332(4) . ? N35 C44 1.346(3) . ? N36 C50 1.343(4) . ? N36 C54 1.348(4) . ? C1 C2 1.502(4) . ? C2 C3 1.389(4) . ? C3 C4 1.374(5) . ? C4 C5 1.365(5) . ? C5 C6 1.371(5) . ? C7 C8 1.499(5) . ? C8 C9 1.391(4) . ? C9 C10 1.369(6) . ? C10 C11 1.364(6) . ? C11 C12 1.387(5) . ? C13 C14 1.495(5) . ? C14 C15 1.387(5) . ? C15 C16 1.368(7) . ? C16 C17 1.360(8) . ? C17 C18 1.371(6) . ? C19 C20 1.497(4) . ? C20 C21 1.388(4) . ? C21 C22 1.379(5) . ? C22 C23 1.366(5) . ? C23 C24 1.376(4) . ? C25 C26 1.506(4) . ? C31 C32 1.511(4) . ? C32 C33 1.381(4) . ? C33 C34 1.375(5) . ? C34 C35 1.379(5) . ? C35 C36 1.367(4) . ? C37 C38 1.507(4) . ? C38 C39 1.387(4) . ? C39 C40 1.372(5) . ? C40 C41 1.368(5) . ? C41 C42 1.378(4) . ? C43 C44 1.497(4) . ? C44 C45 1.388(4) . ? C45 C46 1.365(5) . ? C46 C47 1.379(5) . ? C47 C48 1.377(4) . ? C49 C50 1.502(5) . ? C50 C51 1.387(4) . ? C51 C52 1.371(6) . ? C52 C53 1.375(6) . ? C53 C54 1.384(5) . ? C55 C56 1.510(4) . ? S1 O3S1 1.414(3) . ? S1 O1S1 1.444(2) . ? S1 O2S1 1.447(2) . ? S1 C1S 1.825(4) . ? F1S1 C1S 1.297(5) . ? F2S1 C1S 1.314(5) . ? F3S1 C1S 1.318(5) . ? S2A O1S2 1.336(4) . ? S2A O2S2 1.367(4) . ? S2A O3S2 1.394(7) . ? S2A C2SA 1.813(8) . ? C2SA F3S2 1.243(13) . ? C2SA F1S2 1.277(10) . ? C2SA F2S2 1.325(9) . ? S2B O2S2 1.363(5) . ? S2B O1S2 1.441(6) . ? S2B O4S2 1.448(18) . ? S2B C2SB 1.85(3) . ? C2SB F1S2 1.253(19) . ? C2SB F2S2 1.26(2) . ? C2SB F4S2 1.29(2) . ? S3A O2S3 1.335(4) . ? S3A O1S3 1.404(3) . ? S3A O3S3 1.518(9) . ? S3A C3SA 1.764(5) . ? F3S3 C3SA 1.331(7) . ? C3SA F2S3 1.446(5) . ? C3SA F1S3 1.497(5) . ? S3B O4S3 1.336(10) . ? S3B O2S3 1.416(5) . ? S3B O1S3 1.469(4) . ? S3B C3SB 1.817(8) . ? F4S3 C3SB 1.327(9) . ? C3SB F1S3 1.377(8) . ? C3SB F2S3 1.479(8) . ? S4 O1S4 1.274(8) . ? S4 O5S4 1.282(8) . ? S4 O4S4 1.427(9) . ? S4 O3S4 1.431(6) . ? S4 O2S4 1.438(8) . ? S4 O6S4 1.549(8) . ? S4 C4SB 1.753(19) . ? S4 C4SA 1.836(15) . ? C4SA F1S4 1.17(2) . ? C4SA F3S4 1.303(16) . ? C4SA F2S4 1.336(17) . ? C4SB F4S4 1.26(2) . ? C4SB F6S4 1.37(3) . ? C4SB F5S4 1.42(3) . ? N101 C101 1.104(5) . ? C101 C102 1.430(6) . ? N102 C103 1.120(6) . ? C103 C104 1.424(7) . ? N103 C105 1.122(5) . ? C105 C106 1.463(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 La1 O1 67.91(7) . . ? O2 La1 O1S1 75.83(7) . . ? O1 La1 O1S1 81.77(7) . . ? O2 La1 N6 79.64(7) . . ? O1 La1 N6 82.91(7) . . ? O1S1 La1 N6 154.57(7) . . ? O2 La1 N5 139.62(8) . . ? O1 La1 N5 82.93(8) . . ? O1S1 La1 N5 72.77(8) . . ? N6 La1 N5 125.12(8) . . ? O2 La1 N3 75.89(7) . . ? O1 La1 N3 142.47(7) . . ? O1S1 La1 N3 99.06(8) . . ? N6 La1 N3 81.19(8) . . ? N5 La1 N3 133.49(8) . . ? O2 La1 N2 130.90(7) . . ? O1 La1 N2 76.80(7) . . ? O1S1 La1 N2 132.08(7) . . ? N6 La1 N2 62.68(7) . . ? N5 La1 N2 62.49(8) . . ? N3 La1 N2 123.65(7) . . ? O2 La1 N1 132.93(7) . . ? O1 La1 N1 140.74(7) . . ? O1S1 La1 N1 130.92(7) . . ? N6 La1 N1 72.07(7) . . ? N5 La1 N1 87.26(8) . . ? N3 La1 N1 63.37(7) . . ? N2 La1 N1 65.02(7) . . ? O2 La1 N4 118.73(8) . . ? O1 La1 N4 145.96(8) . . ? O1S1 La1 N4 69.15(8) . . ? N6 La1 N4 130.39(8) . . ? N5 La1 N4 72.08(8) . . ? N3 La1 N4 62.58(8) . . ? N2 La1 N4 109.73(8) . . ? N1 La1 N4 62.07(8) . . ? O2 La1 La2 34.23(5) . . ? O1 La1 La2 34.04(5) . . ? O1S1 La1 La2 72.75(5) . . ? N6 La1 La2 83.22(5) . . ? N5 La1 La2 110.60(6) . . ? N3 La1 La2 110.06(5) . . ? N2 La1 La2 106.94(5) . . ? N1 La1 La2 155.02(5) . . ? N4 La1 La2 138.90(6) . . ? O1 La2 O2 68.29(7) . . ? O1 La2 O2S1 77.80(7) . . ? O2 La2 O2S1 77.82(7) . . ? O1 La2 N33 144.48(7) . . ? O2 La2 N33 76.19(7) . . ? O2S1 La2 N33 95.45(8) . . ? O1 La2 N35 93.55(7) . . ? O2 La2 N35 76.15(7) . . ? O2S1 La2 N35 153.95(7) . . ? N33 La2 N35 77.28(8) . . ? O1 La2 N32 80.17(7) . . ? O2 La2 N32 125.98(7) . . ? O2S1 La2 N32 137.23(8) . . ? N33 La2 N32 122.80(7) . . ? N35 La2 N32 62.92(7) . . ? O1 La2 N36 79.75(8) . . ? O2 La2 N36 143.62(7) . . ? O2S1 La2 N36 78.86(8) . . ? N33 La2 N36 133.74(8) . . ? N35 La2 N36 124.21(8) . . ? N32 La2 N36 61.35(8) . . ? O1 La2 N31 145.81(7) . . ? O2 La2 N31 131.74(7) . . ? O2S1 La2 N31 128.59(7) . . ? N33 La2 N31 63.21(7) . . ? N35 La2 N31 70.64(7) . . ? N32 La2 N31 65.66(7) . . ? N36 La2 N31 84.61(8) . . ? O1 La2 N34 138.73(7) . . ? O2 La2 N34 121.85(7) . . ? O2S1 La2 N34 67.34(7) . . ? N33 La2 N34 63.14(7) . . ? N35 La2 N34 127.30(7) . . ? N32 La2 N34 110.95(7) . . ? N36 La2 N34 72.63(8) . . ? N31 La2 N34 61.27(7) . . ? O1 La2 La1 34.36(5) . . ? O2 La2 La1 34.30(5) . . ? O2S1 La2 La1 71.45(5) . . ? N33 La2 La1 110.28(5) . . ? N35 La2 La1 87.47(5) . . ? N32 La2 La1 107.29(5) . . ? N36 La2 La1 111.02(6) . . ? N31 La2 La1 157.94(5) . . ? N34 La2 La1 137.01(6) . . ? La2 O1 La1 111.60(9) . . ? La2 O2 La1 111.47(8) . . ? C1 N1 C25 107.3(2) . . ? C1 N1 C7 110.0(2) . . ? C25 N1 C7 107.7(2) . . ? C1 N1 La1 110.89(16) . . ? C25 N1 La1 111.64(16) . . ? C7 N1 La1 109.25(18) . . ? C19 N2 C13 107.3(2) . . ? C19 N2 C26 111.3(2) . . ? C13 N2 C26 108.2(2) . . ? C19 N2 La1 108.74(16) . . ? C13 N2 La1 108.28(17) . . ? C26 N2 La1 112.86(17) . . ? C2 N3 C6 117.5(3) . . ? C2 N3 La1 119.08(18) . . ? C6 N3 La1 119.7(2) . . ? C8 N4 C12 117.1(3) . . ? C8 N4 La1 117.4(2) . . ? C12 N4 La1 125.0(2) . . ? C14 N5 C18 118.4(3) . . ? C14 N5 La1 119.0(2) . . ? C18 N5 La1 122.6(2) . . ? C20 N6 C24 117.9(3) . . ? C20 N6 La1 120.62(19) . . ? C24 N6 La1 121.48(19) . . ? C37 N31 C31 109.5(2) . . ? C37 N31 C55 107.6(2) . . ? C31 N31 C55 109.2(2) . . ? C37 N31 La2 109.27(18) . . ? C31 N31 La2 110.62(16) . . ? C55 N31 La2 110.64(15) . . ? C49 N32 C43 107.1(2) . . ? C49 N32 C56 108.1(2) . . ? C43 N32 C56 111.2(2) . . ? C49 N32 La2 108.82(17) . . ? C43 N32 La2 108.47(16) . . ? C56 N32 La2 113.00(16) . . ? C36 N33 C32 118.2(2) . . ? C36 N33 