Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Peter Junk' _publ_contact_author_address ; School of Chemistry Monash University Clayton VIC 3800 AUSTRALIA ; _publ_contact_author_email PETER.JUNK@SCI.MONASH.EDU.AU _publ_section_title ; Structural Variations in Rare Earth-Benzoate Complexes: Part I - Lanthanum ; loop_ _publ_author_name 'Peter Junk' 'Hendrik Busskamp' 'G. Deacon' 'Matthias Hilder' 'Ulrich Kynast' 'Winnie Lee' 'David Turner' data_hb31dmso _database_code_depnum_ccdc_archive 'CCDC 634364' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (La(BA)3(DMSO))n _chemical_melting_point ? _chemical_formula_moiety 'C23 H21 La1 O7 S1' _chemical_formula_sum 'C23 H21 La1 O7 S1' _chemical_formula_weight 580.37 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' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 '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 8.8927(6) _cell_length_b 22.5574(15) _cell_length_c 22.7642(15) _cell_angle_alpha 90.00 _cell_angle_beta 95.590(2) _cell_angle_gamma 90.00 _cell_volume 4544.7(5) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 2.013 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6436 _exptl_absorpt_correction_T_max 0.7942 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _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 37102 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7960 _reflns_number_gt 7603 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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. Data shows signs of significant twinning (large Fo2 vs Fc2) resulting in large residual peaks in non-sensical positions. ; _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^)+(0.0001P)^2^+205.2310P] 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 7960 _refine_ls_number_parameters 597 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.1096 _refine_ls_R_factor_gt 0.1055 _refine_ls_wR_factor_ref 0.2228 _refine_ls_wR_factor_gt 0.2212 _refine_ls_goodness_of_fit_ref 1.437 _refine_ls_restrained_S_all 1.434 _refine_ls_shift/su_max 0.000 _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 0.25827(9) 0.49609(3) 0.97309(4) 0.0090(2) Uani 1 1 d . . . O1 O 0.0250(11) 0.4373(4) 0.9712(5) 0.016(2) Uani 1 1 d . . . C1 C -0.0223(17) 0.3983(6) 1.0056(7) 0.016(3) Uani 1 1 d . . . S1A S 0.0686(5) 0.53678(17) 0.82549(18) 0.0124(13) Uani 0.871(14) 1 d P A 1 S1B S 0.011(6) 0.477(2) 0.830(2) 0.060(16) Uani 0.129(14) 1 d PU A 2 La2 La 0.23640(9) 0.52581(3) 0.50371(3) 0.0090(2) Uani 1 1 d . . . S2 S 0.3712(5) 0.67656(17) 0.46799(17) 0.0189(8) Uani 1 1 d . . . O2 O -0.1052(12) 0.4112(4) 1.0458(5) 0.020(2) Uani 1 1 d . . . C2 C 0.0201(16) 0.3349(6) 0.9993(8) 0.017(3) Uani 1 1 d . . . O3 O 0.2942(12) 0.4193(4) 1.0512(4) 0.015(2) Uani 1 1 d . . . C3 C 0.096(2) 0.3175(9) 0.9515(8) 0.031(4) Uani 1 1 d . . . H3 H 0.1255 0.3454 0.9248 0.038 Uiso 1 1 calc R . . O4 O 0.5389(11) 0.4426(4) 1.0554(4) 0.014(2) Uani 1 1 d U . . C4 C 0.126(2) 0.2585(10) 0.9448(10) 0.047(6) Uani 1 1 d . . . H4 H 0.1733 0.2463 0.9121 0.056 Uiso 1 1 calc R . . O5 O 0.3348(11) 0.5576(4) 1.0599(4) 0.012(2) Uani 1 1 d U . . C5 C 0.090(2) 0.2174(9) 0.9842(10) 0.039(5) Uani 1 1 d U . . H5 H 0.1170 0.1779 0.9798 0.046 Uiso 1 1 calc R . . O6 O 0.5852(12) 0.5760(4) 1.0710(5) 0.017(2) Uani 1 1 d . . . C6 C 0.013(2) 0.2349(9) 1.0312(11) 0.048(6) Uani 1 1 d . . . H6 H -0.0176 0.2066 1.0573 0.057 Uiso 1 1 calc R . . O7 O 0.1668(12) 0.4973(5) 0.8673(5) 0.023(2) Uani 1 1 d . . . C7 C -0.020(2) 0.2932(7) 1.0394(9) 0.030(4) Uani 1 1 d . . . H7 H -0.0692 0.3048 1.0718 0.036 Uiso 1 1 calc R . . O8 O 0.5127(13) 0.4731(5) 0.4375(5) 0.025(3) Uani 1 1 d . . . C8 C 0.4276(15) 0.4091(6) 1.0666(6) 0.008(3) Uani 1 1 d U . . O9 O 0.3558(12) 0.5469(4) 0.4110(4) 0.017(2) Uani 1 1 d . . . C9 C 0.4706(16) 0.3556(6) 1.1040(6) 0.014(3) Uani 1 1 d . . . O10 O 0.2351(12) 0.4459(4) 0.5788(4) 0.017(2) Uani 1 1 d . . . C10 C 0.3546(18) 0.3183(7) 1.1201(8) 0.023(4) Uani 1 1 d . . . H10 H 0.2540 0.3281 1.1097 0.028 Uiso 1 1 calc R . . O11 O -0.0059(13) 0.4425(5) 0.5544(5) 0.020(2) Uani 1 1 d . . . C11 C 0.390(2) 0.2675(8) 1.1511(9) 0.035(5) Uani 1 1 d . . . H11 H 0.3127 0.2434 1.1620 0.042 Uiso 1 1 calc R . . O12 O 0.0874(12) 0.5691(5) 0.5770(5) 0.019(2) Uani 1 1 d . . . C12 C 0.536(2) 0.2515(7) 1.1664(7) 0.029(4) Uani 1 1 d . . . H12 H 0.5589 0.2168 1.1875 0.035 Uiso 1 1 calc R . . O13 O -0.1614(12) 0.5592(4) 0.5591(4) 0.016(2) Uani 1 1 d . . . C13 C 0.6508(19) 0.2874(7) 1.1502(7) 0.022(4) Uani 1 1 d . . . H13 H 0.7506 0.2761 1.1602 0.027 Uiso 1 1 calc R . . O14 O 0.2988(13) 0.6316(4) 0.5067(5) 0.022(3) Uani 1 1 d . . . C14 C 0.6215(18) 0.3399(6) 1.1194(7) 0.019(3) Uani 1 1 d . . . H14 H 0.6998 0.3639 1.1092 0.022 Uiso 1 1 calc R . . C15 C 0.4496(17) 0.5881(6) 1.0794(6) 0.014(3) Uani 1 1 d U . . C16 C 0.4214(17) 0.6436(6) 1.1136(6) 0.012(3) Uani 1 1 d . . . C17 C 0.2775(17) 0.6609(6) 1.1232(7) 0.017(3) Uani 1 1 d . . . H17 H 0.1954 0.6377 1.1090 0.020 Uiso 1 1 calc R . . C18 C 0.2543(19) 0.7124(7) 1.1536(7) 0.023(4) Uani 1 1 d . . . H18 H 0.1566 0.7241 1.1595 0.028 Uiso 1 1 calc R . . C19 C 0.374(2) 0.7461(7) 1.1750(7) 0.022(4) Uani 1 1 d . . . H19 H 0.3577 0.7809 1.1954 0.027 Uiso 1 1 calc R . . C20 C 0.521(2) 0.7287(6) 1.1664(7) 0.024(4) Uani 1 1 d . . . H20 H 0.6025 0.7516 1.1816 0.028 Uiso 1 1 calc R . . C21 C 0.5435(18) 0.6773(7) 1.1353(6) 0.017(3) Uani 1 1 d . . . H21 H 0.6410 0.6656 1.1292 0.021 Uiso 1 1 calc R . . C22A C 0.040(2) 0.4959(8) 0.7589(7) 0.030(4) Uani 0.871(14) 1 d P A 1 H22D H 0.1360 0.4883 0.7443 0.046 Uiso 0.871(14) 1 calc PR A 1 H22E H -0.0224 0.5183 0.7302 0.046 Uiso 0.871(14) 1 calc PR A 1 H22F H -0.0082 0.4589 0.7662 0.046 Uiso 0.871(14) 1 calc PR A 1 C22B C 0.040(2) 0.4959(8) 0.7589(7) 0.030(4) Uani 0.13 1 d P A 2 H22A H 0.1149 0.5267 0.7597 0.046 Uiso 0.129(14) 1 calc PR A 2 H22B H -0.0527 0.5099 0.7386 0.046 Uiso 0.129(14) 1 calc PR A 2 H22C H 0.0750 0.4619 0.7387 0.046 Uiso 0.129(14) 1 calc PR A 2 C23A C -0.1177(18) 0.5283(11) 0.8469(8) 0.041(10) Uani 0.871(14) 1 d P A 1 H23A H -0.1291 0.4892 0.8624 0.061 Uiso 0.871(14) 1 calc PR A 1 H23B H -0.1898 0.5340 0.8131 0.061 Uiso 0.871(14) 1 calc PR A 1 H23C H -0.1347 0.5572 0.8765 0.061 Uiso 0.871(14) 1 calc PR A 1 C23B C -0.1177(18) 0.5283(11) 0.8469(8) 0.04(5) Uani 0.129(14) 1 d P A 2 H23D H -0.0795 0.5491 0.8819 0.056 Uiso 0.129(14) 1 calc PR A 2 H23E H -0.2109 0.5090 0.8534 0.056 Uiso 0.129(14) 1 calc PR A 2 H23F H -0.1353 0.5559 0.8148 0.056 Uiso 0.129(14) 1 calc PR A 2 C24 C 0.4488(16) 0.5068(6) 0.3982(6) 0.016(3) Uani 1 1 d U . . C25 C 0.4801(15) 0.4997(7) 0.3355(6) 0.013(3) Uani 1 1 d . . . C26 C 0.5676(18) 0.4528(7) 0.3189(8) 0.021(3) Uani 1 1 d . . . H26 H 0.6112 0.4262 0.3468 0.026 Uiso 1 1 calc R . . C27 C 0.588(2) 0.4466(9) 0.2610(8) 0.033(5) Uani 1 1 d . . . H27 H 0.6444 0.4145 0.2498 0.040 Uiso 1 1 calc R . . C28 C 0.531(2) 0.4846(10) 0.2185(7) 0.037(5) Uani 1 1 d . . . H28 H 0.5501 0.4798 0.1794 0.044 Uiso 1 1 calc R . . C29 C 0.445(2) 0.5301(10) 0.2356(8) 0.037(5) Uani 1 1 d . . . H29 H 0.4033 0.5566 0.2071 0.044 Uiso 1 1 calc R . . C30 C 0.4160(17) 0.5385(7) 0.2936(7) 0.020(3) Uani 1 1 d . . . H30 H 0.3549 0.5694 0.3041 0.024 Uiso 1 1 calc R . . C31 C 0.1080(15) 0.4311(6) 0.5892(6) 0.009(3) Uani 1 1 d . . . C32 C 0.0896(16) 0.3949(6) 0.6436(6) 0.010(3) Uani 1 1 d U . . C33 C 0.2142(18) 0.3817(6) 0.6811(6) 0.015(3) Uani 1 1 d . . . H33 H 0.3090 0.3939 0.6718 0.018 Uiso 1 1 calc R . . C34 C 0.202(2) 0.3506(8) 0.7325(7) 0.028(4) Uani 1 1 d . . . H34 H 0.2879 0.3422 0.7579 0.033 Uiso 1 1 calc R . . C35 C 0.061(2) 0.3319(8) 0.7459(7) 0.029(4) Uani 1 1 d . . . H35 H 0.0519 0.3114 0.7807 0.035 Uiso 1 1 calc R . . C36 C -0.064(2) 0.3437(7) 0.7080(7) 0.024(4) Uani 1 1 d . . . H36 H -0.1576 0.3302 0.7170 0.029 Uiso 1 1 calc R . . C37 C -0.0532(18) 0.3753(7) 0.6566(7) 0.019(3) Uani 1 1 d . . . H37 H -0.1389 0.3834 0.6311 0.022 Uiso 1 1 calc R . . C38 C -0.0454(17) 0.5768(6) 0.5888(7) 0.015(3) Uani 1 1 d . . . C39 C -0.0682(18) 0.6129(6) 0.6445(7) 0.017(3) Uani 1 1 d . . . C40 C 0.0577(19) 0.6408(7) 0.6743(7) 0.022(3) Uani 1 1 d . . . H40 H 0.1513 0.6393 0.6594 0.026 Uiso 1 1 calc R . . C41 C 0.0405(19) 0.6707(7) 0.7266(7) 0.022(4) Uani 1 1 d . . . H41 H 0.1223 0.6901 0.7467 0.027 Uiso 1 1 calc R . . C42 C -0.100(2) 0.6713(8) 0.7486(7) 0.025(4) Uani 1 1 d . . . H42 H -0.1105 0.6899 0.7845 0.030 Uiso 1 1 calc R . . C43 C -0.2224(18) 0.6455(7) 0.7189(7) 0.021(3) Uani 1 1 d . . . H43 H -0.3159 0.6472 0.7339 0.025 Uiso 1 1 calc R . . C44 C -0.2077(19) 0.6162(6) 0.6657(8) 0.021(3) Uani 1 1 d . . . H44 H -0.2917 0.5991 0.6447 0.025 Uiso 1 1 calc R . . C45 C 0.562(2) 0.6557(9) 0.4712(10) 0.042(5) Uani 1 1 d . . . H45A H 0.5713 0.6201 0.4487 0.064 Uiso 1 1 calc R . . H45B H 0.6004 0.6488 0.5115 0.064 Uiso 1 1 calc R . . H45C H 0.6193 0.6869 0.4551 0.064 Uiso 1 1 calc R . . C46 C 0.393(2) 0.7399(8) 0.5114(8) 0.035(5) Uani 1 1 d . . . H46A H 0.2967 0.7580 0.5141 0.053 Uiso 1 1 calc R . . H46B H 0.4588 0.7672 0.4940 0.053 Uiso 1 1 calc R . . H46C H 0.4371 0.7293 0.5503 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0097(4) 0.0039(4) 0.0133(4) 0.0004(3) 0.0006(3) -0.0006(3) O1 0.011(5) 0.009(5) 0.028(6) 0.005(4) -0.006(4) -0.005(4) C1 0.016(8) 0.013(7) 0.018(8) -0.008(6) -0.001(6) -0.004(6) S1A 0.015(2) 0.007(2) 0.015(2) -0.0002(15) -0.0024(16) 0.0029(15) S1B 0.062(17) 0.059(17) 0.060(17) -0.001(7) 0.006(7) 0.001(7) La2 0.0084(4) 0.0100(4) 0.0085(4) 0.0005(3) 0.0001(3) -0.0014(3) S2 0.024(2) 0.0141(18) 0.0180(19) -0.0003(15) -0.0004(16) -0.0057(15) O2 0.018(6) 0.003(5) 0.038(7) -0.003(4) 0.003(5) 0.002(4) C2 0.002(7) 0.011(7) 0.037(9) -0.002(7) -0.007(6) 0.001(5) O3 0.019(6) 0.009(5) 0.017(5) -0.002(4) -0.001(4) 0.000(4) C3 0.023(9) 0.038(11) 0.032(10) -0.013(8) -0.003(8) 0.004(8) O4 0.018(4) 0.004(4) 0.020(4) 0.002(3) -0.004(4) -0.003(3) C4 0.035(12) 0.051(13) 0.052(14) -0.031(11) -0.006(10) 0.025(10) O5 0.011(5) 0.006(4) 0.020(5) -0.005(4) 0.005(4) -0.006(4) C5 0.035(8) 0.023(7) 0.054(9) -0.009(7) -0.013(7) 0.015(6) O6 0.015(6) 0.016(5) 0.019(6) -0.007(4) -0.003(4) 0.002(4) C6 0.036(12) 0.023(10) 0.080(17) 0.024(10) -0.013(11) -0.012(9) O7 0.026(6) 0.025(6) 0.017(6) 0.002(5) 0.001(5) 0.017(5) C7 0.025(9) 0.017(9) 0.048(12) 0.008(8) 0.004(8) 0.003(7) O8 0.028(6) 0.026(6) 0.020(6) 0.008(5) -0.006(5) -0.007(5) C8 0.010(5) 0.003(5) 0.011(5) 0.002(4) 0.001(4) -0.001(4) O9 0.023(6) 0.013(5) 0.013(5) -0.005(4) -0.004(4) 0.005(4) C9 0.013(8) 0.016(8) 0.012(7) 0.007(6) 0.001(6) 0.002(6) O10 0.023(6) 0.015(5) 0.012(5) 0.004(4) 0.003(4) -0.007(4) C10 0.013(8) 0.021(8) 0.037(10) 0.014(7) 0.011(7) 0.006(6) O11 0.029(7) 0.015(5) 0.015(5) -0.001(4) -0.001(5) 0.007(5) C11 0.034(11) 0.036(11) 0.040(11) 0.023(9) 0.020(9) 0.008(8) O12 0.013(6) 0.025(6) 0.020(6) 0.002(5) -0.004(4) -0.004(4) C12 0.052(12) 0.013(8) 0.024(9) 0.013(7) 0.010(8) 0.017(8) O13 0.024(6) 0.012(5) 0.013(5) -0.006(4) -0.003(4) -0.005(4) C13 0.027(9) 0.018(8) 0.020(8) -0.001(7) -0.007(7) 0.017(7) O14 0.036(7) 0.005(5) 0.026(6) 0.000(4) 0.015(5) -0.008(4) C14 0.022(9) 0.011(7) 0.023(8) -0.003(6) 0.006(7) 0.001(6) C15 0.018(6) 0.017(6) 0.007(6) 0.008(5) -0.001(5) 0.008(5) C16 0.017(8) 0.006(7) 0.012(7) 0.003(5) 0.003(6) 0.003(6) C17 0.015(8) 0.013(7) 0.023(8) -0.005(6) 0.003(6) -0.005(6) C18 0.023(9) 0.021(8) 0.024(9) -0.004(7) 0.003(7) 0.012(7) C19 0.039(10) 0.007(7) 0.020(8) -0.006(6) -0.001(7) 0.008(7) C20 0.034(10) 0.005(7) 0.028(9) -0.008(6) -0.015(8) 0.005(6) C21 0.020(8) 0.018(8) 0.012(7) 0.003(6) -0.005(6) 0.009(6) C22A 0.040(11) 0.027(9) 0.025(9) -0.005(8) 0.003(8) -0.005(8) C22B 0.040(11) 0.027(9) 0.025(9) -0.005(8) 0.003(8) -0.005(8) C23A 0.008(16) 0.09(2) 0.029(14) 0.04(3) 0.01(3) 0.02(3) C23B 0.04(12) 0.04(5) 0.04(5) 0.00(17) 0.0(2) 0.00(19) C24 0.015(6) 0.014(6) 0.018(6) -0.002(5) 0.002(5) -0.013(5) C25 0.009(7) 0.019(7) 0.010(7) 0.001(6) -0.008(5) -0.005(6) C26 0.020(8) 0.013(8) 0.033(9) -0.005(7) 0.007(7) -0.004(6) C27 0.019(9) 0.054(12) 0.026(10) -0.023(9) 0.003(7) -0.001(8) C28 0.028(10) 0.069(15) 0.012(8) -0.013(9) 0.000(7) -0.019(10) C29 0.026(10) 0.066(14) 0.017(9) 0.009(9) -0.007(7) -0.002(9) C30 0.014(8) 0.026(9) 0.020(8) -0.003(7) -0.003(6) -0.009(6) C31 0.006(7) 0.008(7) 0.013(7) -0.007(5) -0.007(6) 0.003(5) C32 0.017(6) 0.004(5) 0.010(6) -0.002(5) 0.001(5) 0.000(5) C33 0.020(8) 0.009(7) 0.017(8) -0.004(6) 0.003(6) -0.007(6) C34 0.034(10) 0.029(10) 0.019(9) 0.010(7) 0.002(8) 0.015(8) C35 0.050(12) 0.024(9) 0.014(8) 0.002(7) 0.004(8) 0.001(8) C36 0.027(9) 0.019(8) 0.030(9) 0.003(7) 0.014(8) -0.007(7) C37 0.016(8) 0.017(8) 0.023(8) -0.005(6) 0.000(6) 0.001(6) C38 0.017(8) 0.011(7) 0.017(8) 0.001(6) 0.006(6) -0.001(6) C39 0.023(8) 0.007(7) 0.020(8) 0.001(6) 0.001(7) -0.001(6) C40 0.025(9) 0.016(8) 0.025(9) 0.003(7) 0.007(7) 0.002(7) C41 0.019(9) 0.026(9) 0.020(8) -0.005(7) -0.007(7) -0.004(7) C42 0.033(10) 0.031(9) 0.011(8) -0.002(7) -0.001(7) 0.002(8) C43 0.021(9) 0.017(8) 0.027(9) 0.003(7) 0.012(7) 0.006(6) C44 0.024(9) 0.004(7) 0.036(10) 0.004(6) 0.006(7) -0.001(6) C45 0.021(10) 0.036(11) 0.070(15) -0.005(10) 0.008(10) -0.008(8) C46 0.057(13) 0.021(9) 0.025(10) -0.014(7) -0.012(9) -0.007(9) _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 O4 2.412(10) 3_667 ? La1 O6 2.420(10) 3_667 ? La1 O5 2.456(9) . ? La1 O1 2.459(10) . ? La1 O7 2.466(10) . ? La1 O3 2.481(10) . ? La1 O2 2.509(10) 3_567 ? O1 C1 1.276(18) . ? C1 O2 1.265(18) . ? C1 C2 1.49(2) . ? S1A O7 1.517(11) . ? S1A C22A 1.771(17) . ? S1A C23A 1.782(17) . ? S1B O7 1.62(5) . ? La2 O12 2.435(11) . ? La2 O11 2.435(11) 3_566 ? La2 O13 2.446(9) 3_566 ? La2 O14 2.450(10) . ? La2 O10 2.484(10) . ? La2 O8 2.488(11) 3_666 ? La2 O9 2.498(10) . ? S2 O14 1.526(10) . ? S2 C46 1.737(16) . ? S2 C45 1.757(19) . ? O2 La1 2.509(10) 3_567 ? C2 C7 1.38(2) . ? C2 C3 1.39(2) . ? O3 C8 1.225(17) . ? C3 C4 1.37(3) . ? C3 H3 0.9300 . ? O4 C8 1.290(17) . ? O4 La1 2.412(10) 3_667 ? C4 C5 1.35(3) . ? C4 H4 0.9300 . ? O5 C15 1.275(18) . ? C5 C6 1.39(3) . ? C5 H5 0.9300 . ? O6 C15 1.269(18) . ? O6 La1 2.420(10) 3_667 ? C6 C7 1.36(3) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? O8 C24 1.263(19) . ? O8 La2 2.488(11) 3_666 ? C8 C9 1.506(18) . ? O9 C24 1.278(18) . ? C9 C14 1.40(2) . ? C9 C10 1.41(2) . ? O10 C31 1.223(17) . ? C10 C11 1.36(2) . ? C10 H10 0.9300 . ? O11 C31 1.250(17) . ? O11 La2 2.435(11) 3_566 ? C11 C12 1.36(3) . ? C11 H11 0.9300 . ? O12 C38 1.248(18) . ? C12 C13 1.38(3) . ? C12 H12 0.9300 . ? O13 C38 1.242(18) . ? O13 La2 2.446(9) 3_566 ? C13 C14 1.39(2) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.51(2) . ? C16 C17 1.38(2) . ? C16 C21 1.38(2) . ? C17 C18 1.38(2) . ? C17 H17 0.9300 . ? C18 C19 1.36(2) . ? C18 H18 0.9300 . ? C19 C20 1.39(2) . ? C19 H19 0.9300 . ? C20 C21 1.38(2) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22A H22D 0.9600 . ? C22A H22E 0.9600 . ? C22A H22F 0.9600 . ? C23A H23A 0.9600 . ? C23A H23B 0.9600 . ? C23A H23C 0.9600 . ? C24 C25 1.49(2) . ? C25 C30 1.38(2) . ? C25 C26 1.39(2) . ? C26 C27 1.35(2) . ? C26 H26 0.9300 . ? C27 C28 1.35(3) . ? C27 H27 0.9300 . ? C28 C29 1.36(3) . ? C28 H28 0.9300 . ? C29 C30 1.38(2) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.506(19) . ? C32 C33 1.37(2) . ? C32 C37 1.40(2) . ? C33 C34 1.38(2) . ? C33 H33 0.9300 . ? C34 C35 1.38(3) . ? C34 H34 0.9300 . ? C35 C36 1.37(3) . ? C35 H35 0.9300 . ? C36 C37 1.38(2) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C39 1.54(2) . ? C39 C44 1.38(2) . ? C39 C40 1.40(2) . ? C40 C41 1.39(2) . ? C40 H40 0.9300 . ? C41 C42 1.39(2) . ? C41 H41 0.9300 . ? C42 C43 1.36(2) . ? C42 H42 0.9300 . ? C43 C44 1.40(2) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 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 O4 La1 O6 78.3(3) 3_667 3_667 ? O4 La1 O5 74.8(3) 3_667 . ? O6 La1 O5 126.0(3) 3_667 . ? O4 La1 O1 163.0(3) 3_667 . ? O6 La1 O1 98.6(4) 3_667 . ? O5 La1 O1 119.0(3) . . ? O4 La1 O7 85.1(4) 3_667 . ? O6 La1 O7 75.5(3) 3_667 . ? O5 La1 O7 145.0(4) . . ? O1 La1 O7 78.0(4) . . ? O4 La1 O3 123.1(3) 3_667 . ? O6 La1 O3 77.9(3) 3_667 . ? O5 La1 O3 79.1(3) . . ? O1 La1 O3 71.7(3) . . ? O7 La1 O3 135.6(4) . . ? O4 La1 O2 83.3(3) 3_667 3_567 ? O6 La1 O2 144.3(4) 3_667 3_567 ? O5 La1 O2 76.7(3) . 