# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email dfsun@sdu.edu.cn _publ_contact_author_name 'Daofeng Sun' loop_ _publ_author_name 'Daofeng Sun' 'Di Sun' data_p1 _database_code_depnum_ccdc_archive 'CCDC 832546' #TrackingRef '- p1-3-r2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H95 La2 N2 O17 S6' _chemical_formula_weight 1898.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.036(3) _cell_length_b 34.721(6) _cell_length_c 23.393(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.699(4) _cell_angle_gamma 90.00 _cell_volume 10576(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3691 _cell_measurement_theta_min 4.602 _cell_measurement_theta_max 39.894 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3884 _exptl_absorpt_coefficient_mu 0.969 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9093 _exptl_absorpt_correction_T_max 0.9265 _exptl_absorpt_process_details sadabs _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 'Bruker SMART APEXII' _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 44869 _diffrn_reflns_av_R_equivalents 0.0821 _diffrn_reflns_av_sigmaI/netI 0.1053 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 23.33 _reflns_number_total 15049 _reflns_number_gt 8223 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+ (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2001)' _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. During the refinement, the command 'isor' was used to restrain the non-H atoms (C52)with ADP problems. Furthermore, the command 'dfix' was used for C01 C02 to restrain its bond distance in the rational range. The voids in the framework are filled with many disordered solvent molecules, which can not be located. Hence reflect on a high R(int) value. In the refinement we used SQEEZE procedure (Spek, A.L. (2008) Utrecht University, Utrecht, The Netherlands) to remove solvent electron density from voids which give a smaller final R(int) and R-value compared with the original R(int) and R-value. ; _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^)+(0.0772P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15049 _refine_ls_number_parameters 1030 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1127 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1567 _refine_ls_wR_factor_gt 0.1380 _refine_ls_goodness_of_fit_ref 0.918 _refine_ls_restrained_S_all 0.920 _refine_ls_shift/su_max 0.004 _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 O1 O 0.2007(4) 0.20791(13) 0.2073(2) 0.0579(14) Uani 1 1 d . . . O2 O 0.3422(5) 0.23920(15) 0.2298(3) 0.083(2) Uani 1 1 d . . . O3 O 0.9144(6) 0.25053(15) 0.3314(3) 0.096(2) Uani 1 1 d . . . O4 O 1.0603(5) 0.22624(15) 0.3057(3) 0.086(2) Uani 1 1 d . . . O5 O 0.2318(4) 0.12460(14) 0.2223(2) 0.0599(14) Uani 1 1 d . . . O6 O 0.3853(4) 0.09897(14) 0.2187(3) 0.0678(16) Uani 1 1 d . . . O7 O 1.0060(6) 0.09124(19) 0.2736(4) 0.134(3) Uani 1 1 d . . . O8 O 1.1106(5) 0.11322(16) 0.3353(3) 0.091(2) Uani 1 1 d . . . O9 O 0.2507(4) 0.17807(13) 0.3203(2) 0.0516(13) Uani 1 1 d . . . O10 O 0.3706(4) 0.13564(14) 0.3449(2) 0.0611(15) Uani 1 1 d . . . O11 O -0.0491(5) 0.19627(18) 0.1848(3) 0.096(2) Uani 1 1 d . . . O12 O 0.0254(5) 0.14423(15) 0.1581(2) 0.0792(19) Uani 1 1 d . . . O13 O 0.5518(7) 0.2094(3) 0.2024(4) 0.165(4) Uani 1 1 d . . . O14 O 0.4829(6) 0.2087(2) 0.3287(3) 0.107(2) Uani 1 1 d . . . O15 O 0.5642(6) 0.1368(2) 0.2688(4) 0.132(3) Uani 1 1 d . . . O16 O -0.0876(7) 0.1677(3) 0.3124(5) 0.202(5) Uani 1 1 d . . . O22 O 0.3733(6) 0.1701(2) 0.1403(3) 0.106(3) Uani 1 1 d . . . La1 La 0.39594(4) 0.170029(12) 0.24692(2) 0.05122(16) Uani 1 1 d . . . La2 La 0.08232(4) 0.164557(12) 0.26036(2) 0.05013(16) Uani 1 1 d . . . S1 S 0.38170(18) 0.31407(6) 0.23152(10) 0.0667(7) Uani 1 1 d . . . S2 S 0.87353(17) 0.32699(5) 0.31422(11) 0.0694(7) Uani 1 1 d . . . S3 S 0.43198(16) 0.02350(5) 0.21412(9) 0.0544(6) Uani 1 1 d . . . S4 S 0.9371(2) 0.01180(6) 0.28312(14) 0.0962(10) Uani 1 1 d . . . S5 S 0.4004(2) 0.10116(6) 0.44856(9) 0.0764(7) Uani 1 1 d . . . S6 S -0.0238(2) 0.10625(6) 0.05730(10) 0.0880(9) Uani 1 1 d . . . C1 C 0.2507(7) 0.2393(2) 0.2134(3) 0.056(2) Uani 1 1 d . . . C01 C 0.5524(17) 0.2394(5) 0.3626(13) 0.223(13) Uani 1 1 d D . . C2 C 0.2006(7) 0.2775(2) 0.1991(3) 0.050(2) Uani 1 1 d . . . C02 C 0.6254(19) 0.2696(8) 0.3801(11) 0.324(16) Uani 1 1 d D . . C3 C 0.0980(7) 0.2768(2) 0.1791(3) 0.060(2) Uani 1 1 d . . . H3 H 0.0652 0.2532 0.1744 0.072 Uiso 1 1 calc R . . C03 C 0.5867(14) 0.1098(6) 0.3105(9) 0.204(8) Uani 1 1 d . . . C4 C 0.0439(7) 0.3099(2) 0.1662(4) 0.068(2) Uani 1 1 d . . . H4 H -0.0239 0.3088 0.1519 0.082 Uiso 1 1 calc R . . C04 C 0.715(2) 0.0754(13) 0.264(2) 0.56(4) Uani 1 1 d . . . C5 C 0.0927(7) 0.3445(2) 0.1748(4) 0.071(3) Uani 1 1 d . . . H5 H 0.0575 0.3673 0.1666 0.085 Uiso 1 1 calc R . . C05 C 0.668(3) 0.0586(6) 0.3599(8) 0.341(19) Uani 1 1 d . . . C6 C 0.1952(7) 0.3459(2) 0.1957(4) 0.068(3) Uani 1 1 d . . . H6 H 0.2263 0.3697 0.2023 0.082 Uiso 1 1 calc R . . C06 C 0.2974(13) 0.1686(4) 0.1070(6) 0.135(5) Uani 1 1 d . . . C7 C 0.2515(6) 0.3122(2) 0.2069(3) 0.053(2) Uani 1 1 d . . . C07 C 0.1953(15) 0.1843(7) 0.0197(8) 0.256(11) Uani 1 1 d . . . C8 C 0.4112(7) 0.3657(2) 0.2295(4) 0.073(3) Uani 1 1 d . . . H8A H 0.3994 0.3757 0.1911 0.087 Uiso 1 1 calc R . . H8B H 0.3683 0.3797 0.2550 0.087 Uiso 1 1 calc R . . C08 C 0.351(2) 0.2173(8) 0.0448(13) 0.333(16) Uani 1 1 d . . . C9 C 0.5242(7) 0.3697(2) 0.2487(4) 0.057(2) Uani 1 1 d . . . C10 C 0.5527(7) 0.3759(2) 0.3048(4) 0.058(2) Uani 1 1 d . . . C11 C 0.4729(7) 0.3769(2) 0.3492(4) 0.082(3) Uani 1 1 d . . . H11A H 0.4936 0.3949 0.3787 0.123 Uiso 1 1 calc R . . H11B H 0.4661 0.3517 0.3655 0.123 Uiso 1 1 calc R . . H11C H 0.4083 0.3848 0.3316 0.123 Uiso 1 1 calc R . . C12 C 0.6562(7) 0.3793(2) 0.3214(4) 0.059(2) Uani 1 1 d . . . C13 C 0.6880(7) 0.3856(3) 0.3839(4) 0.084(3) Uani 1 1 d . . . H13A H 0.7612 0.3885 0.3878 0.126 Uiso 1 1 calc R . . H13B H 0.6675 0.3638 0.4059 0.126 Uiso 1 1 calc R . . H13C H 0.6555 0.4084 0.3975 0.126 Uiso 1 1 calc R . . C14 C 0.7309(7) 0.3767(2) 0.2802(5) 0.064(2) Uani 1 1 d . . . C15 C 0.8446(6) 0.3773(2) 0.2990(4) 0.073(3) Uani 1 1 d . . . H15A H 0.8566 0.3931 0.3329 0.088 Uiso 1 1 calc R . . H15B H 0.8859 0.3870 0.2687 0.088 Uiso 1 1 calc R . . C16 C 0.7033(7) 0.3696(2) 0.2235(4) 0.068(3) Uani 1 1 d . . . C17 C 0.7858(8) 0.3651(3) 0.1772(5) 0.104(4) Uani 1 1 d . . . H17A H 0.7756 0.3411 0.1575 0.156 Uiso 1 1 calc R . . H17B H 0.8533 0.3656 0.1955 0.156 Uiso 1 1 calc R . . H17C H 0.7790 0.3860 0.1503 0.156 Uiso 1 1 calc R . . C18 C 0.5981(8) 0.3660(2) 0.2068(4) 0.070(3) Uani 1 1 d . . . C19 C 0.5660(8) 0.3570(3) 0.1441(4) 0.095(3) Uani 1 1 d . . . H19A H 0.4942 0.3624 0.1375 0.142 Uiso 1 1 calc R . . H19B H 0.5786 0.3303 0.1365 0.142 Uiso 1 1 calc R . . H19C H 0.6052 0.3726 0.1192 0.142 Uiso 1 1 calc R . . C20 C 1.0066(6) 0.3260(2) 0.3319(3) 0.054(2) Uani 1 1 d . . . C21 C 1.0627(7) 0.3595(2) 0.3433(4) 0.073(3) Uani 1 1 d . . . H21 H 1.0289 0.3831 0.3417 0.087 Uiso 1 1 calc R . . C22 C 1.1672(7) 0.3588(3) 0.3568(4) 0.084(3) Uani 1 1 d . . . H22 H 1.2031 0.3816 0.3636 0.101 Uiso 1 1 calc R . . C23 C 1.2177(8) 0.3237(3) 0.3603(4) 0.087(3) Uani 1 1 d . . . H23 H 1.2871 0.3224 0.3714 0.104 Uiso 1 1 calc R . . C24 C 1.1624(7) 0.2905(3) 0.3467(4) 0.068(2) Uani 1 1 d . . . H24 H 1.1968 0.2670 0.3461 0.082 Uiso 1 1 calc R . . C25 C 1.0584(6) 0.2911(2) 0.3341(3) 0.049(2) Uani 1 1 d . . . C26 C 1.0062(9) 0.2531(2) 0.3234(4) 0.067(3) Uani 1 1 d . . . C27 C 0.2908(7) 0.0960(2) 0.2113(3) 0.049(2) Uani 1 1 d . . . C28 C 0.2440(6) 0.05918(19) 0.1907(3) 0.0410(18) Uani 1 1 d . . . C29 C 0.1426(6) 0.0589(2) 0.1691(3) 0.048(2) Uani 1 1 d . . . H29 H 0.1061 0.0819 0.1678 0.057 Uiso 1 1 calc R . . C30 C 0.0952(6) 0.0264(2) 0.1499(3) 0.055(2) Uani 1 1 d . . . H30 H 0.0277 0.0274 0.1352 0.066 Uiso 1 1 calc R . . C31 C 0.1465(6) -0.0077(2) 0.1522(3) 0.059(2) Uani 1 1 d . . . H31 H 0.1134 -0.0302 0.1401 0.070 Uiso 1 1 calc R . . C32 C 0.2485(7) -0.0090(2) 0.1727(3) 0.058(2) Uani 1 1 d . . . H32 H 0.2829 -0.0325 0.1745 0.069 Uiso 1 1 calc R . . C33 C 0.2995(6) 0.02461(19) 0.1908(3) 0.0448(19) Uani 1 1 d . . . C34 C 0.4643(6) -0.02755(18) 0.2102(3) 0.053(2) Uani 1 1 d . . . H34A H 0.4258 -0.0422 0.2373 0.064 Uiso 1 1 calc R . . H34B H 0.4484 -0.0374 0.1721 0.064 Uiso 1 1 calc R . . C35 C 0.5781(6) -0.03061(19) 0.2248(4) 0.049(2) Uani 1 1 d . . . C36 C 0.6099(6) -0.03706(19) 0.2819(4) 0.051(2) Uani 1 1 d . . . C37 C 0.5336(7) -0.0394(2) 0.3291(4) 0.076(3) Uani 1 1 d . . . H37A H 0.4840 -0.0592 0.3200 0.114 Uiso 1 1 calc R . . H37B H 0.4990 -0.0151 0.3322 0.114 Uiso 1 1 calc R . . H37C H 0.5695 -0.0453 0.3648 0.114 Uiso 1 1 calc R . . C38 C 0.7150(7) -0.0411(2) 0.2970(4) 0.058(2) Uani 1 1 d . . . C39 C 0.7530(7) -0.0466(3) 0.3602(3) 0.080(3) Uani 1 1 d . . . H39A H 0.8244 -0.0399 0.3644 0.120 Uiso 1 1 calc R . . H39B H 0.7441 -0.0730 0.3711 0.120 Uiso 1 1 calc R . . H39C H 0.7141 -0.0303 0.3843 0.120 Uiso 1 1 calc R . . C40 C 0.7870(6) -0.0375(2) 0.2542(4) 0.048(2) Uani 1 1 d . . . C41 C 0.9019(6) -0.0384(2) 