La2 116.32(18) . . ? C32 N33 La2 120.09(18) . . ? C42 N34 C38 117.1(3) . . ? C42 N34 La2 125.2(2) . . ? C38 N34 La2 116.67(19) . . ? C48 N35 C44 117.2(2) . . ? C48 N35 La2 123.08(18) . . ? C44 N35 La2 118.65(19) . . ? C50 N36 C54 117.8(3) . . ? C50 N36 La2 118.0(2) . . ? C54 N36 La2 124.0(2) . . ? N1 C1 C2 113.9(2) . . ? N3 C2 C3 122.2(3) . . ? N3 C2 C1 117.5(2) . . ? C3 C2 C1 120.3(3) . . ? C4 C3 C2 118.9(3) . . ? C5 C4 C3 119.4(3) . . ? C4 C5 C6 118.7(3) . . ? N3 C6 C5 123.3(3) . . ? N1 C7 C8 114.5(3) . . ? N4 C8 C9 122.7(3) . . ? N4 C8 C7 117.9(3) . . ? C9 C8 C7 119.3(3) . . ? C10 C9 C8 118.9(4) . . ? C11 C10 C9 119.4(3) . . ? C10 C11 C12 118.9(4) . . ? N4 C12 C11 122.9(4) . . ? N2 C13 C14 112.6(3) . . ? N5 C14 C15 121.4(4) . . ? N5 C14 C13 117.8(3) . . ? C15 C14 C13 120.7(4) . . ? C16 C15 C14 118.8(5) . . ? C17 C16 C15 120.2(4) . . ? C16 C17 C18 118.4(5) . . ? N5 C18 C17 122.7(4) . . ? N2 C19 C20 114.3(2) . . ? N6 C20 C21 121.6(3) . . ? N6 C20 C19 117.7(2) . . ? C21 C20 C19 120.6(3) . . ? C22 C21 C20 119.8(3) . . ? C23 C22 C21 118.4(3) . . ? C22 C23 C24 119.3(3) . . ? N6 C24 C23 123.0(3) . . ? N1 C25 C26 112.2(2) . . ? N2 C26 C25 113.3(2) . . ? N31 C31 C32 113.4(2) . . ? N33 C32 C33 122.2(3) . . ? N33 C32 C31 116.9(2) . . ? C33 C32 C31 120.9(3) . . ? C34 C33 C32 118.5(3) . . ? C33 C34 C35 119.8(3) . . ? C36 C35 C34 118.0(3) . . ? N33 C36 C35 123.3(3) . . ? N31 C37 C38 114.1(2) . . ? N34 C38 C39 122.3(3) . . ? N34 C38 C37 117.5(3) . . ? C39 C38 C37 120.1(3) . . ? C40 C39 C38 119.2(3) . . ? C41 C40 C39 119.0(3) . . ? C40 C41 C42 118.7(3) . . ? N34 C42 C41 123.7(3) . . ? N32 C43 C44 112.6(2) . . ? N35 C44 C45 122.4(3) . . ? N35 C44 C43 115.8(3) . . ? C45 C44 C43 121.8(3) . . ? C46 C45 C44 119.3(3) . . ? C45 C46 C47 118.7(3) . . ? C48 C47 C46 118.9(3) . . ? N35 C48 C47 123.4(3) . . ? N32 C49 C50 112.5(2) . . ? N36 C50 C51 122.3(3) . . ? N36 C50 C49 117.2(3) . . ? C51 C50 C49 120.5(3) . . ? C52 C51 C50 119.0(4) . . ? C51 C52 C53 119.7(4) . . ? C52 C53 C54 118.5(4) . . ? N36 C54 C53 122.8(4) . . ? N31 C55 C56 112.9(2) . . ? N32 C56 C55 114.2(2) . . ? O3S1 S1 O1S1 115.43(17) . . ? O3S1 S1 O2S1 115.03(16) . . ? O1S1 S1 O2S1 113.65(12) . . ? O3S1 S1 C1S 105.6(2) . . ? O1S1 S1 C1S 102.57(17) . . ? O2S1 S1 C1S 102.36(17) . . ? S1 O1S1 La1 135.36(11) . . ? S1 O2S1 La2 134.35(12) . . ? F1S1 C1S F2S1 108.8(4) . . ? F1S1 C1S F3S1 107.7(4) . . ? F2S1 C1S F3S1 109.0(3) . . ? F1S1 C1S S1 110.8(3) . . ? F2S1 C1S S1 110.4(3) . . ? F3S1 C1S S1 110.0(3) . . ? O1S2 S2A O2S2 126.8(4) . . ? O1S2 S2A O3S2 108.2(4) . . ? O2S2 S2A O3S2 106.5(4) . . ? O1S2 S2A C2SA 105.7(3) . . ? O2S2 S2A C2SA 105.2(4) . . ? O3S2 S2A C2SA 101.8(5) . . ? F3S2 C2SA F1S2 110.5(8) . . ? F3S2 C2SA F2S2 103.3(7) . . ? F1S2 C2SA F2S2 104.7(9) . . ? F3S2 C2SA S2A 111.4(10) . . ? F1S2 C2SA S2A 113.5(5) . . ? F2S2 C2SA S2A 112.8(5) . . ? O2S2 S2B O1S2 119.0(5) . . ? O2S2 S2B O4S2 107.3(6) . . ? O1S2 S2B O4S2 106.6(7) . . ? O2S2 S2B C2SB 114.5(8) . . ? O1S2 S2B C2SB 105.3(7) . . ? O4S2 S2B C2SB 102.8(12) . . ? F1S2 C2SB F2S2 109.9(18) . . ? F1S2 C2SB F4S2 117.1(17) . . ? F2S2 C2SB F4S2 111.5(18) . . ? F1S2 C2SB S2B 103.9(15) . . ? F2S2 C2SB S2B 106.6(13) . . ? F4S2 C2SB S2B 107.0(19) . . ? C2SB F1S2 C2SA 38.5(9) . . ? C2SB F2S2 C2SA 37.5(9) . . ? S2A O1S2 S2B 25.6(2) . . ? S2B O2S2 S2A 26.4(2) . . ? O2S3 S3A O1S3 121.6(3) . . ? O2S3 S3A O3S3 104.0(3) . . ? O1S3 S3A O3S3 110.7(4) . . ? O2S3 S3A C3SA 110.1(3) . . ? O1S3 S3A C3SA 106.6(3) . . ? O3S3 S3A C3SA 102.4(4) . . ? F3S3 C3SA F2S3 128.0(5) . . ? F3S3 C3SA F1S3 117.2(4) . . ? F2S3 C3SA F1S3 94.0(3) . . ? F3S3 C3SA S3A 107.2(5) . . ? F2S3 C3SA S3A 104.4(3) . . ? F1S3 C3SA S3A 103.0(3) . . ? O4S3 S3B O2S3 111.1(4) . . ? O4S3 S3B O1S3 118.5(5) . . ? O2S3 S3B O1S3 112.0(3) . . ? O4S3 S3B C3SB 106.3(5) . . ? O2S3 S3B C3SB 106.7(4) . . ? O1S3 S3B C3SB 100.9(3) . . ? F4S3 C3SB F1S3 115.8(6) . . ? F4S3 C3SB F2S3 122.6(7) . . ? F1S3 C3SB F2S3 97.7(5) . . ? F4S3 C3SB S3B 115.4(6) . . ? F1S3 C3SB S3B 103.8(5) . . ? F2S3 C3SB S3B 98.3(5) . . ? C3SB F1S3 C3SA 51.0(4) . . ? C3SA F2S3 C3SB 50.3(3) . . ? S3A O1S3 S3B 25.90(13) . . ? S3A O2S3 S3B 26.99(14) . . ? O1S4 S4 O5S4 145.9(6) . . ? O1S4 S4 O4S4 60.7(7) . . ? O5S4 S4 O4S4 118.1(9) . . ? O1S4 S4 O3S4 119.4(7) . . ? O5S4 S4 O3S4 53.2(8) . . ? O4S4 S4 O3S4 166.5(5) . . ? O1S4 S4 O2S4 118.2(8) . . ? O5S4 S4 O2S4 56.0(8) . . ? O4S4 S4 O2S4 63.3(6) . . ? O3S4 S4 O2S4 109.1(6) . . ? O1S4 S4 O6S4 43.3(6) . . ? O5S4 S4 O6S4 115.0(8) . . ? O4S4 S4 O6S4 101.9(7) . . ? O3S4 S4 O6S4 76.2(5) . . ? O2S4 S4 O6S4 138.6(5) . . ? O1S4 S4 C4SB 99.3(8) . . ? O5S4 S4 C4SB 113.0(9) . . ? O4S4 S4 C4SB 104.1(10) . . ? O3S4 S4 C4SB 89.4(10) . . ? O2S4 S4 C4SB 117.8(8) . . ? O6S4 S4 C4SB 103.0(7) . . ? O1S4 S4 C4SA 108.5(7) . . ? O5S4 S4 C4SA 105.6(8) . . ? O4S4 S4 C4SA 91.7(7) . . ? O3S4 S4 C4SA 100.6(6) . . ? O2S4 S4 C4SA 96.9(6) . . ? O6S4 S4 C4SA 123.0(6) . . ? C4SB S4 C4SA 21.2(6) . . ? F1S4 C4SA F3S4 110.4(15) . . ? F1S4 C4SA F2S4 100.0(16) . . ? F3S4 C4SA F2S4 105.6(13) . . ? F1S4 C4SA S4 121.3(12) . . ? F3S4 C4SA S4 112.4(11) . . ? F2S4 C4SA S4 105.1(12) . . ? F4S4 C4SB F6S4 103.5(15) . . ? F4S4 C4SB F5S4 117(3) . . ? F6S4 C4SB F5S4 110.0(19) . . ? F4S4 C4SB S4 115.2(15) . . ? F6S4 C4SB S4 110.1(17) . . ? F5S4 C4SB S4 101.2(16) . . ? N101 C101 C102 178.0(6) . . ? N102 C103 C104 178.1(6) . . ? N103 C105 C106 178.5(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1O N103 0.64(3) 2.43(3) 3.065(4) 172(4) 1_455 O2 H2O O6S4 0.65(3) 2.59(4) 3.237(8) 174(4) . _diffrn_measured_fraction_theta_max 0.851 _diffrn_reflns_theta_full 28.68 _diffrn_measured_fraction_theta_full 0.851 _refine_diff_density_max 0.712 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.062 # Attachment 'cifstruc3.doc' data_struc_[La6(tpen)4(CO3)6(OTF)6]8CH3CN.2H20,_3 _database_code_depnum_ccdc_archive 'CCDC 285415' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (La6(tpen)4(CO3)6(OTF)6)8CH3CN.2H20 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C132 H140 F18 La6 N32 O38 S6' _chemical_formula_weight 4150.58 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.965(3) _cell_length_b 16.947(3) _cell_length_c 18.924(4) _cell_angle_alpha 100.72(3) _cell_angle_beta 105.91(3) _cell_angle_gamma 118.09(3) _cell_volume 4033.1(14) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2060 _exptl_absorpt_coefficient_mu 1.735 _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 298(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 19405 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.68 _reflns_number_total 16219 _reflns_number_gt 12508 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0439P)^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 16219 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0866 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.360762(18) 0.375811(17) 0.219254(12) 0.02708(6) Uani 1 1 d . . . La2 La 0.637239(17) 0.797076(16) 0.499336(13) 0.02510(6) Uani 1 1 d . . . La3 La 0.346606(17) 0.462535(16) 0.430976(12) 0.02442(6) Uani 1 1 d . . . N1 N 0.3038(3) 0.3172(2) 0.05587(19) 0.0342(8) Uani 1 1 d . . . N2 N 0.2995(3) 0.4796(2) 0.14907(19) 0.0341(8) Uani 1 1 d . . . N3 N 0.4457(3) 0.2883(3) 0.1601(2) 0.0429(9) Uani 1 1 d . . . N4 N 0.2268(3) 0.1814(3) 0.1322(2) 0.0400(9) Uani 1 1 d . . . N5 N 0.5063(3) 0.5189(3) 0.1951(2) 0.0396(9) Uani 1 1 d . . . N6 N 0.1641(3) 0.3361(3) 0.1890(2) 0.0400(9) Uani 1 1 d . . . N31 N 0.7060(3) 0.9895(2) 0.5718(2) 0.0342(8) Uani 1 1 d . . . N32 N 0.7232(2) 0.9206(2) 0.42384(19) 0.0310(8) Uani 1 1 d . . . N33 N 0.8356(3) 0.9237(3) 0.6186(2) 0.0379(9) Uani 1 1 d . . . N34 N 0.5143(3) 0.8334(3) 0.5567(2) 0.0352(8) Uani 1 1 d . . . N35 N 0.5070(3) 0.8132(2) 0.3788(2) 0.0340(8) Uani 1 1 d . . . N36 N 0.7757(3) 0.7883(3) 0.4429(2) 0.0346(8) Uani 1 1 d . . . C1 C 0.3815(4) 0.3049(4) 0.0353(3) 0.0465(12) Uani 1 1 d . . . H1A H 0.4377 0.3672 0.0413 0.056 Uiso 1 1 calc R . . H1B H 0.3481 0.2636 -0.0201 0.056 Uiso 1 1 calc R . . C2 C 0.4280(3) 0.2630(3) 0.0833(2) 0.0374(10) Uani 1 1 d . . . C3 C 0.4573(4) 0.2067(4) 0.0498(3) 0.0545(13) Uani 1 1 d . . . H3 H 0.4431 0.1896 -0.0038 0.065 Uiso 1 1 calc R . . C4 C 0.5083(5) 0.1759(4) 0.0972(3) 0.0690(17) Uani 1 1 d . . . H4 H 0.5304 0.1389 0.0765 0.083 Uiso 1 1 calc R . . C5 C 0.5255(5) 0.2009(4) 0.1753(3) 0.0686(17) Uani 1 1 d . . . H5 H 0.5588 0.1805 0.2083 0.082 Uiso 1 1 calc R . . C6 C 0.4932(4) 0.2562(4) 0.2040(3) 0.0573(15) Uani 1 1 d . . . H6 H 0.5050 0.2723 0.2571 0.069 Uiso 1 1 calc R . . C7 C 0.1996(3) 0.2247(3) 0.0168(2) 0.0416(11) Uani 1 1 d . . . H7A H 0.1846 0.1977 -0.0385 0.050 Uiso 1 1 calc R . . H7B H 0.1472 0.2378 0.0187 0.050 Uiso 1 1 calc R . . C8 C 0.1901(3) 0.1510(3) 0.0529(2) 0.0367(10) Uani 1 1 d . . . C9 C 0.1395(4) 0.0548(3) 0.0063(3) 0.0517(13) Uani 1 1 d . . . H9 H 0.1143 0.0351 -0.0485 0.062 Uiso 1 1 calc R . . C10 C 0.1271(5) -0.0106(4) 0.0419(3) 0.0607(15) Uani 1 1 d . . . H10 H 0.0927 -0.0755 0.0114 0.073 Uiso 1 1 calc R . . C11 C 0.1652(5) 0.0195(4) 0.1221(3) 0.0617(15) Uani 1 1 d . . . H11 H 0.1583 -0.0240 0.1473 0.074 Uiso 1 1 calc R . . C12 C 0.2140(4) 0.1154(4) 0.1649(3) 0.0540(14) Uani 1 1 d . . . H12 H 0.2397 0.1357 0.2198 0.065 Uiso 1 1 calc R . . C13 C 0.3923(3) 0.5771(3) 0.1695(3) 0.0413(11) Uani 1 1 d . . . H13A H 0.4074 0.6186 0.2204 0.050 Uiso 1 1 calc R . . H13B H 0.3738 0.6030 0.1307 0.050 Uiso 1 1 calc R . . C14 C 0.4903(4) 0.5833(3) 0.1736(2) 0.0417(11) Uani 1 1 d . . . C15 C 0.5654(4) 0.6596(4) 0.1622(3) 0.0556(14) Uani 1 1 d . . . H15 H 0.5514 0.7021 0.1457 0.067 Uiso 1 1 calc R . . C16 C 0.6598(5) 0.6712(5) 0.1758(3) 0.0752(19) Uani 1 1 d . . . H16 H 0.7115 0.7224 0.1695 0.090 Uiso 1 1 calc R . . C17 C 0.6774(4) 0.6046(5) 0.1992(3) 0.0708(17) Uani 1 1 d . . . H17 H 0.7408 0.6105 0.2085 0.085 Uiso 1 1 calc R . . C18 C 0.5986(4) 0.5301(4) 0.2080(3) 0.0541(13) Uani 1 1 d . . . H18 H 0.6101 0.4858 0.2236 0.065 Uiso 1 1 calc R . . C19 C 0.2278(3) 0.4925(3) 0.1786(3) 0.0388(10) Uani 1 1 d . . . H19A H 0.1980 0.5195 0.1472 0.047 Uiso 1 1 calc R . . H19B H 0.2676 0.5382 0.2329 0.047 Uiso 1 1 calc R . . C20 C 0.1409(3) 0.3998(3) 0.1752(2) 0.0391(11) Uani 1 1 d . . . C21 C 0.0449(4) 0.3857(4) 0.1628(3) 0.0582(14) Uani 1 1 d . . . H21 H 0.0319 0.4321 0.1548 0.070 Uiso 1 1 calc R . . C22 C -0.0325(5) 0.2997(5) 0.1627(4) 0.0744(18) Uani 1 1 d . . . H22 H -0.0985 0.2873 0.1538 0.089 Uiso 1 1 calc R . . C23 C -0.0096(4) 0.2339(4) 0.1760(3) 0.0613(15) Uani 1 1 d . . . H23 H -0.0600 0.1764 0.1765 0.074 Uiso 1 1 calc R . . C24 C 0.0872(4) 0.2535(4) 0.1886(3) 0.0523(13) Uani 1 1 d . . . H24 H 0.1016 0.2081 0.1973 0.063 Uiso 1 1 calc R . . C25 C 0.2951(4) 0.3891(3) 0.0254(2) 0.0379(10) Uani 1 1 d . . . H25A H 0.2560 0.3595 -0.0316 0.045 Uiso 1 1 calc R . . H25B H 0.3644 0.4425 0.0371 0.045 Uiso 1 1 calc R . . C26 C 0.2415(3) 0.4271(3) 0.0614(2) 0.0376(10) Uani 1 1 d . . . H26A H 0.2336 0.4702 0.0371 0.045 Uiso 1 1 calc R . . H26B H 0.1721 0.3736 0.0495 0.045 Uiso 1 1 calc R . . C31 C 0.7684(4) 1.0197(3) 0.6572(2) 0.0414(11) Uani 1 1 d . . . H31A H 0.7227 0.9849 0.6804 0.050 Uiso 1 1 calc R . . H31B H 0.7992 1.0878 0.6833 0.050 Uiso 1 1 calc R . . C32 C 0.8539(3) 1.0012(3) 0.6715(2) 0.0371(10) Uani 1 1 d . . . C33 C 0.9469(4) 1.0603(4) 0.7403(3) 0.0534(13) Uani 1 1 d . . . H33 H 0.9597 1.1152 0.7753 0.064 Uiso 1 1 calc R . . C34 C 1.0192(4) 1.0360(4) 0.7553(3) 0.0591(15) Uani 1 1 d . . . H34 H 1.0814 1.0744 0.8008 0.071 Uiso 1 1 calc R . . C35 C 0.9986(4) 0.9541(4) 0.7024(3) 0.0552(14) Uani 1 1 d . . . H35 H 1.0453 0.9352 0.7122 0.066 Uiso 1 1 calc R . . C36 C 0.9072(4) 0.9016(3) 0.6347(3) 0.0458(12) Uani 1 1 d . . . H36 H 0.8943 0.8477 0.5982 0.055 Uiso 1 1 calc R . . C37 C 0.6150(4) 0.9970(3) 0.5623(3) 0.0419(11) Uani 1 1 d . . . H37A H 0.5809 0.9882 0.5078 0.050 Uiso 1 1 calc R . . H37B H 0.6393 1.0610 0.5957 0.050 Uiso 1 1 calc R . . C38 C 0.5365(3) 0.9230(3) 0.5837(2) 0.0359(10) Uani 1 1 d . . . C39 C 0.4890(4) 0.9464(4) 0.6267(3) 0.0468(12) Uani 1 1 d . . . H39 H 0.5079 1.0097 0.6460 0.056 Uiso 1 1 calc R . . C40 C 0.4137(4) 0.8762(4) 0.6411(3) 0.0566(14) Uani 1 1 d . . . H40 H 0.3798 0.8907 0.6690 0.068 Uiso 1 1 calc R . . C41 C 0.3899(4) 0.7843(4) 0.6132(3) 0.0533(13) Uani 1 1 d . . . H41 H 0.3391 0.7350 0.6217 0.064 Uiso 1 1 calc R . . C42 C 0.4422(3) 0.7660(3) 0.5724(3) 0.0410(11) Uani 1 1 d . . . H42 H 0.4267 0.7037 0.5549 0.049 Uiso 1 1 calc R . . C43 C 0.6510(3) 0.8651(3) 0.3386(2) 0.0365(10) Uani 1 1 d . . . H43A H 0.6527 0.8087 0.3206 0.044 Uiso 1 1 calc R . . H43B H 0.6752 0.9046 0.3085 0.044 Uiso 1 1 calc R . . C44 C 0.5399(3) 0.8335(3) 0.3223(2) 0.0303(9) Uani 1 1 d . . . C45 C 0.4743(4) 0.8227(3) 0.2504(3) 0.0428(11) Uani 1 1 d . . . H45 H 0.4991 0.8381 0.2127 0.051 Uiso 1 1 calc R . . C46 C 0.3716(4) 0.7887(3) 0.2360(3) 0.0465(12) Uani 1 1 d . . . H46 H 0.3260 0.7802 0.1880 0.056 Uiso 1 1 calc R . . C47 C 0.3374(3) 0.7678(3) 0.2933(3) 0.0464(12) Uani 1 1 d . . . H47 H 0.2685 0.7451 0.2849 0.056 Uiso 1 1 calc R . . C48 C 0.4071(3) 0.7809(3) 0.3637(3) 0.0401(11) Uani 1 1 d . . . H48 H 0.3837 0.7668 0.4024 0.048 Uiso 1 1 calc R . . C49 C 0.8280(3) 0.9442(3) 0.4339(3) 0.0386(11) Uani 1 1 d . . . H49A H 0.8779 0.9912 0.4869 0.046 Uiso 1 1 calc R . . H49B H 0.8469 0.9736 0.3967 0.046 Uiso 1 1 calc R . . C50 C 0.8360(3) 0.8587(3) 0.4217(2) 0.0334(10) Uani 1 1 d . . . C51 C 0.9042(4) 0.8540(4) 0.3927(3) 0.0498(13) Uani 1 1 d . . . H51 H 0.9445 0.9032 0.3780 0.060 Uiso 1 1 calc R . . C52 C 0.9126(4) 0.7765(4) 0.3856(4) 0.0658(16) Uani 1 1 d . . . H52 H 0.9598 0.7733 0.3674 0.079 Uiso 1 1 calc R . . C53 C 0.8500(4) 0.7027(4) 0.4060(3) 0.0566(14) Uani 1 1 d . . . H53 H 0.8537 0.6490 0.4012 0.068 Uiso 1 1 calc R . . C54 C 0.7823(4) 0.7114(4) 0.4335(3) 0.0450(12) Uani 1 1 d . . . H54 H 0.7392 0.6616 0.4463 0.054 Uiso 1 1 calc R . . C55 C 0.7716(3) 1.0552(3) 0.5395(3) 0.0411(11) Uani 1 1 d . . . H55A H 0.8419 1.0699 0.5626 0.049 Uiso 1 1 calc R . . H55B H 0.7754 1.1152 0.5544 0.049 Uiso 1 1 calc R . . C56 C 0.7285(3) 1.0115(3) 0.4504(3) 0.0386(10) Uani 1 1 d . . . H56A H 0.6590 0.9987 0.4272 0.046 Uiso 1 1 calc R . . H56B H 0.7725 1.0572 0.4318 0.046 Uiso 1 1 calc R . . C201 C 0.4725(3) 0.6051(3) 0.3743(2) 0.0291(9) Uani 1 1 d . . . O201 O 0.3977(2) 0.51858(18) 0.32397(15) 0.0291(6) Uani 1 1 d . . . O202 O 0.5504(2) 0.6611(2) 0.36450(16) 0.0361(7) Uani 1 1 d . . . O203 O 0.4640(2) 0.63388(18) 0.43990(15) 0.0292(6) Uani 1 1 d . . . C202 C 0.4367(3) 0.5420(3) 0.6028(2) 0.0290(9) Uani 1 1 d . . . O211 O 0.4855(2) 0.5259(2) 0.56284(15) 0.0311(6) Uani 1 1 d . . . O212 O 0.3458(2) 0.5211(2) 0.56141(16) 0.0420(8) Uani 1 1 d . . . O213 O 0.4776(2) 0.5764(2) 0.67763(15) 0.0389(7) Uani 1 1 d . . . C203 C 0.3225(3) 0.2771(3) 0.3730(2) 0.0283(9) Uani 1 1 d . . . O221 O 0.3153(2) 0.30553(19) 0.43875(15) 0.0284(6) Uani 1 1 d . . . O222 O 0.3030(2) 0.31386(19) 0.32102(15) 0.0308(6) Uani 1 1 d . . . O223 O 0.3468(2) 0.2165(2) 0.36320(16) 0.0381(7) Uani 1 1 d . . . N104 N 0.1383(3) 0.3484(3) 0.3984(3) 0.0543(11) Uani 1 1 d . . . C61 C 0.0545(4) 0.3127(4) 0.3880(3) 0.0590(14) Uani 1 1 d . . . C62 C -0.0543(5) 0.2677(6) 0.3754(5) 0.120(3) Uani 1 1 d . . . H10J H -0.0851 0.2935 0.3443 0.181 Uiso 1 1 calc R . . H10K H -0.0583 0.2804 0.4256 0.181 Uiso 1 1 calc R . . H10L H -0.0914 0.1994 0.3481 0.181 Uiso 1 1 calc R . . O1 O 0.2388(3) 0.5361(3) 0.3862(2) 0.0562(9) Uani 1 1 d . . . H1O H 0.1602 0.5289 0.3871 0.050 Uiso 1 1 d . . . H2O H 0.2579 0.5521 0.4383 0.050 Uiso 1 1 d . . . S1 S 0.72513(10) -0.01786(10) 0.18168(8) 0.0538(3) Uani 1 1 d . . . F1S1 F 0.5938(4) 0.0300(4) 0.1831(3) 0.1245(16) Uani 1 1 d . . . F2S1 F 0.7241(4) 0.1313(3) 0.1686(3) 0.1322(18) Uani 1 1 d . . . F3S1 F 0.6031(3) 0.0015(3) 0.0724(2) 0.1067(14) Uani 1 1 d . . . O1S1 O 0.6438(3) -0.1163(3) 0.1558(2) 0.0691(11) Uani 1 1 d . . . O2S1 O 0.7772(3) 0.0322(3) 0.2657(2) 0.0796(12) Uani 1 1 d . . . O3S1 O 0.7934(3) 0.0004(4) 0.1425(3) 0.0949(15) Uani 1 1 d . . . C1S C 0.6598(5) 0.0387(5) 0.1492(4) 0.0723(17) Uani 1 1 d . . . S2 S 0.12017(11) 0.65942(12) 0.41321(9) 0.0600(4) Uani 1 1 d . . . F1S2 F -0.0588(3) 0.5927(3) 0.2985(3) 0.1108(14) Uani 1 1 d . . . F2S2 F 0.0530(4) 0.5830(4) 0.2616(3) 0.1354(18) Uani 1 1 d . . . F3S2 F 0.0702(3) 0.7181(3) 0.3020(2) 0.1055(14) Uani 1 1 d . . . O1S2 O 0.2238(3) 0.7142(3) 0.4198(3) 0.0878(14) Uani 1 1 d . . . O2S2 O 0.0911(4) 0.7098(3) 0.4602(3) 0.0859(13) Uani 1 1 d . . . O3S2 O 0.0881(4) 0.5644(3) 0.4130(3) 0.0997(16) Uani 1 1 d . . . C2S C 0.0421(5) 0.6359(5) 0.3140(4) 0.0721(17) Uani 1 1 d . . . S3 S 0.04655(12) 0.74308(10) 0.10126(8) 0.0601(4) Uani 1 1 d . . . F1S3 F -0.0341(3) 0.5667(2) 0.0100(2) 0.0922(12) Uani 1 1 d . . . F2S3 F 0.1274(3) 0.6610(3) 0.0421(3) 0.1161(15) Uani 1 1 d . . . F3S3 F 0.0789(4) 0.6111(3) 0.1254(2) 0.1120(15) Uani 1 1 d . . . O1S3 O -0.0398(4) 0.7047(3) 0.1233(3) 0.0946(14) Uani 1 1 d . . . O2S3 O 0.0247(4) 0.7655(3) 0.0323(2) 0.0850(14) Uani 1 1 d . . . O3S3 O 0.1467(3) 0.8123(3) 0.1652(2) 0.0856(13) Uani 1 1 d . . . C3S C 0.0540(5) 0.6402(4) 0.0692(3) 0.0616(15) Uani 1 1 d . . . N111 N 0.6234(7) 0.4198(6) 