3_567 ? O1 La1 O2 90.2(3) . 3_567 ? O7 La1 O2 72.6(4) . 3_567 ? O3 La1 O2 137.3(4) . 3_567 ? C1 O1 La1 133.5(9) . . ? O2 C1 O1 122.4(13) . . ? O2 C1 C2 117.5(13) . . ? O1 C1 C2 120.1(13) . . ? O7 S1A C22A 104.8(8) . . ? O7 S1A C23A 105.1(7) . . ? C22A S1A C23A 96.9(10) . . ? O12 La2 O11 76.6(3) . 3_566 ? O12 La2 O13 125.4(4) . 3_566 ? O11 La2 O13 75.3(3) 3_566 3_566 ? O12 La2 O14 74.2(4) . . ? O11 La2 O14 84.6(4) 3_566 . ? O13 La2 O14 145.9(4) 3_566 . ? O12 La2 O10 77.3(3) . . ? O11 La2 O10 121.7(4) 3_566 . ? O13 La2 O10 79.3(3) 3_566 . ? O14 La2 O10 134.7(4) . . ? O12 La2 O8 98.4(4) . 3_666 ? O11 La2 O8 162.3(4) 3_566 3_666 ? O13 La2 O8 120.1(4) 3_566 3_666 ? O14 La2 O8 77.7(4) . 3_666 ? O10 La2 O8 72.6(4) . 3_666 ? O12 La2 O9 143.8(3) . . ? O11 La2 O9 83.7(3) 3_566 . ? O13 La2 O9 76.7(3) 3_566 . ? O14 La2 O9 74.0(3) . . ? O10 La2 O9 138.6(3) . . ? O8 La2 O9 91.2(4) 3_666 . ? O14 S2 C46 104.4(8) . . ? O14 S2 C45 105.0(9) . . ? C46 S2 C45 98.1(10) . . ? C1 O2 La1 114.4(10) . 3_567 ? C7 C2 C3 120.1(16) . . ? C7 C2 C1 120.4(15) . . ? C3 C2 C1 119.5(15) . . ? C8 O3 La1 112.9(9) . . ? C4 C3 C2 118.5(19) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C8 O4 La1 175.7(9) . 3_667 ? C5 C4 C3 122(2) . . ? C5 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? C15 O5 La1 137.3(9) . . ? C4 C5 C6 119.1(17) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C15 O6 La1 143.2(10) . 3_667 ? C7 C6 C5 120.7(19) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? S1A O7 S1B 55.1(19) . . ? S1A O7 La1 137.2(6) . . ? S1B O7 La1 134(2) . . ? C6 C7 C2 119.5(19) . . ? C6 C7 H7 120.3 . . ? C2 C7 H7 120.3 . . ? C24 O8 La2 133.9(9) . 3_666 ? O3 C8 O4 125.0(12) . . ? O3 C8 C9 119.8(12) . . ? O4 C8 C9 115.1(12) . . ? C24 O9 La2 113.3(9) . . ? C14 C9 C10 119.5(14) . . ? C14 C9 C8 121.9(13) . . ? C10 C9 C8 118.4(13) . . ? C31 O10 La2 113.4(9) . . ? C11 C10 C9 119.8(16) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C31 O11 La2 172.4(9) . 3_566 ? C12 C11 C10 121.5(17) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C38 O12 La2 142.4(10) . . ? C11 C12 C13 119.1(15) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C38 O13 La2 137.2(10) . 3_566 ? C12 C13 C14 122.0(15) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? S2 O14 La2 137.6(6) . . ? C13 C14 C9 118.1(15) . . ? C13 C14 H14 121.0 . . ? C9 C14 H14 121.0 . . ? O6 C15 O5 124.8(13) . . ? O6 C15 C16 117.8(13) . . ? O5 C15 C16 117.4(13) . . ? C17 C16 C21 119.9(13) . . ? C17 C16 C15 121.5(13) . . ? C21 C16 C15 118.6(13) . . ? C16 C17 C18 120.4(14) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 120.1(15) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 120.2(14) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 119.6(15) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C16 C21 C20 119.7(15) . . ? C16 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? O8 C24 O9 121.4(14) . . ? O8 C24 C25 120.0(14) . . ? O9 C24 C25 118.6(13) . . ? C30 C25 C26 120.0(14) . . ? C30 C25 C24 119.6(14) . . ? C26 C25 C24 120.3(14) . . ? C27 C26 C25 118.4(16) . . ? C27 C26 H26 120.8 . . ? C25 C26 H26 120.8 . . ? C28 C27 C26 123.6(18) . . ? C28 C27 H27 118.2 . . ? C26 C27 H27 118.2 . . ? C27 C28 C29 117.2(16) . . ? C27 C28 H28 121.4 . . ? C29 C28 H28 121.4 . . ? C28 C29 C30 122.4(18) . . ? C28 C29 H29 118.8 . . ? C30 C29 H29 118.8 . . ? C25 C30 C29 118.3(16) . . ? C25 C30 H30 120.9 . . ? C29 C30 H30 120.9 . . ? O10 C31 O11 121.9(14) . . ? O10 C31 C32 118.9(12) . . ? O11 C31 C32 119.1(13) . . ? C33 C32 C37 119.7(13) . . ? C33 C32 C31 119.1(13) . . ? C37 C32 C31 121.2(13) . . ? C32 C33 C34 121.2(15) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C33 C34 C35 119.3(16) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C36 C35 C34 120.0(16) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 121.2(16) . . ? C35 C36 H36 119.4 . . ? C37 C36 H36 119.4 . . ? C36 C37 C32 118.6(15) . . ? C36 C37 H37 120.7 . . ? C32 C37 H37 120.7 . . ? O13 C38 O12 126.3(14) . . ? O13 C38 C39 116.7(13) . . ? O12 C38 C39 117.0(13) . . ? C44 C39 C40 120.7(15) . . ? C44 C39 C38 120.9(14) . . ? C40 C39 C38 118.3(14) . . ? C41 C40 C39 118.9(15) . . ? C41 C40 H40 120.5 . . ? C39 C40 H40 120.5 . . ? C40 C41 C42 119.4(15) . . ? C40 C41 H41 120.3 . . ? C42 C41 H41 120.3 . . ? C43 C42 C41 121.4(15) . . ? C43 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? C42 C43 C44 119.9(15) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C39 C44 C43 119.6(16) . . ? C39 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? S2 C45 H45A 109.5 . . ? S2 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? S2 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? S2 C46 H46A 109.5 . . ? S2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? S2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.489 _refine_diff_density_min -5.195 _refine_diff_density_rms 0.267 # Attachment '10.CIF' data_HB16DMF _database_code_depnum_ccdc_archive 'CCDC 634365' _audit_creation_method SHELXL-97 _chemical_name_systematic ; poly[tris(dimethylformamide)hexakis(3-nitrobenzoato)bis-lanthanum (III)] DMF/H2O solvate ; _chemical_name_common ; poly(tris(dimethylformamide)hexakis(3-nitrobenzoato)bis- lanthanum (iii)) DMF/H2O solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C51 H49 La2 N9 O27, C3 H7 N1 O1, H2 O1' _chemical_formula_sum 'C54 H58 La2 N10 O29' _chemical_formula_weight 1588.92 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' 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 13.5370(3) _cell_length_b 15.4019(4) _cell_length_c 17.2256(4) _cell_angle_alpha 69.5800(10) _cell_angle_beta 73.3540(10) _cell_angle_gamma 71.9100(10) _cell_volume 3134.80(13) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 1.442 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7145 _exptl_absorpt_correction_T_max 0.8021 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _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 56223 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14345 _reflns_number_gt 13168 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0195P)^2^+5.5414P] 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 14345 _refine_ls_number_parameters 888 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0671 _refine_ls_wR_factor_gt 0.0654 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _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 La1 La 0.514670(11) 0.626264(10) 0.320928(8) 0.01325(4) Uani 1 1 d . . . O1 O 0.36895(15) 0.74275(14) 0.39177(11) 0.0212(4) Uani 1 1 d . . . N1 N 0.7026(2) 0.4406(2) -0.07180(17) 0.0305(6) Uani 1 1 d . . . C1 C 0.3544(2) 0.81317(19) 0.32758(16) 0.0171(5) Uani 1 1 d . . . La2 La 0.534700(11) 0.870064(9) 0.113538(8) 0.01183(4) Uani 1 1 d . . . O2 O 0.41362(15) 0.81468(13) 0.25586(11) 0.0194(4) Uani 1 1 d . . . N2 N 0.8419(3) 0.6364(3) 0.50503(19) 0.0471(8) Uani 1 1 d . . . C2 C 0.2627(2) 0.89530(19) 0.33730(17) 0.0189(5) Uani 1 1 d . . . O3 O 0.0293(2) 1.1708(2) 0.2109(2) 0.0737(11) Uani 1 1 d . . . N3 N 0.0994(2) 1.0997(2) 0.2020(2) 0.0417(8) Uani 1 1 d . . . C3 C 0.2240(2) 0.95807(19) 0.26637(17) 0.0212(5) Uani 1 1 d . . . H3 H 0.2557 0.9500 0.2117 0.025 Uiso 1 1 calc R . . O4 O 0.1397(2) 1.08279(19) 0.13408(17) 0.0452(7) Uani 1 1 d . . . N4 N 0.4316(2) 0.94391(17) 0.47420(17) 0.0275(5) Uani 1 1 d . . . C4 C 0.1382(2) 1.0324(2) 0.2778(2) 0.0294(7) Uani 1 1 d . . . O5 O 0.57994(18) 0.53981(13) 0.20202(12) 0.0271(5) Uani 1 1 d . . . N5 N 0.1451(2) 1.40190(19) 0.1619(2) 0.0343(6) Uani 1 1 d . . . C5 C 0.0906(3) 1.0477(2) 0.3557(2) 0.0384(8) Uani 1 1 d . . . H5 H 0.0316 1.0998 0.3612 0.046 Uiso 1 1 calc R . . O6 O 0.53281(15) 0.69592(12) 0.15475(11) 0.0187(4) Uani 1 1 d . . . N6 N 0.06514(19) 1.07356(19) -0.16232(16) 0.0298(6) Uani 1 1 d . . . C6 C 0.1310(3) 0.9851(3) 0.4258(2) 0.0378(8) Uani 1 1 d . . . H6 H 0.1002 0.9944 0.4801 0.045 Uiso 1 1 calc R . . O7 O 0.75431(19) 0.37892(17) -0.02230(16) 0.0402(6) Uani 1 1 d . . . N7 N 0.2207(2) 0.7623(2) 0.73795(18) 0.0376(7) Uani 1 1 d . . . C7 C 0.2163(2) 0.9091(2) 0.41634(18) 0.0269(6) Uani 1 1 d . . . H7 H 0.2434 0.8660 0.4645 0.032 Uiso 1 1 calc R . . O8 O 0.7078(2) 0.4381(2) -0.14276(17) 0.0592(8) Uani 1 1 d . . . C8 C 0.5580(2) 0.61373(18) 0.14433(16) 0.0173(5) Uani 1 1 d . . . O9 O 0.62750(16) 0.73726(14) 0.27978(12) 0.0235(4) Uani 1 1 d . . . C9 C 0.5602(2) 0.60653(18) 0.05919(15) 0.0164(5) Uani 1 1 d . . . O10 O 0.62052(16) 0.89151(14) 0.21827(12) 0.0239(4) Uani 1 1 d . . . C10 C 0.6276(2) 0.52861(19) 0.03373(16) 0.0188(5) Uani 1 1 d . . . H10 H 0.6717 0.4805 0.0695 0.023 Uiso 1 1 calc R . . O11 O 0.8159(4) 0.5654(3) 0.5083(3) 0.0943(14) Uani 1 1 d . . . C11 C 0.6294(2) 0.52233(19) -0.04462(17) 0.0209(5) Uani 1 1 d . . . O12 O 0.8952(2) 0.6359(2) 0.55216(16) 0.0549(8) Uani 1 1 d . . . C12 C 0.5645(2) 0.5893(2) -0.09778(17) 0.0247(6) Uani 1 1 d . . . H12 H 0.5665 0.5828 -0.1511 0.030 Uiso 1 1 calc R . . O13 O 0.54825(15) 0.60560(13) 0.46139(11) 0.0201(4) Uani 1 1 d . . . C13 C 0.4966(2) 0.6660(2) -0.07106(17) 0.0237(6) Uani 1 1 d . . . H13 H 0.4507 0.7126 -0.1062 0.028 Uiso 1 1 calc R . . O14 O 0.54895(17) 0.51593(13) 0.59340(12) 0.0241(4) Uani 1 1 d . . . C14 C 0.4950(2) 0.67545(19) 0.00670(16) 0.0191(5) Uani 1 1 d . . . H14 H 0.4492 0.7291 0.0240 0.023 Uiso 1 1 calc R . . O15 O 0.4540(2) 0.94768(15) 0.39917(14) 0.0362(5) Uani 1 1 d . . . C15 C 0.6484(2) 0.8147(2) 0.27203(16) 0.0200(5) Uani 1 1 d . . . O16 O 0.38469(19) 1.01289(15) 0.50147(16) 0.0378(5) Uani 1 1 d . . . C16 C 0.7126(2) 0.8124(2) 0.33159(16) 0.0200(5) Uani 1 1 d . . . O17 O 0.42862(15) 1.02158(13) 0.13960(11) 0.0209(4) Uani 1 1 d . . . C17 C 0.7474(2) 0.7270(2) 0.38934(17) 0.0247(6) Uani 1 1 d . . . H17 H 0.7312 0.6701 0.3921 0.030 Uiso 1 1 calc R . . O18 O 0.41324(16) 1.15315(13) 0.02980(11) 0.0203(4) Uani 1 1 d . . . C18 C 0.8066(2) 0.7267(2) 0.44301(18) 0.0298(7) Uani 1 1 d . . . O19 O 0.0977(2) 1.4487(2) 0.2116(2) 0.0615(8) Uani 1 1 d . . . C19 C 0.8326(2) 0.8073(3) 0.4407(2) 0.0345(7) Uani 1 1 d . . . H19 H 0.8741 0.8045 0.4780 0.041 Uiso 1 1 calc R . . O20 O 0.1395(2) 1.43009(17) 0.08743(18) 0.0443(6) Uani 1 1 d . . . C20 C 0.7973(3) 0.8918(3) 0.3833(2) 0.0355(7) Uani 1 1 d . . . H20 H 0.8138 0.9484 0.3809 0.043 Uiso 1 1 calc R . . O21 O 0.36228(15) 0.87291(14) 0.08331(12) 0.0212(4) Uani 1 1 d . . . C21 C 0.7374(2) 0.8943(2) 0.32871(19) 0.0280(6) Uani 1 1 d . . . H21 H 0.7133 0.9529 0.2890 0.034 Uiso 1 1 calc R . . O22 O 0.37183(15) 1.00787(14) -0.01926(12) 0.0234(4) Uani 1 1 d . . . C22 C 0.5392(2) 0.59447(18) 0.53787(15) 0.0154(5) Uani 1 1 d . . . O23 O 0.07851(18) 1.15286(16) -0.17622(15) 0.0363(5) Uani 1 1 d . . . C23 C 0.5148(2) 0.68248(18) 0.56604(15) 0.0162(5) Uani 1 1 d . . . O24 O 0.0165(2) 1.05434(19) -0.20172(16) 0.0460(6) Uani 1 1 d . . . C24 C 0.4901(2) 0.77108(18) 0.50843(16) 0.0175(5) Uani 1 1 d . . . H24 H 0.4921 0.7764 0.4514 0.021 Uiso 1 1 calc R . . O25 O 0.69022(17) 0.50826(16) 0.34228(12) 0.0303(5) Uani 1 1 d . . . C25 C 0.4627(2) 0.85131(19) 0.53533(17) 0.0215(5) Uani 1 1 d . . . O26 O 0.34564(18) 0.63552(16) 0.28579(14) 0.0346(5) Uani 1 1 d . . . C26 C 0.4617(3) 0.8478(2) 0.61675(19) 0.0288(6) Uani 1 1 d . . . H26 H 0.4429 0.9043 0.6336 0.035 Uiso 1 1 calc R . . O27 O 0.72520(16) 0.77595(17) 0.09727(13) 0.0348(5) Uani 1 1 d . . . C27 C 0.4892(3) 0.7588(2) 0.67293(18) 0.0316(7) Uani 1 1 d . . . H27 H 0.4911 0.7541 0.7290 0.038 Uiso 1 1 calc R . . O28 O 0.1819(3) 0.8837(2) 0.6194(2) 0.0677(9) Uani 1 1 d . . . C28 C 0.5141(2) 0.6766(2) 0.64876(16) 0.0235(6) Uani 1 1 d . . . H28 H 0.5306 0.6160 0.6886 0.028 Uiso 1 1 calc R . . O29 O 0.6006(3) 1.0975(3) 0.1927(3) 0.0927(12) Uani 1 1 d . . . C29 C 0.3978(2) 1.10927(18) 0.10682(16) 0.0165(5) Uani 1 1 d . . . C30 C 0.3349(2) 1.16754(18) 0.16697(15) 0.0155(5) Uani 1 1 d . . . C31 C 0.2714(2) 1.25693(18) 0.13680(17) 0.0179(5) Uani 1 1 d . . . H31 H 0.2678 1.2823 0.0786 0.021 Uiso 1 1 calc R . . C32 C 0.2134(2) 1.3080(2) 0.19371(19) 0.0241(6) Uani 1 1 d . . . C33 C 0.2183(2) 1.2750(2) 0.2785(2) 0.0308(7) Uani 1 1 d . . . H33 H 0.1786 1.3125 0.3157 0.037 Uiso 1 1 calc R . . C34 C 0.2823(3) 1.1864(2) 0.30760(19) 0.0315(7) Uani 1 1 d . . . H34 H 0.2871 1.1622 0.3656 0.038 Uiso 1 1 calc R . . C35 C 0.3397(2) 1.1325(2) 0.25221(17) 0.0219(6) Uani 1 1 d . . . H35 H 0.3827 1.0711 0.2728 0.026 Uiso 1 1 calc R . . C36 C 0.3308(2) 0.93854(18) 0.02140(16) 0.0167(5) Uani 1 1 d . . . C37 C 0.2376(2) 0.93222(18) -0.00603(16) 0.0164(5) Uani 1 1 d . . . C38 C 0.1940(2) 1.00628(19) -0.06930(16) 0.0184(5) Uani 1 1 d . . . H38 H 0.2203 1.0624 -0.0946 0.022 Uiso 1 1 calc R . . C39 C 0.1110(2) 0.9961(2) -0.09446(17) 0.0208(5) Uani 1 1 d . . . C40 C 0.0692(2) 0.9167(2) -0.05907(19) 0.0261(6) Uani 1 1 d . . . H40 H 0.0120 0.9121 -0.0779 0.031 Uiso 1 1 calc R . . C41 C 0.1130(2) 0.8434(2) 0.00492(19) 0.0268(6) Uani 1 1 d . . . H41 H 0.0853 0.7881 0.0310 0.032 Uiso 1 1 calc R . . C42 C 0.1973(2) 0.85120(19) 0.03063(17) 0.0218(6) Uani 1 1 d . . . H42 H 0.2277 0.8006 0.0738 0.026 Uiso 1 1 calc R . . N43 N 0.1739(2) 0.64707(18) 0.29410(15) 0.0264(5) Uani 1 1 d . . . C43 C 0.7170(2) 0.4512(2) 0.40848(17) 0.0229(6) Uani 1 1 d . . . H43 H 0.6623 0.4357 0.4560 0.027 Uiso 1 1 calc R . . N44 N 0.8799(2) 0.67653(19) 0.06048(17) 0.0317(6) Uani 1 1 d . . . C44 C 0.9028(4) 0.4345(6) 0.3494(3) 0.121(3) Uani 1 1 d . . . H44A H 0.9697 0.3980 0.3677 0.182 Uiso 1 1 calc R . . H44B H 0.8991 0.5028 0.3342 0.182 Uiso 1 1 calc R . . H44C H 0.8992 0.4185 0.3001 0.182 Uiso 1 1 calc R . . C45 C 0.8422(3) 0.3449(3) 0.4959(2) 0.0376(8) Uani 1 1 d . . . H45A H 0.9196 0.3232 0.4887 0.056 Uiso 0.50 1 calc PR . . H45B H 0.8113 0.2900 0.5112 0.056 Uiso 0.50 1 calc PR . . H45C H 0.8145 0.3767 0.5407 0.056 Uiso 0.50 1 calc PR . . H45D H 0.7773 0.3367 0.5384 0.056 Uiso 0.50 1 calc PR . . H45E H 0.8856 0.3699 0.5158 0.056 Uiso 0.50 1 calc PR . . H45F H 0.8824 0.2833 0.4864 0.056 Uiso 0.50 1 calc PR . . N46 N 0.8146(2) 0.4112(2) 0.41752(16) 0.0386(7) Uani 1 1 d . . . C46 C 0.2695(2) 0.5997(2) 0.30219(18) 0.0282(6) Uani 1 1 d . . . H46 H 0.2821 0.5322 0.3223 0.034 Uiso 1 1 calc R . . C47 C 0.1475(4) 0.7499(3) 0.2669(3) 0.0572(11) Uani 1 1 d . . . H47A H 0.0722 0.7733 0.2642 0.086 Uiso 1 1 calc R . . H47B H 0.1904 0.7724 0.2108 0.086 Uiso 1 1 calc R . . H47C H 0.1622 0.7739 0.3072 0.086 Uiso 1 1 calc R . . H47D H 0.2110 0.7731 0.2573 0.086 Uiso 1 1 calc R . . H47E H 0.0927 0.7740 0.3107 0.086 Uiso 1 1 calc R . . H47F H 0.1210 0.7725 0.2143 0.086 Uiso 1 1 calc R . . C48 C 0.0889(3) 0.6018(3) 0.3102(3) 0.0529(10) Uani 1 1 d . . . H48A H 0.0237 0.6506 0.2999 