0.2712(4) 0.063(2) Uani 1 1 d . . . H41A H 0.9407 -0.0494 0.2408 0.076 Uiso 1 1 calc R . . H41B H 0.9148 -0.0534 0.3057 0.076 Uiso 1 1 calc R . . C42 C 0.7560(7) -0.0304(2) 0.1978(4) 0.055(2) Uani 1 1 d . . . C43 C 0.8345(7) -0.0246(2) 0.1510(4) 0.078(3) Uani 1 1 d . . . H43A H 0.8053 -0.0081 0.1215 0.118 Uiso 1 1 calc R . . H43B H 0.8513 -0.0491 0.1348 0.118 Uiso 1 1 calc R . . H43C H 0.8957 -0.0129 0.1676 0.118 Uiso 1 1 calc R . . C44 C 0.6506(7) -0.0263(2) 0.1836(3) 0.053(2) Uani 1 1 d . . . C45 C 0.6155(7) -0.0180(2) 0.1222(3) 0.076(3) Uani 1 1 d . . . H45A H 0.5433 -0.0125 0.1203 0.114 Uiso 1 1 calc R . . H45B H 0.6286 -0.0401 0.0989 0.114 Uiso 1 1 calc R . . H45C H 0.6524 0.0037 0.1085 0.114 Uiso 1 1 calc R . . C46 C 1.0674(6) 0.0107(2) 0.3071(4) 0.058(2) Uani 1 1 d . . . C47 C 1.1253(7) -0.0233(2) 0.3112(4) 0.065(2) Uani 1 1 d . . . H47 H 1.0940 -0.0466 0.3017 0.078 Uiso 1 1 calc R . . C48 C 1.2268(7) -0.0230(2) 0.3291(3) 0.062(2) Uani 1 1 d . . . H48 H 1.2635 -0.0459 0.3310 0.074 Uiso 1 1 calc R . . C49 C 1.2749(7) 0.0110(3) 0.3443(3) 0.067(2) Uani 1 1 d . . . H49 H 1.3437 0.0112 0.3567 0.080 Uiso 1 1 calc R . . C50 C 1.2201(7) 0.0448(2) 0.3408(3) 0.056(2) Uani 1 1 d . . . H50 H 1.2523 0.0677 0.3520 0.067 Uiso 1 1 calc R . . C51 C 1.1186(7) 0.0458(2) 0.3211(3) 0.055(2) Uani 1 1 d . . . C52 C 1.0716(8) 0.0847(3) 0.3152(4) 0.076(3) Uani 1 1 d U . . C53 C 0.2973(7) 0.1572(2) 0.3586(3) 0.050(2) Uani 1 1 d . . . C54 C 0.2703(7) 0.1620(2) 0.4192(3) 0.056(2) Uani 1 1 d . . . C55 C 0.1983(8) 0.1895(2) 0.4315(4) 0.080(3) Uani 1 1 d . . . H55 H 0.1671 0.2034 0.4014 0.096 Uiso 1 1 calc R . . C56 C 0.1705(10) 0.1974(3) 0.4870(5) 0.116(4) Uani 1 1 d . . . H56 H 0.1216 0.2160 0.4944 0.139 Uiso 1 1 calc R . . C57 C 0.2183(11) 0.1764(3) 0.5308(5) 0.122(5) Uani 1 1 d . . . H57 H 0.2017 0.1812 0.5683 0.147 Uiso 1 1 calc R . . C58 C 0.2918(9) 0.1479(3) 0.5197(4) 0.097(4) Uani 1 1 d . . . H58 H 0.3244 0.1346 0.5499 0.117 Uiso 1 1 calc R . . C59 C 0.3157(7) 0.1395(2) 0.4638(3) 0.066(2) Uani 1 1 d . . . C60 C 0.4096(9) 0.0756(2) 0.5169(4) 0.097(4) Uani 1 1 d . . . H60A H 0.4521 0.0900 0.5445 0.116 Uiso 1 1 calc R . . H60B H 0.3419 0.0726 0.5319 0.116 Uiso 1 1 calc R . . C61 C 0.4561(11) 0.0369(3) 0.5068(4) 0.085(3) Uani 1 1 d . . . C62 C 0.3932(11) 0.0050(4) 0.4968(4) 0.091(3) Uani 1 1 d . . . C63 C 0.2783(10) 0.0103(3) 0.4911(4) 0.111(4) Uani 1 1 d . . . H63A H 0.2509 -0.0049 0.4597 0.166 Uiso 1 1 calc R . . H63B H 0.2627 0.0369 0.4842 0.166 Uiso 1 1 calc R . . H63C H 0.2483 0.0022 0.5258 0.166 Uiso 1 1 calc R . . C64 C 0.5633(12) 0.0319(3) 0.5105(4) 0.092(3) Uani 1 1 d . . . C65 C 0.6353(9) 0.0663(3) 0.5205(4) 0.116(4) Uani 1 1 d . . . H65A H 0.6940 0.0635 0.4976 0.175 Uiso 1 1 calc R . . H65B H 0.6575 0.0675 0.5602 0.175 Uiso 1 1 calc R . . H65C H 0.5996 0.0897 0.5100 0.175 Uiso 1 1 calc R . . C66 C -0.0247(7) 0.1736(2) 0.1464(4) 0.066(2) Uani 1 1 d . . . C67 C -0.0551(7) 0.1821(2) 0.0853(4) 0.073(3) Uani 1 1 d . . . C68 C -0.0827(8) 0.2202(3) 0.0714(5) 0.100(4) Uani 1 1 d . . . H68 H -0.0889 0.2381 0.1006 0.120 Uiso 1 1 calc R . . C69 C -0.1010(10) 0.2317(3) 0.0144(5) 0.123(5) Uani 1 1 d . . . H69 H -0.1175 0.2572 0.0059 0.148 Uiso 1 1 calc R . . C70 C -0.0945(9) 0.2055(3) -0.0285(5) 0.104(4) Uani 1 1 d . . . H70 H -0.1042 0.2130 -0.0665 0.125 Uiso 1 1 calc R . . C71 C -0.0737(8) 0.1678(2) -0.0151(4) 0.095(3) Uani 1 1 d . . . H71 H -0.0722 0.1499 -0.0446 0.113 Uiso 1 1 calc R . . C72 C -0.0543(7) 0.1552(2) 0.0419(4) 0.073(3) Uani 1 1 d . . . C73 C -0.0329(9) 0.0824(2) -0.0131(4) 0.095(3) Uani 1 1 d . . . H73A H -0.1005 0.0865 -0.0311 0.114 Uiso 1 1 calc R . . H73B H 0.0178 0.0931 -0.0377 0.114 Uiso 1 1 calc R . . C74 C -0.0137(10) 0.0397(2) -0.0042(3) 0.070(3) Uani 1 1 d . . . C75 C -0.1001(9) 0.0152(3) -0.0031(3) 0.071(3) Uani 1 1 d . . . C76 C -0.0852(10) -0.0251(3) -0.0003(3) 0.077(3) Uani 1 1 d . . . C77 C -0.1773(8) -0.0523(3) -0.0052(4) 0.098(3) Uani 1 1 d . . . H77A H -0.2370 -0.0395 0.0080 0.147 Uiso 1 1 calc R . . H77B H -0.1633 -0.0748 0.0177 0.147 Uiso 1 1 calc R . . H77C H -0.1895 -0.0598 -0.0445 0.147 Uiso 1 1 calc R . . C78 C -0.2097(9) 0.0315(3) -0.0052(4) 0.102(4) Uani 1 1 d . . . H78A H -0.2509 0.0169 0.0201 0.153 Uiso 1 1 calc R . . H78B H -0.2388 0.0298 -0.0435 0.153 Uiso 1 1 calc R . . H78C H -0.2079 0.0580 0.0067 0.153 Uiso 1 1 calc R . . N01 N 0.6582(11) 0.0876(4) 0.3169(10) 0.232(9) Uani 1 1 d . . . N02 N 0.2844(10) 0.1856(5) 0.0594(6) 0.174(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.076(4) 0.043(3) 0.054(4) 0.001(3) -0.003(3) 0.001(3) O2 0.074(5) 0.045(3) 0.125(6) 0.006(3) -0.038(4) 0.005(3) O3 0.088(5) 0.043(3) 0.156(7) -0.026(4) 0.003(5) -0.002(4) O4 0.116(6) 0.054(3) 0.085(5) -0.028(3) -0.017(4) 0.040(4) O5 0.059(4) 0.050(3) 0.070(4) -0.017(3) -0.010(3) 0.013(3) O6 0.049(4) 0.050(3) 0.103(5) -0.026(3) -0.006(3) 0.001(3) O7 0.121(7) 0.087(5) 0.189(9) -0.036(6) -0.033(6) 0.018(5) O8 0.087(5) 0.047(3) 0.138(6) 0.002(4) 0.013(4) -0.011(3) O9 0.059(4) 0.045(3) 0.051(3) 0.001(3) -0.005(3) 0.002(3) O10 0.071(4) 0.054(3) 0.059(4) 0.006(3) -0.002(3) 0.021(3) O11 0.105(6) 0.092(5) 0.088(5) -0.031(4) -0.036(4) 0.043(4) O12 0.115(5) 0.059(4) 0.060(4) -0.010(3) -0.027(4) 0.027(4) O13 0.124(8) 0.225(10) 0.149(8) 0.022(7) 0.020(6) 0.009(7) O14 0.132(7) 0.087(5) 0.101(6) -0.006(4) -0.019(5) -0.016(5) O15 0.068(5) 0.104(6) 0.219(10) -0.021(6) -0.044(6) 0.026(5) O16 0.102(7) 0.215(10) 0.293(13) 0.125(9) 0.060(8) 0.026(7) O22 0.115(7) 0.135(6) 0.067(5) 0.012(5) -0.005(4) 0.030(5) La1 0.0546(3) 0.0416(3) 0.0567(3) 0.0000(2) -0.0050(2) 0.0049(2) La2 0.0507(3) 0.0400(3) 0.0588(3) -0.0111(2) -0.0067(2) 0.0077(2) S1 0.0659(16) 0.0424(11) 0.0898(18) 0.0069(11) -0.0161(13) 0.0089(11) S2 0.0587(15) 0.0403(11) 0.1076(19) -0.0021(12) -0.0122(13) 0.0058(10) S3 0.0525(14) 0.0367(10) 0.0728(15) -0.0058(10) -0.0102(11) 0.0044(10) S4 0.0640(17) 0.0591(14) 0.161(3) -0.0378(16) -0.0387(17) 0.0136(13) S5 0.113(2) 0.0647(14) 0.0500(15) 0.0064(12) -0.0124(13) 0.0255(14) S6 0.159(3) 0.0544(13) 0.0482(15) -0.0063(11) -0.0194(15) 0.0270(15) C1 0.072(7) 0.046(5) 0.049(6) -0.003(4) -0.006(5) -0.006(5) C01 0.17(2) 0.130(14) 0.38(4) 0.056(18) 0.13(2) -0.003(12) C2 0.070(6) 0.042(5) 0.040(5) -0.003(4) 0.005(4) 0.002(4) C02 0.34(4) 0.44(4) 0.19(2) -0.06(3) 0.00(2) 0.18(3) C3 0.069(7) 0.051(5) 0.059(6) -0.004(4) -0.005(5) -0.012(5) C03 0.146(17) 0.206(19) 0.26(2) 0.033(17) 0.004(15) 0.069(15) C4 0.060(6) 0.065(6) 0.078(7) 0.002(5) -0.014(5) 0.006(5) C04 0.24(3) 0.64(7) 0.80(9) -0.46(7) -0.10(4) 0.21(4) C5 0.057(6) 0.061(6) 0.095(7) 0.013(5) -0.011(5) 0.017(5) C05 0.74(6) 0.135(14) 0.147(16) 0.035(13) 0.00(2) 0.13(2) C6 0.063(6) 0.052(5) 0.090(7) 0.003(5) 0.007(5) 0.003(5) C06 0.170(16) 0.170(13) 0.068(9) 0.013(10) 0.026(9) 0.066(12) C7 0.060(6) 0.048(5) 0.050(5) -0.002(4) 0.000(4) 0.016(4) C07 0.148(16) 0.46(3) 0.155(16) 0.063(19) -0.064(13) -0.049(19) C8 0.074(7) 0.038(4) 0.103(8) 0.005(5) -0.022(6) 0.005(4) C08 0.24(3) 0.38(3) 0.38(4) 0.16(3) 0.04(3) -0.03(2) C9 0.063(6) 0.044(5) 0.064(7) 0.011(4) -0.003(5) 0.003(4) C10 0.062(6) 0.042(5) 0.070(7) 0.008(4) 0.001(5) 0.009(4) C11 0.081(7) 0.068(6) 0.098(8) 0.007(5) 0.010(6) 0.006(5) C12 0.067(7) 0.039(4) 0.070(7) 0.008(4) -0.012(6) 0.012(4) C13 0.063(7) 0.084(6) 0.105(9) 0.012(6) -0.012(6) 0.009(5) C14 0.064(7) 0.034(4) 0.094(8) 0.009(5) -0.008(6) 0.006(4) C15 0.052(6) 0.046(5) 0.120(8) 0.011(5) -0.010(5) 0.003(4) C16 0.056(6) 0.058(5) 0.090(8) 0.007(5) -0.005(6) 0.004(5) C17 0.085(8) 0.095(7) 0.134(10) 0.016(7) 0.025(7) 0.018(6) C18 0.089(8) 0.045(5) 0.072(7) 0.008(5) -0.020(6) 0.006(5) C19 0.104(9) 0.101(7) 0.079(8) 0.014(6) 0.005(6) 0.012(7) C20 0.056(5) 0.037(4) 0.069(6) -0.007(4) -0.002(4) -0.002(4) C21 0.067(7) 0.063(6) 0.089(7) -0.010(5) 0.000(5) 0.009(5) C22 0.052(7) 0.088(7) 0.111(9) -0.004(6) -0.014(6) -0.007(6) C23 0.055(6) 0.121(9) 0.083(8) 0.017(7) -0.003(5) -0.003(7) C24 0.061(7) 0.073(6) 0.070(7) 0.000(5) 0.004(5) 0.014(5) C25 0.055(6) 0.049(5) 0.041(5) -0.004(4) -0.006(4) 0.011(4) C26 0.094(8) 0.054(6) 0.052(6) -0.002(4) -0.016(6) 0.018(6) C27 0.056(6) 0.041(5) 0.049(5) -0.007(4) -0.012(4) 0.009(4) C28 0.043(5) 0.050(4) 0.030(4) -0.001(4) 0.001(4) 0.008(4) C29 0.053(5) 0.049(5) 0.041(5) -0.006(4) -0.005(4) 0.011(4) C30 0.038(5) 0.059(5) 0.066(6) 0.005(4) -0.009(4) 0.002(4) C31 0.058(6) 0.052(5) 0.065(6) -0.003(4) -0.010(5) -0.007(5) C32 0.068(6) 0.042(5) 0.062(6) -0.003(4) -0.002(5) 0.006(4) C33 0.045(5) 0.042(4) 0.046(5) -0.006(4) -0.003(4) 0.004(4) C34 0.054(6) 0.040(4) 0.066(6) 0.001(4) 0.000(4) 0.010(4) C35 0.055(6) 0.041(4) 0.050(6) -0.001(4) -0.010(5) 0.008(4) C36 0.052(6) 0.035(4) 0.066(6) -0.004(4) 0.009(5) 0.001(4) C37 0.072(7) 0.081(6) 0.076(7) 0.016(5) 0.014(5) 0.003(5) C38 0.070(7) 0.047(5) 0.058(6) -0.001(4) 0.001(5) 0.007(4) C39 0.071(7) 0.111(7) 0.057(6) -0.005(5) -0.006(5) 0.004(6) C40 0.038(5) 0.044(4) 0.060(6) -0.012(4) -0.007(5) -0.003(4) C41 0.068(6) 0.050(5) 0.070(6) -0.013(4) -0.012(5) -0.004(4) C42 0.057(6) 0.050(5) 0.056(6) 0.000(4) -0.001(5) 0.001(4) C43 0.070(7) 0.092(6) 0.074(7) 0.000(5) 0.017(5) -0.014(5) C44 0.069(6) 