0.0320(5) 0.126(3) Uani 1 1 d . . . C101 C 0.6929(8) 0.4187(7) 0.0661(6) 0.111(3) Uani 1 1 d . . . C102 C 0.7794(8) 0.4179(9) 0.1085(6) 0.200(6) Uani 1 1 d . . . H10A H 0.8290 0.4782 0.1524 0.301 Uiso 1 1 calc R . . H10B H 0.8115 0.4087 0.0744 0.301 Uiso 1 1 calc R . . H10C H 0.7569 0.3663 0.1278 0.301 Uiso 1 1 calc R . . N112 N 0.3594(11) 0.8035(10) 0.0356(9) 0.209(6) Uani 1 1 d . . . C103 C 0.3318(10) 0.8567(10) 0.0480(8) 0.146(5) Uani 1 1 d . . . C104 C 0.3057(11) 0.9189(9) 0.0729(10) 0.245(10) Uani 1 1 d . . . H10D H 0.2695 0.9271 0.0281 0.368 Uiso 1 1 calc R . . H10E H 0.3679 0.9800 0.1089 0.368 Uiso 1 1 calc R . . H10F H 0.2612 0.8936 0.0991 0.368 Uiso 1 1 calc R . . N113 N 0.2016(10) 0.6455(9) 0.7182(8) 0.220(6) Uani 1 1 d . . . C105 C 0.1817(9) 0.5911(10) 0.6579(9) 0.163(5) Uani 1 1 d . . . C106 C 0.1537(7) 0.5313(7) 0.5821(6) 0.121(3) Uani 1 1 d . . . H10G H 0.1822 0.4927 0.5866 0.182 Uiso 1 1 calc R . . H10H H 0.1807 0.5702 0.5530 0.182 Uiso 1 1 calc R . . H10I H 0.0789 0.4901 0.5549 0.182 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 La1 0.03283(12) 0.02552(14) 0.02295(11) 0.00876(9) 0.01081(9) 0.01669(10) La2 0.02837(12) 0.02013(13) 0.02732(11) 0.00968(9) 0.01105(9) 0.01375(10) La3 0.02546(11) 0.02377(13) 0.02517(11) 0.00919(9) 0.00990(9) 0.01470(10) N1 0.044(2) 0.032(2) 0.0262(17) 0.0117(15) 0.0131(15) 0.0213(17) N2 0.040(2) 0.030(2) 0.0290(17) 0.0097(15) 0.0111(15) 0.0194(17) N3 0.055(2) 0.050(3) 0.0311(19) 0.0104(18) 0.0169(17) 0.036(2) N4 0.056(2) 0.028(2) 0.036(2) 0.0123(17) 0.0193(18) 0.0231(19) N5 0.041(2) 0.033(2) 0.038(2) 0.0143(17) 0.0169(17) 0.0159(18) N6 0.036(2) 0.039(2) 0.044(2) 0.0167(18) 0.0156(17) 0.0207(18) N31 0.039(2) 0.025(2) 0.0378(19) 0.0104(16) 0.0149(16) 0.0182(16) N32 0.0283(17) 0.029(2) 0.0361(18) 0.0145(16) 0.0127(14) 0.0154(15) N33 0.035(2) 0.029(2) 0.040(2) 0.0084(17) 0.0086(16) 0.0156(17) N34 0.042(2) 0.032(2) 0.040(2) 0.0144(17) 0.0187(16) 0.0250(18) N35 0.0345(19) 0.031(2) 0.040(2) 0.0158(17) 0.0150(16) 0.0199(16) N36 0.038(2) 0.034(2) 0.0373(19) 0.0142(17) 0.0177(16) 0.0225(17) C1 0.065(3) 0.062(3) 0.032(2) 0.021(2) 0.028(2) 0.043(3) C2 0.039(2) 0.038(3) 0.035(2) 0.011(2) 0.0152(19) 0.023(2) C3 0.075(4) 0.059(4) 0.041(3) 0.014(3) 0.028(3) 0.044(3) C4 0.097(5) 0.082(5) 0.065(4) 0.023(3) 0.037(3) 0.075(4) C5 0.100(5) 0.087(5) 0.046(3) 0.022(3) 0.020(3) 0.077(4) C6 0.085(4) 0.075(4) 0.032(2) 0.016(3) 0.018(3) 0.063(3) C7 0.046(3) 0.034(3) 0.032(2) 0.010(2) 0.0075(19) 0.019(2) C8 0.040(2) 0.030(3) 0.034(2) 0.009(2) 0.0128(19) 0.017(2) C9 0.065(3) 0.037(3) 0.037(3) 0.005(2) 0.013(2) 0.023(3) C10 0.088(4) 0.027(3) 0.053(3) 0.010(2) 0.024(3) 0.027(3) C11 0.093(4) 0.038(3) 0.059(3) 0.028(3) 0.035(3) 0.035(3) C12 0.082(4) 0.037(3) 0.040(3) 0.014(2) 0.025(3) 0.031(3) C13 0.054(3) 0.028(3) 0.038(2) 0.016(2) 0.015(2) 0.021(2) C14 0.044(3) 0.034(3) 0.030(2) 0.008(2) 0.0141(19) 0.012(2) C15 0.064(3) 0.041(3) 0.048(3) 0.023(2) 0.025(3) 0.016(3) C16 0.054(4) 0.066(4) 0.067(4) 0.022(3) 0.031(3) 0.004(3) C17 0.045(3) 0.078(5) 0.068(4) 0.018(3) 0.024(3) 0.021(3) C18 0.044(3) 0.053(3) 0.055(3) 0.016(3) 0.022(2) 0.020(3) C19 0.049(3) 0.038(3) 0.035(2) 0.011(2) 0.015(2) 0.031(2) C20 0.041(2) 0.045(3) 0.035(2) 0.015(2) 0.0154(19) 0.026(2) C21 0.052(3) 0.067(4) 0.074(4) 0.033(3) 0.029(3) 0.041(3) C22 0.049(3) 0.090(5) 0.097(5) 0.044(4) 0.034(3) 0.041(4) C23 0.046(3) 0.061(4) 0.070(4) 0.029(3) 0.026(3) 0.021(3) C24 0.047(3) 0.054(3) 0.060(3) 0.029(3) 0.024(2) 0.027(3) C25 0.049(3) 0.034(3) 0.028(2) 0.0128(19) 0.0124(19) 0.023(2) C26 0.048(3) 0.034(3) 0.028(2) 0.0125(19) 0.0094(19) 0.024(2) C31 0.047(3) 0.029(3) 0.038(2) 0.004(2) 0.013(2) 0.019(2) C32 0.037(2) 0.029(3) 0.037(2) 0.012(2) 0.0131(19) 0.014(2) C33 0.048(3) 0.051(3) 0.039(3) 0.005(2) 0.011(2) 0.020(3) C34 0.043(3) 0.067(4) 0.040(3) 0.010(3) 0.005(2) 0.021(3) C35 0.039(3) 0.060(4) 0.057(3) 0.022(3) 0.010(2) 0.026(3) C36 0.044(3) 0.041(3) 0.046(3) 0.013(2) 0.013(2) 0.024(2) C37 0.052(3) 0.031(3) 0.055(3) 0.015(2) 0.025(2) 0.031(2) C38 0.042(2) 0.039(3) 0.036(2) 0.016(2) 0.0150(19) 0.029(2) C39 0.058(3) 0.045(3) 0.054(3) 0.018(2) 0.028(2) 0.038(3) C40 0.071(4) 0.070(4) 0.061(3) 0.029(3) 0.043(3) 0.052(3) C41 0.051(3) 0.065(4) 0.057(3) 0.029(3) 0.031(3) 0.033(3) C42 0.044(3) 0.037(3) 0.046(3) 0.018(2) 0.022(2) 0.024(2) C43 0.040(2) 0.041(3) 0.036(2) 0.019(2) 0.0215(19) 0.023(2) C44 0.037(2) 0.024(2) 0.035(2) 0.0151(18) 0.0156(18) 0.0197(19) C45 0.049(3) 0.047(3) 0.036(2) 0.018(2) 0.013(2) 0.030(2) C46 0.043(3) 0.051(3) 0.041(3) 0.019(2) 0.006(2) 0.027(2) C47 0.032(2) 0.044(3) 0.058(3) 0.016(2) 0.013(2) 0.021(2) C48 0.042(3) 0.038(3) 0.044(3) 0.017(2) 0.019(2) 0.023(2) C49 0.031(2) 0.036(3) 0.048(3) 0.020(2) 0.019(2) 0.016(2) C50 0.028(2) 0.034(3) 0.036(2) 0.0128(19) 0.0128(17) 0.0167(19) C51 0.042(3) 0.043(3) 0.070(3) 0.025(3) 0.031(3) 0.022(2) C52 0.059(3) 0.071(4) 0.096(5) 0.036(4) 0.051(3) 0.043(3) C53 0.066(3) 0.046(3) 0.085(4) 0.030(3) 0.042(3) 0.042(3) C54 0.055(3) 0.041(3) 0.050(3) 0.022(2) 0.028(2) 0.029(2) C55 0.042(3) 0.020(2) 0.056(3) 0.013(2) 0.021(2) 0.014(2) C56 0.042(2) 0.029(3) 0.051(3) 0.023(2) 0.022(2) 0.020(2) C201 0.033(2) 0.024(2) 0.030(2) 0.0103(18) 0.0092(17) 0.0172(19) O201 0.0341(15) 0.0215(15) 0.0274(14) 0.0084(12) 0.0092(12) 0.0146(13) O202 0.0360(16) 0.0277(17) 0.0375(16) 0.0098(13) 0.0194(13) 0.0113(13) O203 0.0366(15) 0.0231(16) 0.0270(14) 0.0071(12) 0.0142(12) 0.0161(13) C202 0.035(2) 0.028(2) 0.030(2) 0.0108(18) 0.0154(17) 0.0203(19) O211 0.0298(14) 0.0374(17) 0.0263(14) 0.0091(13) 0.0105(11) 0.0204(13) O212 0.0348(16) 0.062(2) 0.0335(16) 0.0119(15) 0.0137(13) 0.0325(16) O213 0.0404(17) 0.051(2) 0.0273(15) 0.0095(14) 0.0134(13) 0.0291(15) C203 