0.079 Uiso 1 1 calc R . . H48B H 0.0782 0.5624 0.3691 0.079 Uiso 1 1 calc R . . H48C H 0.1070 0.5617 0.2725 0.079 Uiso 1 1 calc R . . H48D H 0.1156 0.5325 0.3277 0.079 Uiso 1 1 calc R . . H48E H 0.0611 0.6207 0.2586 0.079 Uiso 1 1 calc R . . H48F H 0.0322 0.6215 0.3552 0.079 Uiso 1 1 calc R . . C49 C 0.8089(2) 0.7579(2) 0.04878(18) 0.0246(6) Uani 1 1 d . . . H49 H 0.8240 0.8068 -0.0017 0.030 Uiso 1 1 calc R . . C50 C 0.8592(4) 0.5969(4) 0.1318(4) 0.135(4) Uani 1 1 d . . . H50A H 0.9207 0.5426 0.1307 0.202 Uiso 1 1 calc R . . H50B H 0.7967 0.5794 0.1294 0.202 Uiso 1 1 calc R . . H50C H 0.8462 0.6141 0.1841 0.202 Uiso 1 1 calc R . . C51 C 0.9781(3) 0.6590(3) 0.0004(2) 0.0391(8) Uani 1 1 d . . . H51A H 1.0192 0.5940 0.0215 0.059 Uiso 0.50 1 calc PR . . H51B H 1.0194 0.7046 -0.0071 0.059 Uiso 0.50 1 calc PR . . H51C H 0.9623 0.6666 -0.0540 0.059 Uiso 0.50 1 calc PR . . H51D H 0.9814 0.7161 -0.0479 0.059 Uiso 0.50 1 calc PR . . H51E H 0.9812 0.6055 -0.0193 0.059 Uiso 0.50 1 calc PR . . H51F H 1.0383 0.6435 0.0276 0.059 Uiso 0.50 1 calc PR . . C52A C 0.2014(6) 0.8559(6) 0.6951(5) 0.039(2) Uani 0.439(6) 1 d P A 1 H52A H 0.2020 0.9016 0.7204 0.047 Uiso 0.439(6) 1 calc PR A 1 C52B C 0.2144(5) 0.7918(5) 0.6549(4) 0.0378(16) Uani 0.561(6) 1 d P A 2 H52B H 0.2330 0.7473 0.6233 0.045 Uiso 0.561(6) 1 calc PR A 2 C53A C 0.2438(8) 0.7324(7) 0.8222(5) 0.047(2) Uani 0.439(6) 1 d P A 1 H53D H 0.1962 0.6923 0.8618 0.071 Uiso 0.439(6) 1 calc PR A 1 H53E H 0.2330 0.7887 0.8406 0.071 Uiso 0.439(6) 1 calc PR A 1 H53F H 0.3175 0.6960 0.8210 0.071 Uiso 0.439(6) 1 calc PR A 1 C53B C 0.2551(9) 0.6634(5) 0.7774(6) 0.078(3) Uani 0.561(6) 1 d P A 2 H53A H 0.3088 0.6536 0.8095 0.117 Uiso 0.561(6) 1 calc PR A 2 H53B H 0.2857 0.6295 0.7341 0.117 Uiso 0.561(6) 1 calc PR A 2 H53C H 0.1945 0.6389 0.8158 0.117 Uiso 0.561(6) 1 calc PR A 2 C54A C 0.2069(13) 0.6978(8) 0.7060(10) 0.096(5) Uani 0.439(6) 1 d P A 1 H54A H 0.1731 0.7319 0.6570 0.145 Uiso 0.439(6) 1 calc PR A 1 H54B H 0.1616 0.6581 0.7495 0.145 Uiso 0.439(6) 1 calc PR A 1 H54C H 0.2759 0.6573 0.6887 0.145 Uiso 0.439(6) 1 calc PR A 1 C54B C 0.2070(7) 0.8278(7) 0.7823(5) 0.070(3) Uani 0.561(6) 1 d P A 2 H54D H 0.1317 0.8471 0.8069 0.105 Uiso 0.561(6) 1 calc PR A 2 H54E H 0.2321 0.8840 0.7435 0.105 Uiso 0.561(6) 1 calc PR A 2 H54F H 0.2477 0.7979 0.8275 0.105 Uiso 0.561(6) 1 calc PR A 2 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 0.01755(7) 0.01104(7) 0.01056(7) 0.00151(5) -0.00677(5) -0.00414(5) O1 0.0196(9) 0.0225(10) 0.0139(8) 0.0004(7) -0.0043(7) -0.0001(8) N1 0.0280(14) 0.0351(15) 0.0341(14) -0.0214(12) 0.0048(11) -0.0120(12) C1 0.0155(12) 0.0201(13) 0.0169(12) -0.0033(10) -0.0059(10) -0.0055(10) La2 0.01302(7) 0.00898(7) 0.01153(7) -0.00017(5) -0.00355(5) -0.00201(5) O2 0.0204(9) 0.0198(9) 0.0145(8) -0.0033(7) -0.0011(7) -0.0040(8) N2 0.0456(18) 0.059(2) 0.0370(16) 0.0020(15) -0.0272(14) -0.0130(16) C2 0.0145(12) 0.0195(13) 0.0215(13) -0.0036(10) -0.0045(10) -0.0039(10) O3 0.0313(15) 0.0518(18) 0.085(2) 0.0228(16) -0.0088(15) 0.0119(13) N3 0.0180(13) 0.0329(16) 0.059(2) 0.0147(14) -0.0167(13) -0.0087(12) C3 0.0160(12) 0.0210(13) 0.0239(13) 0.0005(11) -0.0054(10) -0.0073(11) O4 0.0421(14) 0.0476(15) 0.0413(14) 0.0152(12) -0.0261(12) -0.0200(12) N4 0.0285(13) 0.0154(11) 0.0393(15) -0.0042(10) -0.0138(11) -0.0038(10) C4 0.0157(13) 0.0260(15) 0.0388(17) 0.0044(13) -0.0108(12) -0.0050(12) O5 0.0468(13) 0.0134(9) 0.0181(9) -0.0005(7) -0.0157(9) 0.0009(9) N5 0.0161(12) 0.0231(13) 0.0567(19) -0.0145(13) 0.0022(12) -0.0004(10) C5 0.0199(15) 0.0310(17) 0.055(2) -0.0125(15) -0.0040(14) 0.0044(13) O6 0.0308(10) 0.0104(8) 0.0155(8) -0.0010(7) -0.0084(8) -0.0051(8) N6 0.0188(12) 0.0321(14) 0.0303(13) -0.0001(11) -0.0101(10) -0.0002(11) C6 0.0251(16) 0.045(2) 0.0369(18) -0.0176(15) 0.0011(14) 0.0013(15) O7 0.0362(13) 0.0305(13) 0.0535(15) -0.0224(12) -0.0054(12) 0.0013(11) N7 0.0383(16) 0.0371(16) 0.0379(15) -0.0171(13) -0.0154(13) 0.0050(13) C7 0.0197(14) 0.0350(17) 0.0227(14) -0.0085(12) -0.0049(11) -0.0011(12) O8 0.0651(19) 0.075(2) 0.0416(15) -0.0434(15) 0.0001(13) -0.0017(16) C8 0.0211(13) 0.0161(12) 0.0153(12) -0.0029(10) -0.0086(10) -0.0024(10) O9 0.0267(10) 0.0263(10) 0.0216(9) -0.0017(8) -0.0093(8) -0.0135(9) C9 0.0229(13) 0.0136(12) 0.0144(11) -0.0011(9) -0.0053(10) -0.0083(10) O10 0.0265(10) 0.0252(10) 0.0200(9) 0.0007(8) -0.0104(8) -0.0088(9) C10 0.0213(13) 0.0157(12) 0.0201(12) -0.0032(10) -0.0055(10) -0.0061(10) O11 0.138(4) 0.062(2) 0.101(3) 0.033(2) -0.097(3) -0.045(2) C11 0.0235(14) 0.0208(13) 0.0221(13) -0.0094(11) 0.0001(11) -0.0105(11) O12 0.0462(16) 0.083(2) 0.0372(14) -0.0073(14) -0.0299(12) -0.0086(15) C12 0.0327(16) 0.0332(16) 0.0140(12) -0.0059(11) -0.0048(11) -0.0164(13) O13 0.0259(10) 0.0168(9) 0.0181(9) -0.0042(7) -0.0118(8) 0.0003(8) C13 0.0302(15) 0.0233(14) 0.0197(13) 0.0016(11) -0.0123(11) -0.0114(12) O14 0.0364(11) 0.0160(9) 0.0196(9) 0.0031(7) -0.0097(8) -0.0115(9) C14 0.0239(13) 0.0162(12) 0.0180(12) -0.0010(10) -0.0065(10) -0.0078(11) O15 0.0576(15) 0.0198(11) 0.0310(12) 0.0028(9) -0.0232(11) -0.0071(10) C15 0.0198(13) 0.0271(14) 0.0136(12) -0.0025(10) -0.0035(10) -0.0099(11) O16 0.0344(13) 0.0190(11) 0.0559(15) -0.0132(10) -0.0095(11) 0.0029(9) C16 0.0181(13) 0.0275(14) 0.0162(12) -0.0062(10) -0.0027(10) -0.0084(11) O17 0.0266(10) 0.0122(9) 0.0204(9) -0.0023(7) -0.0048(8) -0.0022(8) C17 0.0230(14) 0.0318(16) 0.0214(13) -0.0032(11) -0.0087(11) -0.0105(12) O18 0.0295(10) 0.0146(9) 0.0139(8) -0.0041(7) 0.0001(7) -0.0053(8) C18 0.0219(14) 0.0462(19) 0.0212(14) -0.0075(13) -0.0087(11) -0.0060(13) O19 0.0505(17) 0.0412(16) 0.076(2) -0.0336(15) 0.0070(15) 0.0140(13) C19 0.0247(15) 0.060(2) 0.0302(16) -0.0225(16) -0.0091(13) -0.0109(15) O20 0.0367(14) 0.0247(12) 0.0594(17) -0.0056(11) -0.0155(12) 0.0074(10) C20 0.0362(18) 0.0427(19) 0.0412(18) -0.0233(16) -0.0083(15) -0.0143(15) O21 0.0193(9) 0.0226(10) 0.0213(9) -0.0018(8) -0.0102(8) -0.0037(8) C21 0.0285(15) 0.0291(16) 0.0301(15) -0.0115(12) -0.0068(12) -0.0074(13) O22 0.0234(10) 0.0263(10) 0.0226(10) -0.0028(8) -0.0026(8) -0.0152(8) C22 0.0161(12) 0.0141(12) 0.0164(12) 0.0000(9) -0.0066(9) -0.0059(10) O23 0.0265(11) 0.0288(12) 0.0401(13) 0.0064(10) -0.0128(10) -0.0009(10) C23 0.0163(12) 0.0171(12) 0.0165(12) -0.0038(10) -0.0032(9) -0.0069(10) O24 0.0423(14) 0.0525(16) 0.0454(14) 0.0000(12) -0.0322(12) -0.0085(12) C24 0.0199(13) 0.0169(12) 0.0164(12) -0.0027(10) -0.0057(10) -0.0056(10) O25 0.0270(11) 0.0358(12) 0.0206(10) -0.0051(9) -0.0108(8) 0.0051(9) C25 0.0221(14) 0.0188(13) 0.0224(13) -0.0025(10) -0.0061(11) -0.0055(11) O26 0.0328(12) 0.0379(13) 0.0360(12) 0.0074(10) -0.0206(10) -0.0200(10) C26 0.0366(17) 0.0244(15) 0.0267(15) -0.0117(12) -0.0009(13) -0.0090(13) O27 0.0189(10) 0.0418(13) 0.0274(11) -0.0039(10) -0.0045(9) 0.0082(9) C27 0.049(2) 0.0326(17) 0.0157(13) -0.0078(12) -0.0040(13) -0.0142(15) O28 0.065(2) 0.068(2) 0.0567(19) 0.0027(16) -0.0256(16) -0.0089(17) C28 0.0329(16) 0.0229(14) 0.0140(12) -0.0003(10) -0.0059(11) -0.0100(12) O29 0.095(3) 0.091(3) 0.099(3) -0.037(2) -0.014(2) -0.023(2) C29 0.0163(12) 0.0156(12) 0.0181(12) -0.0044(10) -0.0046(10) -0.0040(10) C30 0.0150(12) 0.0155(12) 0.0156(11) -0.0032(9) -0.0034(9) -0.0040(10) C31 0.0142(12) 0.0166(12) 0.0219(13) -0.0038(10) -0.0034(10) -0.0045(10) C32 0.0150(13) 0.0199(13) 0.0362(16) -0.0101(12) -0.0001(11) -0.0047(11) C33 0.0269(15) 0.0350(17) 0.0332(16) -0.0221(14) 0.0054(13) -0.0075(13) C34 0.0353(17) 0.0417(18) 0.0193(14) -0.0117(13) -0.0015(12) -0.0117(15) C35 0.0255(14) 0.0204(13) 0.0183(13) -0.0037(10) -0.0059(11) -0.0043(11) C36 0.0151(12) 0.0181(12) 0.0177(12) -0.0059(10) -0.0023(10) -0.0048(10) C37 0.0153(12) 0.0170(12) 0.0177(12) -0.0046(10) -0.0043(10) -0.0043(10) C38 0.0162(12) 0.0166(12) 0.0207(12) -0.0032(10) -0.0042(10) -0.0034(10) C39 0.0161(13) 0.0218(13) 0.0215(13) -0.0038(11) -0.0074(10) 0.0002(11) C40 0.0194(14) 0.0317(16) 0.0321(15) -0.0092(12) -0.0099(12) -0.0081(12) C41 0.0260(15) 0.0236(14) 0.0343(16) -0.0031(12) -0.0109(12) -0.0122(12) C42 0.0226(14) 0.0176(13) 0.0246(13) -0.0004(11) -0.0090(11) -0.0063(11) N43 0.0251(13) 0.0298(13) 0.0253(12) -0.0006(10) -0.0130(10) -0.0088(11) C43 0.0216(14) 0.0239(14) 0.0210(13) -0.0065(11) -0.0062(11) -0.0005(11) N44 0.0193(12) 0.0267(13) 0.0348(14) -0.0003(11) -0.0046(11) 0.0038(10) C44 0.032(2) 0.214(8) 0.046(3) 0.060(4) -0.015(2) -0.036(3) C45 0.0266(16) 0.047(2) 0.0272(16) 0.0087(14) -0.0122(13) -0.0076(15) N46 0.0202(13) 0.0601(19) 0.0219(13) 0.0092(12) -0.0082(10) -0.0109(13) C46 0.0332(16) 0.0281(15) 0.0237(14) -0.0017(12) -0.0105(12) -0.0099(13) C47 0.050(2) 0.044(2) 0.072(3) -0.002(2) -0.035(2) 0.0003(19) C48 0.035(2) 0.069(3) 0.059(2) -0.013(2) -0.0140(18) -0.020(2) C49 0.0234(14) 0.0215(14) 0.0248(14) -0.0030(11) -0.0083(11) -0.0005(11) C50 0.062(3) 0.084(4) 0.113(5) 0.067(4) 0.023(3) 0.036(3) C51 0.0223(16) 0.0377(19) 0.055(2) -0.0209(16) -0.0012(15) -0.0009(14) C52A 0.028(4) 0.044(5) 0.037(4) -0.005(3) -0.009(3) -0.002(3) C52B 0.040(3) 0.040(4) 0.034(3) -0.014(3) -0.012(3) -0.001(3) C53A 0.048(5) 0.050(6) 0.034(4) -0.002(4) -0.010(4) -0.009(4) C53B 0.123(9) 0.035(4) 0.059(5) 0.001(4) -0.035(5) 0.004(5) C54A 0.143(13) 0.044(6) 0.133(13) -0.046(8) -0.079(11) 0.007(7) C54B 0.064(5) 0.115(8) 0.042(4) -0.054(5) -0.012(4) 0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O14 2.4297(18) 2_666 ? La1 O9 2.4318(19) . ? La1 O26 2.481(2) . ? La1 O13 2.4829(18) . ? La1 O25 2.537(2) . ? La1 O1 2.5592(19) . ? La1 O5 2.6239(19) . ? La1 O6 2.6502(17) . ? La1 O2 2.7735(18) . ? La1 C8 2.992(2) . ? La1 C1 3.036(3) . ? La1 La2 4.2015(2) . ? O1 C1 1.262(3) . ? N1 O7 1.218(4) . ? N1 O8 1.218(3) . ? N1 C11 1.468(4) . ? C1 O2 1.262(3) . ? C1 C2 1.491(4) . ? La2 O22 2.4377(18) 2_675 ? La2 O17 2.4475(18) . ? La2 O18 2.4867(17) 2_675 ? La2 O21 2.5175(18) . ? La2 O27 2.525(2) . ? La2 O6 2.5303(17) . ? La2 O2 2.5557(17) . ? La2 O10 2.5628(19) . ? N2 O12 1.228(4) . ? N2 O11 1.228(5) . ? N2 C18 1.466(4) . ? C2 C7 1.386(4) . ? C2 C3 1.389(4) . ? O3 N3 1.229(4) . ? N3 O4 1.221(4) . ? N3 C4 1.471(4) . ? C3 C4 1.378(4) . ? C3 H3 0.9500 . ? N4 O15 1.225(3) . ? N4 O16 1.229(3) . ? N4 C25 1.467(3) . ? C4 C5 1.380(5) . ? O5 C8 1.242(3) . ? N5 O20 1.220(4) . ? N5 O19 1.222(4) . ? N5 C32 1.468(4) . ? C5 C6 1.387(5) . ? C5 H5 0.9500 . ? O6 C8 1.267(3) . ? N6 O23 1.221(3) . ? N6 O24 1.224(4) . ? N6 C39 1.469(4) . ? C6 C7 1.385(4) . ? C6 H6 0.9500 . ? N7 C52A 1.351(9) . ? N7 C52B 1.362(6) . ? N7 C54A 1.372(11) . ? N7 C54B 1.406(8) . ? N7 C53B 1.420(8) . ? N7 C53A 1.456(9) . ? C7 H7 0.9500 . ? C8 C9 1.500(3) . ? O9 C15 1.264(3) . ? C9 C10 1.387(4) . ? C9 C14 1.389(4) . ? O10 C15 1.249(3) . ? C10 C11 1.379(4) . ? C10 H10 0.9500 . ? C11 C12 1.383(4) . ? C12 C13 1.384(4) . ? C12 H12 0.9500 . ? O13 C22 1.242(3) . ? C13 C14 1.390(4) . ? C13 H13 0.9500 . ? O14 C22 1.250(3) . ? O14 La1 2.4297(18) 2_666 ? C14 H14 0.9500 . ? C15 C16 1.508(4) . ? C16 C17 1.382(4) . ? C16 C21 1.385(4) . ? O17 C29 1.253(3) . ? C17 C18 1.384(4) . ? C17 H17 0.9500 . ? O18 C29 1.250(3) . ? O18 La2 2.4867(17) 2_675 ? C18 C19 1.377(5) . ? C19 C20 1.372(5) . ? C19 H19 0.9500 . ? C20 C21 1.392(4) . ? C20 H20 0.9500 . ? O21 C36 1.258(3) . ? C21 H21 0.9500 . ? O22 C36 1.250(3) . ? O22 La2 2.4377(18) 2_675 ? C22 C23 1.507(4) . ? C23 C24 1.386(3) . ? C23 C28 1.393(4) . ? C24 C25 1.377(4) . ? C24 H24 0.9500 . ? O25 C43 1.242(3) . ? C25 C26 1.381(4) . ? O26 C46 1.235(4) . ? C26 C27 1.385(4) . ? C26 H26 0.9500 . ? O27 C49 1.218(4) . ? C27 C28 1.383(4) . ? C27 H27 0.9500 . ? O28 C52A 1.301(8) . ? O28 C52B 1.317(7) . ? C28 H28 0.9500 . ? C29 C30 1.508(4) . ? C30 C31 1.388(4) . ? C30 C35 1.390(4) . ? C31 C32 1.381(4) . ? C31 H31 0.9500 . ? C32 C33 1.383(4) . ? C33 C34 1.378(5) . ? C33 H33 0.9500 . ? C34 C35 1.390(4) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.507(3) . ? C37 C38 1.386(4) . ? C37 C42 1.390(4) . ? C38 C39 1.382(4) . ? C38 H38 0.9500 . ? C39 C40 1.379(4) . ? C40 C41 1.390(4) . ? C40 H40 0.9500 . ? C41 C42 1.387(4) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? N43 C46 1.293(4) . ? N43 C48 1.437(4) . ? N43 C47 1.443(5) . ? C43 N46 1.302(4) . ? C43 H43 0.9500 . ? N44 C49 1.313(4) . ? N44 C50 1.435(5) . ? N44 C51 1.448(4) . ? C44 N46 1.450(5) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 N46 1.447(4) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C45 H45D 0.9800 . ? C45 H45E 0.9800 . ? C45 H45F 0.9800 . ? C46 H46 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C47 H47D 0.9800 . ? C47 H47E 0.9800 . ? C47 H47F 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C48 H48D 0.9800 . ? C48 H48E 0.9800 . ? C48 H48F 0.9800 . ? C49 H49 0.9500 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C51 H51D 0.9800 . ? C51 H51E 0.9800 . ? C51 H51F 0.9800 . ? C52A H52A 0.9500 . ? C52B H52B 0.9500 . ? C53A H53D 0.9800 . ? C53A H53E 0.9800 . ? C53A H53F 0.9800 . ? C53B H53A 0.9800 . ? C53B H53B 0.9800 . ? C53B H53C 0.9800 . ? C54A H54A 0.9800 . ? C54A H54B 0.9800 . ? C54A H54C 0.9800 . ? C54B H54D 0.9800 . ? C54B H54E 0.9800 . ? C54B H54F 0.9800 . ? 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 O14 La1 O9 155.09(7) 2_666 . ? O14 La1 O26 70.61(7) 2_666 . ? O9 La1 O26 133.68(7) . . ? O14 La1 O13 78.19(6) 2_666 . ? O9 La1 O13 80.33(6) . . ? O26 La1 O13 127.87(7) . . ? O14 La1 O25 80.26(7) 2_666 . ? O9 La1 O25 80.59(7) . . ? O26 La1 O25 139.33(8) . . ? O13 La1 O25 69.78(6) . . ? O14 La1 O1 96.57(6) 2_666 . ? O9 La1 O1 88.05(7) . . ? O26 La1 O1 72.65(7) . . ? O13 La1 O1 70.67(6) . . ? O25 La1 O1 140.12(6) . . ? O14 La1 O5 84.18(6) 2_666 . ? O9 La1 O5 104.58(7) . . ? O26 La1 O5 77.74(8) . . ? O13 La1 O5 139.53(6) . . ? O25 La1 O5 71.50(7) . . ? O1 La1 O5 148.18(6) . . ? O14 La1 O6 124.96(6) 2_666 . ? O9 La1 O6 75.61(6) . . ? O26 La1 O6 71.95(7) . . ? O13 La1 O6 155.92(6) . . ? O25 La1 O6 104.96(6) . . ? O1 La1 O6 108.97(6) . . ? O5 La1 O6 49.25(5) . . ? O14 La1 O2 133.38(6) 2_666 . ? O9 La1 O2 66.24(6) . . ? O26 La1 O2 69.56(7) . . ? O13 La1 O2 108.92(6) . . ? O25 La1 O2 146.20(6) . . ? O1 La1 O2 48.68(5) . . ? O5 La1 O2 109.67(5) . . ? O6 La1 O2 61.78(5) . . ? O14 La1 C8 103.49(7) 2_666 . ? O9 La1 C8 92.16(7) . . ? O26 La1 C8 71.00(8) . . ? O13 La1 C8 158.92(7) . . ? O25 La1 C8 89.64(7) . . ? O1 La1 C8 129.14(6) . . ? O5 La1 C8 24.43(6) . . ? O6 La1 C8 25.03(6) . . ? O2 La1 C8 85.46(6) . . ? O14 La1 C1 114.95(7) 2_666 . ? O9 La1 C1 77.59(7) . . ? O26 La1 C1 67.65(7) . . ? O13 La1 C1 90.58(6) . . ? O25 La1 C1 152.80(7) . . ? O1 La1 C1 24.20(6) . . ? O5 La1 C1 129.87(6) . . ? O6 La1 C1 85.16(6) . . ? O2 La1 C1 24.57(6) . . ? C8 La1 C1 107.13(7) . . ? O14 La1 La2 155.09(5) 2_666 . ? O9 La1 La2 49.67(4) . . ? O26 La1 La2 85.90(5) . . ? O13 La1 La2 124.60(4) . . ? O25 La1 La2 115.16(5) . . ? O1 La1 La2 83.76(4) . . ? O5 La1 La2 82.77(4) . . ? O6 La1 La2 34.86(4) . . ? O2 La1 La2 36.17(4) . . ? C8 La1 La2 59.46(5) . . ? C1 La1 La2 60.32(5) . . ? C1 O1 La1 99.56(15) . . ? O7 N1 O8 123.6(3) . . ? O7 N1 C11 118.5(2) . . ? O8 N1 C11 117.9(3) . . ? O1 C1 O2 121.9(2) . . ? O1 C1 C2 118.4(2) . . ? O2 C1 C2 119.7(2) . . ? O1 C1 La1 56.23(13) . . ? O2 C1 La1 66.00(14) . . ? C2 C1 La1 170.67(17) . . ? O22 La2 O17 73.22(6) 2_675 . ? O22 La2 O18 72.13(6) 2_675 2_675 ? O17 La2 O18 122.22(6) . 