0.047(5) 0.042(5) 0.002(4) 0.000(5) 0.012(4) C45 0.066(6) 0.097(7) 0.064(6) 0.009(5) 0.000(5) -0.005(5) C46 0.051(5) 0.043(5) 0.080(6) -0.006(4) -0.015(4) 0.012(4) C47 0.059(6) 0.055(5) 0.080(7) -0.015(5) -0.013(5) -0.001(5) C48 0.055(6) 0.066(6) 0.063(6) -0.004(5) -0.007(5) 0.014(5) C49 0.057(6) 0.084(7) 0.060(6) -0.018(5) 0.000(5) -0.005(5) C50 0.066(6) 0.057(5) 0.044(5) -0.003(4) -0.007(4) -0.008(5) C51 0.065(6) 0.049(5) 0.049(5) -0.001(4) -0.007(4) -0.002(4) C52 0.074(5) 0.074(4) 0.076(4) -0.006(4) -0.027(4) 0.008(4) C53 0.070(6) 0.031(4) 0.048(5) -0.004(4) -0.021(4) -0.006(4) C54 0.081(6) 0.049(5) 0.039(5) 0.000(4) -0.007(4) 0.002(5) C55 0.120(9) 0.058(5) 0.063(7) -0.001(5) 0.004(6) 0.031(6) C56 0.167(13) 0.094(8) 0.090(9) -0.005(7) 0.031(9) 0.043(8) C57 0.203(15) 0.107(9) 0.058(8) 0.002(7) 0.025(8) 0.038(9) C58 0.154(11) 0.073(6) 0.065(7) 0.009(6) 0.002(7) 0.046(7) C59 0.100(7) 0.059(5) 0.035(5) -0.013(4) -0.019(5) 0.007(5) C60 0.156(11) 0.072(6) 0.061(7) 0.002(5) -0.010(6) 0.039(7) C61 0.131(11) 0.073(8) 0.048(6) 0.014(5) -0.024(6) 0.022(8) C62 0.134(11) 0.092(8) 0.044(6) 0.014(6) -0.011(6) 0.029(9) C63 0.161(13) 0.113(9) 0.057(7) 0.018(6) -0.007(7) 0.013(9) C64 0.148(12) 0.073(8) 0.055(7) 0.005(5) -0.009(7) 0.009(8) C65 0.166(12) 0.086(8) 0.093(9) 0.003(6) -0.042(8) 0.024(8) C66 0.073(6) 0.052(5) 0.071(7) -0.021(5) -0.011(5) 0.018(5) C67 0.093(7) 0.048(5) 0.075(7) -0.008(5) -0.039(5) 0.018(5) C68 0.126(10) 0.069(7) 0.100(9) -0.028(6) -0.054(7) 0.023(6) C69 0.191(13) 0.066(7) 0.104(10) 0.003(7) -0.080(9) 0.012(7) C70 0.158(11) 0.066(7) 0.084(8) 0.002(6) -0.043(7) 0.000(7) C71 0.141(10) 0.050(6) 0.088(8) -0.014(6) -0.042(7) 0.016(6) C72 0.086(7) 0.051(5) 0.079(7) 0.003(5) -0.024(5) 0.016(5) C73 0.150(10) 0.076(6) 0.059(6) -0.023(5) 0.001(6) 0.015(6) C74 0.117(9) 0.060(6) 0.032(5) -0.009(4) -0.003(5) 0.012(7) C75 0.115(9) 0.070(6) 0.027(5) -0.012(4) -0.003(5) 0.012(7) C76 0.132(10) 0.065(7) 0.035(5) -0.005(5) 0.005(6) 0.017(7) C77 0.126(10) 0.085(7) 0.084(8) -0.013(6) 0.008(7) 0.004(7) C78 0.142(11) 0.085(7) 0.080(8) -0.007(6) 0.011(7) 0.020(7) N01 0.119(12) 0.106(9) 0.47(3) -0.004(13) -0.045(15) 0.063(8) N02 0.128(11) 0.281(17) 0.115(10) 0.080(11) 0.008(9) -0.014(11) _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 O1 C1 1.273(8) . ? O1 La2 2.524(5) . ? O1 La1 2.974(5) . ? O2 C1 1.236(9) . ? O2 La1 2.528(5) . ? O3 C26 1.224(10) . ? O4 C26 1.252(9) . ? O4 La2 2.413(5) 1_655 ? O5 C27 1.288(8) . ? O5 La2 2.584(5) . ? O5 La1 2.698(5) . ? O6 C27 1.240(8) . ? O6 La1 2.556(5) . ? O7 C52 1.286(11) . ? O7 La2 2.756(7) 1_655 ? O8 C52 1.199(10) . ? O8 La2 2.515(6) 1_655 ? O9 C53 1.284(8) . ? O9 La2 2.591(5) . ? O9 La1 2.630(5) . ? O10 C53 1.266(8) . ? O10 La1 2.620(5) . ? O11 C66 1.247(9) . ? O11 La2 2.643(6) . ? O12 C66 1.236(9) . ? O12 La2 2.570(5) . ? O13 La1 2.698(9) . ? O14 C01 1.59(3) . ? O14 La1 2.557(7) . ? O15 C03 1.38(2) . ? O15 La1 2.509(7) . ? O16 La2 2.580(9) . ? O22 C06 1.232(16) . ? O22 La1 2.497(8) . ? La1 C53 3.000(8) . ? La1 C27 3.011(8) . ? La2 O4 2.413(5) 1_455 ? La2 O8 2.515(6) 1_455 ? La2 O7 2.756(7) 1_455 ? La2 C66 2.968(9) . ? La2 C52 3.062(10) 1_455 ? S1 C7 1.768(8) . ? S1 C8 1.833(7) . ? S2 C20 1.765(8) . ? S2 C15 1.818(7) . ? S3 C33 1.787(8) . ? S3 C34 1.825(6) . ? S4 C46 1.765(8) . ? S4 C41 1.819(7) . ? S5 C59 1.776(8) . ? S5 C60 1.828(9) . ? S6 C72 1.779(8) . ? S6 C73 1.840(8) . ? C1 C2 1.509(10) . ? C01 C02 1.461(10) . ? C2 C7 1.385(10) . ? C2 C3 1.395(11) . ? C3 C4 1.374(10) . ? C03 N01 1.214(18) . ? C4 C5 1.369(11) . ? C04 N01 1.53(4) . ? C5 C6 1.402(11) . ? C05 N01 1.42(2) . ? C6 C7 1.398(10) . ? C06 N02 1.266(15) . ? C07 N02 1.452(19) . ? C8 C9 1.526(11) . ? C08 N02 1.45(2) . ? C9 C10 1.363(11) . ? C9 C18 1.413(12) . ? C10 C12 1.392(11) . ? C10 C11 1.505(11) . ? C12 C14 1.404(12) . ? C12 C13 1.516(11) . ? C14 C16 1.380(12) . ? C14 C15 1.526(11) . ? C16 C18 1.413(12) . ? C16 C17 1.570(12) . ? C18 C19 1.539(12) . ? C20 C25 1.385(9) . ? C20 C21 1.393(10) . ? C21 C22 1.385(11) . ? C22 C23 1.386(12) . ? C23 C24 1.389(11) . ? C24 C25 1.374(11) . ? C25 C26 1.500(11) . ? C27 C28 1.488(9) . ? C28 C29 1.392(9) . ? C28 C33 1.402(9) . ? C29 C30 1.353(9) . ? C30 C31 1.359(10) . ? C31 C32 1.393(10) . ? C32 C33 1.400(9) . ? C34 C35 1.509(10) . ? C35 C44 1.390(10) . ? C35 C36 1.397(11) . ? C36 C38 1.407(11) . ? C36 C37 1.522(10) . ? C38 C40 1.409(10) . ? C38 C39 1.548(11) . ? C40 C42 1.385(10) . ? C40 C41 1.532(10) . ? C42 C44 1.406(11) . ? C42 C43 1.546(10) . ? C44 C45 1.514(10) . ? C46 C47 1.401(10) . ? C46 C51 1.420(10) . ? C47 C48 1.369(10) . ? C48 C49 1.375(10) . ? C49 C50 1.374(10) . ? C50 C51 1.381(10) . ? C51 C52 1.488(11) . ? C52 La2 3.062(10) 1_655 ? C53 C54 1.484(10) . ? C54 C55 1.380(11) . ? C54 C59 1.411(10) . ? C55 C56 1.393(12) . ? C56 C57 1.380(14) . ? C57 C58 1.411(13) . ? C58 C59 1.388(11) . ? C60 C61 1.497(12) . ? C61 C62 1.393(14) . ? C61 C64 1.406(14) . ? C62 C64 1.414(14) 3_656 ? C62 C63 1.508(14) . ? C64 C62 1.414(14) 3_656 ? C64 C65 1.533(14) . ? C66 C67 1.493(12) . ? C67 C72 1.379(11) . ? C67 C68 1.404(11) . ? C68 C69 1.403(13) . ? C69 C70 1.362(13) . ? C70 C71 1.368(11) . ? C71 C72 1.417(12) . ? C73 C74 1.519(11) . ? C74 C76 1.384(13) 3 ? C74 C75 1.411(12) . ? C75 C76 1.413(11) . ? C75 C78 1.535(13) . ? C76 C74 1.384(13) 3 ? C76 C77 1.529(13) . ? 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 C1 O1 La2 140.9(5) . . ? C1 O1 La1 85.2(5) . . ? La2 O1 La1 96.71(15) . . ? C1 O2 La1 107.9(5) . . ? C26 O4 La2 152.6(7) . 1_655 ? C27 O5 La2 161.6(5) . . ? C27 O5 La1 91.1(5) . . ? La2 O5 La1 102.48(16) . . ? C27 O6 La1 99.0(4) . . ? C52 O7 La2 91.0(6) . 1_655 ? C52 O8 La2 105.5(7) . 1_655 ? C53 O9 La2 129.5(4) . . ? C53 O9 La1 93.7(5) . . ? La2 O9 La1 104.19(17) . . ? C53 O10 La1 94.6(4) . . ? C66 O11 La2 92.3(5) . . ? C66 O12 La2 96.1(5) . . ? C01 O14 La1 161.7(9) . . ? C03 O15 La1 127.8(10) . . ? C06 O22 La1 133.3(9) . . ? O22 La1 O15 105.4(3) . . ? O22 La1 O2 79.8(2) . . ? O15 La1 O2 134.5(2) . . ? O22 La1 O6 74.9(2) . . ? O15 La1 O6 69.3(2) . . ? O2 La1 O6 149.8(2) . . ? O22 La1 O14 140.7(3) . . ? O15 La1 O14 74.7(2) . . ? O2 La1 O14 74.3(2) . . ? O6 La1 O14 135.8(2) . . ? O22 La1 O10 149.3(2) . . ? O15 La1 O10 76.0(3) . . ? O2 La1 O10 121.73(19) . . ? O6 La1 O10 77.22(17) . . ? O14 La1 O10 69.8(2) . . ? O22 La1 O9 126.6(2) . . ? O15 La1 O9 124.4(3) . . ? O2 La1 O9 78.45(19) . . ? O6 La1 O9 103.84(16) . . ? O14 La1 O9 76.3(2) . . ? O10 La1 O9 49.66(15) . . ? O22 La1 O5 74.5(2) . . ? O15 La1 O5 116.9(2) . . ? O2 La1 O5 108.10(18) . . ? O6 La1 O5 49.28(16) . . ? O14 La1 O5 141.8(2) . . ? O10 La1 O5 77.79(17) . . ? O9 La1 O5 67.24(15) . . ? O22 La1 O13 70.8(3) . . ? O15 La1 O13 69.2(3) . . ? O2 La1 O13 70.5(3) . . ? O6 La1 O13 115.0(2) . . ? O14 La1 O13 73.0(3) . . ? O10 La1 O13 134.2(2) . . ? O9 La1 O13 140.9(2) . . ? O5 La1 O13 144.9(2) . . ? O22 La1 O1 68.2(2) . . ? O15 La1 O1 173.6(2) . . ? O2 La1 O1 45.89(17) . . ? O6 La1 O1 108.11(17) . . ? O14 La1 O1 110.10(19) . . ? O10 La1 O1 109.46(15) . . ? O9 La1 O1 61.62(15) . . ? O5 La1 O1 62.21(15) . . ? O13 La1 O1 107.7(2) . . ? O22 La1 C53 146.6(2) . . ? O15 La1 C53 99.2(3) . . ? O2 La1 C53 98.8(2) . . ? O6 La1 C53 93.51(18) . . ? O14 La1 C53 67.7(2) . . ? O10 La1 C53 24.88(16) . . ? O9 La1 C53 25.29(17) . . ? O5 La1 C53 74.37(18) . . ? O13 La1 C53 140.6(2) . . ? O1 La1 C53 86.67(19) . . ? O22 La1 C27 72.1(2) . . ? O15 La1 C27 92.7(2) . . ? O2 La1 C27 130.4(2) . . ? O6 La1 C27 24.00(17) . . ? O14 La1 C27 146.6(2) . . ? O10 La1 C27 77.20(18) . . ? O9 La1 C27 86.49(19) . . ? O5 La1 C27 25.32(17) . . ? O13 La1 C27 131.8(3) . . ? O1 La1 C27 85.37(18) . . ? C53 La1 C27 84.59(19) . . ? O4 La2 O8 109.9(2) 1_455 1_455 ? O4 La2 O1 77.00(19) 1_455 . ? O8 La2 O1 133.85(19) 1_455 . ? O4 La2 O12 128.13(19) 1_455 . ? O8 La2 O12 118.7(2) 1_455 . ? O1 La2 O12 82.08(18) . . ? O4 La2 O16 68.5(3) 1_455 . ? O8 La2 O16 78.6(2) 1_455 . ? O1 La2 O16 140.0(2) . . ? O12 La2 O16 103.5(3) . . ? O4 La2 O5 137.3(2) 1_455 . ? O8 La2 O5 76.77(18) 1_455 . ? O1 La2 O5 70.26(16) . . ? O12 La2 O5 73.83(18) . . ? O16 La2 O5 149.7(2) . . ? O4 La2 O9 73.56(18) 1_455 . ? O8 La2 O9 70.04(18) 1_455 . ? O1 La2 O9 68.67(16) . . ? O12 La2 O9 138.90(18) . . ? O16 La2 O9 117.5(3) . . ? O5 La2 O9 69.52(15) . . ? O4 La2 O11 80.6(2) 1_455 . ? O8 La2 O11 146.1(2) 1_455 . ? O1 La2 O11 79.3(2) . . ? O12 La2 O11 48.88(18) . . ? O16 La2 O11 75.8(3) . . ? O5 La2 O11 117.98(19) . . ? O9 La2 O11 142.39(18) . . ? O4 La2 O7 136.0(2) 1_455 1_455 ? O8 La2 O7 46.3(2) 1_455 1_455 ? O1 La2 O7 147.0(2) . 1_455 ? O12 La2 O7 76.2(2) . 1_455 ? O16 La2 O7 70.3(3) . 1_455 ? O5 La2 O7 79.91(19) . 1_455 ? O9 La2 O7 114.1(2) . 1_455 ? O11 La2 O7 103.5(2) . 1_455 ? O4 La2 C66 103.9(2) 1_455 . ? O8 La2 C66 138.5(2) 1_455 . ? O1 La2 C66 76.5(2) . . ? O12 La2 C66 24.46(17) . . ? O16 La2 C66 92.4(3) . . ? O5 La2 C66 94.5(2) . . ? O9 La2 C66 144.8(2) . . ? O11 La2 C66 24.83(18) . . ? O7 La2 C66 92.4(3) 1_455 . ? O4 La2 C52 127.7(2) 1_455 1_455 ? O8 La2 C52 22.2(2) 1_455 1_455 ? O1 La2 C52 142.0(2) . 1_455 ? O12 La2 C52 97.2(2) . 1_455 ? O16 La2 C52 77.4(3) . 