0.0255(19) 0.022(2) 0.030(2) 0.0079(17) 0.0097(16) 0.0099(17) O221 0.0397(15) 0.0256(15) 0.0260(13) 0.0121(12) 0.0164(12) 0.0200(13) O222 0.0375(15) 0.0256(16) 0.0282(14) 0.0122(12) 0.0115(12) 0.0173(13) O223 0.0527(19) 0.0402(19) 0.0344(16) 0.0139(14) 0.0191(14) 0.0341(16) N104 0.040(2) 0.050(3) 0.075(3) 0.027(2) 0.025(2) 0.024(2) C61 0.046(3) 0.055(4) 0.058(3) 0.011(3) 0.017(3) 0.022(3) C62 0.044(4) 0.135(7) 0.117(6) -0.003(5) 0.036(4) 0.021(4) O1 0.052(2) 0.065(2) 0.076(2) 0.036(2) 0.0278(18) 0.0449(19) S1 0.0477(7) 0.0577(9) 0.0509(7) 0.0257(7) 0.0204(6) 0.0236(7) F1S1 0.124(4) 0.160(4) 0.131(4) 0.038(3) 0.061(3) 0.109(4) F2S1 0.136(4) 0.061(3) 0.157(5) 0.034(3) 0.022(3) 0.047(3) F3S1 0.130(3) 0.110(3) 0.071(3) 0.032(2) 0.007(2) 0.079(3) O1S1 0.079(3) 0.049(2) 0.062(2) 0.0191(19) 0.023(2) 0.026(2) O2S1 0.074(3) 0.074(3) 0.055(2) 0.017(2) 0.014(2) 0.025(2) O3S1 0.077(3) 0.126(4) 0.105(4) 0.056(3) 0.060(3) 0.056(3) C1S 0.075(4) 0.061(5) 0.073(4) 0.019(3) 0.023(3) 0.037(4) S2 0.0576(8) 0.0757(11) 0.0749(9) 0.0409(8) 0.0403(7) 0.0453(8) F1S2 0.065(3) 0.111(3) 0.110(3) 0.022(3) 0.015(2) 0.034(2) F2S2 0.176(5) 0.143(4) 0.087(3) 0.007(3) 0.058(3) 0.099(4) F3S2 0.128(4) 0.105(3) 0.093(3) 0.061(3) 0.041(3) 0.065(3) O1S2 0.051(2) 0.113(4) 0.103(3) 0.050(3) 0.040(2) 0.041(3) O2S2 0.101(3) 0.116(4) 0.077(3) 0.039(3) 0.056(3) 0.074(3) O3S2 0.111(4) 0.100(4) 0.166(5) 0.095(4) 0.089(4) 0.081(3) C2S 0.068(4) 0.069(4) 0.078(4) 0.018(4) 0.035(3) 0.037(4) S3 0.0653(9) 0.0432(9) 0.0553(8) 0.0052(7) 0.0109(7) 0.0308(7) F1S3 0.078(2) 0.047(2) 0.101(3) -0.0085(19) -0.006(2) 0.0352(18) F2S3 0.101(3) 0.112(4) 0.149(4) 0.028(3) 0.068(3) 0.066(3) F3S3 0.161(4) 0.101(3) 0.090(3) 0.045(3) 0.025(3) 0.096(3) O1S3 0.083(3) 0.108(4) 0.091(3) 0.018(3) 0.044(3) 0.054(3) O2S3 0.108(3) 0.050(3) 0.081(3) 0.027(2) 0.013(3) 0.044(2) O3S3 0.074(3) 0.058(3) 0.073(3) -0.008(2) 0.002(2) 0.028(2) C3S 0.063(4) 0.054(4) 0.060(3) 0.018(3) 0.010(3) 0.036(3) N111 0.130(7) 0.121(6) 0.139(7) 0.075(6) 0.069(6) 0.060(6) C101 0.095(7) 0.121(7) 0.101(7) 0.051(6) 0.042(6) 0.045(6) C102 0.142(10) 0.241(15) 0.134(10) 0.024(9) -0.012(8) 0.101(10) N112 0.184(11) 0.209(13) 0.223(13) 0.043(10) 0.113(10) 0.100(10) C103 0.122(9) 0.146(12) 0.150(10) 0.060(9) 0.088(8) 0.041(8) C104 0.264(17) 0.183(13) 0.49(3) 0.197(17) 0.30(2) 0.162(13) N113 0.171(11) 0.161(11) 0.206(14) 0.024(9) 0.039(10) 0.044(9) C105 0.104(8) 0.127(12) 0.178(14) 0.062(10) 0.060(10) 0.004(8) C106 0.112(7) 0.117(8) 0.180(10) 0.078(8) 0.087(8) 0.073(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 La1 O213 2.409(3) 2_666 ? La1 O201 2.522(3) . ? La1 O222 2.544(3) . ? La1 N5 2.678(4) . ? La1 N3 2.720(4) . ? La1 N6 2.742(4) . ? La1 N4 2.749(4) . ? La1 N2 2.756(3) . ? La1 N1 2.800(3) . ? La1 La3 4.1089(11) . ? La2 O221 2.546(3) 2_666 ? La2 O203 2.549(3) . ? La2 O202 2.571(3) . ? La2 O223 2.608(3) 2_666 ? La2 N34 2.733(4) . ? La2 N36 2.756(3) . ? La2 N33 2.758(4) . ? La2 N35 2.787(3) . ? La2 N32 2.791(3) . ? La2 N31 2.804(4) . ? La2 C201 2.961(5) . ? La2 C203 2.978(4) 2_666 ? La3 O211 2.455(3) . ? La3 O212 2.489(3) . ? La3 O221 2.507(3) . ? La3 O203 2.548(3) . ? La3 O211 2.561(3) 2_666 ? La3 O201 2.561(3) . ? La3 O222 2.601(3) . ? La3 O1 2.617(3) . ? La3 N104 2.748(4) . ? La3 C202 2.904(4) . ? La3 C203 2.928(4) . ? La3 C201 2.932(4) . ? N1 C7 1.487(5) . ? N1 C1 1.488(6) . ? N1 C25 1.487(5) . ? N2 C19 1.487(5) . ? N2 C13 1.489(5) . ? N2 C26 1.495(5) . ? N3 C6 1.332(6) . ? N3 C2 1.343(5) . ? N4 C12 1.337(5) . ? N4 C8 1.344(5) . ? N5 C18 1.338(6) . ? N5 C14 1.339(6) . ? N6 C20 1.342(6) . ? N6 C24 1.355(6) . ? N31 C37 1.481(5) . ? N31 C31 1.482(5) . ? N31 C55 1.489(5) . ? N32 C49 1.471(5) . ? N32 C56 1.482(5) . ? N32 C43 1.486(5) . ? N33 C36 1.340(6) . ? N33 C32 1.342(5) . ? N34 C42 1.338(5) . ? N34 C38 1.340(6) . ? N35 C48 1.340(5) . ? N35 C44 1.345(5) . ? N36 C54 1.340(6) . ? N36 C50 1.349(5) . ? C1 C2 1.500(6) . ? C2 C3 1.375(6) . ? C3 C4 1.384(7) . ? C4 C5 1.369(7) . ? C5 C6 1.362(7) . ? C7 C8 1.499(6) . ? C8 C9 1.386(6) . ? C9 C10 1.367(7) . ? C10 C11 1.360(7) . ? C11 C12 1.369(7) . ? C13 C14 1.498(6) . ? C14 C15 1.393(6) . ? C15 C16 1.366(8) . ? C16 C17 1.402(9) . ? C17 C18 1.380(7) . ? C19 C20 1.503(6) . ? C20 C21 1.378(6) . ? C21 C22 1.397(7) . ? C22 C23 1.370(8) . ? C23 C24 1.358(7) . ? C25 C26 1.512(6) . ? C31 C32 1.504(6) . ? C32 C33 1.400(6) . ? C33 C34 1.376(7) . ? C34 C35 1.382(7) . ? C35 C36 1.375(6) . ? C37 C38 1.515(6) . ? C38 C39 1.376(6) . ? C39 C40 1.375(7) . ? C40 C41 1.369(7) . ? C41 C42 1.379(6) . ? C43 C44 1.507(6) . ? C44 C45 1.388(6) . ? C45 C46 1.379(6) . ? C46 C47 1.373(6) . ? C47 C48 1.380(6) . ? C49 C50 1.495(6) . ? C50 C51 1.374(6) . ? C51 C52 1.367(7) . ? C52 C53 1.386(7) . ? C53 C54 1.374(7) . ? C55 C56 1.512(6) . ? C201 O202 1.251(5) . ? C201 O201 1.300(5) . ? C201 O203 1.313(5) . ? C202 O213 1.265(4) . ? C202 O212 1.278(5) . ? C202 O211 1.304(5) . ? O211 La3 2.561(3) 2_666 ? O213 La1 2.409(3) 2_666 ? C203 O223 1.259(5) . ? C203 O222 1.302(5) . ? C203 O221 1.303(4) . ? C203 La2 2.978(4) 2_666 ? O221 La2 2.546(3) 2_666 ? O223 La2 2.608(3) 2_666 ? N104 C61 1.116(6) . ? C61 C62 1.454(8) . ? S1 O1S1 1.420(4) . ? S1 O3S1 1.430(4) . ? S1 O2S1 1.432(4) . ? S1 C1S 1.787(7) . ? F1S1 C1S 1.344(7) . ? F2S1 C1S 1.309(7) . ? F3S1 C1S 1.316(7) . ? S2 O1S2 1.419(4) . ? S2 O2S2 1.433(4) . ? S2 O3S2 1.440(4) . ? S2 C2S 1.791(7) . ? F1S2 C2S 1.330(7) . ? F2S2 C2S 1.312(7) . ? F3S2 C2S 1.335(7) . ? S3 O2S3 1.425(4) . ? S3 O3S3 1.429(4) . ? S3 O1S3 1.438(5) . ? S3 C3S 1.806(6) . ? F1S3 C3S 1.323(6) . ? F2S3 C3S 1.330(7) . ? F3S3 C3S 1.297(6) . ? N111 C101 1.131(10) . ? C101 C102 1.402(13) . ? N112 C103 1.188(16) . ? C103 C104 1.358(15) . ? N113 C105 1.178(16) . ? C105 C106 1.401(15) . ? 