2_675 ? O22 La2 O21 117.56(6) 2_675 . ? O17 La2 O21 80.60(6) . . ? O18 La2 O21 76.45(6) 2_675 . ? O22 La2 O27 78.14(7) 2_675 . ? O17 La2 O27 139.57(8) . . ? O18 La2 O27 73.08(7) 2_675 . ? O21 La2 O27 138.88(7) . . ? O22 La2 O6 144.83(6) 2_675 . ? O17 La2 O6 141.76(6) . . ? O18 La2 O6 80.97(6) 2_675 . ? O21 La2 O6 75.98(6) . . ? O27 La2 O6 72.55(7) . . ? O22 La2 O2 146.72(6) 2_675 . ? O17 La2 O2 78.01(6) . . ? O18 La2 O2 139.40(6) 2_675 . ? O21 La2 O2 72.77(6) . . ? O27 La2 O2 116.07(6) . . ? O6 La2 O2 66.44(6) . . ? O22 La2 O10 80.06(6) 2_675 . ? O17 La2 O10 75.84(6) . . ? O18 La2 O10 138.56(6) 2_675 . ? O21 La2 O10 144.80(6) . . ? O27 La2 O10 71.55(7) . . ? O6 La2 O10 107.86(6) . . ? O2 La2 O10 76.98(6) . . ? O22 La2 La1 150.86(5) 2_675 . ? O17 La2 La1 115.80(4) . . ? O18 La2 La1 117.10(4) 2_675 . ? O21 La2 La1 91.55(4) . . ? O27 La2 La1 78.70(5) . . ? O6 La2 La1 36.77(4) . . ? O2 La2 La1 39.83(4) . . ? O10 La2 La1 76.00(4) . . ? C1 O2 La2 161.32(17) . . ? C1 O2 La1 89.43(15) . . ? La2 O2 La1 104.00(6) . . ? O12 N2 O11 123.2(3) . . ? O12 N2 C18 118.0(3) . . ? O11 N2 C18 118.8(3) . . ? C7 C2 C3 120.2(3) . . ? C7 C2 C1 120.4(2) . . ? C3 C2 C1 119.4(2) . . ? O4 N3 O3 124.0(3) . . ? O4 N3 C4 118.5(3) . . ? O3 N3 C4 117.6(3) . . ? C4 C3 C2 117.9(3) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? O15 N4 O16 124.1(3) . . ? O15 N4 C25 118.0(2) . . ? O16 N4 C25 118.0(3) . . ? C3 C4 C5 123.0(3) . . ? C3 C4 N3 117.4(3) . . ? C5 C4 N3 119.5(3) . . ? C8 O5 La1 94.63(16) . . ? O20 N5 O19 123.2(3) . . ? O20 N5 C32 118.8(3) . . ? O19 N5 C32 118.0(3) . . ? C4 C5 C6 118.4(3) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? C8 O6 La2 155.16(17) . . ? C8 O6 La1 92.75(14) . . ? La2 O6 La1 108.37(6) . . ? O23 N6 O24 124.1(3) . . ? O23 N6 C39 118.0(3) . . ? O24 N6 C39 117.9(3) . . ? C7 C6 C5 119.8(3) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C52A N7 C52B 59.1(5) . . ? C52A N7 C54A 119.8(7) . . ? C52B N7 C54A 62.9(7) . . ? C52A N7 C54B 62.4(5) . . ? C52B N7 C54B 121.4(5) . . ? C54A N7 C54B 164.7(9) . . ? C52A N7 C53B 172.5(6) . . ? C52B N7 C53B 118.9(5) . . ? C54A N7 C53B 61.0(7) . . ? C54B N7 C53B 119.1(6) . . ? C52A N7 C53A 119.4(6) . . ? C52B N7 C53A 171.4(5) . . ? C54A N7 C53A 120.4(8) . . ? C54B N7 C53A 57.8(5) . . ? C53B N7 C53A 61.3(5) . . ? C6 C7 C2 120.7(3) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? O5 C8 O6 122.3(2) . . ? O5 C8 C9 119.4(2) . . ? O6 C8 C9 118.3(2) . . ? O5 C8 La1 60.94(14) . . ? O6 C8 La1 62.22(13) . . ? C9 C8 La1 170.13(18) . . ? C15 O9 La1 155.28(19) . . ? C10 C9 C14 120.0(2) . . ? C10 C9 C8 118.9(2) . . ? C14 C9 C8 121.1(2) . . ? C15 O10 La2 111.95(17) . . ? C11 C10 C9 118.7(3) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C10 C11 C12 122.6(3) . . ? C10 C11 N1 118.3(3) . . ? C12 C11 N1 119.1(2) . . ? C11 C12 C13 118.1(2) . . ? C11 C12 H12 121.0 . . ? C13 C12 H12 121.0 . . ? C22 O13 La1 164.34(17) . . ? C12 C13 C14 120.6(3) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C22 O14 La1 150.66(18) . 2_666 ? C9 C14 C13 120.0(3) . . ? C9 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? O10 C15 O9 124.4(2) . . ? O10 C15 C16 118.7(2) . . ? O9 C15 C16 117.0(2) . . ? C17 C16 C21 119.8(3) . . ? C17 C16 C15 119.3(2) . . ? C21 C16 C15 120.9(3) . . ? C29 O17 La2 145.36(17) . . ? C16 C17 C18 118.2(3) . . ? C16 C17 H17 120.9 . . ? C18 C17 H17 120.9 . . ? C29 O18 La2 142.71(17) . 2_675 ? C19 C18 C17 122.8(3) . . ? C19 C18 N2 119.2(3) . . ? C17 C18 N2 118.0(3) . . ? C20 C19 C18 118.6(3) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? C19 C20 C21 119.9(3) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C36 O21 La2 116.92(16) . . ? C16 C21 C20 120.7(3) . . ? C16 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C36 O22 La2 171.61(18) . 2_675 ? O13 C22 O14 125.1(2) . . ? O13 C22 C23 117.5(2) . . ? O14 C22 C23 117.3(2) . . ? C24 C23 C28 119.6(2) . . ? C24 C23 C22 118.8(2) . . ? C28 C23 C22 121.6(2) . . ? C25 C24 C23 118.8(2) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C43 O25 La1 129.46(18) . . ? C24 C25 C26 122.9(3) . . ? C24 C25 N4 117.6(2) . . ? C26 C25 N4 119.4(3) . . ? C46 O26 La1 147.4(2) . . ? C25 C26 C27 117.5(3) . . ? C25 C26 H26 121.2 . . ? C27 C26 H26 121.2 . . ? C49 O27 La2 146.6(2) . . ? C28 C27 C26 121.1(3) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C52A O28 C52B 61.4(5) . . ? C27 C28 C23 120.1(3) . . ? C27 C28 H28 120.0 . . ? C23 C28 H28 120.0 . . ? O18 C29 O17 126.9(2) . . ? O18 C29 C30 116.9(2) . . ? O17 C29 C30 116.2(2) . . ? C31 C30 C35 119.8(2) . . ? C31 C30 C29 119.6(2) . . ? C35 C30 C29 120.7(2) . . ? C32 C31 C30 118.2(3) . . ? C32 C31 H31 120.9 . . ? C30 C31 H31 120.9 . . ? C31 C32 C33 122.9(3) . . ? C31 C32 N5 118.1(3) . . ? C33 C32 N5 118.9(3) . . ? C34 C33 C32 118.3(3) . . ? C34 C33 H33 120.8 . . ? C32 C33 H33 120.8 . . ? C33 C34 C35 120.0(3) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 C30 120.7(3) . . ? C34 C35 H35 119.6 . . ? C30 C35 H35 119.6 . . ? O22 C36 O21 124.6(2) . . ? O22 C36 C37 117.9(2) . . ? O21 C36 C37 117.4(2) . . ? C38 C37 C42 120.0(2) . . ? C38 C37 C36 120.0(2) . . ? C42 C37 C36 120.0(2) . . ? C39 C38 C37 118.0(2) . . ? C39 C38 H38 121.0 . . ? C37 C38 H38 121.0 . . ? C40 C39 C38 123.2(3) . . ? C40 C39 N6 118.3(2) . . ? C38 C39 N6 118.5(2) . . ? C39 C40 C41 118.2(3) . . ? C39 C40 H40 120.9 . . ? C41 C40 H40 120.9 . . ? C42 C41 C40 119.8(3) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C41 C42 C37 120.8(3) . . ? C41 C42 H42 119.6 . . ? C37 C42 H42 119.6 . . ? C46 N43 C48 122.9(3) . . ? C46 N43 C47 120.8(3) . . ? C48 N43 C47 116.3(3) . . ? O25 C43 N46 124.8(3) . . ? O25 C43 H43 117.6 . . ? N46 C43 H43 117.6 . . ? C49 N44 C50 120.6(3) . . ? C49 N44 C51 123.0(3) . . ? C50 N44 C51 116.2(3) . . ? N46 C44 H44A 109.5 . . ? N46 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N46 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N46 C45 H45A 109.5 . . ? N46 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N46 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N46 C45 H45D 109.5 . . ? H45A C45 H45D 141.1 . . ? H45B C45 H45D 56.3 . . ? H45C C45 H45D 56.3 . . ? N46 C45 H45E 109.5 . . ? H45A C45 H45E 56.3 . . ? H45B C45 H45E 141.1 . . ? H45C C45 H45E 56.3 . . ? H45D C45 H45E 109.5 . . ? N46 C45 H45F 109.5 . . ? H45A C45 H45F 56.3 . . ? H45B C45 H45F 56.3 . . ? H45C C45 H45F 141.1 . . ? H45D C45 H45F 109.5 . . ? H45E C45 H45F 109.5 . . ? C43 N46 C45 122.9(3) . . ? C43 N46 C44 121.0(3) . . ? C45 N46 C44 116.0(3) . . ? O26 C46 N43 125.0(3) . . ? O26 C46 H46 117.5 . . ? N43 C46 H46 117.5 . . ? N43 C47 H47A 109.5 . . ? N43 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N43 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N43 C47 H47D 109.5 . . ? H47A C47 H47D 141.1 . . ? H47B C47 H47D 56.3 . . ? H47C C47 H47D 56.3 . . ? N43 C47 H47E 109.5 . . ? H47A C47 H47E 56.3 . . ? H47B C47 H47E 141.1 . . ? H47C C47 H47E 56.3 . . ? H47D C47 H47E 109.5 . . ? N43 C47 H47F 109.5 . . ? H47A C47 H47F 56.3 . . ? H47B C47 H47F 56.3 . . ? H47C C47 H47F 141.1 . . ? H47D C47 H47F 109.5 . . ? H47E C47 H47F 109.5 . . ? N43 C48 H48A 109.5 . . ? N43 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N43 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N43 C48 H48D 109.5 . . ? H48A C48 H48D 141.1 . . ? H48B C48 H48D 56.3 . . ? H48C C48 H48D 56.3 . . ? N43 C48 H48E 109.5 . . ? H48A C48 H48E 56.3 . . ? H48B C48 H48E 141.1 . . ? H48C C48 H48E 56.3 . . ? H48D C48 H48E 109.5 . . ? N43 C48 H48F 109.5 . . ? H48A C48 H48F 56.3 . . ? H48B C48 H48F 56.3 . . ? H48C C48 H48F 141.1 . . ? H48D C48 H48F 109.5 . . ? H48E C48 H48F 109.5 . . ? O27 C49 N44 125.4(3) . . ? O27 C49 H49 117.3 . . ? N44 C49 H49 117.3 . . ? N44 C50 H50A 109.5 . . ? N44 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N44 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N44 C51 H51A 109.5 . . ? N44 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N44 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N44 C51 H51D 109.5 . . ? H51A C51 H51D 141.1 . . ? H51B C51 H51D 56.3 . . ? H51C C51 H51D 56.3 . . ? N44 C51 H51E 109.5 . . ? H51A C51 H51E 56.3 . . ? H51B C51 H51E 141.1 . . ? H51C C51 H51E 56.3 . . ? H51D C51 H51E 109.5 . . ? N44 C51 H51F 109.5 . . ? H51A C51 H51F 56.3 . . ? H51B C51 H51F 56.3 . . ? H51C C51 H51F 141.1 . . ? H51D C51 H51F 109.5 . . ? H51E C51 H51F 109.5 . . ? O28 C52A N7 120.1(7) . . ? O28 C52A H52A 119.9 . . ? N7 C52A H52A 119.9 . . ? O28 C52B N7 118.2(5) . . ? O28 C52B H52B 120.9 . . ? N7 C52B H52B 120.9 . . ? N7 C53A H53D 109.5 . . ? N7 C53A H53E 109.5 . . ? N7 C53A H53F 109.5 . . ? N7 C53B H53A 109.5 . . ? N7 C53B H53B 109.5 . . ? H53A C53B H53B 109.5 . . ? N7 C53B H53C 109.5 . . ? H53A C53B H53C 109.5 . . ? H53B C53B H53C 109.5 . . ? N7 C54A H54A 109.5 . . ? N7 C54A H54B 109.5 . . ? N7 C54A H54C 109.5 . . ? N7 C54B H54D 109.5 . . ? N7 C54B H54E 109.5 . . ? H54D C54B H54E 109.5 . . ? N7 C54B H54F 109.5 . . ? H54D C54B H54F 109.5 . . ? H54E C54B H54F 109.5 . . ? 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 C6 H6 O28 0.95 2.72 3.324(5) 122.4 . C7 H7 O28 0.95 2.64 3.290(4) 125.9 . C43 H43 O14 0.95 2.88 3.602(3) 134.1 . C43 H43 O13 0.95 2.95 3.828(3) 153.8 2_666 C49 H49 O4 0.95 2.35 3.292(4) 174.0 2_675 C46 H46 O11 0.95 2.91 3.511(5) 122.0 2_666 C46 H46 O14 0.95 2.83 3.167(4) 102.2 2_666 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.039 _refine_diff_density_min -0.985 _refine_diff_density_rms 0.083 # Attachment '11.CIF' data_HB15DMSO _database_code_depnum_ccdc_archive 'CCDC 634366' _audit_creation_method SHELXL-97 _chemical_name_systematic ; poly[(aqua)(dimethylsulphoxide)tris(4-nitrobenzoato)lanthanum(III)] DMSO solvate ; _chemical_name_common ; poly((aqua)(dimethylsulphoxide)tris(4- nitrobenzoato)lanthanum(iii)) DMSO solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C23 H20 La1 N3 O14 S1, C2 H6 O1 S1' _chemical_formula_sum 'C25 H26 La1 N3 O15 S2' _chemical_formula_weight 811.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' N N 0.0061 0.0033 '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 16.4013(10) _cell_length_b 9.6954(5) _cell_length_c 20.2097(11) _cell_angle_alpha 90.00 _cell_angle_beta 108.461(2) _cell_angle_gamma 90.00 _cell_volume 3048.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 1.616 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6978 _exptl_absorpt_correction_T_max 0.8551 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 X8 Apex II CCD' _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 19202 _diffrn_reflns_av_R_equivalents 0.1093 _diffrn_reflns_av_sigmaI/netI 0.1246 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7002 _reflns_number_gt 5006 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^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_extinction_expression ? _refine_ls_number_reflns 7002 _refine_ls_number_parameters 423 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0859 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.0988 _refine_ls_wR_factor_gt 0.0812 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _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 0.004286(18) 0.76828(3) 0.981179(16) 0.01468(9) Uani 1 1 d . . . S1 S 0.04473(9) 0.69166(13) 0.81498(7) 0.0206(3) Uani 1 1 d . . . O1 O 0.1127(2) 0.8814(4) 0.93477(19) 0.0253(9) Uani 1 1 d . . . N1 N 0.4395(4) 1.2273(7) 0.9195(3) 0.0501(17) Uani 1 1 d . . . C1 C 0.1296(3) 1.0078(5) 0.9464(3) 0.0177(11) Uani 1 1 d . . . H1O H 0.038(4) 0.656(6) 1.133(3) 0.04(2) Uiso 1 1 d . . . S2 S 0.21252(9) 0.61239(14) 1.20413(7) 0.0222(3) Uani 1 1 d . . . O2 O 0.0851(2) 1.0891(4) 0.96853(19) 0.0270(9) Uani 1 1 d . . . N2 N -0.5069(3) 1.0475(5) 0.7599(3) 0.0302(12) Uani 1 1 d . . . C2 C 0.2088(3) 1.0626(5) 0.9338(3) 0.0154(11) Uani 1 1 d . . . H2O H -0.007(3) 0.564(5) 1.094(2) 0.004(13) Uiso 1 1 d . . . O3 O 0.5046(3) 1.1596(7) 0.9440(3) 0.0715(18) Uani 1 1 d . . . N3 N 0.4953(3) 0.2874(5) 1.0928(3) 0.0308(12) Uani 1 1 d . . . C3 C 0.2797(3) 0.9778(6) 0.9453(3) 0.0216(12) Uani 1 1 d . . . H3 H 0.2762 0.8835 0.9567 0.026 Uiso 1 1 calc R . . O4 O 0.4369(3) 1.3420(6) 0.8940(2) 0.0614(16) Uani 1 1 d . . . C4 C 0.3563(3) 1.0311(6) 0.9401(3) 0.0290(14) Uani 1 1 d . . . H4 H 0.4061 0.9751 0.9493 0.035 Uiso 1 1 calc R . . O5 O -0.1063(2) 0.8973(3) 0.88281(18) 0.0210(8) Uani 1 1 d . . . C5 C 0.3577(4) 1.1664(7) 0.9213(3) 0.0329(15) Uani 1 1 d . . . O6 O -0.1042(2) 1.1171(3) 0.91775(18) 0.0208(8) Uani 1 1 d . . . C6 C 0.2869(4) 1.2516(6) 0.9067(3) 0.0270(14) Uani 1 1 d . . . H6 H 0.2894 1.3437 0.8914 0.032 Uiso 1 1 calc R . . O7 O -0.5412(3) 0.9662(5) 0.7142(2) 0.0420(11) Uani 1 1 d . . . C7 C 0.2120(3) 1.1998(5) 0.9150(3) 0.0210(12) Uani 1 1 d . . . H7 H 0.1632 1.2576 0.9078 0.025 Uiso 1 1 calc R . . O8 O -0.5464(3) 1.1314(5) 0.7833(3) 0.0510(13) Uani 1 1 d . . . C8 C -0.1406(3) 1.0125(5) 0.8858(3) 0.0171(11) Uani 1 1 d . . . O9 O 0.1362(2) 0.6160(4) 1.00786(19) 0.0225(8) Uani 1 1 d . . . C9 C -0.2365(3) 1.0254(5) 0.8499(3) 0.0172(11) Uani 1 1 d . . . O10 O 0.0999(2) 0.4178(4) 1.04662(18) 0.0209(8) Uani 1 1 d . . . C10 C -0.2785(3) 0.9409(5) 0.7935(3) 0.0217(12) Uani 1 1 d . . . H10 H -0.2468 0.8766 0.7758 0.026 Uiso 1 1 calc R . . O11 O 0.5479(3) 0.3511(5) 1.0747(3) 0.0615(15) Uani 1 1 d . . . C11 C -0.3673(3) 0.9517(5) 0.7632(3) 0.0224(12) Uani 1 1 d . . . H11 H -0.3968 0.8961 0.7243 0.027 Uiso 1 1 calc R . . O12 O 0.5113(3) 0.1767(5) 1.1233(3) 0.0593(15) Uani 1 1 d . . . C12 C -0.4116(3) 1.0440(6) 0.7907(3) 0.0242(13) Uani 1 1 d . . . O13 O 0.0001(3) 0.6471(4) 1.0950(2) 0.0197(8) Uani 1 1 d . . . C13 C -0.3719(4) 1.1313(5) 0.8447(3) 0.0233(12) Uani 1 1 d . . . H13 H -0.4039 1.1966 0.8614 0.028 Uiso 1 1 calc R . . O14 O 0.0004(2) 0.6459(3) 0.86746(18) 0.0213(8) Uani 1 1 d . . . C14 C -0.2832(3) 1.1210(5) 0.8740(3) 0.0198(11) Uani 1 1 d . . . H14 H -0.2541 1.1806 0.9114 0.024 Uiso 1 1 calc R . . O15 O 0.1328(2) 0.6716(4) 1.21651(18) 0.0257(9) Uani 1 1 d . . . C15 C 0.1533(3) 0.4974(5) 1.0333(3) 0.0133(10) Uani 1 1 d . . . C16 C 0.2442(3) 0.4463(5) 1.0489(2) 0.0141(10) Uani 1 1 d . . . C17 C 0.3069(3) 0.5239(5) 1.0338(3) 0.0197(11) Uani 1 1 d . . . H17 H 0.2930 0.6129 1.0136 0.024 Uiso 1 1 calc R . . C18 C 0.3895(3) 0.4732(5) 1.0476(3) 0.0228(12) Uani 1 1 d . . . H18 H 0.4328 0.5265 1.0377 0.027 Uiso 1 1 calc R . . C19 C 0.4072(3) 0.3431(6) 1.0763(3) 0.0218(12) Uani 1 1 d . . . C20 C 0.3469(3) 0.2623(6) 1.0918(3) 0.0218(12) Uani 1 1 d . . . H20 H 0.3613 0.1733 1.1117 0.026 Uiso 1 1 calc R . . C21 C 0.2645(3) 0.3140(5) 1.0776(3) 0.0183(11) Uani 1 1 d . . . H21 H 0.2214 0.2597 1.0874 0.022 Uiso 1 1 calc R . . C22 C -0.0053(4) 0.5944(6) 0.7387(3) 0.0376(16) Uani 1 1 d . . . H22A H -0.0637 0.6292 0.7163 0.056 Uiso 1 1 calc R . . H22B H -0.0081 0.4972 0.7512 0.056 Uiso 1 1 calc R . . H22C H 0.0280 0.6028 0.7063 0.056 Uiso 1 1 calc R . . C23 C 0.1450(4) 0.6058(6) 0.8417(3) 0.0369(16) Uani 1 1 d . . . H23A H 0.1820 0.6474 0.8850 0.055 Uiso 1 1 calc R . . H23B H 0.1723 0.6145 0.8053 0.055 Uiso 1 1 calc R . . H23C H 0.1361 0.5081 0.8497 0.055 Uiso 1 1 calc R . . C24 C 0.3009(3) 0.6742(6) 1.2744(3) 0.0303(14) Uani 1 1 d . . . H24A H 0.3078 0.7735 1.2688 0.045 Uiso 1 1 calc R . . H24B H 0.3535 0.6261 1.2744 0.045 Uiso 1 1 calc R . . H24C H 0.2900 0.6571 1.3187 0.045 Uiso 1 1 calc R . . C25 C 0.2188(4) 0.4360(5) 1.2305(3) 0.0292(14) Uani 1 1 d . . . H25A H 0.1732 0.3833 1.1969 0.044 Uiso 1 1 calc R . . H25B H 0.2117 0.4295 1.2768 0.044 Uiso 1 1 calc R . . H25C H 0.2749 0.3983 1.2323 0.044 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 0.01224(15) 