1_455 ? O5 La2 C52 73.0(2) . 1_455 ? O9 La2 C52 89.5(2) . 1_455 ? O11 La2 C52 128.1(3) . 1_455 ? O7 La2 C52 24.8(2) 1_455 1_455 ? C66 La2 C52 116.4(3) . 1_455 ? O4 La2 La1 97.58(16) 1_455 . ? O8 La2 La1 88.42(14) 1_455 . ? O1 La2 La1 45.81(12) . . ? O12 La2 La1 100.70(14) . . ? O16 La2 La1 155.7(3) . . ? O5 La2 La1 39.75(11) . . ? O9 La2 La1 38.24(10) . . ? O11 La2 La1 122.96(16) . . ? O7 La2 La1 114.58(16) 1_455 . ? C66 La2 La1 110.67(18) . . ? C52 La2 La1 97.99(19) 1_455 . ? C7 S1 C8 103.1(4) . . ? C20 S2 C15 104.9(4) . . ? C33 S3 C34 103.2(3) . . ? C46 S4 C41 105.0(4) . . ? C59 S5 C60 101.8(4) . . ? C72 S6 C73 104.1(4) . . ? O2 C1 O1 121.0(8) . . ? O2 C1 C2 118.2(8) . . ? O1 C1 C2 120.8(8) . . ? O2 C1 La1 50.1(4) . . ? O1 C1 La1 70.9(4) . . ? C2 C1 La1 168.2(6) . . ? C02 C01 O14 166(2) . . ? C7 C2 C3 120.3(7) . . ? C7 C2 C1 122.5(8) . . ? C3 C2 C1 117.2(7) . . ? C4 C3 C2 122.3(8) . . ? N01 C03 O15 131(2) . . ? C5 C4 C3 118.1(8) . . ? C4 C5 C6 120.7(8) . . ? C7 C6 C5 121.3(8) . . ? O22 C06 N02 127.5(17) . . ? C2 C7 C6 117.4(8) . . ? C2 C7 S1 121.5(6) . . ? C6 C7 S1 121.2(6) . . ? C9 C8 S1 106.4(5) . . ? C10 C9 C18 121.1(9) . . ? C10 C9 C8 120.9(8) . . ? C18 C9 C8 117.9(8) . . ? C9 C10 C12 120.0(8) . . ? C9 C10 C11 120.1(9) . . ? C12 C10 C11 119.9(9) . . ? C10 C12 C14 119.8(9) . . ? C10 C12 C13 119.9(9) . . ? C14 C12 C13 120.2(9) . . ? C16 C14 C12 120.8(9) . . ? C16 C14 C15 119.0(9) . . ? C12 C14 C15 119.8(9) . . ? C14 C15 S2 103.6(5) . . ? C14 C16 C18 119.2(9) . . ? C14 C16 C17 121.6(9) . . ? C18 C16 C17 119.2(9) . . ? C9 C18 C16 119.0(9) . . ? C9 C18 C19 121.0(9) . . ? C16 C18 C19 119.9(9) . . ? C25 C20 C21 118.2(8) . . ? C25 C20 S2 119.8(6) . . ? C21 C20 S2 122.0(6) . . ? C22 C21 C20 122.1(8) . . ? C21 C22 C23 119.2(9) . . ? C22 C23 C24 118.5(9) . . ? C25 C24 C23 122.1(8) . . ? C24 C25 C20 119.8(8) . . ? C24 C25 C26 117.1(8) . . ? C20 C25 C26 123.1(8) . . ? O3 C26 O4 124.4(9) . . ? O3 C26 C25 118.6(8) . . ? O4 C26 C25 117.0(9) . . ? O6 C27 O5 120.4(7) . . ? O6 C27 C28 120.3(7) . . ? O5 C27 C28 119.2(7) . . ? O6 C27 La1 57.0(4) . . ? O5 C27 La1 63.6(4) . . ? C28 C27 La1 176.1(5) . . ? C29 C28 C33 118.4(7) . . ? C29 C28 C27 119.5(7) . . ? C33 C28 C27 122.1(7) . . ? C30 C29 C28 122.5(7) . . ? C29 C30 C31 119.8(7) . . ? C30 C31 C32 120.2(7) . . ? C31 C32 C33 120.6(7) . . ? C32 C33 C28 118.4(7) . . ? C32 C33 S3 120.9(6) . . ? C28 C33 S3 120.7(6) . . ? C35 C34 S3 106.5(5) . . ? C44 C35 C36 120.0(7) . . ? C44 C35 C34 121.9(7) . . ? C36 C35 C34 118.1(7) . . ? C35 C36 C38 119.9(7) . . ? C35 C36 C37 121.8(8) . . ? C38 C36 C37 118.3(8) . . ? C36 C38 C40 119.1(7) . . ? C36 C38 C39 121.1(8) . . ? C40 C38 C39 119.7(8) . . ? C42 C40 C38 121.2(8) . . ? C42 C40 C41 119.2(7) . . ? C38 C40 C41 119.4(7) . . ? C40 C41 S4 104.9(5) . . ? C40 C42 C44 118.8(7) . . ? C40 C42 C43 121.7(8) . . ? C44 C42 C43 119.5(8) . . ? C35 C44 C42 121.0(7) . . ? C35 C44 C45 119.6(8) . . ? C42 C44 C45 119.4(7) . . ? C47 C46 C51 117.4(7) . . ? C47 C46 S4 123.2(6) . . ? C51 C46 S4 119.3(6) . . ? C48 C47 C46 121.6(8) . . ? C47 C48 C49 120.5(8) . . ? C50 C49 C48 119.2(8) . . ? C49 C50 C51 121.8(8) . . ? C50 C51 C46 119.3(7) . . ? C50 C51 C52 115.9(8) . . ? C46 C51 C52 124.8(8) . . ? O8 C52 O7 113.9(9) . . ? O8 C52 C51 123.3(9) . . ? O7 C52 C51 119.1(9) . . ? O8 C52 La2 52.3(5) . 1_655 ? O7 C52 La2 64.1(6) . 1_655 ? C51 C52 La2 146.6(6) . 1_655 ? O10 C53 O9 119.7(7) . . ? O10 C53 C54 121.5(7) . . ? O9 C53 C54 118.5(7) . . ? O10 C53 La1 60.5(4) . . ? O9 C53 La1 61.0(4) . . ? C54 C53 La1 160.9(5) . . ? C55 C54 C59 119.7(8) . . ? C55 C54 C53 118.1(8) . . ? C59 C54 C53 122.3(7) . . ? C54 C55 C56 122.7(9) . . ? C57 C56 C55 117.4(10) . . ? C56 C57 C58 121.4(10) . . ? C59 C58 C57 120.3(9) . . ? C58 C59 C54 118.4(8) . . ? C58 C59 S5 121.0(7) . . ? C54 C59 S5 120.6(6) . . ? C61 C60 S5 107.9(6) . . ? C62 C61 C64 119.1(10) . . ? C62 C61 C60 120.1(12) . . ? C64 C61 C60 120.8(12) . . ? C61 C62 C64 120.3(12) . 3_656 ? C61 C62 C63 119.5(11) . . ? C64 C62 C63 120.1(14) 3_656 . ? C61 C64 C62 120.6(11) . 3_656 ? C61 C64 C65 120.8(11) . . ? C62 C64 C65 118.6(14) 3_656 . ? O12 C66 O11 120.7(9) . . ? O12 C66 C67 119.3(7) . . ? O11 C66 C67 120.0(8) . . ? O12 C66 La2 59.4(4) . . ? O11 C66 La2 62.8(5) . . ? C67 C66 La2 166.6(6) . . ? C72 C67 C68 118.5(8) . . ? C72 C67 C66 124.0(7) . . ? C68 C67 C66 117.5(8) . . ? C69 C68 C67 121.4(9) . . ? C70 C69 C68 119.7(10) . . ? C69 C70 C71 119.4(10) . . ? C70 C71 C72 122.3(9) . . ? C67 C72 C71 118.5(8) . . ? C67 C72 S6 120.5(7) . . ? C71 C72 S6 120.9(7) . . ? C74 C73 S6 108.3(6) . . ? C76 C74 C75 121.3(9) 3 . ? C76 C74 C73 121.0(10) 3 . ? C75 C74 C73 117.7(10) . . ? C74 C75 C76 119.2(10) . . ? C74 C75 C78 121.3(9) . . ? C76 C75 C78 119.4(11) . . ? C74 C76 C75 119.4(10) 3 . ? C74 C76 C77 120.3(9) 3 . ? C75 C76 C77 120.2(11) . . ? C03 N01 C05 125(3) . . ? C03 N01 C04 118(3) . . ? C05 N01 C04 110(2) . . ? C06 N02 C08 120.3(19) . . ? C06 N02 C07 128.1(17) . . ? C08 N02 C07 110.0(17) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 23.33 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.279 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.085 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.001 0.001 0.500 1534.0 78.4 2 -0.129 0.371 0.000 1528.6 78.0 _platon_squeeze_details ; Disordered, independent solvent molecules were eliminated from the refinement using SQUEEZE/PLATON [Spek, A.L. (2003), J. Appl. Cryst. 36, 7-13]. ; data_p2 _database_code_depnum_ccdc_archive 'CCDC 832547' #TrackingRef '- p1-3-r2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H84 La2 O17 S6' _chemical_formula_weight 1763.63 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' La La -0.2871 2.4523 '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' S S 0.1246 0.1234 '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 9.8233(5) _cell_length_b 13.2039(7) _cell_length_c 15.9391(8) _cell_angle_alpha 113.8630(10) _cell_angle_beta 96.3080(10) _cell_angle_gamma 92.6770(10) _cell_volume 1869.74(17) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3688 _cell_measurement_theta_min 5.121 _cell_measurement_theta_max 52.168 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 898 _exptl_absorpt_coefficient_mu 1.363 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8757 _exptl_absorpt_correction_T_max 0.8987 _exptl_absorpt_process_details sadabs _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 'Bruker SMART APEXII' _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 9305 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6479 _reflns_number_gt 5493 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+ (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2001)' _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^)+(0.0505P)^2^+0.2485P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6479 _refine_ls_number_parameters 475 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0830 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.941 _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 La La 0.22666(2) 0.500512(17) 0.495510(14) 0.02501(8) Uani 1 1 d . . . S1 S 0.14038(11) 0.30484(10) 0.16473(7) 0.0454(3) Uani 1 1 d . . . S2 S 0.71623(11) 0.63588(11) 0.26486(7) 0.0471(3) Uani 1 1 d . . . S3 S 0.31309(10) 0.88008(8) 0.58521(7) 0.0405(3) Uani 1 1 d . . . O1 O 0.0874(3) 0.3586(2) 0.34823(17) 0.0362(6) Uani 1 1 d . . . O2 O -0.1328(3) 0.3824(2) 0.3651(2) 0.0470(8) Uani 1 1 d . . . O3 O 0.8388(3) 0.6312(2) 0.43235(19) 0.0436(7) Uani 1 1 d . . . O4 O 1.0584(3) 0.6037(2) 0.4471(2) 0.0600(9) Uani 1 1 d . . . O5 O 0.3915(3) 0.6675(2) 0.53676(19) 0.0400(7) Uani 1 1 d . . . O6 O 0.6070(3) 0.6343(2) 0.55914(19) 0.0420(7) Uani 1 1 d . . . O7 O 0.3148(3) 0.5140(3) 0.34616(19) 0.0499(8) Uani 1 1 d . . . H7B H 0.2473 0.4981 0.3032 0.060 Uiso 1 1 d R . . H7A H 0.3510 0.5797 0.3609 0.060 Uiso 1 1 d R . . O8 O 0.4002(3) 0.5329(3) 0.6460(2) 0.0510(8) Uani 1 1 d . . . H8D H 0.3683 0.4959 0.6737 0.061 Uiso 1 1 d R . . H8E H 0.4091 0.6015 0.6828 0.061 Uiso 1 1 d R . . C1 C -0.0397(4) 0.3357(3) 0.3207(2) 0.0301(8) Uani 1 1 d . . . C2 C -0.0871(4) 0.2439(3) 0.2258(3) 0.0305(8) Uani 1 1 d . . . C3 C -0.2079(4) 0.1788(3) 0.2143(3) 0.0401(10) Uani 1 1 d . . . H3 H -0.2569 0.1940 0.2641 0.048 Uiso 1 1 calc R . . C4 C -0.2575(5) 0.0918(4) 0.1306(3) 0.0515(12) Uani 1 1 d . . . H4 H -0.3376 0.0473 0.1242 0.062 Uiso 1 1 calc R . . C5 C -0.1859(5) 0.0719(4) 0.0561(3) 0.0563(13) Uani 1 1 d . . . H5 H -0.2191 0.0141 -0.0009 0.068 Uiso 1 1 calc R . . C6 C -0.0673(4) 0.1361(4) 0.0654(3) 0.0465(11) Uani 1 1 d . . . H6 H -0.0213 0.1217 0.0144 0.056 Uiso 1 1 calc R . . C7 C -0.0142(4) 0.2227(3) 0.1500(3) 0.0335(9) Uani 1 1 d . . . C8 C 0.1692(4) 0.2890(4) 0.0494(3) 0.0452(11) Uani 1 1 d . . . H8A H 0.1838 0.2129 0.0111 0.054 Uiso 1 1 calc R . . H8B H 0.0921 0.3107 0.0191 0.054 Uiso 1 1 calc R . . C9 C 0.2979(4) 0.3671(4) 0.0682(3) 0.0398(10) Uani 1 1 d . . . C10 C 0.2854(4) 0.4806(4) 0.0931(3) 0.0413(10) Uani 1 1 d . . . C11 C 0.1461(5) 0.5233(5) 0.0951(4) 0.0670(15) Uani 1 1 d . . . H11A H 0.1359 0.5618 0.0553 0.100 Uiso 1 1 calc R . . H11B H 0.1374 0.5735 