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 O213 La1 O201 77.76(10) 2_666 . ? O213 La1 O222 77.00(9) 2_666 . ? O201 La1 O222 73.85(9) . . ? O213 La1 N5 76.53(11) 2_666 . ? O201 La1 N5 80.34(11) . . ? O222 La1 N5 146.23(10) . . ? O213 La1 N3 70.65(11) 2_666 . ? O201 La1 N3 145.39(10) . . ? O222 La1 N3 111.25(10) . . ? N5 La1 N3 78.90(12) . . ? O213 La1 N6 143.83(10) 2_666 . ? O201 La1 N6 77.86(11) . . ? O222 La1 N6 70.80(10) . . ? N5 La1 N6 124.61(12) . . ? N3 La1 N6 136.71(12) . . ? O213 La1 N4 115.26(12) 2_666 . ? O201 La1 N4 146.22(10) . . ? O222 La1 N4 78.94(10) . . ? N5 La1 N4 131.86(11) . . ? N3 La1 N4 64.16(12) . . ? N6 La1 N4 74.51(12) . . ? O213 La1 N2 131.88(11) 2_666 . ? O201 La1 N2 70.07(9) . . ? O222 La1 N2 124.11(10) . . ? N5 La1 N2 63.76(11) . . ? N3 La1 N2 122.81(10) . . ? N6 La1 N2 61.00(11) . . ? N4 La1 N2 111.36(11) . . ? O213 La1 N1 127.75(10) 2_666 . ? O201 La1 N1 135.12(9) . . ? O222 La1 N1 140.59(10) . . ? N5 La1 N1 73.08(11) . . ? N3 La1 N1 62.54(11) . . ? N6 La1 N1 88.21(11) . . ? N4 La1 N1 63.15(11) . . ? N2 La1 N1 65.90(10) . . ? O213 La1 La3 73.11(7) 2_666 . ? O201 La1 La3 36.38(6) . . ? O222 La1 La3 37.50(6) . . ? N5 La1 La3 113.59(9) . . ? N3 La1 La3 137.31(8) . . ? N6 La1 La3 71.38(9) . . ? N4 La1 La3 114.47(8) . . ? N2 La1 La3 98.16(7) . . ? N1 La1 La3 158.82(7) . . ? O221 La2 O203 76.81(9) 2_666 . ? O221 La2 O202 87.31(9) 2_666 . ? O203 La2 O202 51.10(9) . . ? O221 La2 O223 50.75(9) 2_666 2_666 ? O203 La2 O223 86.73(10) . 2_666 ? O202 La2 O223 128.38(9) . 2_666 ? O221 La2 N34 110.97(9) 2_666 . ? O203 La2 N34 76.27(10) . . ? O202 La2 N34 118.94(10) . . ? O223 La2 N34 65.38(10) 2_666 . ? O221 La2 N36 75.62(9) 2_666 . ? O203 La2 N36 111.04(10) . . ? O202 La2 N36 65.66(10) . . ? O223 La2 N36 118.25(10) 2_666 . ? N34 La2 N36 171.52(11) . . ? O221 La2 N33 74.18(10) 2_666 . ? O203 La2 N33 148.84(10) . . ? O202 La2 N33 137.15(11) . . ? O223 La2 N33 66.12(10) 2_666 . ? N34 La2 N33 103.80(11) . . ? N36 La2 N33 72.35(11) . . ? O221 La2 N35 150.54(10) 2_666 . ? O203 La2 N35 75.99(10) . . ? O202 La2 N35 66.77(10) . . ? O223 La2 N35 137.68(10) 2_666 . ? N34 La2 N35 73.02(10) . . ? N36 La2 N35 104.03(10) . . ? N33 La2 N35 134.51(11) . . ? O221 La2 N32 134.29(9) 2_666 . ? O203 La2 N32 128.43(9) . . ? O202 La2 N32 85.42(10) . . ? O223 La2 N32 144.22(10) 2_666 . ? N34 La2 N32 111.97(10) . . ? N36 La2 N32 60.32(10) . . ? N33 La2 N32 81.12(10) . . ? N35 La2 N32 60.26(10) . . ? O221 La2 N31 128.06(10) 2_666 . ? O203 La2 N31 136.17(10) . . ? O202 La2 N31 143.49(10) . . ? O223 La2 N31 86.64(10) 2_666 . ? N34 La2 N31 61.67(11) . . ? N36 La2 N31 110.20(11) . . ? N33 La2 N31 60.46(11) . . ? N35 La2 N31 80.33(11) . . ? N32 La2 N31 64.00(10) . . ? O221 La2 C201 80.99(10) 2_666 . ? O203 La2 C201 26.24(9) . . ? O202 La2 C201 24.87(9) . . ? O223 La2 C201 108.55(11) 2_666 . ? N34 La2 C201 98.64(11) . . ? N36 La2 C201 87.52(11) . . ? N33 La2 C201 151.12(11) . . ? N35 La2 C201 69.60(11) . . ? N32 La2 C201 107.10(10) . . ? N31 La2 C201 148.21(11) . . ? O221 La2 C203 25.81(10) 2_666 2_666 ? O203 La2 C203 80.96(10) . 2_666 ? O202 La2 C203 108.85(10) . 2_666 ? O223 La2 C203 24.94(10) 2_666 2_666 ? N34 La2 C203 87.73(11) . 2_666 ? N36 La2 C203 97.55(11) . 2_666 ? N33 La2 C203 67.96(11) . 2_666 ? N35 La2 C203 152.80(10) . 2_666 ? N32 La2 C203 146.80(10) . 2_666 ? N31 La2 C203 107.65(11) . 2_666 ? C201 La2 C203 95.33(11) . 2_666 ? O211 La3 O212 52.47(9) . . ? O211 La3 O221 81.66(10) . . ? O212 La3 O221 94.78(10) . . ? O211 La3 O203 81.27(10) . . ? O212 La3 O203 91.96(10) . . ? O221 La3 O203 152.26(9) . . ? O211 La3 O211 62.86(10) . 2_666 ? O212 La3 O211 115.31(9) . 2_666 ? O221 La3 O211 76.29(9) . 2_666 ? O203 La3 O211 76.50(9) . 2_666 ? O211 La3 O201 118.43(9) . . ? O212 La3 O201 142.58(10) . . ? O221 La3 O201 121.19(9) . . ? O203 La3 O201 51.55(9) . . ? O211 La3 O201 68.77(9) 2_666 . ? O211 La3 O222 119.37(9) . . ? O212 La3 O222 145.14(10) . . ? O221 La3 O222 51.46(8) . . ? O203 La3 O222 121.79(9) . . ? O211 La3 O222 69.59(9) 2_666 . ? O201 La3 O222 72.26(8) . . ? O211 La3 O1 125.62(11) . . ? O212 La3 O1 83.61(11) . . ? O221 La3 O1 138.93(10) . . ? O203 La3 O1 68.56(10) . . ? O211 La3 O1 140.88(10) 2_666 . ? O201 La3 O1 75.83(10) . . ? O222 La3 O1 114.97(10) . . ? O211 La3 N104 122.45(11) . . ? O212 La3 N104 78.27(12) . . ? O221 La3 N104 74.06(11) . . ? O203 La3 N104 133.68(11) . . ? O211 La3 N104 148.33(11) 2_666 . ? O201 La3 N104 118.84(11) . . ? O222 La3 N104 83.25(12) . . ? O1 La3 N104 65.41(12) . . ? O211 La3 C202 26.50(10) . . ? O212 La3 C202 25.97(10) . . ? O221 La3 C202 88.00(11) . . ? O203 La3 C202 86.39(11) . . ? O211 La3 C202 89.35(10) 2_666 . ? O201 La3 C202 135.30(10) . . ? O222 La3 C202 137.01(10) . . ? O1 La3 C202 105.07(12) . . ? N104 La3 C202 100.43(13) . . ? O211 La3 C203 97.03(11) . . ? O212 La3 C203 121.03(11) . . ? O221 La3 C203 26.32(9) . . ? O203 La3 C203 137.02(10) . . ? O211 La3 C203 65.15(10) 2_666 . ? O201 La3 C203 95.03(10) . . ? O222 La3 C203 26.40(9) . . ? O1 La3 C203 135.83(12) . . ? N104 La3 C203 83.26(12) . . ? C202 La3 C203 110.87(11) . . ? O211 La3 C201 96.34(11) . . ? O212 La3 C201 118.43(12) . . ? O221 La3 C201 136.44(10) . . ? O203 La3 C201 26.57(10) . . ? O211 La3 C201 64.69(10) 2_666 . ? O201 La3 C201 26.29(10) . . ? O222 La3 C201 95.29(10) . . ? O1 La3 C201 76.21(11) . . ? N104 La3 C201 136.31(12) . . ? C202 La3 C201 109.29(12) . . ? C203 La3 C201 113.47(11) . . ? C7 N1 C1 110.2(4) . . ? C7 N1 C25 108.2(3) . . ? C1 N1 C25 108.0(3) . . ? C7 N1 La1 107.8(2) . . ? C1 N1 La1 111.7(2) . . ? C25 N1 La1 110.9(2) . . ? C19 N2 C13 107.7(3) . . ? C19 N2 C26 107.4(3) . . ? C13 