0.01143(15) 0.01993(17) -0.00071(12) 0.00445(12) -0.00034(12) S1 0.0241(7) 0.0169(7) 0.0228(7) 0.0004(5) 0.0103(6) -0.0013(6) O1 0.027(2) 0.018(2) 0.031(2) 0.0002(17) 0.0102(18) -0.0116(18) N1 0.037(3) 0.079(5) 0.030(3) 0.006(3) 0.004(3) -0.032(4) C1 0.018(3) 0.019(3) 0.017(3) 0.007(2) 0.005(2) 0.004(2) S2 0.0252(7) 0.0211(7) 0.0213(7) 0.0010(6) 0.0086(6) 0.0006(6) O2 0.028(2) 0.032(2) 0.024(2) 0.0070(18) 0.0128(18) 0.0145(19) N2 0.020(3) 0.030(3) 0.037(3) 0.011(2) 0.004(2) -0.001(2) C2 0.016(3) 0.016(3) 0.017(3) -0.006(2) 0.010(2) -0.006(2) O3 0.021(3) 0.133(5) 0.058(4) 0.038(3) 0.009(2) -0.011(3) N3 0.017(2) 0.043(3) 0.033(3) 0.000(2) 0.009(2) 0.005(2) C3 0.024(3) 0.025(3) 0.020(3) 0.003(2) 0.013(2) 0.000(2) O4 0.055(3) 0.088(4) 0.042(3) 0.009(3) 0.014(3) -0.049(3) C4 0.018(3) 0.047(4) 0.024(3) 0.002(3) 0.009(2) 0.003(3) O5 0.0185(19) 0.0175(19) 0.025(2) 0.0011(16) 0.0036(16) 0.0030(16) C5 0.024(3) 0.052(4) 0.021(3) -0.003(3) 0.004(3) -0.020(3) O6 0.0207(19) 0.0158(19) 0.025(2) -0.0040(16) 0.0060(16) -0.0109(16) C6 0.033(3) 0.029(3) 0.017(3) 0.005(2) 0.005(2) -0.022(3) O7 0.026(2) 0.057(3) 0.036(3) -0.006(2) 0.000(2) -0.012(2) C7 0.024(3) 0.023(3) 0.016(3) -0.005(2) 0.007(2) -0.003(2) O8 0.022(2) 0.050(3) 0.073(4) 0.004(3) 0.003(2) 0.012(2) C8 0.017(3) 0.015(3) 0.019(3) 0.008(2) 0.006(2) 0.000(2) O9 0.0204(19) 0.0166(19) 0.032(2) 0.0081(16) 0.0098(17) 0.0089(16) C9 0.023(3) 0.009(2) 0.020(3) 0.003(2) 0.006(2) -0.002(2) O10 0.0130(18) 0.020(2) 0.028(2) -0.0001(16) 0.0037(16) -0.0057(16) C10 0.026(3) 0.016(3) 0.023(3) 0.003(2) 0.007(2) -0.001(2) O11 0.026(3) 0.074(4) 0.095(4) 0.030(3) 0.033(3) 0.012(3) C11 0.019(3) 0.023(3) 0.020(3) 0.002(2) 0.000(2) -0.008(2) O12 0.029(3) 0.073(4) 0.078(4) 0.044(3) 0.020(3) 0.025(3) C12 0.015(3) 0.023(3) 0.030(3) 0.010(2) 0.001(2) -0.002(2) O13 0.022(2) 0.015(2) 0.021(2) 0.0000(17) 0.0060(18) -0.0050(18) C13 0.029(3) 0.018(3) 0.027(3) 0.003(2) 0.015(3) -0.002(3) O14 0.024(2) 0.0166(19) 0.026(2) -0.0034(16) 0.0116(17) -0.0068(16) C14 0.019(3) 0.016(3) 0.021(3) 0.001(2) 0.002(2) -0.002(2) O15 0.026(2) 0.029(2) 0.021(2) -0.0038(17) 0.0063(17) 0.0035(18) C15 0.013(2) 0.011(2) 0.013(3) -0.0035(19) 0.000(2) -0.001(2) C16 0.013(2) 0.016(3) 0.013(3) -0.003(2) 0.003(2) -0.001(2) C17 0.019(3) 0.015(3) 0.025(3) -0.001(2) 0.008(2) 0.000(2) C18 0.022(3) 0.018(3) 0.031(3) 0.001(2) 0.012(2) -0.001(2) C19 0.016(3) 0.028(3) 0.018(3) -0.001(2) 0.002(2) 0.005(2) C20 0.025(3) 0.021(3) 0.021(3) 0.009(2) 0.010(2) 0.008(2) C21 0.014(2) 0.019(3) 0.020(3) 0.003(2) 0.003(2) 0.000(2) C22 0.044(4) 0.043(4) 0.026(4) -0.014(3) 0.012(3) -0.010(3) C23 0.036(4) 0.037(4) 0.048(4) 0.011(3) 0.028(3) 0.009(3) C24 0.023(3) 0.024(3) 0.043(4) -0.001(3) 0.009(3) -0.007(3) C25 0.030(3) 0.024(3) 0.029(3) -0.003(3) 0.004(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O10 2.426(3) 3_567 ? La1 O6 2.444(3) 3_577 ? La1 O2 2.457(3) 3_577 ? La1 O1 2.510(3) . ? La1 O9 2.532(3) . ? La1 O5 2.554(3) . ? La1 O14 2.569(3) . ? La1 O13 2.602(4) . ? La1 La1 4.5668(6) 3_577 ? La1 La1 5.2658(6) 3_567 ? S1 O14 1.529(4) . ? S1 C23 1.767(6) . ? S1 C22 1.772(6) . ? O1 C1 1.262(6) . ? N1 O3 1.216(7) . ? N1 O4 1.221(7) . ? N1 C5 1.477(7) . ? C1 O2 1.250(6) . ? C1 C2 1.498(6) . ? S2 O15 1.519(4) . ? S2 C24 1.782(6) . ? S2 C25 1.785(6) . ? O2 La1 2.457(3) 3_577 ? N2 O7 1.210(6) . ? N2 O8 1.224(6) . ? N2 C12 1.488(7) . ? C2 C3 1.382(7) . ? C2 C7 1.389(7) . ? N3 O11 1.208(6) . ? N3 O12 1.224(6) . ? N3 C19 1.479(6) . ? C3 C4 1.392(7) . ? C3 H3 0.9500 . ? C4 C5 1.367(8) . ? C4 H4 0.9500 . ? O5 C8 1.261(6) . ? C5 C6 1.380(8) . ? O6 C8 1.247(6) . ? O6 La1 2.444(3) 3_577 ? C6 C7 1.385(7) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.514(7) . ? O9 C15 1.255(5) . ? C9 C14 1.386(7) . ? C9 C10 1.397(7) . ? O10 C15 1.258(6) . ? O10 La1 2.426(3) 3_567 ? C10 C11 1.394(7) . ? C10 H10 0.9500 . ? C11 C12 1.375(7) . ? C11 H11 0.9500 . ? C12 C13 1.372(7) . ? O13 H1O 0.82(6) . ? O13 H2O 0.81(5) . ? C13 C14 1.390(7) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.508(6) . ? C16 C17 1.383(7) . ? C16 C21 1.404(7) . ? C17 C18 1.384(7) . ? C17 H17 0.9500 . ? C18 C19 1.381(7) . ? C18 H18 0.9500 . ? C19 C20 1.374(7) . ? C20 C21 1.383(7) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? 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 O10 La1 O6 140.24(12) 3_567 3_577 ? O10 La1 O2 92.60(12) 3_567 3_577 ? O6 La1 O2 74.26(12) 3_577 3_577 ? O10 La1 O1 140.27(12) 3_567 . ? O6 La1 O1 75.31(12) 3_577 . ? O2 La1 O1 119.64(12) 3_577 . ? O10 La1 O9 96.17(12) 3_567 . ? O6 La1 O9 77.61(12) 3_577 . ? O2 La1 O9 145.23(12) 3_577 . ? O1 La1 O9 71.09(12) . . ? O10 La1 O5 84.80(11) 3_567 . ? O6 La1 O5 123.43(11) 3_577 . ? O2 La1 O5 71.13(11) 3_577 . ? O1 La1 O5 84.70(12) . . ? O9 La1 O5 143.10(11) . . ? O10 La1 O14 68.49(11) 3_567 . ? O6 La1 O14 141.04(11) 3_577 . ? O2 La1 O14 141.33(12) 3_577 . ? O1 La1 O14 71.79(11) . . ? O9 La1 O14 72.47(11) . . ? O5 La1 O14 73.71(11) . . ? O10 La1 O13 69.82(12) 3_567 . ? O6 La1 O13 70.44(12) 3_577 . ? O2 La1 O13 72.69(12) 3_577 . ? O1 La1 O13 138.37(12) . . ? O9 La1 O13 78.95(12) . . ? O5 La1 O13 134.26(12) . . ? O14 La1 O13 125.58(12) . . ? O10 La1 La1 135.54(8) 3_567 3_577 ? O6 La1 La1 57.40(8) 3_577 3_577 ? O2 La1 La1 47.44(9) 3_577 3_577 ? O1 La1 La1 72.24(8) . 3_577 ? O9 La1 La1 127.40(8) . 3_577 ? O5 La1 La1 66.18(8) . 3_577 ? O14 La1 La1 127.59(8) . 3_577 ? O13 La1 La1 106.63(9) . 3_577 ? O10 La1 La1 41.37(8) 3_567 3_567 ? O6 La1 La1 111.72(8) 3_577 3_567 ? O2 La1 La1 116.70(9) 3_577 3_567 ? O1 La1 La1 122.71(8) . 3_567 ? O9 La1 La1 56.86(8) . 3_567 ? O5 La1 La1 123.46(8) . 3_567 ? O14 La1 La1 71.27(8) . 3_567 ? O13 La1 La1 54.33(9) . 3_567 ? La1 La1 La1 160.787(14) 3_577 3_567 ? O14 S1 C23 104.6(2) . . ? O14 S1 C22 105.0(3) . . ? C23 S1 C22 98.3(3) . . ? C1 O1 La1 119.7(3) . . ? O3 N1 O4 124.9(6) . . ? O3 N1 C5 117.5(6) . . ? O4 N1 C5 117.6(6) . . ? O2 C1 O1 124.1(5) . . ? O2 C1 C2 118.3(5) . . ? O1 C1 C2 117.7(4) . . ? O15 S2 C24 105.5(2) . . ? O15 S2 C25 106.5(2) . . ? C24 S2 C25 97.4(3) . . ? C1 O2 La1 174.8(4) . 3_577 ? O7 N2 O8 123.5(5) . . ? O7 N2 C12 118.5(5) . . ? O8 N2 C12 118.0(5) . . ? C3 C2 C7 120.8(5) . . ? C3 C2 C1 119.3(5) . . ? C7 C2 C1 119.7(5) . . ? O11 N3 O12 122.8(5) . . ? O11 N3 C19 119.1(5) . . ? O12 N3 C19 118.1(5) . . ? C2 C3 C4 119.8(5) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 118.2(5) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? C8 O5 La1 127.9(3) . . ? C4 C5 C6 123.1(5) . . ? C4 C5 N1 119.1(6) . . ? C6 C5 N1 117.7(6) . . ? C8 O6 La1 152.4(3) . 3_577 ? C5 C6 C7 118.4(5) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? C6 C7 C2 119.5(5) . . ? C6 C7 H7 120.2 . . ? C2 C7 H7 120.2 . . ? O6 C8 O5 126.7(5) . . ? O6 C8 C9 115.8(4) . . ? O5 C8 C9 117.5(4) . . ? C15 O9 La1 133.3(3) . . ? C14 C9 C10 119.7(5) . . ? C14 C9 C8 119.5(5) . . ? C10 C9 C8 120.8(5) . . ? C15 O10 La1 153.3(3) . 3_567 ? C11 C10 C9 119.4(5) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C12 C11 C10 119.0(5) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C13 C12 C11 123.0(5) . . ? C13 C12 N2 119.3(5) . . ? C11 C12 N2 117.8(5) . . ? La1 O13 H1O 123(5) . . ? La1 O13 H2O 118(3) . . ? H1O O13 H2O 101(5) . . ? C12 C13 C14 117.7(5) . . ? C12 C13 H13 121.2 . . ? C14 C13 H13 121.2 . . ? S1 O14 La1 127.15(18) . . ? C9 C14 C13 121.2(5) . . ? C9 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? O9 C15 O10 124.7(4) . . ? O9 C15 C16 117.7(4) . . ? O10 C15 C16 117.6(4) . . ? C17 C16 C21 119.6(4) . . ? C17 C16 C15 122.0(4) . . ? C21 C16 C15 118.4(4) . . ? C16 C17 C18 120.6(5) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C19 C18 C17 118.2(5) . . ? C19 C18 H18 120.9 . . ? C17 C18 H18 120.9 . . ? C20 C19 C18 123.1(5) . . ? C20 C19 N3 117.6(5) . . ? C18 C19 N3 119.3(5) . . ? C19 C20 C21 118.3(5) . . ? C19 C20 H20 120.9 . . ? C21 C20 H20 120.9 . . ? C20 C21 C16 120.2(5) . . ? C20 C21 H21 119.9 . . ? C16 C21 H21 119.9 . . ? S1 C22 H22A 109.5 . . ? S1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? S1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? S1 C23 H23A 109.5 . . ? S1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? S1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? S2 C24 H24A 109.5 . . ? S2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? S2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? S2 C25 H25A 109.5 . . ? S2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? S2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? 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 O13 H2O O14 0.81(5) 2.17(5) 2.941(5) 159(4) 3_567 O13 H1O O15 0.82(6) 1.91(6) 2.728(5) 174(6) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.052 _refine_diff_density_min -1.515 _refine_diff_density_rms 0.226 # Attachment '12.CIF' data_HB21DMSO _database_code_depnum_ccdc_archive 'CCDC 634367' _audit_creation_method SHELXL-97 _chemical_name_systematic ; poly[(aqua)(dimethylsulphoxide)tris(3-methoxybenzoato)lanthanum (III)], DMSO solvate. ; _chemical_name_common ; poly((aqua)(dimethylsulphoxide)tris(3- methoxybenzoato)lanthanum (iii)), DMSO solvate. ; _chemical_melting_point ? _chemical_formula_moiety 'C26 H29 La1 O11 S1, C2 H6 S1 O1' _chemical_formula_sum 'C28 H35 La1 O12 S2' _chemical_formula_weight 766.59 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' 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 9.6514(4) _cell_length_b 21.4458(5) _cell_length_c 15.9922(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.028(1) _cell_angle_gamma 90.00 _cell_volume 3297.36(17) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 1.480 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6652 _exptl_absorpt_correction_T_max 0.8085 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 30583 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7552 _reflns_number_gt 5430 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^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 7552 _refine_ls_number_parameters 554 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.025 _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 La1 La 0.275910(17) 0.003252(8) 0.490326(12) 0.03032(7) Uani 1 1 d . . . S1 S 0.22853(11) -0.14366(5) 0.36457(8) 0.0574(3) Uani 1 1 d . . . O1 O 0.4013(3) 0.04892(12) 0.61838(18) 0.0565(7) Uani 1 1 d . A . C1 C 0.5074(3) 0.03884(15) 0.6670(2) 0.0377(8) Uani 1 1 d . . . O2 O 0.6247(2) 0.02319(12) 0.64525(15) 0.0431(6) Uani 1 1 d . . . C2A C 0.5070(9) 0.0497(7) 0.7651(4) 0.038(3) Uani 0.608(8) 1 d PD A 1 C3A C 0.3821(7) 0.0652(4) 0.7981(5) 0.044(2) Uani 0.608(8) 1 d PD A 1 H3A H 0.2995 0.0673 0.7636 0.053 Uiso 0.608(8) 1 calc PR A 1 C4A C 0.3839(10) 0.0774(5) 0.8839(5) 0.063(2) Uani 0.608(8) 1 d PD A 1 C5A C 0.5022(9) 0.0705(5) 0.9344(4) 0.079(3) Uani 0.608(8) 1 d PD A 1 H5A H 0.5018 0.0789 0.9914 0.095 Uiso 0.608(8) 1 calc PR A 1 C6A C 0.6248(10) 0.0512(4) 0.9030(4) 0.075(3) Uani 0.608(8) 1 d PD A 1 H6A H 0.7048 0.0456 0.9390 0.090 Uiso 0.608(8) 1 calc PR A 1 C7A C 0.6274(10) 0.0403(6) 0.8165(4) 0.053(3) Uani 0.608(8) 1 d PD A 1 H7A H 0.7085 0.0270 0.7945 0.063 Uiso 0.608(8) 1 calc PR A 1 O3A O 0.2668(7) 0.0947(4) 0.9216(4) 0.101(3) Uani 0.608(8) 1 d PD A 1 C2B C 0.4732(12) 0.0430(11) 0.7493(6) 0.035(4) Uani 0.392(8) 1 d PD A 2 C3B C 0.3387(11) 0.0619(7) 0.7639(6) 0.046(3) Uani 0.392(8) 1 d PD A 2 H3B H 0.2750 0.0734 0.7195 0.055 Uiso 0.392(8) 1 calc PR A 2 C4B C 0.3022(11) 0.0632(5) 0.8464(7) 0.058(3) Uani 0.392(8) 1 d PD A 2 C5B C 0.3958(12) 0.0477(5) 0.9105(6) 0.063(5) Uani 0.392(8) 1 d PD A 2 H5B H 0.3682 0.0461 0.9647 0.076 Uiso 0.392(8) 1 calc PR A 2 C6B C 0.5327(12) 0.0339(5) 0.8971(6) 0.058(3) Uani 0.392(8) 1 d PD A 2 H6B H 0.5971 0.0254 0.9424 0.070 Uiso 0.392(8) 1 calc PR A 2 C7B C 0.5733(13) 0.0328(7) 0.8148(6) 0.050(5) Uani 0.392(8) 1 d PD A 2 H7B H 0.6654 0.0254 0.8048 0.060 Uiso 0.392(8) 1 calc PR A 2 O3B O 0.1730(16) 0.0821(16) 0.8670(10) 0.103(6) Uani 0.392(8) 1 d PD A 2 O4 O 0.1441(2) -0.04683(11) 0.59711(15) 0.0432(6) Uani 1 1 d . . . O5 O -0.0718(2) -0.01587(12) 0.60893(16) 0.0463(6) Uani 1 1 d . . . O6 O 0.3149(6) -0.1210(3) 0.8890(3) 0.138(2) Uani 1 1 d . . . O7 O 0.4582(2) -0.07057(10) 0.54306(15) 0.0415(6) Uani 1 1 d . C . O8 O 0.6686(2) -0.10876(11) 0.56924(18) 0.0517(7) Uani 1 1 d . . . C8A C 0.136(2) 0.1016(15) 0.8587(12) 0.111(9) Uani 0.608(8) 1 d P A 1 H8A1 H 0.0577 0.1133 0.8885 0.167 Uiso 0.608(8) 1 calc PR A 1 H8A2 H 0.1165 0.0626 0.8306 0.167 Uiso 0.608(8) 1 calc PR A 1 H8A3 H 0.1520 0.1331 0.8181 0.167 Uiso 0.608(8) 1 calc PR A 1 C9 C 0.0406(3) -0.03978(14) 0.6378(2) 0.0328(7) Uani 1 1 d . . . O11 O 0.11913(10) 0.08921(5) 0.55006(18) 0.0542(7) Uani 1 1 d D . . C10 C 0.0517(4) -0.06143(17) 0.7271(2) 0.0454(9) Uani 1 1 d . . . O10 O 0.1814(2) -0.10818(11) 0.43837(15) 0.0425(6) Uani 1 1 d . . . C11 C 0.1809(5) -0.0794(2) 0.7650(3) 0.0639(12) Uani 1 1 d . . . H11 H 0.2592 -0.0770 0.7351 0.077 Uiso 1 1 calc R . . C12 C 0.1933(7) -0.1007(3) 0.8466(4) 0.0920(19) Uani 1 1 d . . . C13 C 0.0769(11) -0.1036(3) 0.8901(4) 0.118(3) Uani 1 1 d . . . H13 H 0.0846 -0.1180 0.9452 0.141 Uiso 1 1 calc R . . C14 C -0.0492(9) -0.0859(3) 0.8535(4) 0.112(2) Uani 1 1 d . . . H14 H -0.1266 -0.0881 0.8842 0.134 Uiso 1 1 calc R . . C15 C -0.0650(5) -0.0645(2) 0.7712(3) 0.0722(13) Uani 1 1 d . . . H15 H -0.1517 -0.0526 0.7464 0.087 Uiso 1 1 calc R . . C16 C 0.4319(8) -0.1208(4) 0.8452(6) 0.152(4) Uani 1 1 d . . . H16A H 0.5098 -0.1363 0.8806 0.228 Uiso 1 1 calc R . . H16B H 0.4509 -0.0791 0.8279 0.228 Uiso 1 1 calc R . . H16C H 0.4164 -0.1471 0.7966 0.228 Uiso 1 1 calc R . . C17 C 0.5393(4) -0.11376(15) 0.5675(2) 0.0368(8) Uani 1 1 d . . . C25 C 0.1036(6) -0.1246(2) 0.2790(3) 0.0862(16) Uani 1 1 d . . . H25A H 0.1166 -0.0821 0.2624 0.129 Uiso 1 1 calc R . . H25B H 0.0115 -0.1296 0.2963 0.129 Uiso 1 1 calc R . . H25C H 0.1158 -0.1518 0.2325 0.129 Uiso 1 1 calc R . . C26 C 0.1760(5) -0.22287(19) 0.3781(3) 0.0718(13) Uani 1 1 d . . . H26A H 0.2343 -0.2416 0.4230 0.108 Uiso 1 1 calc R . . H26B H 0.1846 -0.2456 0.3271 0.108 Uiso 1 1 calc R . . H26C H 0.0810 -0.2238 0.3915 0.108 Uiso 1 1 calc R . . S2 S 0.26637(15) 0.25109(8) 0.63322(11) 0.0928(5) Uani 1 1 d D . . O12A O 0.2074(17) 0.2027(6) 0.6769(10) 0.179(8) Uani 0.503(12) 1 d P B 1 C25A C 0.4246(11) 0.2086(6) 0.6034(9) 0.075(4) Uani 0.503(12) 1 d P B 1 H25D H 0.4822 0.1976 0.6532 0.113 Uiso 0.503(12) 1 calc PR B 1 H25E H 0.4759 0.2350 0.5687 0.113 Uiso 0.503(12) 1 calc PR B 1 H25F H 0.3966 0.1714 0.5730 0.113 Uiso 0.503(12) 1 calc PR B 1 C23A C 0.3426(4) -0.18464(17) 0.5995(2) 0.039(7) Uani 0.525(7) 1 d P C 1 H23A H 0.2795 -0.1566 0.5732 0.047 Uiso 0.525(7) 1 calc PR C 1 C22A C 0.301(2) -0.2360(8) 0.6294(13) 0.036(3) Uani 0.525(7) 1 d P C 1 C18A C 0.484(2) -0.1716(9) 0.6071(7) 0.033(3) Uani 0.525(7) 1 d P C 1 C19A C 0.5790(8) -0.2119(3) 0.6422(5) 0.051(2) Uani 0.525(7) 1 d P C 1 H19A H 0.6734 -0.2025 0.6461 0.061 Uiso 0.525(7) 1 calc PR C 1 C20A C 0.5319(9) -0.2675(4) 0.6724(6) 0.065(3) Uani 0.525(7) 1 d P C 1 H20A H 0.5949 -0.2959 0.6979 0.078 Uiso 0.525(7) 1 calc PR C 1 O9B O 0.161(3) -0.2598(17) 0.621(3) 0.071(7) Uani 0.475(7) 1 d P C 2 C24A C 0.0548(13) -0.2135(7) 0.5962(8) 0.072(3) Uani 0.525(7) 1 d P C 1 H24A H -0.0364 -0.2291 0.6038 0.108 Uiso 0.525(7) 1 calc PR C 1 H24B H 0.0659 -0.2099 0.5373 0.108 Uiso 0.525(7) 1 calc PR C 1 H24C H 0.0664 -0.1732 0.6221 0.108 Uiso 0.525(7) 1 calc PR C 1 C21A C 