0.1573 0.100 Uiso 1 1 calc R . . H11C H 0.0759 0.4619 0.0740 0.100 Uiso 1 1 calc R . . C12 C 0.4063(4) 0.5547(3) 0.1170(3) 0.0399(10) Uani 1 1 d . . . C13 C 0.3974(5) 0.6787(4) 0.1467(4) 0.0601(13) Uani 1 1 d . . . H13A H 0.3041 0.6949 0.1540 0.090 Uiso 1 1 calc R . . H13B H 0.4266 0.7003 0.1002 0.090 Uiso 1 1 calc R . . H13C H 0.4559 0.7192 0.2045 0.090 Uiso 1 1 calc R . . C14 C 0.5346(4) 0.5139(3) 0.1151(3) 0.0383(9) Uani 1 1 d . . . C15 C 0.6621(5) 0.5937(4) 0.1412(3) 0.0468(11) Uani 1 1 d . . . H15A H 0.6424 0.6580 0.1287 0.056 Uiso 1 1 calc R . . H15B H 0.7339 0.5579 0.1060 0.056 Uiso 1 1 calc R . . C16 C 0.5463(4) 0.4005(4) 0.0924(3) 0.0437(10) Uani 1 1 d . . . C17 C 0.6883(5) 0.3598(5) 0.0961(4) 0.0678(15) Uani 1 1 d . . . H17A H 0.7575 0.4217 0.1164 0.102 Uiso 1 1 calc R . . H17B H 0.7004 0.3067 0.0356 0.102 Uiso 1 1 calc R . . H17C H 0.6966 0.3251 0.1388 0.102 Uiso 1 1 calc R . . C18 C 0.4276(5) 0.3271(4) 0.0692(3) 0.0467(11) Uani 1 1 d . . . C19 C 0.4380(6) 0.2048(4) 0.0469(5) 0.0807(18) Uani 1 1 d . . . H19A H 0.5301 0.1947 0.0671 0.121 Uiso 1 1 calc R . . H19B H 0.4158 0.1621 -0.0187 0.121 Uiso 1 1 calc R . . H19C H 0.3748 0.1804 0.0783 0.121 Uiso 1 1 calc R . . C20 C 0.8869(4) 0.6980(3) 0.2819(3) 0.0372(9) Uani 1 1 d . . . C21 C 0.9225(5) 0.7522(4) 0.2274(3) 0.0495(11) Uani 1 1 d . . . H21 H 0.8566 0.7539 0.1816 0.059 Uiso 1 1 calc R . . C22 C 1.0529(5) 0.8032(4) 0.2399(4) 0.0586(13) Uani 1 1 d . . . H22 H 1.0749 0.8389 0.2027 0.070 Uiso 1 1 calc R . . C23 C 1.1508(5) 0.8011(4) 0.3078(4) 0.0598(14) Uani 1 1 d . . . H23 H 1.2390 0.8363 0.3174 0.072 Uiso 1 1 calc R . . C24 C 1.1171(4) 0.7464(4) 0.3614(3) 0.0502(12) Uani 1 1 d . . . H24 H 1.1844 0.7441 0.4062 0.060 Uiso 1 1 calc R . . C25 C 0.9857(4) 0.6946(3) 0.3507(3) 0.0354(9) Uani 1 1 d . . . C26 C 0.9588(4) 0.6391(3) 0.4139(3) 0.0392(10) Uani 1 1 d . . . C27 C 0.5124(4) 0.6969(3) 0.5768(3) 0.0289(8) Uani 1 1 d . . . C28 C 0.5458(4) 0.8125(3) 0.6523(2) 0.0288(8) Uani 1 1 d . . . C29 C 0.6663(4) 0.8311(3) 0.7137(3) 0.0353(9) Uani 1 1 d . . . H29 H 0.7220 0.7736 0.7052 0.042 Uiso 1 1 calc R . . C30 C 0.7048(4) 0.9336(4) 0.7873(3) 0.0444(11) Uani 1 1 d . . . H30 H 0.7856 0.9447 0.8275 0.053 Uiso 1 1 calc R . . C31 C 0.6229(5) 1.0186(4) 0.8003(3) 0.0481(11) Uani 1 1 d . . . H31 H 0.6477 1.0872 0.8501 0.058 Uiso 1 1 calc R . . C32 C 0.5041(4) 1.0028(3) 0.7399(3) 0.0414(10) Uani 1 1 d . . . H32 H 0.4502 1.0615 0.7491 0.050 Uiso 1 1 calc R . . C33 C 0.4631(4) 0.9008(3) 0.6654(3) 0.0306(8) Uani 1 1 d . . . C34 C 0.2392(4) 1.0132(3) 0.6305(3) 0.0414(10) Uani 1 1 d . . . H34A H 0.2119 1.0279 0.6907 0.050 Uiso 1 1 calc R . . H34B H 0.3061 1.0733 0.6370 0.050 Uiso 1 1 calc R . . C35 C 0.1147(4) 1.0042(3) 0.5614(3) 0.0372(9) Uani 1 1 d . . . C36 C 0.1285(4) 1.0472(3) 0.4955(3) 0.0369(9) Uani 1 1 d . . . C37 C 0.2679(4) 1.0941(4) 0.4871(3) 0.0528(12) Uani 1 1 d . . . H37A H 0.2746 1.0755 0.4231 0.079 Uiso 1 1 calc R . . H37B H 0.3393 1.0629 0.5123 0.079 Uiso 1 1 calc R . . H37C H 0.2779 1.1736 0.5208 0.079 Uiso 1 1 calc R . . C38 C -0.0116(4) 0.9557(3) 0.5658(3) 0.0371(9) Uani 1 1 d . . . C39 C -0.0250(5) 0.9038(4) 0.6325(3) 0.0539(12) Uani 1 1 d . . . H39A H -0.0871 0.8370 0.6033 0.081 Uiso 1 1 calc R . . H39B H -0.0602 0.9550 0.6859 0.081 Uiso 1 1 calc R . . H39C H 0.0636 0.8861 0.6513 0.081 Uiso 1 1 calc R . . O01 O 0.4437(11) 0.7255(9) 0.3730(7) 0.116(3) Uani 0.50 1 d P . . 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 0.01910(11) 0.02746(12) 0.02491(12) 0.00698(9) 0.00291(8) 0.00484(8) S1 0.0370(6) 0.0630(7) 0.0285(5) 0.0126(5) 0.0042(4) -0.0094(5) S2 0.0337(6) 0.0745(8) 0.0384(6) 0.0314(6) -0.0011(5) -0.0054(5) S3 0.0360(6) 0.0337(5) 0.0423(6) 0.0077(5) -0.0051(4) 0.0138(4) O1 0.0332(15) 0.0387(15) 0.0272(14) 0.0058(12) -0.0011(11) -0.0008(12) O2 0.0387(17) 0.0447(17) 0.0463(18) 0.0033(14) 0.0202(13) 0.0086(13) O3 0.0448(18) 0.0515(18) 0.0401(17) 0.0249(14) 0.0053(13) 0.0027(14) O4 0.059(2) 0.0441(18) 0.065(2) 0.0175(16) -0.0241(17) 0.0132(15) O5 0.0309(15) 0.0277(14) 0.0510(18) 0.0083(13) -0.0041(13) 0.0008(11) O6 0.0325(15) 0.0354(15) 0.0485(18) 0.0058(13) 0.0077(12) 0.0142(12) O7 0.0481(18) 0.0552(19) 0.0399(17) 0.0155(15) 0.0002(13) -0.0049(14) O8 0.0390(17) 0.065(2) 0.0516(19) 0.0283(16) 0.0014(14) -0.0014(15) C1 0.033(2) 0.029(2) 0.028(2) 0.0110(16) 0.0048(16) 0.0060(16) C2 0.029(2) 0.030(2) 0.030(2) 0.0105(17) 0.0030(16) 0.0033(16) C3 0.037(2) 0.040(2) 0.041(2) 0.016(2) 0.0051(18) -0.0003(18) C4 0.050(3) 0.044(3) 0.050(3) 0.014(2) -0.002(2) -0.018(2) C5 0.070(3) 0.043(3) 0.038(3) 0.001(2) -0.002(2) -0.014(2) C6 0.047(3) 0.045(3) 0.032(2) 0.000(2) 0.0070(19) -0.002(2) C7 0.027(2) 0.036(2) 0.034(2) 0.0113(18) 0.0043(16) 0.0053(16) C8 0.046(3) 0.050(3) 0.032(2) 0.010(2) 0.0045(19) 0.000(2) C9 0.042(2) 0.050(3) 0.024(2) 0.0119(19) 0.0065(17) 0.0004(19) C10 0.039(2) 0.052(3) 0.028(2) 0.013(2) -0.0004(17) 0.005(2) C11 0.041(3) 0.071(4) 0.088(4) 0.034(3) -0.002(3) 0.008(2) C12 0.044(2) 0.044(2) 0.032(2) 0.0174(19) 0.0011(18) 0.0063(19) C13 0.054(3) 0.058(3) 0.067(3) 0.025(3) 0.005(2) 0.013(2) C14 0.041(2) 0.047(2) 0.027(2) 0.0156(19) 0.0028(17) 0.0045(19) C15 0.047(3) 0.059(3) 0.039(2) 0.028(2) 0.000(2) -0.001(2) C16 0.042(2) 0.053(3) 0.040(2) 0.022(2) 0.0080(19) 0.006(2) C17 0.043(3) 0.075(4) 0.093(4) 0.040(3) 0.015(3) 0.018(3) C18 0.051(3) 0.046(3) 0.046(3) 0.019(2) 0.016(2) 0.008(2) C19 0.063(4) 0.051(3) 0.127(5) 0.032(3) 0.026(3) 0.008(3) C20 0.038(2) 0.040(2) 0.035(2) 0.0143(19) 0.0107(17) 0.0084(18) C21 0.050(3) 0.051(3) 0.052(3) 0.025(2) 0.011(2) 0.006(2) C22 0.065(3) 0.051(3) 0.062(3) 0.022(3) 0.024(3) -0.003(2) C23 0.043(3) 0.056(3) 0.065(3) 0.011(3) 0.013(2) -0.018(2) C24 0.037(2) 0.047(3) 0.050(3) 0.005(2) 0.002(2) 0.004(2) C25 0.030(2) 0.034(2) 0.035(2) 0.0075(18) 0.0056(17) 0.0063(17) C26 0.043(3) 0.029(2) 0.034(2) 0.0036(18) -0.0046(18) 0.0083(18) C27 0.025(2) 0.031(2) 0.033(2) 0.0162(17) 0.0052(16) 0.0016(16) C28 0.0273(19) 0.0278(19) 0.033(2) 0.0133(17) 0.0063(15) 0.0035(15) C29 0.033(2) 0.037(2) 0.034(2) 0.0133(18) 0.0018(17) 0.0095(17) C30 0.039(2) 0.047(3) 0.037(2) 0.010(2) -0.0076(18) 0.0056(19) C31 0.052(3) 0.035(2) 0.040(3) 0.001(2) -0.005(2) 0.000(2) C32 0.042(2) 0.031(2) 0.045(3) 0.0090(19) 0.0041(19) 0.0112(18) C33 0.0241(19) 0.032(2) 0.036(2) 0.0157(18) 0.0022(15) 0.0020(15) C34 0.042(2) 0.038(2) 0.044(2) 0.015(2) 0.0037(19) 0.0207(19) C35 0.037(2) 0.032(2) 0.046(2) 0.0185(19) 0.0069(18) 0.0160(17) C36 0.036(2) 0.031(2) 0.046(2) 0.0161(19) 0.0111(18) 0.0123(17) C37 0.042(3) 0.058(3) 0.068(3) 0.035(3) 0.011(2) 0.005(2) C38 0.040(2) 0.035(2) 0.043(2) 0.0214(19) 0.0088(18) 0.0143(18) C39 0.053(3) 0.064(3) 0.060(3) 0.040(3) 0.012(2) 0.016(2) O01 0.108(8) 0.136(9) 0.111(8) 0.065(7) 0.001(6) -0.009(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 La O6 2.434(2) 2_666 ? La O4 2.442(3) 1_455 ? La O2 2.445(3) 2_566 ? La O5 2.485(3) . ? La O1 2.528(2) . ? La O3 2.537(3) 2_666 ? La O8 2.655(3) . ? La O7 2.689(3) . ? S1 C7 1.760(4) . ? S1 C8 1.820(4) . ? S2 C20 1.774(4) . ? S2 C15 1.825(4) . ? S3 C33 1.774(4) . ? S3 C34 1.828(4) . ? O1 C1 1.257(4) . ? O2 C1 1.250(4) . ? O2 La 2.445(3) 2_566 ? O3 C26 1.256(5) . ? O3 La 2.537(3) 2_666 ? O4 C26 1.259(5) . ? O4 La 2.442(3) 1_655 ? O5 C27 1.249(4) . ? O6 C27 1.252(4) . ? O6 La 2.434(2) 2_666 ? O7 H7B 0.8500 . ? O7 H7A 0.8501 . ? O8 H8D 0.8500 . ? O8 H8E 0.8500 . ? C1 C2 1.511(5) . ? C2 C3 1.382(5) . ? C2 C7 1.410(5) . ? C3 C4 1.380(6) . ? C3 H3 0.9300 . ? C4 C5 1.385(7) . ? C4 H4 0.9300 . ? C5 C6 1.366(6) . ? C5 H5 0.9300 . ? C6 C7 1.393(5) . ? C6 H6 0.9300 . ? C8 C9 1.515(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.402(6) . ? C9 C18 1.403(6) . ? C10 C12 1.415(6) . ? C10 C11 1.503(6) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C14 1.393(6) . ? C12 C13 1.519(6) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C16 1.404(6) . ? C14 C15 1.503(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C18 1.395(6) . ? C16 C17 1.522(6) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.517(7) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.391(6) . ? C20 C25 1.399(5) . ? C21 C22 1.376(6) . ? C21 H21 0.9300 . ? C22 C23 1.376(7) . ? C22 H22 0.9300 . ? C23 C24 1.379(7) . ? C23 H23 0.9300 . ? C24 C25 1.393(6) . ? C24 H24 0.9300 . ? C25 C26 1.503(6) . ? C27 C28 1.505(5) . ? C28 C29 1.395(5) . ? C28 C33 1.410(5) . ? C29 C30 1.386(5) . ? C29 H29 0.9300 . ? C30 C31 1.372(6) . ? C30 H30 0.9300 . ? C31 C32 1.379(6) . ? C31 H31 0.9300 . ? C32 C33 1.392(5) . ? C32 H32 0.9300 . ? C34 C35 1.519(5) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C38 1.391(6) . ? C35 C36 1.397(6) . ? C36 C38 1.413(5) 2_576 ? C36 C37 1.518(6) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C36 1.413(5) 2_576 ? C38 C39 1.493(6) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? 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 O6 La O4 143.66(11) 2_666 1_455 ? O6 La O2 142.61(10) 2_666 2_566 ? O4 La O2 73.71(11) 1_455 2_566 ? O6 La O5 95.68(9) 2_666 . ? O4 La O5 85.55(10) 1_455 . ? O2 La O5 84.02(9) 2_566 . ? O6 La O1 79.57(9) 2_666 . ? O4 La O1 74.69(9) 1_455 . ? O2 La O1 125.44(9) 2_566 . ? O5 La O1 135.74(9) . . ? O6 La O3 80.01(10) 2_666 2_666 ? O4 La O3 122.30(11) 1_455 2_666 ? O2 La O3 75.55(10) 2_566 2_666 ? O5 La O3 137.43(9) . 