N2 C26 111.0(3) . . ? C19 N2 La1 110.2(2) . . ? C13 N2 La1 110.0(2) . . ? C26 N2 La1 110.5(2) . . ? C6 N3 C2 117.3(4) . . ? C6 N3 La1 120.2(3) . . ? C2 N3 La1 121.7(3) . . ? C12 N4 C8 117.5(4) . . ? C12 N4 La1 122.4(3) . . ? C8 N4 La1 118.7(3) . . ? C18 N5 C14 118.5(4) . . ? C18 N5 La1 120.5(3) . . ? C14 N5 La1 120.9(3) . . ? C20 N6 C24 117.1(4) . . ? C20 N6 La1 120.5(3) . . ? C24 N6 La1 122.4(3) . . ? C37 N31 C31 109.0(3) . . ? C37 N31 C55 108.8(3) . . ? C31 N31 C55 109.1(3) . . ? C37 N31 La2 109.9(2) . . ? C31 N31 La2 106.9(2) . . ? C55 N31 La2 113.0(2) . . ? C49 N32 C56 108.8(3) . . ? C49 N32 C43 108.7(3) . . ? C56 N32 C43 109.6(3) . . ? C49 N32 La2 112.5(2) . . ? C56 N32 La2 112.8(2) . . ? C43 N32 La2 104.4(2) . . ? C36 N33 C32 118.2(4) . . ? C36 N33 La2 122.2(3) . . ? C32 N33 La2 118.2(3) . . ? C42 N34 C38 117.2(4) . . ? C42 N34 La2 120.4(3) . . ? C38 N34 La2 121.2(3) . . ? C48 N35 C44 117.9(4) . . ? C48 N35 La2 124.4(3) . . ? C44 N35 La2 115.8(3) . . ? C54 N36 C50 118.1(4) . . ? C54 N36 La2 120.2(3) . . ? C50 N36 La2 121.7(3) . . ? N1 C1 C2 115.4(3) . . ? N3 C2 C3 122.7(4) . . ? N3 C2 C1 117.3(4) . . ? C3 C2 C1 119.9(4) . . ? C2 C3 C4 118.7(5) . . ? C5 C4 C3 118.7(5) . . ? C6 C5 C4 119.1(5) . . ? N3 C6 C5 123.5(4) . . ? N1 C7 C8 114.5(3) . . ? N4 C8 C9 121.7(4) . . ? N4 C8 C7 116.9(4) . . ? C9 C8 C7 121.3(4) . . ? C10 C9 C8 119.1(4) . . ? C9 C10 C11 119.7(5) . . ? C10 C11 C12 118.4(5) . . ? N4 C12 C11 123.6(5) . . ? N2 C13 C14 116.7(4) . . ? N5 C14 C15 122.2(5) . . ? N5 C14 C13 117.8(4) . . ? C15 C14 C13 119.7(5) . . ? C16 C15 C14 119.1(5) . . ? C15 C16 C17 118.9(5) . . ? C18 C17 C16 118.4(6) . . ? N5 C18 C17 122.7(5) . . ? N2 C19 C20 112.7(4) . . ? N6 C20 C21 123.1(4) . . ? N6 C20 C19 116.6(4) . . ? C21 C20 C19 120.2(4) . . ? C20 C21 C22 118.1(5) . . ? C23 C22 C21 119.1(5) . . ? C24 C23 C22 119.3(5) . . ? C23 C24 N6 123.2(5) . . ? N1 C25 C26 112.2(3) . . ? N2 C26 C25 113.2(3) . . ? N31 C31 C32 112.3(4) . . ? N33 C32 C33 121.5(4) . . ? N33 C32 C31 118.0(4) . . ? C33 C32 C31 120.5(4) . . ? C34 C33 C32 119.1(5) . . ? C33 C34 C35 119.5(5) . . ? C36 C35 C34 118.1(5) . . ? N33 C36 C35 123.6(5) . . ? N31 C37 C38 112.4(4) . . ? N34 C38 C39 122.3(4) . . ? N34 C38 C37 116.1(4) . . ? C39 C38 C37 121.6(4) . . ? C40 C39 C38 120.0(5) . . ? C41 C40 C39 118.2(5) . . ? C40 C41 C42 119.0(5) . . ? N34 C42 C41 123.3(5) . . ? N32 C43 C44 113.0(3) . . ? N35 C44 C45 122.2(4) . . ? N35 C44 C43 117.2(3) . . ? C45 C44 C43 120.6(4) . . ? C46 C45 C44 118.9(4) . . ? C47 C46 C45 119.3(4) . . ? C46 C47 C48 118.7(4) . . ? N35 C48 C47 123.0(4) . . ? N32 C49 C50 113.5(3) . . ? N36 C50 C51 121.8(4) . . ? N36 C50 C49 116.9(4) . . ? C51 C50 C49 121.3(4) . . ? C52 C51 C50 119.6(5) . . ? C51 C52 C53 119.4(5) . . ? C54 C53 C52 118.1(5) . . ? N36 C54 C53 123.1(4) . . ? N31 C55 C56 112.1(3) . . ? N32 C56 C55 111.8(3) . . ? O202 C201 O201 124.7(4) . . ? O202 C201 O203 118.9(4) . . ? O201 C201 O203 116.4(3) . . ? O202 C201 La3 158.9(3) . . ? O201 C201 La3 60.72(19) . . ? O203 C201 La3 60.19(19) . . ? O202 C201 La2 59.8(2) . . ? O201 C201 La2 175.2(3) . . ? O203 C201 La2 59.07(19) . . ? La3 C201 La2 114.45(13) . . ? C201 O201 La1 142.4(3) . . ? C201 O201 La3 93.0(2) . . ? La1 O201 La3 107.86(10) . . ? C201 O202 La2 95.3(2) . . ? C201 O203 La3 93.2(2) . . ? C201 O203 La2 94.7(2) . . ? La3 O203 La2 152.92(12) . . ? O213 C202 O212 122.7(4) . . ? O213 C202 O211 121.6(4) . . ? O212 C202 O211 115.7(3) . . ? O213 C202 La3 178.7(3) . . ? O212 C202 La3 58.5(2) . . ? O211 C202 La3 57.13(18) . . ? C202 O211 La3 96.4(2) . . ? C202 O211 La3 146.5(2) . 2_666 ? La3 O211 La3 117.14(10) . 2_666 ? C202 O212 La3 95.5(2) . . ? C202 O213 La1 135.9(3) . 2_666 ? O223 C203 O222 124.1(4) . . ? O223 C203 O221 119.1(3) . . ? O222 C203 O221 116.8(4) . . ? O223 C203 La3 159.4(3) . . ? O222 C203 La3 62.7(2) . . ? O221 C203 La3 58.5(2) . . ? O223 C203 La2 60.8(2) . 2_666 ? O222 C203 La2 175.1(3) . 2_666 ? O221 C203 La2 58.24(19) . 2_666 ? La3 C203 La2 112.82(13) . 2_666 ? C203 O221 La3 95.2(2) . . ? C203 O221 La2 96.0(2) . 2_666 ? La3 O221 La2 153.63(12) . 2_666 ? C203 O222 La1 143.0(2) . . ? C203 O222 La3 90.9(2) . . ? La1 O222 La3 105.97(10) . . ? C203 O223 La2 94.2(2) . 2_666 ? C61 N104 La3 171.1(5) . . ? N104 C61 C62 179.0(7) . . ? O1S1 S1 O3S1 114.5(3) . . ? O1S1 S1 O2S1 114.8(2) . . ? O3S1 S1 O2S1 114.5(3) . . ? O1S1 S1 C1S 104.6(3) . . ? O3S1 S1 C1S 103.3(3) . . ? O2S1 S1 C1S 103.2(3) . . ? F2S1 C1S F3S1 107.3(6) . . ? F2S1 C1S F1S1 105.9(6) . . ? F3S1 C1S F1S1 106.0(6) . . ? F2S1 C1S S1 112.8(5) . . ? F3S1 C1S S1 113.9(5) . . ? F1S1 C1S S1 110.5(5) . . ? O1S2 S2 O2S2 115.9(3) . . ? O1S2 S2 O3S2 113.2(3) . . ? O2S2 S2 O3S2 115.8(3) . . ? O1S2 S2 C2S 103.2(3) . . ? O2S2 S2 C2S 103.3(3) . . ? O3S2 S2 C2S 103.0(3) . . ? F2S2 C2S F1S2 108.7(6) . . ? F2S2 C2S F3S2 107.2(6) . . ? F1S2 C2S F3S2 105.8(6) . . ? F2S2 C2S S2 111.8(5) . . ? F1S2 C2S S2 112.5(5) . . ? F3S2 C2S S2 110.5(4) . . ? O2S3 S3 O3S3 116.1(3) . . ? O2S3 S3 O1S3 113.3(3) . . ? O3S3 S3 O1S3 115.4(3) . . ? O2S3 S3 C3S 103.9(3) . . ? O3S3 S3 C3S 103.2(3) . . ? O1S3 S3 C3S 102.4(3) . . ? F3S3 C3S F1S3 108.8(5) . . ? F3S3 C3S F2S3 105.1(5) . . ? F1S3 C3S F2S3 105.6(5) . . ? F3S3 C3S S3 113.6(4) . . ? F1S3 C3S S3 112.1(4) . . ? F2S3 C3S S3 111.0(4) . . ? N111 C101 C102 179.6(12) . . ? N112 C103 C104 172.0(18) . . ? N113 C105 C106 174(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1O O3S2 1.21 1.67 2.817(5) 156.9 . O1 H2O O212 0.89 2.65 3.405(4) 142.8 . _diffrn_measured_fraction_theta_max 0.779 _diffrn_reflns_theta_full 28.68 _diffrn_measured_fraction_theta_full 0.779 _refine_diff_density_max 1.177 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.091