0.3928(10) -0.2810(4) 0.6649(7) 0.064(3) Uani 0.525(7) 1 d P C 1 H21A H 0.3604 -0.3192 0.6828 0.077 Uiso 0.525(7) 1 calc PR C 1 C19B C 0.5601(9) -0.2323(4) 0.5670(6) 0.051(2) Uani 0.475(7) 1 d P C 2 H19B H 0.6513 -0.2287 0.5532 0.061 Uiso 0.475(7) 1 calc PR C 2 C20B C 0.5030(11) -0.2910(4) 0.5774(7) 0.071(3) Uani 0.475(7) 1 d P C 2 H20B H 0.5568 -0.3263 0.5705 0.085 Uiso 0.475(7) 1 calc PR C 2 C21B C 0.3681(11) -0.2979(4) 0.5977(8) 0.065(3) Uani 0.475(7) 1 d P C 2 H21B H 0.3339 -0.3381 0.6033 0.078 Uiso 0.475(7) 1 calc PR C 2 C24B C 0.0699(15) -0.2080(7) 0.6474(10) 0.072(4) Uani 0.475(7) 1 d P C 2 H24D H -0.0193 -0.2245 0.6582 0.108 Uiso 0.475(7) 1 calc PR C 2 H24E H 0.0582 -0.1774 0.6036 0.108 Uiso 0.475(7) 1 calc PR C 2 H24F H 0.1127 -0.1890 0.6976 0.108 Uiso 0.475(7) 1 calc PR C 2 C18B C 0.480(2) -0.1776(10) 0.5774(7) 0.035(3) Uani 0.475(7) 1 d P C 2 C22B C 0.282(3) -0.2492(10) 0.6101(17) 0.045(4) Uani 0.475(7) 1 d P C 2 O9A O 0.157(3) -0.2554(16) 0.634(2) 0.077(8) Uani 0.525(7) 1 d P C 1 C26A C 0.1905(15) 0.2457(10) 0.5443(15) 0.183(12) Uani 0.503(12) 1 d P B 1 H26D H 0.1040 0.2680 0.5424 0.275 Uiso 0.503(12) 1 calc PR B 1 H26E H 0.1725 0.2026 0.5313 0.275 Uiso 0.503(12) 1 calc PR B 1 H26F H 0.2477 0.2632 0.5041 0.275 Uiso 0.503(12) 1 calc PR B 1 C8B C 0.1203(17) 0.0810(10) 0.9349(10) 0.113(7) Uani 0.392(8) 1 d P A 2 H8B1 H 0.0276 0.0975 0.9275 0.170 Uiso 0.392(8) 1 calc PR A 2 H8B2 H 0.1753 0.1059 0.9752 0.170 Uiso 0.392(8) 1 calc PR A 2 H8B3 H 0.1174 0.0388 0.9547 0.170 Uiso 0.392(8) 1 calc PR A 2 O12B O 0.1729(9) 0.1991(4) 0.6363(10) 0.197(11) Uani 0.497(12) 1 d PD B 2 C25B C 0.2130(17) 0.2741(8) 0.7382(9) 0.146(7) Uani 0.497(12) 1 d P B 2 H25G H 0.1253 0.2955 0.7314 0.220 Uiso 0.497(12) 1 calc PR B 2 H25H H 0.2821 0.3011 0.7656 0.220 Uiso 0.497(12) 1 calc PR B 2 H25I H 0.2040 0.2374 0.7718 0.220 Uiso 0.497(12) 1 calc PR B 2 C26B C 0.4229(13) 0.2160(7) 0.6683(13) 0.109(6) Uani 0.497(12) 1 d P B 2 H26G H 0.4704 0.2031 0.6209 0.164 Uiso 0.497(12) 1 calc PR B 2 H26H H 0.4051 0.1803 0.7020 0.164 Uiso 0.497(12) 1 calc PR B 2 H26I H 0.4797 0.2452 0.7013 0.164 Uiso 0.497(12) 1 calc PR B 2 C23B C 0.3426(4) -0.18464(17) 0.5995(2) 0.045(8) Uiso 0.475(7) 1 d P C 2 H23B H 0.2888 -0.1496 0.6076 0.054 Uiso 0.475(7) 1 calc PR C 2 H2O H 0.0272 0.0889 0.5456 0.060 Uiso 1 1 d D . . H1O H 0.1284 0.1290 0.5618 0.077 Uiso 1 1 d 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 La1 0.02162(9) 0.03302(11) 0.03628(11) -0.00324(9) 0.00226(7) 0.00092(7) S1 0.0502(6) 0.0459(5) 0.0794(8) -0.0212(5) 0.0246(5) -0.0063(4) O1 0.0404(14) 0.0598(17) 0.066(2) -0.0244(14) -0.0102(13) 0.0068(12) C1 0.0364(19) 0.0345(17) 0.043(2) -0.0082(15) 0.0059(16) -0.0065(14) O2 0.0332(13) 0.0571(14) 0.0396(15) -0.0082(12) 0.0071(10) -0.0036(11) C2A 0.044(5) 0.037(5) 0.034(5) -0.005(4) 0.003(4) -0.004(5) C3A 0.044(4) 0.063(4) 0.026(4) -0.005(4) 0.002(3) 0.002(4) C4A 0.064(6) 0.092(7) 0.035(5) -0.015(5) 0.018(4) -0.005(5) C5A 0.090(7) 0.120(8) 0.028(4) -0.007(5) 0.003(4) -0.007(6) C6A 0.064(6) 0.122(8) 0.035(4) 0.005(4) -0.016(4) -0.008(5) C7A 0.046(5) 0.079(7) 0.033(5) 0.006(4) 0.004(3) -0.003(5) O3A 0.077(5) 0.181(7) 0.048(4) -0.040(4) 0.024(3) 0.009(4) C2B 0.043(7) 0.034(7) 0.028(6) -0.005(6) 0.000(5) -0.016(6) C3B 0.054(8) 0.062(7) 0.025(6) 0.003(6) 0.014(5) -0.001(6) C4B 0.060(8) 0.069(7) 0.047(8) 0.001(6) 0.018(6) -0.003(6) C5B 0.103(13) 0.041(7) 0.047(9) 0.008(5) 0.020(8) -0.021(7) C6B 0.066(9) 0.053(7) 0.054(8) 0.003(6) -0.008(7) 0.000(6) C7B 0.055(10) 0.043(7) 0.058(10) 0.003(6) 0.034(8) -0.005(8) O3B 0.058(13) 0.176(16) 0.075(11) 0.021(9) 0.012(9) 0.034(11) O4 0.0378(13) 0.0508(14) 0.0422(15) 0.0085(12) 0.0102(11) 0.0112(11) O5 0.0324(13) 0.0585(15) 0.0469(16) 0.0035(12) -0.0028(11) 0.0060(11) O6 0.134(4) 0.166(5) 0.099(3) 0.076(3) -0.067(3) -0.036(4) O7 0.0378(13) 0.0318(12) 0.0537(16) 0.0024(11) -0.0019(11) 0.0035(10) O8 0.0337(14) 0.0492(15) 0.0725(19) 0.0119(13) 0.0055(12) 0.0034(11) C8A 0.041(8) 0.20(3) 0.085(10) 0.020(10) -0.006(6) 0.019(9) C9 0.0334(17) 0.0310(16) 0.0331(19) 0.0000(14) -0.0013(14) -0.0016(13) O11 0.0303(13) 0.0477(15) 0.085(2) -0.0151(14) 0.0094(13) 0.0017(11) C10 0.052(2) 0.045(2) 0.039(2) 0.0068(17) 0.0041(17) -0.0064(17) O10 0.0388(13) 0.0419(13) 0.0470(15) -0.0100(11) 0.0042(11) -0.0010(10) C11 0.067(3) 0.072(3) 0.049(3) 0.023(2) -0.017(2) -0.015(2) C12 0.111(5) 0.102(4) 0.056(3) 0.037(3) -0.031(3) -0.030(3) C13 0.176(8) 0.131(6) 0.045(4) 0.029(4) 0.005(4) -0.027(5) C14 0.129(6) 0.149(6) 0.064(4) 0.027(4) 0.045(4) -0.005(5) C15 0.078(3) 0.091(3) 0.051(3) 0.018(3) 0.026(2) 0.005(3) C16 0.110(6) 0.156(7) 0.172(8) 0.096(6) -0.093(6) -0.033(5) C17 0.0373(19) 0.0377(18) 0.035(2) 0.0033(15) 0.0037(14) 0.0041(14) C25 0.141(5) 0.075(3) 0.042(3) -0.012(2) 0.007(3) -0.004(3) C26 0.076(3) 0.045(2) 0.095(4) -0.017(2) 0.008(3) -0.004(2) S2 0.0623(8) 0.1082(12) 0.1083(13) 0.0092(10) 0.0100(8) 0.0009(8) O12A 0.257(17) 0.133(11) 0.169(12) 0.102(9) 0.150(12) 0.091(10) C25A 0.049(6) 0.095(8) 0.083(9) -0.029(7) 0.018(6) 0.003(5) C23A 0.045(8) 0.036(8) 0.037(7) 0.005(3) 0.005(3) 0.004(3) C22A 0.039(7) 0.023(8) 0.043(8) -0.001(5) -0.003(5) -0.016(5) C18A 0.039(5) 0.043(5) 0.018(7) 0.014(6) 0.012(6) 0.006(4) C19A 0.043(4) 0.044(4) 0.066(6) 0.013(4) 0.011(4) 0.007(3) C20A 0.073(6) 0.041(4) 0.081(7) 0.023(4) 0.015(5) 0.013(4) O9B 0.070(15) 0.045(9) 0.094(13) 0.002(7) -0.005(10) -0.011(7) C24A 0.052(6) 0.082(8) 0.082(9) 0.001(8) 0.011(7) -0.019(5) C21A 0.081(7) 0.036(4) 0.076(8) 0.016(4) 0.016(5) -0.013(4) C19B 0.056(5) 0.037(4) 0.059(7) 0.002(4) 0.001(4) 0.011(4) C20B 0.084(7) 0.025(4) 0.104(9) 0.009(5) 0.014(6) 0.013(4) C21B 0.087(8) 0.026(4) 0.083(9) 0.009(5) 0.005(6) -0.011(4) C24B 0.055(7) 0.062(7) 0.099(12) 0.001(9) 0.011(8) -0.015(5) C18B 0.045(5) 0.046(6) 0.016(7) 0.016(7) 0.005(7) 0.009(4) C22B 0.052(9) 0.021(8) 0.060(13) -0.009(6) -0.004(8) -0.024(5) O9A 0.073(12) 0.061(13) 0.102(14) 0.025(10) 0.039(10) -0.024(8) C26A 0.051(8) 0.19(2) 0.29(3) -0.167(19) -0.066(12) 0.045(10) C8B 0.087(11) 0.190(19) 0.069(11) -0.001(11) 0.042(9) 0.000(11) O12B 0.027(4) 0.168(12) 0.40(3) -0.228(16) 0.035(8) -0.047(6) C25B 0.145(14) 0.181(16) 0.109(12) -0.067(11) -0.018(10) 0.051(12) C26B 0.065(7) 0.101(10) 0.161(18) -0.008(11) 0.005(9) 0.015(7) _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 O5 2.434(2) 3_556 ? La1 O7 2.460(2) . ? La1 O4 2.464(2) . ? La1 O1 2.487(3) . ? La1 O2 2.511(2) 3_656 ? La1 O8 2.530(2) 3_656 ? La1 O11 2.6181(12) . ? La1 O10 2.665(2) . ? S1 O10 1.508(2) . ? S1 C25 1.790(5) . ? S1 C26 1.791(4) . ? O1 C1 1.249(4) . ? C1 O2 1.258(4) . ? C1 C2B 1.388(9) . ? C1 C2A 1.585(7) . ? O2 La1 2.511(2) 3_656 ? C2A C7A 1.378(8) . ? C2A C3A 1.398(7) . ? C3A C4A 1.397(9) . ? C3A H3A 0.9300 . ? C4A C5A 1.347(12) . ? C4A O3A 1.378(9) . ? C5A C6A 1.388(11) . ? C5A H5A 0.9300 . ? C6A C7A 1.406(8) . ? C6A H6A 0.9300 . ? C7A H7A 0.9300 . ? O3A C8A 1.553(19) . ? C2B C7B 1.378(9) . ? C2B C3B 1.399(7) . ? C3B C4B 1.397(9) . ? C3B H3B 0.9300 . ? C4B C5B 1.347(12) . ? C4B O3B 1.378(9) . ? C5B C6B 1.388(11) . ? C5B H5B 0.9300 . ? C6B C7B 1.406(8) . ? C6B H6B 0.9300 . ? C7B H7B 0.9300 . ? O3B C8B 1.24(2) . ? O4 C9 1.248(4) . ? O5 C9 1.251(4) . ? O5 La1 2.434(2) 3_556 ? O6 C12 1.373(7) . ? O6 C16 1.381(10) . ? O7 C17 1.253(4) . ? O8 C17 1.250(4) . ? O8 La1 2.530(2) 3_656 ? C8A H8A1 0.9600 . ? C8A H8A2 0.9600 . ? C8A H8A3 0.9600 . ? C9 C10 1.498(5) . ? O11 H2O 0.8839 . ? O11 H1O 0.8771 . ? C10 C15 1.381(5) . ? C10 C11 1.392(5) . ? C11 C12 1.377(6) . ? C11 H11 0.9300 . ? C12 C13 1.373(10) . ? C13 C14 1.358(10) . ? C13 H13 0.9300 . ? C14 C15 1.390(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18B 1.50(2) . ? C17 C18A 1.511(19) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? S2 O12A 1.399(10) . ? S2 O12B 1.439(5) . ? S2 C26A 1.545(18) . ? S2 C26B 1.736(13) . ? S2 C25B 1.866(14) . ? S2 C25A 1.875(10) . ? C25A H25D 0.9600 . ? C25A H25E 0.9600 . ? C25A H25F 0.9600 . ? C23A C22A 1.28(2) . ? C23A C18A 1.39(2) . ? C23A H23A 0.9300 . ? C22A C21A 1.40(2) . ? C22A O9A 1.45(3) . ? C18A C19A 1.346(19) . ? C19A C20A 1.378(10) . ? C19A H19A 0.9300 . ? C20A C21A 1.369(12) . ? C20A H20A 0.9300 . ? O9B C22B 1.22(4) . ? O9B C24B 1.50(4) . ? C24A O9A 1.43(4) . ? C24A H24A 0.9600 . ? C24A H24B 0.9600 . ? C24A H24C 0.9600 . ? C21A H21A 0.9300 . ? C19B C20B 1.390(12) . ? C19B C18B 1.43(2) . ? C19B H19B 0.9300 . ? C20B C21B 1.377(14) . ? C20B H20B 0.9300 . ? C21B C22B 1.36(3) . ? C21B H21B 0.9300 . ? C24B H24D 0.9600 . ? C24B H24E 0.9600 . ? C24B H24F 0.9600 . ? C26A H26D 0.9600 . ? C26A H26E 0.9600 . ? C26A H26F 0.9600 . ? C8B H8B1 0.9600 . ? C8B H8B2 0.9600 . ? C8B H8B3 0.9600 . ? C25B H25G 0.9600 . ? C25B H25H 0.9600 . ? C25B H25I 0.9600 . ? C26B H26G 0.9600 . ? C26B H26H 0.9600 . ? C26B H26I 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 O5 La1 O7 143.95(8) 3_556 . ? O5 La1 O4 93.61(8) 3_556 . ? O7 La1 O4 83.05(8) . . ? O5 La1 O1 143.22(8) 3_556 . ? O7 La1 O1 71.90(8) . . ? O4 La1 O1 81.05(9) . . ? O5 La1 O2 79.09(8) 3_556 3_656 ? O7 La1 O2 80.49(8) . 3_656 ? O4 La1 O2 139.42(8) . 3_656 ? O1 La1 O2 127.21(8) . 3_656 ? O5 La1 O8 80.84(8) 3_556 3_656 ? O7 La1 O8 122.41(8) . 3_656 ? O4 La1 O8 142.18(8) . 3_656 ? O1 La1 O8 81.61(9) . 3_656 ? O2 La1 O8 76.56(9) 3_656 3_656 ? O5 La1 O11 72.49(8) 3_556 . ? O7 La1 O11 138.32(8) . . ? O4 La1 O11 72.78(7) . . ? O1 La1 O11 71.18(7) . . ? O2 La1 O11 138.66(9) 3_656 . ? O8 La1 O11 69.87(8) 3_656 . ? O5 La1 O10 70.18(8) 3_556 . ? O7 La1 O10 75.21(7) . . ? O4 La1 O10 69.00(8) . . ? O1 La1 O10 137.61(9) . . ? O2 La1 O10 71.01(8) 3_656 . ? O8 La1 O10 139.68(8) 3_656 . ? O11 La1 O10 123.52(5) . . ? O10 S1 C25 104.7(2) . . ? O10 S1 C26 106.0(2) . . ? C25 S1 C26 97.5(2) . . ? C1 O1 La1 139.3(2) . . ? O1 C1 O2 125.6(3) . . ? O1 C1 C2B 109.2(6) . . ? O2 C1 C2B 125.0(6) . . ? O1 C1 C2A 121.2(4) . . ? O2 C1 C2A 113.1(4) . . ? C2B C1 C2A 14.3(8) . . ? C1 O2 La1 136.1(2) . 3_656 ? C7A C2A C3A 121.3(6) . . ? C7A C2A C1 119.6(5) . . ? C3A C2A C1 119.0(7) . . ? C4A C3A C2A 118.6(7) . . ? C4A C3A H3A 120.7 . . ? C2A C3A H3A 120.7 . . ? C5A C4A O3A 116.9(7) . . ? C5A C4A C3A 120.4(7) . . ? O3A C4A C3A 122.7(8) . . ? C4A C5A C6A 121.3(7) . . ? C4A C5A H5A 119.3 . . ? C6A C5A H5A 119.3 . . ? C5A C6A C7A 119.7(7) . . ? C5A C6A H6A 120.1 . . ? C7A C6A H6A 120.1 . . ? C2A C7A C6A 118.4(8) . . ? C2A C7A H7A 120.8 . . ? C6A C7A H7A 120.8 . . ? C4A O3A C8A 113.3(10) . . ? C7B C2B C1 120.1(8) . . ? C7B C2B C3B 121.2(6) . . ? C1 C2B C3B 118.5(9) . . ? C4B C3B C2B 118.5(7) . . ? C4B C3B H3B 120.7 . . ? C2B C3B H3B 120.7 . . ? C5B C4B O3B 116.9(7) . . ? C5B C4B C3B 120.4(7) . . ? O3B C4B C3B 122.7(8) . . ? C4B C5B C6B 121.3(7) . . ? C4B C5B H5B 119.3 . . ? C6B C5B H5B 119.3 . . ? C5B C6B C7B 119.6(7) . . ? C5B C6B H6B 120.2 . . ? C7B C6B H6B 120.2 . . ? C2B C7B C6B 118.3(8) . . ? C2B C7B H7B 120.8 . . ? C6B C7B H7B 120.8 . . ? C8B O3B C4B 130.7(14) . . ? C9 O4 La1 142.6(2) . . ? C9 O5 La1 155.8(2) . 3_556 ? C12 O6 C16 116.8(5) . . ? C17 O7 La1 172.4(2) . . ? C17 O8 La1 108.2(2) . 3_656 ? O3A C8A H8A1 109.5 . . ? O3A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? O3A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? O4 C9 O5 124.4(3) . . ? O4 C9 C10 117.8(3) . . ? O5 C9 C10 117.8(3) . . ? La1 O11 H2O 125.0 . . ? La1 O11 H1O 135.4 . . ? H2O O11 H1O 96.1 . . ? C15 C10 C11 120.3(4) . . ? C15 C10 C9 120.5(4) . . ? C11 C10 C9 119.2(3) . . ? S1 O10 La1 125.32(13) . . ? C12 C11 C10 120.3(5) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? O6 C12 C13 115.9(6) . . ? O6 C12 C11 124.9(6) . . ? C13 C12 C11 119.2(6) . . ? C14 C13 C12 120.8(6) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 121.3(6) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C10 C15 C14 118.2(5) . . ? C10 C15 H15 120.9 . . ? C14 C15 H15 120.9 . . ? O6 C16 H16A 109.5 . . ? O6 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O6 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O8 C17 O7 122.6(3) . . ? O8 C17 C18B 118.0(9) . . ? O7 C17 C18B 118.2(9) . . ? O8 C17 C18A 116.7(8) . . ? O7 C17 C18A 120.2(8) . . ? C18B C17 C18A 18.7(6) . . ? S1 C25 H25A 109.5 . . ? S1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? S1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? S1 C26 H26A 109.5 . . ? S1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? S1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O12A S2 O12B 28.9(10) . . ? O12A S2 C26A 102.9(13) . . ? O12B S2 C26A 74.1(9) . . ? O12A S2 C26B 84.1(8) . . ? O12B S2 C26B 100.6(7) . . ? C26A S2 C26B 126.4(9) . . ? O12A S2 C25B 65.7(9) . . ? O12B S2 C25B 87.1(8) . . ? C26A S2 C25B 134.6(8) . . ? C26B S2 C25B 97.2(8) . . ? O12A S2 C25A 98.2(6) . . ? O12B S2 C25A 99.2(6) . . ? C26A S2 C25A 93.5(7) . . ? C26B S2 C25A 33.6(6) . . ? C25B S2 C25A 130.7(7) . . ? S2 C25A H25D 109.5 . . ? S2 C25A H25E 109.5 . . ? H25D C25A H25E 109.5 . . ? S2 C25A H25F 109.5 . . ? H25D C25A H25F 109.5 . . ? H25E C25A H25F 109.5 . . ? C22A C23A C18A 118.7(13) . . ? C22A C23A H23A 120.6 . . ? C18A C23A H23A 120.6 . . ? C23A C22A C21A 122.3(16) . . ? C23A C22A O9A 127(2) . . ? C21A C22A O9A 110.9(19) . . ? C19A C18A C23A 122.4(14) . . ? C19A C18A C17 116.6(14) . . ? C23A C18A C17 120.7(12) . . ? C18A C19A C20A 117.9(11) . . ? C18A C19A H19A 121.1 . . ? C20A C19A H19A 121.1 . . ? C21A C20A C19A 120.3(7) . . ? C21A C20A H20A 119.9 . . ? C19A C20A H20A 119.9 . . ? C22B O9B C24B 119(3) . . ? O9A C24A H24A 109.5 . . ? O9A C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? O9A C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? C20A C21A C22A 118.2(10) . . ? C20A C21A H21A 120.9 . . ? C22A C21A H21A 120.9 . . ? C20B C19B C18B 120.4(12) . . ? C20B C19B H19B 119.8 . . ? C18B C19B H19B 119.8 . . ? C21B C20B C19B 121.2(8) . . ? C21B C20B H20B 119.4 . . ? C19B C20B H20B 119.4 . . ? C22B C21B C20B 123.6(12) . . ? C22B C21B H21B 118.2 . . ? C20B C21B H21B 118.2 . . ? O9B C24B H24D 109.5 . . ? O9B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? O9B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C19B C18B C17 121.3(15) . . ? O9B C22B C21B 119(2) . . ? C24A O9A C22A 115(2) . . ? S2 C26A H26D 109.5 . . ? S2 C26A H26E 109.5 . . ? H26D C26A H26E 109.5 . . ? S2 C26A H26F 109.5 . . ? H26D C26A H26F 109.5 . . ? H26E C26A H26F 109.5 . . ? O3B C8B H8B1 109.5 . . ? O3B C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? O3B C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? S2 C25B H25G 109.5 . . ? S2 C25B H25H 109.5 . . ? H25G C25B H25H 109.5 . . ? S2 C25B H25I 109.5 . . ? H25G C25B H25I 109.5 . . ? H25H C25B H25I 109.5 . . ? S2 C26B H26G 109.5 . . ? S2 C26B H26H 109.5 . . ? H26G C26B H26H 109.5 . . ? S2 C26B H26I 109.5 . . ? H26G C26B H26I 109.5 . . ? H26H C26B H26I 109.5 . . ? 