2_666 ? O1 La O3 85.55(9) . 2_666 ? O6 La O8 75.18(9) 2_666 . ? O4 La O8 137.38(10) 1_455 . ? O2 La O8 69.64(10) 2_566 . ? O5 La O8 69.89(9) . . ? O1 La O8 146.02(9) . . ? O3 La O8 68.09(9) 2_666 . ? O6 La O7 71.41(10) 2_666 . ? O4 La O7 75.73(11) 1_455 . ? O2 La O7 139.37(10) 2_566 . ? O5 La O7 67.44(9) . . ? O1 La O7 69.43(9) . . ? O3 La O7 144.64(9) 2_666 . ? O8 La O7 121.55(9) . . ? C7 S1 C8 106.28(19) . . ? C20 S2 C15 102.97(19) . . ? C33 S3 C34 103.96(18) . . ? C1 O1 La 133.1(2) . . ? C1 O2 La 154.6(3) . 2_566 ? C26 O3 La 120.2(3) . 2_666 ? C26 O4 La 169.1(3) . 1_655 ? C27 O5 La 134.5(2) . . ? C27 O6 La 172.4(3) . 2_666 ? La O7 H7B 109.7 . . ? La O7 H7A 109.3 . . ? H7B O7 H7A 109.8 . . ? La O8 H8D 109.6 . . ? La O8 H8E 109.5 . . ? H8D O8 H8E 108.2 . . ? O2 C1 O1 125.7(3) . . ? O2 C1 C2 115.8(3) . . ? O1 C1 C2 118.5(3) . . ? C3 C2 C7 119.5(3) . . ? C3 C2 C1 117.5(3) . . ? C7 C2 C1 123.0(3) . . ? C4 C3 C2 121.4(4) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 118.8(4) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 120.8(4) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 121.1(4) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C6 C7 C2 118.3(4) . . ? C6 C7 S1 122.1(3) . . ? C2 C7 S1 119.6(3) . . ? C9 C8 S1 103.2(3) . . ? C9 C8 H8A 111.1 . . ? S1 C8 H8A 111.1 . . ? C9 C8 H8B 111.1 . . ? S1 C8 H8B 111.1 . . ? H8A C8 H8B 109.1 . . ? C10 C9 C18 121.0(4) . . ? C10 C9 C8 119.0(4) . . ? C18 C9 C8 119.7(4) . . ? C9 C10 C12 119.0(4) . . ? C9 C10 C11 120.6(4) . . ? C12 C10 C11 120.4(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C10 119.7(4) . . ? C14 C12 C13 119.7(4) . . ? C10 C12 C13 120.6(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 C16 121.0(4) . . ? C12 C14 C15 119.1(4) . . ? C16 C14 C15 119.9(4) . . ? C14 C15 S2 106.6(3) . . ? C14 C15 H15A 110.4 . . ? S2 C15 H15A 110.4 . . ? C14 C15 H15B 110.4 . . ? S2 C15 H15B 110.4 . . ? H15A C15 H15B 108.6 . . ? C18 C16 C14 119.6(4) . . ? C18 C16 C17 120.7(4) . . ? C14 C16 C17 119.6(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 C9 119.7(4) . . ? C16 C18 C19 120.4(4) . . ? C9 C18 C19 119.9(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C25 119.6(4) . . ? C21 C20 S2 119.8(3) . . ? C25 C20 S2 120.6(3) . . ? C22 C21 C20 121.5(5) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 119.6(5) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C22 C23 C24 119.4(4) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C23 C24 C25 122.3(4) . . ? C23 C24 H24 118.9 . . ? C25 C24 H24 118.9 . . ? C24 C25 C20 117.7(4) . . ? C24 C25 C26 118.1(4) . . ? C20 C25 C26 124.2(4) . . ? O3 C26 O4 122.8(4) . . ? O3 C26 C25 118.8(3) . . ? O4 C26 C25 118.4(4) . . ? O5 C27 O6 123.5(3) . . ? O5 C27 C28 118.5(3) . . ? O6 C27 C28 118.1(3) . . ? C29 C28 C33 118.8(3) . . ? C29 C28 C27 116.5(3) . . ? C33 C28 C27 124.7(3) . . ? C30 C29 C28 121.2(4) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C31 C30 C29 119.6(4) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C32 120.3(4) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C33 121.3(4) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C32 C33 C28 118.8(3) . . ? C32 C33 S3 121.9(3) . . ? C28 C33 S3 119.3(3) . . ? C35 C34 S3 106.9(3) . . ? C35 C34 H34A 110.3 . . ? S3 C34 H34A 110.3 . . ? C35 C34 H34B 110.3 . . ? S3 C34 H34B 110.3 . . ? H34A C34 H34B 108.6 . . ? C38 C35 C36 121.1(4) . . ? C38 C35 C34 119.8(4) . . ? C36 C35 C34 119.1(4) . . ? C35 C36 C38 119.5(4) . 2_576 ? C35 C36 C37 121.0(4) . . ? C38 C36 C37 119.5(4) 2_576 . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 C36 119.5(4) . 2_576 ? C35 C38 C39 121.1(4) . . ? C36 C38 C39 119.4(4) 2_576 . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.556 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.080 data_p _database_code_depnum_ccdc_archive 'CCDC 832548' #TrackingRef '- p1-3-r2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H122 La2 N6 O22 S6' _chemical_formula_weight 2182.18 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' La La -0.2871 2.4523 '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' S S 0.1246 0.1234 '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' _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 12.668(2) _cell_length_b 14.585(3) _cell_length_c 17.323(3) _cell_angle_alpha 113.754(2) _cell_angle_beta 109.044(2) _cell_angle_gamma 90.263(2) _cell_volume 2734.7(9) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9429 _cell_measurement_theta_min 4.931 _cell_measurement_theta_max 54.641 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1126 _exptl_absorpt_coefficient_mu 0.951 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8705 _exptl_absorpt_correction_T_max 0.9109 _exptl_absorpt_process_details sadabs _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 'Bruker SMART APEXII' _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 19200 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9506 _reflns_number_gt 8192 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+ (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2001)' _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. The voids in the framework are filled with many disordered solvent molecules, which can not be located. Hence reflect on a high R(int) value. In the refinement we used SQEEZE procedure (Spek, A.L. (2008) Utrecht University, Utrecht, The Netherlands) to remove solvent electron density from voids which give a smaller final R(int) and R-value compared with the original R(int) and R-value. ; _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^)+(0.0819P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9506 _refine_ls_number_parameters 607 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1152 _refine_ls_wR_factor_gt 0.1101 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.002 _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 0.817283(15) 0.954903(13) 0.955284(12) 0.03820(9) Uani 1 1 d . . . S1 S 0.88072(9) 1.31958(7) 1.18477(6) 0.0522(2) Uani 1 1 d . . . S2 S 0.74813(8) 1.51803(7) 1.61738(6) 0.0463(2) Uani 1 1 d . . . S3 S 0.71321(9) 0.75130(8) 1.11386(6) 0.0563(3) Uani 1 1 d . . . C1 C 0.9278(3) 1.1695(2) 1.0215(2) 0.0370(7) Uani 1 1 d . . . C01 C 0.270(2) 0.8370(10) 0.3476(15) 0.177(9) Uani 0.50 1 d P . . H01A H 0.3387 0.8501 0.3426 0.213 Uiso 0.50 1 calc PR . . C2 C 0.9790(3) 1.2771(2) 1.0572(2) 0.0367(7) Uani 1 1 d . . . C02 C 0.0860(15) 0.7836(12) 0.2779(11) 0.136(6) Uani 0.50 1 d P . . H02A H 0.0958 0.7223 0.2856 0.204 Uiso 0.50 1 calc PR . . H02B H 0.0309 0.7682 0.2192 0.204 Uiso 0.50 1 calc PR . . H02C H 0.0605 0.8298 0.3235 0.204 Uiso 0.50 1 calc PR . . C3 C 1.0402(3) 1.3022(3) 1.0143(2) 0.0470(8) Uani 1 1 d . . . H3A H 1.0538 1.2509 0.9667 0.056 Uiso 1 1 calc R . . C03 C 0.1862(19) 0.8358(18) 0.2116(11) 0.219(13) Uani 0.50 1 d P . . H03A H 0.2596 0.8596 0.2160 0.329 Uiso 0.50 1 calc PR . . H03B H 0.1355 0.8821 0.2017 0.329 Uiso 0.50 1 calc PR . . H03C H 0.1580 0.7699 0.1619 0.329 Uiso 0.50 1 calc PR . . C4 C 1.0819(3) 1.4010(3) 1.0399(3) 0.0542(9) Uani 1 1 d . . . H4A H 1.1201 1.4169 1.0081 0.065 Uiso 1 1 calc R . . C5 C 1.0668(3) 1.4767(3) 1.1133(3) 0.0534(9) Uani 1 1 d . . . H5A H 1.0958 1.5439 1.1318 0.064 Uiso 1 1 calc R . . C6 C 1.0087(3) 1.4528(3) 1.1591(3) 0.0491(8) Uani 1 1 d . . . H6A H 1.0013 1.5041 1.2098 0.059 Uiso 1 1 calc R . . C7 C 0.9612(3) 1.3541(2) 1.1313(2) 0.0393(7) Uani 1 1 d . . . C8 C 0.9204(3) 1.4299(3) 1.2927(2) 0.0529(9) Uani 1 1 d . . . H8A H 1.0017 1.4419 1.3237 0.063 Uiso 1 1 calc R . . H8B H 0.8987 1.4894 1.2833 0.063 Uiso 1 1 calc R . . C9 C 0.8610(3) 1.4111(3) 1.3494(2) 0.0483(8) Uani 1 1 d . . . C10 C 0.9155(3) 1.3698(3) 1.4088(2) 0.0489(9) Uani 1 1 d . . . C11 C 1.0293(3) 1.3348(3) 1.4106(3) 0.0669(11) Uani 1 1 d . . . H11A H 1.0347 1.3149 1.3522 0.100 Uiso 1 1 calc R . . H11B H 1.0355 1.2782 1.4259 0.100 Uiso 1 1 calc R . . H11C H 1.0892 1.3894 1.4550 0.100 Uiso 1 1 calc R . . C12 C 0.8670(3) 1.3615(3) 1.4681(2) 0.0486(8) Uani 1 1 d . . . C13 C 0.9293(4) 1.3250(3) 1.5372(3) 0.0694(11) Uani 1 1 d . . . H13A H 1.0084 1.3322 1.5463 0.104 Uiso 1 1 calc R . . H13B H 0.9005 1.2550 1.5165 0.104 Uiso 1 1 calc R . . H13C H 0.9191 1.3646 1.5932 0.104 Uiso 1 1 calc R . . C14 C 0.7591(3) 1.3896(3) 1.4621(2) 0.0473(8) Uani 1 1 d . . . C15 C 0.7101(3) 1.3880(3) 1.5299(2) 0.0524(9) Uani 1 1 d . . . H15A H 0.7424 1.3412 1.5546 0.063 Uiso 1 1 calc R . . H15B H 0.6286 1.3683 1.5025 0.063 Uiso 1 1 calc R . . C16 C 0.7023(3) 1.4261(3) 1.3992(2) 0.0522(9) Uani 1 1 d . . . C17 C 0.5839(4) 1.4526(4) 1.3922(3) 0.0792(14) Uani 1 1 d . . . H17A H 0.5643 1.4917 1.3578 0.119 Uiso 1 1 calc R . . H17B H 0.5829 1.4914 1.4517 0.119 Uiso 1 1 calc R . . H17C H 0.5303 1.3913 1.3628 0.119 Uiso 1 1 calc R . . C18 C 0.7530(3) 1.4382(3) 1.3435(2) 0.0524(9) Uani 1 1 d . . . C19 C 0.6957(4) 1.4852(5) 1.2782(3) 0.0855(16) Uani 1 1 d . . . H19A H 0.6151 1.4698 1.2594 0.128 Uiso 1 1 calc