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 O11 H2O O10 0.88 2.09 2.951(2) 163.4 3_556 O11 H1O O12B 0.88 1.94 2.756(8) 153.8 . O11 H1O O12A 0.88 2.50 3.235(18) 142.5 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.707 _refine_diff_density_min -0.793 _refine_diff_density_rms 0.080 # Attachment '13.CIF' data_C:\HB18DMSO.CIF _database_code_depnum_ccdc_archive 'CCDC 634368' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common HB18DMSO _chemical_melting_point ? _chemical_formula_moiety 'C29 H35 La1 O14 S1' _chemical_formula_sum 'C29 H35 La1 O14 S1' _chemical_formula_weight 778.54 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' O O 0.0106 0.0060 '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' 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 9.6002(2) _cell_length_b 11.3814(2) _cell_length_c 14.8606(3) _cell_angle_alpha 95.295(1) _cell_angle_beta 101.131(1) _cell_angle_gamma 95.719(1) _cell_volume 1574.87(5) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 1.491 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7161 _exptl_absorpt_correction_T_max 0.8184 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 X8 Apex II CCD' _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 11366 _diffrn_reflns_av_R_equivalents 0.0150 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7208 _reflns_number_gt 6904 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^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_extinction_expression ? _refine_ls_number_reflns 7208 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0230 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0525 _refine_ls_wR_factor_gt 0.0516 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 La1 La 0.720222(10) 0.514751(9) 0.482088(7) 0.01068(4) Uani 1 1 d . . . S1 S 0.77811(5) 0.66922(5) 0.28154(3) 0.01984(10) Uani 1 1 d . . . O1 O 0.58576(14) 0.47027(13) 0.31599(9) 0.0170(3) Uani 1 1 d . . . C1 C 0.4540(2) 0.45336(16) 0.31484(12) 0.0131(3) Uani 1 1 d . . . O2 O 0.40289(15) 0.46756(12) 0.38685(9) 0.0160(3) Uani 1 1 d . . . C2 C 0.3546(2) 0.41623(16) 0.22372(12) 0.0135(3) Uani 1 1 d . . . O3 O 0.36911(17) 0.34019(14) -0.02201(9) 0.0241(3) Uani 1 1 d . . . C3 C 0.4125(2) 0.39341(17) 0.14478(13) 0.0156(4) Uani 1 1 d . . . H3 H 0.5132 0.4002 0.1502 0.019 Uiso 1 1 calc R . . O4 O 0.09533(17) 0.31399(16) -0.03500(10) 0.0306(4) Uani 1 1 d . . . C4 C 0.3235(2) 0.36118(17) 0.05952(13) 0.0179(4) Uani 1 1 d . . . O5 O 0.59864(15) 0.69467(12) 0.47093(9) 0.0174(3) Uani 1 1 d . . . C5 C 0.1743(2) 0.34900(19) 0.05199(13) 0.0204(4) Uani 1 1 d . . . O6 O 0.39950(15) 0.69300(12) 0.52839(10) 0.0187(3) Uani 1 1 d . . . C6 C 0.1177(2) 0.37253(19) 0.12974(14) 0.0211(4) Uani 1 1 d . . . H6 H 0.0169 0.3660 0.1245 0.025 Uiso 1 1 calc R . . O7 O 0.8583(2) 1.1081(2) 0.57890(13) 0.0567(7) Uani 1 1 d . . . C7 C 0.2081(2) 0.40578(17) 0.21576(13) 0.0169(4) Uani 1 1 d . . . H7 H 0.1687 0.4213 0.2690 0.020 Uiso 1 1 calc R . . O8 O 0.71481(18) 1.20923(13) 0.68810(11) 0.0266(3) Uani 1 1 d . . . C8 C 0.5196(3) 0.3438(2) -0.01636(15) 0.0275(5) Uani 1 1 d . . . H8A H 0.5388 0.3274 -0.0785 0.041 Uiso 1 1 calc R . . H8B H 0.5564 0.2836 0.0220 0.041 Uiso 1 1 calc R . . H8C H 0.5670 0.4227 0.0113 0.041 Uiso 1 1 calc R . . O9 O 0.90536(14) 0.65773(12) 0.58613(9) 0.0175(3) Uani 1 1 d . . . C9 C -0.0553(3) 0.2880(4) -0.04436(18) 0.0553(9) Uani 1 1 d . . . H9A H -0.0995 0.2640 -0.1095 0.083 Uiso 1 1 calc R . . H9B H -0.0944 0.3589 -0.0221 0.083 Uiso 1 1 calc R . . H9C H -0.0757 0.2232 -0.0080 0.083 Uiso 1 1 calc R . . O10 O 1.11747(15) 0.59310(13) 0.59230(10) 0.0208(3) Uani 1 1 d . . . C10 C 0.5184(2) 0.74138(16) 0.51822(13) 0.0152(4) Uani 1 1 d . . . O11 O 0.9838(3) 0.9654(2) 0.86672(17) 0.0655(8) Uani 1 1 d . . . C11 C 0.5687(2) 0.86495(17) 0.56550(13) 0.0156(4) Uani 1 1 d . . . C12 C 0.6918(2) 0.92745(19) 0.54900(14) 0.0208(4) Uani 1 1 d . . . H12 H 0.7452 0.8908 0.5091 0.025 Uiso 1 1 calc R . . O12A O 1.2311(4) 1.0129(4) 0.9268(3) 0.0358(13) Uani 0.493(6) 1 d P A 1 O12B O 1.2817(4) 0.9485(3) 0.9533(2) 0.0275(11) Uani 0.507(6) 1 d P A 2 O13 O 0.84413(15) 0.65271(13) 0.38035(9) 0.0183(3) Uani 1 1 d . . . C13 C 0.7368(2) 1.04211(19) 0.59000(14) 0.0231(4) Uani 1 1 d . . . O14 O 0.86585(17) 0.39835(13) 0.60679(10) 0.0179(3) Uani 1 1 d . . . C14 C 0.6595(2) 1.09566(17) 0.64979(14) 0.0208(4) Uani 1 1 d . . . H1O H 0.944(3) 0.387(3) 0.602(2) 0.033(8) Uiso 1 1 d . . . C15 C 0.5389(2) 1.03378(19) 0.66744(16) 0.0242(4) Uani 1 1 d . . . H15 H 0.4867 1.0698 0.7084 0.029 Uiso 1 1 calc R . . C16 C 0.4934(2) 0.91843(18) 0.62522(15) 0.0208(4) Uani 1 1 d . . . H16 H 0.4100 0.8760 0.6375 0.025 Uiso 1 1 calc R . . C17 C 0.8849(3) 1.1140(3) 0.49332(19) 0.0444(7) Uani 1 1 d . . . H17A H 0.9753 1.1644 0.4973 0.067 Uiso 1 1 calc R . . H17B H 0.8070 1.1479 0.4553 0.067 Uiso 1 1 calc R . . H17C H 0.8917 1.0340 0.4652 0.067 Uiso 1 1 calc R . . C18 C 0.6324(3) 1.2704(2) 0.74278(18) 0.0328(5) Uani 1 1 d . . . H18A H 0.6821 1.3499 0.7664 0.049 Uiso 1 1 calc R . . H18B H 0.6197 1.2260 0.7947 0.049 Uiso 1 1 calc R . . H18C H 0.5386 1.2774 0.7049 0.049 Uiso 1 1 calc R . . C19 C 1.0362(2) 0.66091(16) 0.62042(12) 0.0134(3) Uani 1 1 d . . . H2O H 0.825(4) 0.335(3) 0.611(2) 0.053(10) Uiso 1 1 d . . . C20 C 1.0980(2) 0.75110(17) 0.70271(13) 0.0156(4) Uani 1 1 d . A . C21 C 1.0090(2) 0.82173(18) 0.74065(14) 0.0210(4) Uani 1 1 d . . . H21 H 0.9110 0.8175 0.7118 0.025 Uiso 1 1 calc R . . C22 C 1.0632(3) 0.8984(2) 0.82058(18) 0.0377(6) Uani 1 1 d . A . C23 C 1.2078(3) 0.9069(3) 0.85995(19) 0.0560(10) Uani 1 1 d . . . C24 C 1.2969(3) 0.8410(3) 0.82068(17) 0.0425(7) Uani 1 1 d . A . H24 H 1.3963 0.8499 0.8470 0.051 Uiso 1 1 calc R . . C25 C 1.2422(2) 0.7608(2) 0.74219(15) 0.0248(4) Uani 1 1 d . . . H25 H 1.3033 0.7131 0.7160 0.030 Uiso 1 1 calc R A . C26 C 0.8357(4) 0.9518(3) 0.8330(2) 0.0481(8) Uani 1 1 d . . . H26A H 0.7912 1.0046 0.8719 0.072 Uiso 1 1 calc R . . H26B H 0.7966 0.8691 0.8341 0.072 Uiso 1 1 calc R . . H26C H 0.8159 0.9720 0.7695 0.072 Uiso 1 1 calc R . . C27A C 1.3775(6) 1.0347(5) 0.9708(4) 0.0375(15) Uani 0.493(6) 1 d P A 1 H27A H 1.3929 1.1060 1.0155 0.056 Uiso 0.493(6) 1 calc PR A 1 H27B H 1.4359 1.0469 0.9244 0.056 Uiso 0.493(6) 1 calc PR A 1 H27C H 1.4049 0.9665 1.0028 0.056 Uiso 0.493(6) 1 calc PR A 1 C27B C 1.2881(7) 1.0751(5) 0.9583(4) 0.0352(14) Uani 0.507(6) 1 d P A 2 H27D H 1.3374 1.1107 1.0203 0.053 Uiso 0.507(6) 1 calc PR A 2 H27E H 1.1909 1.0975 0.9454 0.053 Uiso 0.507(6) 1 calc PR A 2 H27F H 1.3405 1.1039 0.9126 0.053 Uiso 0.507(6) 1 calc PR A 2 C28 C 0.8357(3) 0.5555(2) 0.21138(14) 0.0260(5) Uani 1 1 d . . . H28A H 0.7860 0.4782 0.2178 0.039 Uiso 1 1 calc R . . H28B H 0.9391 0.5549 0.2311 0.039 Uiso 1 1 calc R . . H28C H 0.8136 0.5709 0.1467 0.039 Uiso 1 1 calc R . . C29 C 0.8843(3) 0.7936(2) 0.25468(17) 0.0332(5) Uani 1 1 d . . . H29A H 0.8655 0.8664 0.2885 0.050 Uiso 1 1 calc R . . H29B H 0.8601 0.7992 0.1882 0.050 Uiso 1 1 calc R . . H29C H 0.9858 0.7835 0.2726 0.050 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 0.00949(5) 0.01414(6) 0.00819(5) -0.00143(4) 0.00341(4) -0.00022(4) S1 0.0176(2) 0.0263(2) 0.0165(2) 0.00691(19) 0.00382(18) 0.00198(19) O1 0.0127(6) 0.0258(7) 0.0119(6) 0.0000(5) 0.0034(5) 0.0002(5) C1 0.0158(9) 0.0133(8) 0.0106(8) 0.0004(6) 0.0037(7) 0.0017(7) O2 0.0191(7) 0.0199(7) 0.0097(6) -0.0007(5) 0.0062(5) 0.0022(5) C2 0.0163(9) 0.0143(8) 0.0097(8) 0.0002(6) 0.0033(7) 0.0006(7) O3 0.0274(8) 0.0352(8) 0.0088(6) -0.0027(6) 0.0067(6) -0.0020(6) C3 0.0161(9) 0.0187(9) 0.0120(8) 0.0002(7) 0.0047(7) -0.0001(7) O4 0.0241(8) 0.0503(10) 0.0114(7) 0.0015(7) -0.0014(6) -0.0122(7) C4 0.0237(10) 0.0194(9) 0.0109(8) 0.0009(7) 0.0063(7) -0.0013(8) O5 0.0184(7) 0.0166(6) 0.0182(7) 0.0000(5) 0.0066(5) 0.0031(5) C5 0.0218(10) 0.0251(10) 0.0109(9) 0.0025(7) -0.0010(7) -0.0051(8) O6 0.0141(7) 0.0165(6) 0.0248(7) -0.0002(5) 0.0051(6) -0.0015(5) C6 0.0158(9) 0.0294(11) 0.0164(9) 0.0031(8) 0.0023(8) -0.0038(8) O7 0.0630(14) 0.0654(14) 0.0329(10) -0.0215(9) 0.0305(10) -0.0505(11) C7 0.0174(9) 0.0212(9) 0.0122(9) 0.0004(7) 0.0054(7) -0.0007(7) O8 0.0336(9) 0.0151(7) 0.0282(8) -0.0041(6) 0.0055(7) -0.0034(6) C8 0.0319(12) 0.0358(12) 0.0180(10) -0.0003(9) 0.0136(9) 0.0051(10) O9 0.0148(7) 0.0203(7) 0.0153(7) -0.0008(5) 0.0011(5) -0.0018(5) C9 0.0275(14) 0.106(3) 0.0204(12) 0.0008(14) -0.0050(10) -0.0258(16) O10 0.0200(7) 0.0224(7) 0.0218(7) -0.0033(6) 0.0111(6) 0.0028(6) C10 0.0152(9) 0.0158(9) 0.0143(9) 0.0026(7) 0.0018(7) 0.0026(7) O11 0.0609(14) 0.0593(14) 0.0728(16) -0.0474(12) 0.0452(13) -0.0201(11) C11 0.0150(9) 0.0159(9) 0.0156(9) 0.0012(7) 0.0030(7) 0.0016(7) C12 0.0207(10) 0.0247(10) 0.0167(9) -0.0033(8) 0.0084(8) -0.0030(8) O12A 0.041(2) 0.028(2) 0.028(2) -0.0171(17) -0.0059(17) 0.0013(19) O12B 0.034(2) 0.0236(19) 0.0187(16) -0.0054(13) -0.0035(13) 0.0005(15) O13 0.0176(7) 0.0253(7) 0.0128(6) 0.0039(5) 0.0050(5) 0.0004(6) C13 0.0255(11) 0.0237(10) 0.0184(10) -0.0003(8) 0.0083(8) -0.0100(8) O14 0.0137(7) 0.0208(7) 0.0203(7) 0.0052(6) 0.0048(6) 0.0017(6) C14 0.0255(11) 0.0146(9) 0.0197(10) 0.0001(7) 0.0008(8) -0.0005(8) C15 0.0214(10) 0.0217(10) 0.0293(11) -0.0060(8) 0.0089(9) 0.0028(8) C16 0.0154(9) 0.0213(10) 0.0256(10) -0.0024(8) 0.0087(8) -0.0018(8) C17 0.0353(14) 0.0631(19) 0.0337(14) 0.0044(13) 0.0169(11) -0.0183(13) C18 0.0381(13) 0.0204(11) 0.0373(13) -0.0068(9) 0.0053(11) 0.0051(10) C19 0.0143(8) 0.0148(8) 0.0111(8) 0.0000(7) 0.0048(7) -0.0017(7) C20 0.0177(9) 0.0165(9) 0.0111(8) -0.0007(7) 0.0032(7) -0.0032(7) C21 0.0252(10) 0.0181(9) 0.0197(10) -0.0019(8) 0.0095(8) -0.0026(8) C22 0.0447(15) 0.0337(13) 0.0342(13) -0.0165(11) 0.0254(12) -0.0138(11) C23 0.0482(17) 0.080(2) 0.0271(13) -0.0307(14) 0.0173(12) -0.0397(16) C24 0.0262(12) 0.0688(19) 0.0225(12) -0.0037(12) -0.0007(10) -0.0219(13) C25 0.0198(10) 0.0304(11) 0.0214(10) 0.0028(9) 0.0012(8) -0.0039(9) C26 0.071(2) 0.0416(15) 0.0430(16) 0.0022(12) 0.0294(15) 0.0274(15) C27A 0.037(3) 0.034(3) 0.032(3) -0.013(2) -0.004(2) -0.005(2) C27B 0.046(4) 0.027(3) 0.027(3) -0.008(2) -0.002(2) 0.003(3) C28 0.0288(11) 0.0338(12) 0.0156(10) 0.0020(8) 0.0067(8) 0.0009(9) C29 0.0421(14) 0.0320(12) 0.0249(11) 0.0114(10) 0.0070(10) -0.0067(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 La1 O10 2.4397(13) 2_766 ? La1 O5 2.4591(13) . ? La1 O2 2.4687(13) 2_666 ? La1 O9 2.4689(13) . ? La1 O6 2.5014(14) 2_666 ? La1 O1 2.5345(13) . ? La1 O13 2.6319(14) . ? La1 O14 2.6393(14) . ? La1 O2 3.0727(14) . ? La1 La1 4.3468(2) 2_666 ? La1 La1 5.3424(2) 2_766 ? S1 O13 1.5193(14) . ? S1 C29 1.782(2) . ? S1 C28 1.784(2) . ? O1 C1 1.256(2) . ? C1 O2 1.265(2) . ? C1 C2 1.496(3) . ? O2 La1 2.4687(13) 2_666 ? C2 C7 1.381(3) . ? C2 C3 1.406(2) . ? O3 C4 1.374(2) . ? O3 C8 1.427(3) . ? C3 C4 1.380(3) . ? C3 H3 0.9500 . ? O4 C5 1.368(2) . ? O4 C9 1.424(3) . ? C4 C5 1.407(3) . ? O5 C10 1.262(2) . ? C5 C6 1.385(3) . ? O6 C10 1.259(2) . ? O6 La1 2.5014(13) 2_666 ? C6 C7 1.396(3) . ? C6 H6 0.9500 . ? O7 C17 1.351(3) . ? O7 C13 1.369(3) . ? C7 H7 0.9500 . ? O8 C14 1.374(2) . ? O8 C18 1.423(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O9 C19 1.256(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? O10 C19 1.251(2) . ? O10 La1 2.4397(13) 2_766 ? C10 C11 1.502(3) . ? O11 C22 1.361(3) . ? O11 C26 1.401(4) . ? C11 C16 1.385(3) . ? C11 C12 1.392(3) . ? C12 C13 1.378(3) . ? C12 H12 0.9500 . ? O12A C27A 1.417(7) . ? O12A C23 1.460(5) . ? O12B C27B 1.431(7) . ? O12B C23 1.444(4) . ? C13 C14 1.398(3) . ? O14 H1O 0.78(3) . ? O14 H2O 0.80(4) . ? C14 C15 1.377(3) . ? C15 C16 1.391(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.506(2) . ? C20 C25 1.385(3) . ? C20 C21 1.390(3) . ? C21 C22 1.387(3) . ? C21 H21 0.9500 . ? C22 C23 1.389(4) . ? C23 C24 1.370(5) . ? C24 C25 1.393(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27A H27A 0.9800 . ? C27A H27B 0.9800 . ? C27A H27C 0.9800 . ? C27B H27D 0.9800 . ? C27B H27E 0.9800 . ? C27B H27F 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? 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 O10 La1 O5 140.34(5) 2_766 . ? O10 La1 O2 146.36(5) 2_766 2_666 ? O5 La1 O2 73.06(4) . 2_666 ? O10 La1 O9 96.84(5) 2_766 . ? O5 La1 O9 80.85(5) . . ? O2 La1 O9 82.86(5) 2_666 . ? O10 La1 O6 80.06(5) 2_766 2_666 ? O5 La1 O6 125.75(5) . 2_666 ? O2 La1 O6 79.28(5) 2_666 2_666 ? O9 La1 O6 140.55(5) . 2_666 ? O10 La1 O1 76.96(5) 2_766 . ? O5 La1 O1 81.28(5) . . ? O2 La1 O1 122.46(4) 2_666 . ? O9 La1 O1 142.44(5) . . ? O6 La1 O1 75.66(5) 2_666 . ? O10 La1 O13 70.00(5) 2_766 . ? O5 La1 O13 71.77(4) . . ? O2 La1 O13 139.22(4) 2_666 . ? O9 La1 O13 71.82(4) . . ? O6 La1 O13 139.30(4) 2_666 . ? O1 La1 O13 71.28(4) . . ? O10 La1 O14 72.38(5) 2_766 . ? O5 La1 O14 140.38(5) . . ? O2 La1 O14 75.72(5) 2_666 . ? O9 La1 O14 71.57(5) . . ? O6 La1 O14 70.04(5) 2_666 . ? O1 La1 O14 137.03(5) . . ? O13 La1 O14 122.69(5) . . ? O10 La1 O2 115.71(4) 2_766 . ? O5 La1 O2 65.84(4) . . ? O2 La1 O2 77.21(4) 2_666 . ? O9 La1 O2 144.86(4) . . ? O6 La1 O2 62.99(4) 2_666 . ? O1 La1 O2 45.26(4) . . ? O13 La1 O2 105.94(4) . . ? O14 La1 O2 129.03(4) . . ? O10 La1 La1 141.21(3) 2_766 2_666 ? O5 La1 La1 62.94(3) . 2_666 ? O2 La1 La1 43.58(3) 2_666 2_666 ? O9 La1 La1 120.50(3) . 2_666 ? O6 La1 La1 64.75(3) 2_666 2_666 ? O1 La1 La1 78.89(3) . 2_666 ? O13 La1 La1 128.62(3) . 2_666 ? O14 La1 La1 107.76(3) . 2_666 ? O2 La1 La1 33.63(2) . 2_666 ? O10 La1 La1 40.47(4) 2_766 2_766 ? O5 La1 La1 127.48(3) . 2_766 ? O2 La1 La1 124.00(3) 2_666 2_766 ? O9 La1 La1 56.94(3) . 2_766 ? O6 La1 La1 106.72(3) 2_666 2_766 ? O1 La1 La1 112.63(3) . 2_766 ? O13 La1 La1 66.62(3) . 2_766 ? O14 La1 La1 56.63(3) . 2_766 ? O2 La1 La1 155.94(2) . 2_766 ? La1 La1 La1 164.378(5) 2_666 2_766 ? O13 S1 C29 105.31(10) . . ? O13 S1 C28 105.34(9) . . ? C29 S1 C28 98.36(12) . . ? C1 O1 La1 108.90(11) . . ? O1 C1 O2 122.83(17) . . ? O1 C1 C2 117.97(16) . . ? O2 C1 C2 119.19(16) . . ? C1 O2 La1 174.19(13) . 2_666 ? C1 O2 La1 82.80(11) . . ? La1 O2 La1 102.79(4) 2_666 . ? C7 C2 C3 119.75(17) . . ? C7 C2 C1 121.32(16) . . ? C3 C2 C1 118.93(17) . . ? C4 O3 C8 117.01(16) . . ? C4 C3 C2 120.27(18) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 O4 C9 117.28(18) . . ? O3 C4 C3 124.83(18) . . ? O3 C4 C5 115.42(17) . . ? C3 C4 C5 119.75(18) . . ? C10 O5 La1 132.58(12) . . ? O4 C5 C6 124.82(19) . . ? O4 C5 C4 115.36(18) . . ? C6 C5 C4 119.82(18) . . ? C10 O6 La1 136.44(12) . 2_666 ? C5 C6 C7 120.20(19) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C17 O7 C13 119.6(2) . . ? C2 C7 C6 120.19(18) . . ? C2 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C14 O8 C18 116.69(18) . . ? O3 C8 H8A 109.5 . . ? O3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C19 O9 La1 136.17(12) . . ? O4 C9 H9A 109.5 . . ? O4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C19 O10 La1 170.04(13) . 2_766 ? O6 C10 O5 125.23(18) . . ? O6 C10 C11 117.62(17) . . ? O5 C10 C11 117.15(17) . . ? C22 O11 C26 117.4(2) . . ? C16 C11 C12 119.21(18) . . ? C16 C11 C10 120.72(17) . . ? C12 C11 C10 120.07(17) . . ? C13 C12 C11 120.57(19) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C27A O12A C23 109.7(4) . . ? C27B O12B C23 104.3(4) . . ? S1 O13 La1 123.88(8) . . ? O7 C13 C12 123.9(2) . . ? O7 C13 C14 116.21(19) . . ? C12 C13 C14 119.82(19) . . ? La1 O14 H1O 118(2) . . ? La1 O14 H2O 113(3) . . ? H1O O14 H2O 106(3) . . ? O8 C14 C15 124.93(19) . . ? O8 C14 C13 115.14(19) . . ? C15 C14 C13 119.92(19) . . ? C14 C15 C16 119.96(19) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C11 C16 C15 120.50(19) . . ? C11 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? O7 C17 H17A 109.5 . . ? O7 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O7 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O8 C18 H18A 109.5 . . ? O8 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O8 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O10 C19 O9 124.71(17) . . ? O10 C19 C20 117.97(17) . . ? O9 C19 C20 117.30(16) . . ? C25 C20 C21 120.20(19) . . ? C25 C20 C19 119.96(18) . . ? C21 C20 C19 119.81(18) . . ? C22 C21 C20 120.1(2) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? O11 C22 C21 124.8(3) . . ? O11 C22 C23 115.9(2) . . ? C21 C22 C23 119.2(2) . . ? C24 C23 C22 120.8(2) . . ? C24 C23 O12B 106.9(3) . . ? C22 C23 O12B 129.7(3) . . ? C24 C23 O12A 133.8(3) . . ? C22 C23 O12A 103.5(3) . . ? O12B C23 O12A 39.81(19) . . ? C23 C24 C25 120.1(2) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C20 C25 C24 119.4(2) . . ? C20 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? O11 C26 H26A 109.5 . . ? O11 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O11 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O12A C27A H27A 109.5 . . ? O12A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? O12A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? O12B C27B H27D 109.5 . . ? O12B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? O12B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? S1 C28 H28A 109.5 . . ? S1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? S1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? S1 C29 H29A 109.5 . . ? S1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? S1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? 