R . . H19B H 0.7177 1.4576 1.2263 0.128 Uiso 1 1 calc R . . H19C H 0.7186 1.5574 1.3082 0.128 Uiso 1 1 calc R . . C20 C 0.6948(3) 1.5148(2) 1.6988(2) 0.0385(7) Uani 1 1 d . . . C21 C 0.6483(3) 1.4238(3) 1.6919(3) 0.0519(9) Uani 1 1 d . . . H21A H 0.6451 1.3633 1.6435 0.062 Uiso 1 1 calc R . . C22 C 0.6068(4) 1.4223(3) 1.7559(3) 0.0614(10) Uani 1 1 d . . . H22A H 0.5752 1.3609 1.7498 0.074 Uiso 1 1 calc R . . C23 C 0.6118(3) 1.5103(3) 1.8284(3) 0.0566(10) Uani 1 1 d . . . H23A H 0.5841 1.5091 1.8716 0.068 Uiso 1 1 calc R . . C24 C 0.6583(3) 1.6006(3) 1.8362(2) 0.0465(8) Uani 1 1 d . . . H24A H 0.6619 1.6603 1.8855 0.056 Uiso 1 1 calc R . . C25 C 0.6998(3) 1.6054(2) 1.7730(2) 0.0365(7) Uani 1 1 d . . . C26 C 0.7463(3) 1.7069(3) 1.7864(2) 0.0414(7) Uani 1 1 d . . . C27 C 0.8468(3) 0.9420(3) 1.1264(2) 0.0425(8) Uani 1 1 d . . . C28 C 0.8483(3) 0.9398(3) 1.2125(2) 0.0486(8) Uani 1 1 d . . . C29 C 0.9073(4) 1.0224(3) 1.2921(3) 0.0739(13) Uani 1 1 d . . . H29A H 0.9431 1.0770 1.2903 0.089 Uiso 1 1 calc R . . C30 C 0.9142(6) 1.0259(4) 1.3735(3) 0.0968(18) Uani 1 1 d . . . H30A H 0.9563 1.0816 1.4266 0.116 Uiso 1 1 calc R . . C31 C 0.8595(5) 0.9475(4) 1.3774(3) 0.0928(17) Uani 1 1 d . . . H31A H 0.8622 0.9512 1.4329 0.111 Uiso 1 1 calc R . . C32 C 0.8006(4) 0.8633(4) 1.2993(3) 0.0728(13) Uani 1 1 d . . . H32A H 0.7658 0.8095 1.3027 0.087 Uiso 1 1 calc R . . C33 C 0.7924(3) 0.8575(3) 1.2147(2) 0.0524(9) Uani 1 1 d . . . C34 C 0.6505(4) 0.6736(3) 1.1540(3) 0.0644(11) Uani 1 1 d . . . H34A H 0.7094 0.6507 1.1910 0.077 Uiso 1 1 calc R . . H34B H 0.6081 0.7130 1.1900 0.077 Uiso 1 1 calc R . . C35 C 0.5735(3) 0.5843(3) 1.0722(3) 0.0515(9) Uani 1 1 d . . . C36 C 0.4592(3) 0.5905(3) 1.0357(3) 0.0535(9) Uani 1 1 d . . . C37 C 0.4124(5) 0.6885(4) 1.0729(4) 0.0814(14) Uani 1 1 d . . . H37A H 0.3590 0.6980 1.0237 0.122 Uiso 1 1 calc R . . H37B H 0.4733 0.7447 1.1062 0.122 Uiso 1 1 calc R . . H37C H 0.3755 0.6845 1.1121 0.122 Uiso 1 1 calc R . . C38 C 0.6149(3) 0.4946(3) 1.0357(3) 0.0508(9) Uani 1 1 d . . . C39 C 0.7395(3) 0.4893(4) 1.0694(4) 0.0756(13) Uani 1 1 d . . . H39A H 0.7642 0.4599 1.0190 0.113 Uiso 1 1 calc R . . H39B H 0.7528 0.4483 1.1022 0.113 Uiso 1 1 calc R . . H39C H 0.7809 0.5565 1.1086 0.113 Uiso 1 1 calc R . . C40 C 0.5862(5) 0.9176(4) 0.7608(3) 0.0858(15) Uani 1 1 d . . . H40A H 0.5970 0.8501 0.7402 0.103 Uiso 1 1 calc R . . C41 C 0.4720(7) 1.0399(6) 0.7367(6) 0.149(3) Uani 1 1 d . . . H41A H 0.5358 1.0860 0.7864 0.223 Uiso 1 1 calc R . . H41B H 0.4076 1.0435 0.7549 0.223 Uiso 1 1 calc R . . H41C H 0.4553 1.0581 0.6870 0.223 Uiso 1 1 calc R . . C42 C 0.4127(8) 0.8660(6) 0.6283(5) 0.187(4) Uani 1 1 d . . . H42A H 0.4219 0.7991 0.6240 0.281 Uiso 1 1 calc R . . H42B H 0.4206 0.8712 0.5768 0.281 Uiso 1 1 calc R . . H42C H 0.3389 0.8789 0.6297 0.281 Uiso 1 1 calc R . . C43 C 0.6001(4) 1.0797(4) 1.0151(4) 0.0739(13) Uani 1 1 d . . . H43A H 0.5591 1.0850 0.9621 0.089 Uiso 1 1 calc R . . C44 C 0.6589(6) 1.1450(5) 1.1734(4) 0.1064(19) Uani 1 1 d . . . H44A H 0.7374 1.1502 1.1806 0.160 Uiso 1 1 calc R . . H44B H 0.6351 1.0825 1.1735 0.160 Uiso 1 1 calc R . . H44C H 0.6483 1.2010 1.2224 0.160 Uiso 1 1 calc R . . C45 C 0.5173(5) 1.2206(4) 1.0908(5) 0.1025(19) Uani 1 1 d . . . H45A H 0.4662 1.2031 1.0303 0.154 Uiso 1 1 calc R . . H45B H 0.5601 1.2867 1.1148 0.154 Uiso 1 1 calc R . . H45C H 0.4751 1.2209 1.1279 0.154 Uiso 1 1 calc R . . N1 N 0.4974(4) 0.9394(3) 0.7096(3) 0.0888(13) Uani 1 1 d . . . N01 N 0.1934(7) 0.8302(7) 0.2860(6) 0.076(3) Uani 0.50 1 d P . . N2 N 0.5933(3) 1.1471(3) 1.0897(3) 0.0681(10) Uani 1 1 d . . . O1 O 0.98849(19) 1.09956(16) 1.00310(16) 0.0442(5) Uani 1 1 d . . . O01 O 0.2813(13) 0.8308(9) 0.4206(7) 0.184(6) Uani 0.50 1 d P . . O2 O 0.8260(2) 1.14805(18) 1.00679(19) 0.0562(7) Uani 1 1 d . . . O02 O 0.6742(7) 0.8085(10) 0.5091(7) 0.162(5) Uani 0.50 1 d P . . O3 O 0.7950(3) 1.7132(2) 1.73663(19) 0.0669(8) Uani 1 1 d . . . O4 O 0.7325(2) 1.78393(18) 1.84900(16) 0.0522(6) Uani 1 1 d . . . O5 O 0.8960(2) 1.01912(18) 1.13001(16) 0.0506(6) Uani 1 1 d . . . O6 O 0.7960(2) 0.86744(17) 1.05316(16) 0.0486(6) Uani 1 1 d . . . O7 O 0.6539(3) 0.9760(2) 0.8310(2) 0.0823(10) Uani 1 1 d . . . O8 O 0.6559(3) 1.0095(2) 1.0080(3) 0.0770(9) Uani 1 1 d . . . O9 O 0.8783(2) 0.91345(19) 0.81896(16) 0.0553(6) Uani 1 1 d . . . H9A H 0.9497 0.9206 0.8333 0.066 Uiso 1 1 d R . . H9B H 0.8602 0.8496 0.7884 0.066 Uiso 1 1 d 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 0.03738(13) 0.03207(13) 0.04074(13) 0.00847(9) 0.01777(9) -0.00079(8) S1 0.0622(6) 0.0429(5) 0.0495(5) 0.0069(4) 0.0342(5) -0.0051(4) S2 0.0554(5) 0.0396(5) 0.0403(5) 0.0059(4) 0.0271(4) -0.0043(4) S3 0.0659(6) 0.0553(6) 0.0443(5) 0.0210(4) 0.0161(4) -0.0161(5) C1 0.0424(18) 0.0359(17) 0.0324(16) 0.0119(13) 0.0165(14) 0.0035(14) C01 0.32(3) 0.067(9) 0.18(2) 0.055(12) 0.14(2) 0.063(14) C2 0.0357(16) 0.0361(17) 0.0395(17) 0.0169(14) 0.0142(14) 0.0068(13) C02 0.155(15) 0.138(13) 0.142(13) 0.072(11) 0.069(12) 0.071(12) C3 0.053(2) 0.0427(19) 0.050(2) 0.0180(16) 0.0262(17) 0.0039(15) C03 0.24(2) 0.28(3) 0.084(10) 0.067(14) 0.006(12) -0.13(2) C4 0.063(2) 0.053(2) 0.066(2) 0.035(2) 0.035(2) 0.0091(18) C5 0.049(2) 0.041(2) 0.073(3) 0.0287(19) 0.0196(19) 0.0006(16) C6 0.051(2) 0.0350(18) 0.057(2) 0.0102(16) 0.0257(18) 0.0062(15) C7 0.0384(17) 0.0381(17) 0.0448(18) 0.0175(15) 0.0192(14) 0.0061(13) C8 0.058(2) 0.045(2) 0.048(2) 0.0058(17) 0.0276(18) 0.0017(17) C9 0.050(2) 0.047(2) 0.0377(18) 0.0044(16) 0.0212(16) 0.0003(16) C10 0.0455(19) 0.0420(19) 0.047(2) 0.0021(16) 0.0238(16) 0.0015(15) C11 0.058(2) 0.072(3) 0.077(3) 0.028(2) 0.037(2) 0.018(2) C12 0.056(2) 0.0372(18) 0.0417(19) 0.0044(15) 0.0195(16) 0.0024(15) C13 0.078(3) 0.067(3) 0.066(3) 0.027(2) 0.032(2) 0.018(2) C14 0.049(2) 0.0406(18) 0.0391(18) -0.0010(15) 0.0234(16) -0.0020(15) C15 0.059(2) 0.0423(19) 0.047(2) 0.0042(16) 0.0272(18) -0.0028(16) C16 0.0423(19) 0.059(2) 0.0384(19) 0.0049(17) 0.0148(15) 0.0047(16) C17 0.050(2) 0.120(4) 0.066(3) 0.033(3) 0.028(2) 0.017(3) C18 0.052(2) 0.058(2) 0.0409(19) 0.0108(17) 0.0231(17) 0.0091(17) C19 0.079(3) 0.127(5) 0.069(3) 0.050(3) 0.039(3) 0.038(3) C20 0.0356(16) 0.0439(18) 0.0381(17) 0.0158(15) 0.0180(14) 0.0040(14) C21 0.068(2) 0.0352(18) 0.054(2) 0.0135(16) 0.0314(19) 0.0015(16) C22 0.075(3) 0.050(2) 0.073(3) 0.031(2) 0.037(2) 0.0025(19) C23 0.065(2) 0.067(3) 0.055(2) 0.034(2) 0.033(2) 0.006(2) C24 0.0468(19) 0.055(2) 0.0404(19) 0.0193(17) 0.0202(16) 0.0086(16) C25 0.0317(16) 0.0420(18) 0.0369(17) 0.0172(14) 0.0131(13) 0.0050(13) C26 0.0419(18) 0.0426(18) 0.0327(17) 0.0089(15) 0.0141(14) -0.0004(14) C27 0.0399(17) 0.0436(19) 0.0457(19) 0.0158(16) 0.0215(15) 0.0048(15) C28 0.049(2) 0.048(2) 0.0424(19) 0.0118(16) 0.0179(16) -0.0009(16) C29 0.091(3) 0.059(3) 0.050(2) 0.007(2) 0.020(2) -0.016(2) C30 0.130(5) 0.081(4) 0.046(3) 0.007(2) 0.017(3) -0.021(3) C31 0.116(4) 0.103(4) 0.045(3) 0.022(3) 0.024(3) -0.012(3) C32 0.082(3) 0.083(3) 0.046(2) 0.027(2) 0.016(2) -0.012(2) C33 0.051(2) 0.059(2) 0.044(2) 0.0206(18) 0.0149(17) -0.0002(17) C34 0.071(3) 0.069(3) 0.058(2) 0.034(2) 0.021(2) -0.015(2) C35 0.055(2) 0.056(2) 0.054(2) 0.0319(18) 0.0217(18) -0.0082(17) C36 0.061(2) 0.054(2) 0.066(2) 0.035(2) 0.035(2) 0.0070(18) C37 0.099(4) 0.066(3) 0.107(4) 0.044(3) 0.062(3) 0.023(3) C38 0.0444(19) 0.063(2) 0.060(2) 0.042(2) 0.0167(17) -0.0017(17) C39 0.053(2) 0.103(4) 0.099(4) 0.070(3) 0.027(2) 0.011(2) C40 0.099(4) 0.069(3) 0.063(3) 0.013(3) 0.016(3) 0.025(3) C41 0.135(6) 0.120(6) 0.154(7) 0.052(5) 0.014(5) 0.061(5) C42 0.185(9) 0.141(7) 0.106(6) 0.012(5) -0.054(6) -0.013(6) C43 0.065(3) 0.084(3) 0.093(4) 0.046(3) 0.043(3) 0.012(3) C44 0.110(5) 0.106(5) 0.101(5) 0.036(4) 0.045(4) 0.017(4) C45 0.097(4) 0.086(4) 0.137(5) 0.043(4) 0.064(4) 0.042(3) N1 0.087(3) 0.079(3) 0.063(2) 0.019(2) -0.005(2) 0.016(2) N01 0.067(5) 0.115(7) 0.071(5) 0.069(5) 0.020(4) 0.034(5) N2 0.061(2) 0.067(2) 0.087(3) 0.030(2) 0.044(2) 0.0192(18) O1 0.0472(13) 0.0311(12) 0.0546(14) 0.0132(10) 0.0249(11) 0.0078(10) O01 0.284(16) 0.139(9) 0.081(6) 0.061(6) -0.010(8) -0.021(9) O2 0.0415(14) 0.0417(14) 0.0773(18) 0.0135(13) 0.0267(13) 0.0029(11) O02 0.078(5) 0.231(13) 0.131(8) 0.027(8) 0.048(6) 0.004(7) O3 0.099(2) 0.0446(15) 0.0586(16) 0.0063(12) 0.0504(16) -0.0104(14) O4 0.0599(15) 0.0398(13) 0.0483(14) 0.0032(11) 0.0290(12) -0.0009(11) O5 0.0535(14) 0.0428(13) 0.0504(14) 0.0117(11) 0.0230(12) -0.0091(11) O6 0.0622(15) 0.0359(13) 0.0437(13) 0.0087(11) 0.0249(12) -0.0061(11) O7 0.0664(19) 0.072(2) 0.068(2) 0.0096(17) 0.0001(16) 0.0080(16) O8 0.0632(18) 0.0692(19) 0.123(3) 0.0434(19) 0.0599(19) 0.0244(16) O9 0.0527(15) 0.0559(15) 0.0467(14) 0.0097(12) 0.0207(12) -0.0115(12) _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 O4 2.398(2) 1_544 ? La O8 2.509(3) . ? La O1 2.555(2) 2_777 ? La O9 2.566(2) . ? La O6 2.572(2) . ? La O7 2.578(3) . ? La O2 2.579(2) . ? La O5 2.602(2) . ? La O1 2.687(2) . ? La C27 2.948(3) . ? La C1 3.015(3) . ? S1 C7 1.771(3) . ? S1 C8 1.815(4) . ? S2 C20 1.767(3) . ? S2 C15 1.824(4) . ? S3 C33 1.766(4) . ? S3 C34 1.839(4) . ? C1 O2 1.242(4) . ? C1 O1 1.280(4) . ? C1 C2 1.488(4) . ? C01 N01 1.15(3) . ? C01 O01 1.27(2) . ? C01 H01A 0.9300 . ? C2 C3 1.372(5) . ? C2 C7 1.410(4) . ? C02 N01 1.457(19) . ? C02 H02A 0.9600 . ? C02 H02B 0.9600 . ? C02 H02C 0.9600 . ? C3 C4 1.370(5) . ? C3 H3A 0.9300 . ? C03 N01 1.298(17) . ? C03 H03A 0.9600 . ? C03 H03B 0.9600 . ? C03 H03C 0.9600 . ? C4 C5 1.379(5) . ? C4 H4A 0.9300 . ? C5 C6 1.377(5) . ? C5 H5A 0.9300 . ? C6 C7 1.382(5) . ? C6 H6A 0.9300 . ? C8 C9 1.518(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.392(5) . ? C9 C18 1.409(5) . ? C10 C12 1.399(5) . ? C10 C11 1.526(5) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C14 1.412(5) . ? C12 C13 1.497(6) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C16 1.395(5) . ? C14 C15 1.504(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C18 1.383(5) . ? C16 C17 1.529(5) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.539(6) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.393(5) . ? C20 C25 1.407(5) . ? C21 C22 1.381(5) . ? C21 H21A 0.9300 . ? C22 C23 1.370(6) . ? C22 H22A 0.9300 . ? C23 C24 1.377(5) . ? C23 H23A 0.9300 . ? C24 C25 1.385(5) . ? C24 H24A 0.9300 . ? C25 C26 1.491(5) . ? C26 O3 1.242(4) . ? C26 O4 1.270(4) . ? C27 O6 1.248(4) . ? C27 O5 1.252(4) . ? C27 C28 1.499(5) . ? C28 C29 1.375(5) . ? C28 C33 1.411(5) . ? C29 C30 1.364(7) . ? C29 H29A 0.9300 . ? C30 C31 1.371(7) . ? C30 H30A 0.9300 . ? C31 C32 1.373(6) . ? C31 H31A 0.9300 . ? C32 C33 1.403(5) . ? C32 H32A 0.9300 . ? C34 C35 1.501(5) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C38 1.395(5) . ? C35 C36 1.398(5) . ? C36 C38 1.394(5) 2_667 ? C36 C37 1.525(6) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C36 1.394(5) 2_667 ? C38 C39 1.508(5) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 O7 1.191(5) . ? C40 N1 1.316(6) . ? C40 H40A 0.9300 . ? C41 N1 1.422(8) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 N1 1.439(7) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 O8 1.236(5) . ? C43 N2 1.302(6) . ? C43 H43A 0.9300 . ? C44 N2 1.429(7) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 N2 1.443(6) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? O1 La 2.555(2) 2_777 ? O4 La 2.398(2) 1_566 ? O9 H9A 0.8500 . ? O9 H9B 0.8500 . ? 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 O4 La O8 98.51(10) 1_544 . ? O4 La O1 90.93(8) 1_544 2_777 ? O8 La O1 144.40(10) . 2_777 ? O4 La O9 72.53(8) 1_544 . ? O8 La O9 141.69(11) . . ? O1 La O9 73.86(8) 2_777 . ? O4 La O6 75.64(8) 1_544 . ? O8 La O6 69.96(9) . . ? O1 La O6 79.47(8) 2_777 . ? O9 La O6 137.61(8) . . ? O4 La O7 76.27(10) 1_544 . ? O8 La O7 69.37(12) . . ? O1 La O7 146.05(10) 2_777 . ? O9 La O7 72.32(10) . . ? O6 La O7 125.57(10) . . ? O4 La O2 150.97(9) 1_544 . ? O8 La O2 71.10(9) . . ? O1 La O2 113.51(7) 2_777 . ? O9 La O2 98.48(9) . . ? O6 La O2 122.41(8) . . ? O7 La O2 74.70(9) . . ? O4 La O5 124.89(8) 1_544 . ? O8 La O5 73.24(10) . . ? O1 La O5 73.24(8) 2_777 . ? O9 La O5 142.69(8) . . ? O6 La O5 49.95(7) . . ? O7 La O5 139.54(10) . . ? O2 La O5 79.13(8) . . ? O4 La O1 142.21(8) 1_544 . ? O8 La O1 117.59(9) . . ? O1 La O1 66.67(8) 2_777 . ? O9 La O1 72.15(7) . . ? O6 La O1 125.36(8) . . ? O7 La O1 105.05(10) . . ? O2 La O1 49.13(7) . . ? O5 La O1 79.03(7) . . ? O4 La C27 100.49(9) 1_544 . ? O8 La C27 67.96(11) . . ? O1 La C27 76.60(8) 2_777 . ? O9 La C27 149.43(9) . . ? O6 La C27 24.96(8) . . ? O7 La C27 136.17(10) . . ? O2 La C27 100.30(9) . . ? O5 La C27 25.10(8) . . ? O1 La C27 103.03(8) . . ? O4 La C1 157.38(9) 1_544 . ? O8 La C1 93.57(10) . . ? O1 La C1 90.27(8) 2_777 . ? O9 La C1 86.15(8) . . ? O6 La C1 126.71(8) . . ? O7 La C1 90.36(10) . . ? O2 La C1 24.07(8) . . ? O5 La C1 76.92(8) . . ? O1 La C1 25.10(7) . . ? C27 La C1 101.76(9) . . ? C7 S1 C8 101.97(17) . . ? C20 S2 C15 104.24(17) . . ? C33 S3 C34 103.14(19) . . ? O2 C1 O1 120.7(3) . . ? O2 C1 C2 119.9(3) . . ? O1 C1 C2 119.4(3) . . ? O2 C1 La 57.90(17) . . ? O1 C1 La 62.96(16) . . ? C2 C1 La 177.1(2) . . ? N01 C01 O01 134(2) . . ? N01 C01 H01A 112.8 . . ? O01 C01 H01A 112.8 . . ? C3 C2 C7 119.6(3) . . ? C3 C2 C1 119.0(3) . . ? C7 C2 C1 121.3(3) . . ? N01 C02 H02A 109.5 . . ? N01 C02 H02B 109.5 . . ? H02A C02 H02B 109.5 . . ? N01 C02 H02C 109.5 . . ? H02A C02 H02C 109.5 . . ? H02B C02 H02C 109.5 . . ? C4 C3 C2 121.6(3) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? N01 C03 H03A 109.5 . . ? N01 C03 H03B 109.5 . . ? H03A C03 H03B 109.5 . . ? N01 C03 H03C 109.5 . . ? H03A C03 H03C 109.5 . . ? H03B C03 H03C 109.5 . . ? C3 C4 C5 119.3(3) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C6 C5 C4 120.0(3) . . ? C6 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? C5 C6 C7 121.4(3) . . ? C5 C6 H6A 119.3 . . ? C7 C6 H6A 119.3 . . ? C6 C7 C2 118.1(3) . . ? C6 C7 S1 123.3(3) . . ? C2 C7 S1 118.6(2) . . ? C9 C8 S1 108.9(3) . . ? C9 C8 H8A 109.9 . . ? S1 C8 H8A 109.9 . . ? C9 C8 H8B 109.9 . . ? S1 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? C10 C9 C18 120.6(3) . . ? C10 C9 C8 119.4(3) . . ? C18 C9 C8 119.9(3) . . ? C9 C10 C12 120.2(3) . . ? C9 C10 C11 120.2(3) . . ? C12 C10 C11 119.6(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 C14 118.6(3) . . ? C10 C12 C13 120.5(4) . . ? C14 C12 C13 120.9(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C16 C14 C12 120.9(3) . . ? C16 C14 C15 120.1(3) . . ? C12 C14 C15 118.9(3) . . ? C14 C15 S2 104.4(2) . . ? C14 C15 H15A 110.9 . . ? S2 C15 H15A 110.9 . . ? C14 C15 H15B 110.9 . . ? S2 C15 H15B 110.9 . . ? H15A C15 H15B 108.9 . . ? C18 C16 C14 120.2(3) . . ? C18 C16 C17 120.2(4) . . ? C14 C16 C17 119.6(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 C9 119.5(4) . . ? C16 C18 C19 121.1(4) . . ? C9 C18 C19 119.3(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C25 118.6(3) . . ? C21 C20 S2 121.4(3) . . ? C25 C20 S2 120.0(2) . . ? C22 C21 C20 120.9(3) . . ? C22 C21 H21A 119.6 . . ? C20 C21 H21A 119.6 . . ? C23 C22 C21 120.6(4) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C22 C23 C24 119.0(3) . . ? C22 C23 H23A 120.5 . . ? C24 C23 H23A 120.5 . . ? C23 C24 C25 122.1(3) . . ? C23 C24 H24A 118.9 . . ? C25 C24 H24A 118.9 . . ? C24 C25 C20 118.8(3) . . ? C24 C25 C26 118.1(3) . . ? C20 C25 C26 123.1(3) . . ? O3 C26 O4 123.1(3) . . ? O3 C26 C25 119.8(3) . . ? O4 C26 C25 117.1(3) . . ? O6 C27 O5 121.8(3) . . ? O6 C27 C28 119.2(3) . . ? O5 C27 C28 119.0(3) . . ? O6 C27 La 60.41(17) . . ? O5 C27 La 61.83(18) . . ? C28 C27 La 173.1(2) . . ? C29 C28 C33 119.6(4) . . ? C29 C28 C27 117.5(3) . . ? C33 C28 C27 122.9(3) . . ? C30 C29 C28 121.2(5) . . ? C30 C29 H29A 119.4 . . ? C28 C29 H29A 119.4 . . ? C29 C30 C31 120.3(5) . . ? C29 C30 H30A 119.9 . . ? C31 C30 H30A 119.9 . . ? C30 C31 C32 120.1(5) . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C31 C32 C33 120.9(4) . . ? C31 C32 H32A 119.6 . . ? C33 C32 H32A 119.6 . . ? C32 C33 C28 117.9(4) . . ? C32 C33 S3 121.2(3) . . ? C28 C33 S3 120.9(3) . . ? C35 C34 S3 107.5(3) . . ? C35 C34 H34A 110.2 . . ? S3 C34 H34A 110.2 . . ? C35 C34 H34B 110.2 . . ? S3 C34 H34B 110.2 . . ? H34A C34 H34B 108.5 . . ? C38 C35 C36 120.4(3) . . ? C38 C35 C34 120.0(4) . . ? C36 C35 C34 119.5(4) . . ? C38 C36 C35 119.9(4) 2_667 . ? C38 C36 C37 118.7(4) 2_667 . ? C35 C36 C37 121.4(4) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 C35 119.6(3) 2_667 . ? C36 C38 C39 119.3(4) 2_667 . ? C35 C38 C39 121.0(4) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O7 C40 N1 126.2(5) . . ? O7 C40 H40A 116.9 . . ? N1 C40 H40A 116.9 . . ? N1 C41 H41A 109.5 . . ? N1 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N1 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N1 C42 H42A 109.5 . . ? N1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O8 C43 N2 126.1(5) . . ? O8 C43 H43A 116.9 . . ? N2 C43 H43A 116.9 . . ? N2 C44 H44A 109.5 . . ? N2 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N2 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N2 C45 H45A 109.5 . . ? N2 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N2 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C40 N1 C41 121.0(5) . . ? C40 N1 C42 124.9(5) . . ? C41 N1 C42 113.8(6) . . ? C01 N01 C03 132.1(17) . . ? C01 N01 C02 115.3(14) . . ? C03 N01 C02 110.9(12) . . ? C43 N2 C44 119.0(4) . . ? C43 N2 C45 122.3(5) . . ? C44 N2 C45 118.5(5) . . ? C1 O1 La 147.4(2) . 2_777 ? C1 O1 La 91.93(18) . . ? La O1 La 113.33(8) 2_777 . ? C1 O2 La 98.04(19) . . ? C26 O4 La 142.3(2) . 1_566 ? C27 O5 La 93.1(2) . . ? C27 O6 La 94.6(2) . . ? C40 O7 La 133.5(3) . . ? C43 O8 La 136.8(3) . . ? La O9 H9A 112.8 . . ? La O9 H9B 105.4 . . ? H9A O9 H9B 101.3 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.051 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.100 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.179 0.056 0.366 28.3 0.6 2 0.400 0.306 0.414 16.1 1.1 3 0.500 0.000 0.500 51.8 0.1 4 0.465 0.206 0.675 9.6 1.7 5 0.535 0.794 0.325 9.0 1.4 6 0.600 0.694 0.586 16.2 1.1 7 0.821 0.944 0.634 28.4 0.8 _platon_squeeze_details ; Disordered, independent solvent molecules were eliminated from the refinement using SQUEEZE/PLATON [Spek, A.L. (2003), J. Appl. Cryst. 36, 7-13]. ;