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 O14 H1O O13 0.78(3) 2.10(3) 2.875(2) 168(3) 2_766 O14 H2O O8 0.80(4) 2.23(4) 2.955(2) 152(3) 1_545 O14 H2O O7 0.80(4) 2.65(4) 3.283(3) 138(3) 1_545 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.075 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.074 # Attachment '14.CIF' data_c:\docume~1\owner\mydocu~1\xray\hendrik\hb20dmso\trial _database_code_depnum_ccdc_archive 'CCDC 634369' _audit_creation_method SHELXL-97 _chemical_name_systematic ; poly{[bis(aqua)bis(dimethylsulphoxide)hexa(4-methoxybenzoato) dilanthanum].DMSO.H2O} ; _chemical_name_common ; poly((bis(aqua)bis(dimethylsulphoxide)hexa(4-methoxybenzoato) dilanthanum).DMSO.H2O) ; _chemical_melting_point ? _chemical_formula_moiety 'C52 H58 La2 O22 S2, H2 O1, C2 H6 O1 S1' _chemical_formula_sum 'C54 H66 La2 O24 S3' _chemical_formula_weight 1473.07 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' O O 0.0106 0.0060 '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' 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 9.6330(3) _cell_length_b 10.0380(3) _cell_length_c 32.5121(8) _cell_angle_alpha 86.1710(10) _cell_angle_beta 89.5090(10) _cell_angle_gamma 75.7160(10) _cell_volume 3039.70(15) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 1.568 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6505 _exptl_absorpt_correction_T_max 0.7874 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 38157 _diffrn_reflns_av_R_equivalents 0.0808 _diffrn_reflns_av_sigmaI/netI 0.0805 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11759 _reflns_number_gt 8195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0587P)^2^+1.3127P] 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 11759 _refine_ls_number_parameters 877 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1172 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.014 _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 0.84653(3) 1.04577(3) 0.242865(9) 0.01771(9) Uani 1 1 d . . . O1 O 0.6631(3) 1.2035(3) 0.19775(10) 0.0213(8) Uani 1 1 d . A . C1 C 0.5635(5) 1.1862(5) 0.17547(15) 0.0184(11) Uani 1 1 d . . . S1A S 0.8773(4) 1.3983(4) 0.20745(12) 0.0217(7) Uani 0.773(6) 1 d P A 2 S1B S 0.8653(16) 1.4275(14) 0.2137(4) 0.019(3) Uani 0.227(6) 1 d PU A 1 H1O H 1.119(2) 0.811(4) 0.2288(12) 0.003(11) Uiso 1 1 d D . . La2 La 0.42393(3) 0.95752(3) 0.240496(9) 0.01718(9) Uani 1 1 d . . . S2 S 0.47752(16) 0.58778(15) 0.22684(4) 0.0310(3) Uani 1 1 d . . . O2 O 0.4623(3) 1.1372(4) 0.18758(10) 0.0238(8) Uani 1 1 d . A . C2 C 0.5675(5) 1.2292(5) 0.13034(15) 0.0173(11) Uani 1 1 d . A . H2O H 1.065(4) 0.767(4) 0.2597(7) 0.002(12) Uiso 1 1 d D . . S3 S 0.13929(15) 1.30164(15) 0.34715(5) 0.0320(4) Uani 1 1 d . . . O3 O 0.5990(4) 1.3249(4) 0.00478(10) 0.0320(9) Uani 1 1 d . A . C3 C 0.6925(5) 1.2506(5) 0.11247(15) 0.0226(12) Uani 1 1 d . . . H3 H 0.7744 1.2430 0.1294 0.027 Uiso 1 1 calc R A . H3O H 0.154(2) 1.172(5) 0.2529(15) 0.020(14) Uiso 1 1 d D . . O4 O 0.7181(3) 1.1799(4) 0.30134(10) 0.0213(8) Uani 1 1 d . A . C4 C 0.7000(6) 1.2824(5) 0.07082(16) 0.0246(12) Uani 1 1 d . A . H4 H 0.7863 1.2967 0.0591 0.030 Uiso 1 1 calc R . . H4O H 0.245(5) 1.238(4) 0.2676(10) 0.011(13) Uiso 1 1 d D . . O5 O 0.5405(4) 1.0878(3) 0.28467(10) 0.0227(8) Uani 1 1 d . A . C5 C 0.5805(6) 1.2936(5) 0.04588(16) 0.0235(12) Uani 1 1 d . . . O6 O 0.4320(4) 1.1491(4) 0.47667(11) 0.0321(9) Uani 1 1 d . A . C6 C 0.4527(6) 1.2758(5) 0.06315(16) 0.0273(13) Uani 1 1 d . A . H6 H 0.3696 1.2866 0.0465 0.033 Uiso 1 1 calc R . . O7 O 0.8107(3) 0.8650(3) 0.29752(10) 0.0214(8) Uani 1 1 d . A . C7 C 0.4492(6) 1.2420(5) 0.10545(16) 0.0258(13) Uani 1 1 d . . . H7 H 0.3633 1.2274 0.1173 0.031 Uiso 1 1 calc R A . O8 O 0.6169(4) 0.7957(3) 0.27964(10) 0.0230(8) Uani 1 1 d . A . C8 C 0.4788(6) 1.3367(6) -0.02187(17) 0.0373(15) Uani 1 1 d . . . H8A H 0.5048 1.3591 -0.0502 0.056 Uiso 1 1 calc R A . H8B H 0.3987 1.4099 -0.0132 0.056 Uiso 1 1 calc R . . H8C H 0.4506 1.2492 -0.0205 0.056 Uiso 1 1 calc R . . O9 O 0.6990(4) 0.5065(4) 0.45867(11) 0.0358(10) Uani 1 1 d . A . C9 C 0.6074(5) 1.1394(5) 0.31021(15) 0.0190(11) Uani 1 1 d . . . O10 O 0.7284(4) 0.9101(4) 0.20089(10) 0.0254(9) Uani 1 1 d . A . C10 C 0.5568(5) 1.1469(5) 0.35378(15) 0.0185(11) Uani 1 1 d . A . O11 O 0.5533(3) 0.8187(4) 0.18324(11) 0.0249(8) Uani 1 1 d . A . C11 C 0.6120(5) 1.2229(5) 0.38074(16) 0.0215(12) Uani 1 1 d . . . H11 H 0.6778 1.2736 0.3706 0.026 Uiso 1 1 calc R A . O12 O 1.0028(4) 0.5637(4) 0.04982(12) 0.0382(10) Uani 1 1 d . A . C12 C 0.5742(5) 1.2271(5) 0.42194(16) 0.0244(12) Uani 1 1 d . A . H12 H 0.6132 1.2801 0.4398 0.029 Uiso 1 1 calc R . . O13 O 0.2712(3) 0.9250(3) 0.30167(10) 0.0193(8) Uani 1 1 d . A . C13 C 0.4785(5) 1.1525(5) 0.43671(15) 0.0219(12) Uani 1 1 d . . . O14 O 0.0470(3) 1.0441(3) 0.29047(10) 0.0184(8) Uani 1 1 d . . . C14 C 0.4215(5) 1.0752(5) 0.41015(15) 0.0231(12) Uani 1 1 d . A . H14 H 0.3554 1.0248 0.4203 0.028 Uiso 1 1 calc R . . O15 O 0.0151(4) 0.8286(4) 0.47799(10) 0.0280(9) Uani 1 1 d . A . C15 C 0.4611(5) 1.0722(5) 0.36920(16) 0.0236(12) Uani 1 1 d . . . H15 H 0.4229 1.0187 0.3514 0.028 Uiso 1 1 calc R A . O16 O 0.2183(3) 0.9564(4) 0.19514(10) 0.0234(8) Uani 1 1 d . A . C16 C 0.5082(6) 1.2031(6) 0.50618(17) 0.0368(15) Uani 1 1 d . . . H16A H 0.4657 1.1949 0.5334 0.055 Uiso 1 1 calc R A . H16B H 0.5025 1.3003 0.4984 0.055 Uiso 1 1 calc R . . H16C H 0.6087 1.1511 0.5070 0.055 Uiso 1 1 calc R . . O17 O -0.0056(4) 1.0595(4) 0.17826(11) 0.0315(9) Uani 1 1 d . . . C17 C 0.7164(5) 0.8003(5) 0.30426(15) 0.0204(12) Uani 1 1 d . . . C18 C 0.7171(5) 0.7210(5) 0.34531(15) 0.0178(11) Uani 1 1 d . A . O18A O 0.3203(6) 1.0063(5) 0.00451(15) 0.0377(15) Uani 0.773(6) 1 d P A 1 O18B O 0.2025(18) 1.1400(16) -0.0003(5) 0.028(5) Uani 0.227(6) 1 d P A 2 O19 O 1.0322(4) 0.8145(4) 0.23702(11) 0.0268(9) Uani 1 1 d D A . C19 C 0.8253(5) 0.7118(5) 0.37407(15) 0.0193(11) Uani 1 1 d . . . H19 H 0.9015 0.7540 0.3675 0.023 Uiso 1 1 calc R A . O20 O 0.2380(4) 1.1848(4) 0.24797(11) 0.0239(8) Uani 1 1 d D A . C20 C 0.8239(6) 0.6414(5) 0.41264(16) 0.0250(13) Uani 1 1 d . A . H20 H 0.8981 0.6361 0.4322 0.030 Uiso 1 1 calc R . . C21 C 0.7128(6) 0.5796(5) 0.42187(15) 0.0246(12) Uani 1 1 d . . . O21A O 0.9152(12) 1.2698(10) 0.2374(4) 0.025(2) Uani 0.773(6) 1 d P A 2 O21B O 0.896(4) 1.299(4) 0.2400(14) 0.011(7) Uani 0.227(6) 1 d PU A 1 O22 O 0.3768(4) 0.7107(4) 0.24548(11) 0.0247(8) Uani 1 1 d . A . C22 C 0.6034(6) 0.5880(5) 0.39308(16) 0.0243(12) Uani 1 1 d . A . H22 H 0.5274 0.5454 0.3995 0.029 Uiso 1 1 calc R . . O23 O 1.1681(4) 0.6495(4) 0.30538(14) 0.0485(12) Uani 1 1 d . . . C23 C 0.6063(5) 0.6583(5) 0.35544(16) 0.0218(12) Uani 1 1 d . . . H23 H 0.5315 0.6643 0.3360 0.026 Uiso 1 1 calc R A . O24 O 0.1953(4) 1.3690(4) 0.30949(13) 0.0403(11) Uani 1 1 d . . . C24 C 0.8058(7) 0.5013(7) 0.48955(18) 0.0499(18) Uani 1 1 d . . . H24A H 0.7861 0.4474 0.5142 0.075 Uiso 1 1 calc R A . H24B H 0.8038 0.5951 0.4967 0.075 Uiso 1 1 calc R . . H24C H 0.9005 0.4579 0.4789 0.075 Uiso 1 1 calc R . . C25 C 0.6770(5) 0.8364(5) 0.17852(15) 0.0199(12) Uani 1 1 d . . . C26 C 0.7684(5) 0.7645(5) 0.14526(14) 0.0185(11) Uani 1 1 d . A . C27 C 0.8970(5) 0.7926(5) 0.13482(15) 0.0236(12) Uani 1 1 d . . . H27 H 0.9295 0.8582 0.1494 0.028 Uiso 1 1 calc R A . C28 C 0.9820(5) 0.7272(5) 0.10318(16) 0.0258(13) Uani 1 1 d . A . H28 H 1.0712 0.7473 0.0965 0.031 Uiso 1 1 calc R . . C29 C 0.9327(6) 0.6328(6) 0.08200(16) 0.0266(13) Uani 1 1 d . . . C30 C 0.8032(6) 0.6015(6) 0.09258(16) 0.0283(13) Uani 1 1 d . A . H30 H 0.7713 0.5346 0.0785 0.034 Uiso 1 1 calc R . . C31 C 0.7223(5) 0.6679(5) 0.12344(15) 0.0229(12) Uani 1 1 d . . . H31 H 0.6331 0.6478 0.1301 0.027 Uiso 1 1 calc R A . C32 C 1.1308(6) 0.5967(7) 0.0357(2) 0.0496(18) Uani 1 1 d . . . H32A H 1.1698 0.5400 0.0129 0.074 Uiso 1 1 calc R A . H32B H 1.2010 0.5787 0.0583 0.074 Uiso 1 1 calc R . . H32C H 1.1100 0.6944 0.0261 0.074 Uiso 1 1 calc R . . C33 C 0.1449(5) 0.9705(5) 0.31325(15) 0.0148(11) Uani 1 1 d . . . C34 C 0.1107(5) 0.9375(5) 0.35684(14) 0.0160(11) Uani 1 1 d . A . C35 C 0.2080(5) 0.8414(5) 0.38231(15) 0.0188(11) Uani 1 1 d . . . H35 H 0.2995 0.7982 0.3720 0.023 Uiso 1 1 calc R A . C36 C 0.1723(5) 0.8085(5) 0.42256(15) 0.0214(12) Uani 1 1 d . A . H36 H 0.2388 0.7420 0.4394 0.026 Uiso 1 1 calc R . . C37 C 0.0408(5) 0.8719(5) 0.43814(14) 0.0190(11) Uani 1 1 d . . . C38 C -0.0560(5) 0.9693(5) 0.41380(15) 0.0212(12) Uani 1 1 d . A . H38 H -0.1456 1.0148 0.4248 0.025 Uiso 1 1 calc R . . C39 C -0.0221(5) 1.0006(5) 0.37337(15) 0.0182(11) Uani 1 1 d . . . H39 H -0.0901 1.0659 0.3566 0.022 Uiso 1 1 calc R A . C40 C -0.1231(6) 0.8876(6) 0.49448(16) 0.0342(14) Uani 1 1 d . . . H40A H -0.1288 0.8492 0.5228 0.051 Uiso 1 1 calc R A . H40B H -0.1973 0.8662 0.4775 0.051 Uiso 1 1 calc R . . H40C H -0.1378 0.9878 0.4945 0.051 Uiso 1 1 calc R . . C41 C 0.1223(5) 1.0137(5) 0.16948(15) 0.0194(12) Uani 1 1 d . . . C42A C 0.1725(8) 1.0068(9) 0.1255(2) 0.0164(18) Uani 0.773(6) 1 d P A 1 C42B C 0.149(3) 1.063(3) 0.1252(8) 0.004(6) Uani 0.227(6) 1 d PU A 2 C43A C 0.3146(10) 0.9533(9) 0.1153(3) 0.028(2) Uani 0.773(6) 1 d P A 1 H43A H 0.3826 0.9163 0.1367 0.034 Uiso 0.773(6) 1 calc PR A 1 C43B C 0.255(3) 0.959(3) 0.1045(9) 0.021(7) Uani 0.227(6) 1 d PU A 2 H43B H 0.3098 0.8798 0.1195 0.026 Uiso 0.227(6) 1 calc PR A 2 C44A C 0.3596(10) 0.9526(9) 0.0749(2) 0.037(2) Uani 0.773(6) 1 d P A 1 H44A H 0.4569 0.9133 0.0685 0.045 Uiso 0.773(6) 1 calc PR A 1 C44B C 0.274(4) 0.980(3) 0.0613(10) 0.023(8) Uani 0.227(6) 1 d PU A 2 H44B H 0.3383 0.9128 0.0463 0.027 Uiso 0.227(6) 1 calc PR A 2 C45A C 0.2617(10) 1.0095(10) 0.0438(3) 0.025(2) Uani 0.773(6) 1 d P A 1 C45B C 0.192(3) 1.104(3) 0.0416(7) 0.020(6) Uani 0.227(6) 1 d PU A 2 C46A C 0.1206(9) 1.0600(8) 0.0526(2) 0.032(2) Uani 0.773(6) 1 d P A 1 H46A H 0.0528 1.0952 0.0311 0.038 Uiso 0.773(6) 1 calc PR A 1 C46B C 0.094(2) 1.205(2) 0.0629(7) 0.021(6) Uani 0.227(6) 1 d PU A 2 H46B H 0.0435 1.2884 0.0487 0.026 Uiso 0.227(6) 1 calc PR A 2 C47A C 0.0770(7) 1.0597(7) 0.0934(2) 0.0270(18) Uani 0.773(6) 1 d P A 1 H47A H -0.0211 1.0967 0.0995 0.032 Uiso 0.773(6) 1 calc PR A 1 C47B C 0.073(2) 1.181(2) 0.1039(6) 0.013(5) Uani 0.227(6) 1 d PU A 2 H47B H 0.0048 1.2469 0.1180 0.015 Uiso 0.227(6) 1 calc PR A 2 C48A C 0.2418(15) 1.0586(12) -0.0276(3) 0.049(3) Uani 0.773(6) 1 d P A 1 H48D H 0.3013 1.0479 -0.0523 0.074 Uiso 0.773(6) 1 calc PR A 1 H48E H 0.1994 1.1567 -0.0245 0.074 Uiso 0.773(6) 1 calc PR A 1 H48F H 0.1654 1.0107 -0.0301 0.074 Uiso 0.773(6) 1 calc PR A 1 C48B C 0.214(6) 1.021(5) -0.0300(17) 0.066(17) Uani 0.227(6) 1 d PU A 2 H48A H 0.2234 1.0561 -0.0585 0.099 Uiso 0.227(6) 1 calc PR A 2 H48B H 0.1280 0.9856 -0.0276 0.099 Uiso 0.227(6) 1 calc PR A 2 H48C H 0.2987 0.9462 -0.0225 0.099 Uiso 0.227(6) 1 calc PR A 2 C49A C 0.9046(10) 1.5343(8) 0.2367(3) 0.034(2) Uani 0.773(6) 1 d P A 2 H49A H 0.8234 1.5631 0.2552 0.051 Uiso 0.773(6) 1 calc PR A 2 H49B H 0.9125 1.6126 0.2179 0.051 Uiso 0.773(6) 1 calc PR A 2 H49C H 0.9930 1.5017 0.2530 0.051 Uiso 0.773(6) 1 calc PR A 2 C49B C 0.846(3) 1.556(4) 0.2478(11) 0.034(9) Uani 0.227(6) 1 d PU A 1 H49D H 0.7444 1.5899 0.2542 0.051 Uiso 0.227(6) 1 calc PR A 1 H49E H 0.8830 1.6313 0.2353 0.051 Uiso 0.227(6) 1 calc PR A 1 H49F H 0.8997 1.5181 0.2732 0.051 Uiso 0.227(6) 1 calc PR A 1 C50A C 1.0277(8) 1.3827(9) 0.1736(2) 0.035(2) Uani 0.773(6) 1 d P A 2 H50A H 1.1166 1.3575 0.1899 0.052 Uiso 0.773(6) 1 calc PR A 2 H50B H 1.0212 1.4708 0.1579 0.052 Uiso 0.773(6) 1 calc PR A 2 H50C H 1.0274 1.3112 0.1545 0.052 Uiso 0.773(6) 1 calc PR A 2 C50B C 1.040(3) 1.432(3) 0.1925(9) 0.036(7) Uani 0.227(6) 1 d PU A 1 H50D H 1.1009 1.4503 0.2142 0.053 Uiso 0.227(6) 1 calc PR A 1 H50E H 1.0278 1.5042 0.1702 0.053 Uiso 0.227(6) 1 calc PR A 1 H50F H 1.0843 1.3424 0.1816 0.053 Uiso 0.227(6) 1 calc PR A 1 C51 C 0.4585(9) 0.4410(6) 0.2577(2) 0.064(2) Uani 1 1 d . A . H51A H 0.5032 0.4398 0.2847 0.096 Uiso 1 1 calc R . . H51B H 0.5052 0.3574 0.2441 0.096 Uiso 1 1 calc R . . H51C H 0.3565 0.4447 0.2612 0.096 Uiso 1 1 calc R . . C52 C 0.3894(8) 0.5645(7) 0.1813(2) 0.059(2) Uani 1 1 d . A . H52A H 0.3912 0.6400 0.1608 0.088 Uiso 1 1 calc R . . H52B H 0.2898 0.5641 0.1876 0.088 Uiso 1 1 calc R . . H52C H 0.4383 0.4766 0.1704 0.088 Uiso 1 1 calc R . . C53 C 0.1714(7) 1.4015(7) 0.38847(19) 0.0470(18) Uani 1 1 d . . . H53A H 0.2745 1.3816 0.3941 0.071 Uiso 1 1 calc R . . H53B H 0.1221 1.3775 0.4133 0.071 Uiso 1 1 calc R . . H53C H 0.1351 1.4998 0.3805 0.071 Uiso 1 1 calc R . . C54 C -0.0493(6) 1.3577(6) 0.34430(18) 0.0342(14) Uani 1 1 d . . . H54A H -0.0850 1.3115 0.3226 0.051 Uiso 1 1 calc R . . H54B H -0.0773 1.4576 0.3380 0.051 Uiso 1 1 calc R . . H54C H -0.0902 1.3352 0.3708 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.01723(17) 0.02508(19) 0.01290(16) 0.00290(13) -0.00131(12) -0.01021(13) O1 0.0203(19) 0.026(2) 0.0158(19) 0.0053(15) -0.0041(15) -0.0047(16) C1 0.016(3) 0.024(3) 0.014(3) 0.003(2) -0.004(2) -0.002(2) S1A 0.0262(15) 0.0135(17) 0.0255(16) 0.0030(13) -0.0046(11) -0.0059(13) S1B 0.019(3) 0.019(3) 0.019(3) -0.0011(10) 0.0001(10) -0.0046(13) La2 0.01580(17) 0.02282(19) 0.01461(17) 0.00181(12) -0.00001(12) -0.00876(13) S2 0.0414(9) 0.0243(8) 0.0301(8) -0.0051(6) 0.0112(7) -0.0129(7) O2 0.0181(19) 0.032(2) 0.021(2) 0.0082(16) 0.0014(16) -0.0082(16) C2 0.020(3) 0.015(3) 0.016(3) 0.005(2) -0.002(2) -0.004(2) S3 0.0295(8) 0.0232(8) 0.0437(9) -0.0040(7) -0.0022(7) -0.0066(6) O3 0.041(2) 0.042(3) 0.0137(19) 0.0023(17) -0.0018(17) -0.0144(19) C3 0.023(3) 0.025(3) 0.021(3) -0.002(2) -0.006(2) -0.010(2) O4 0.0192(19) 0.030(2) 0.0172(19) 0.0009(15) -0.0001(15) -0.0109(16) C4 0.027(3) 0.025(3) 0.024(3) 0.001(2) 0.002(2) -0.010(2) O5 0.0239(19) 0.025(2) 0.0189(19) -0.0008(16) -0.0049(16) -0.0062(16) C5 0.036(3) 0.016(3) 0.019(3) -0.001(2) 0.001(2) -0.007(2) O6 0.040(2) 0.042(3) 0.017(2) -0.0027(17) 0.0058(18) -0.0169(19) C6 0.034(3) 0.029(3) 0.021(3) 0.006(2) -0.008(3) -0.014(3) O7 0.0176(19) 0.026(2) 0.0214(19) 0.0078(16) 0.0027(15) -0.0089(16) C7 0.026(3) 0.029(3) 0.026(3) 0.008(2) -0.004(2) -0.016(3) O8 0.024(2) 0.028(2) 0.0180(19) 0.0027(16) -0.0043(16) -0.0093(16) C8 0.043(4) 0.044(4) 0.021(3) 0.000(3) -0.004(3) -0.005(3) O9 0.060(3) 0.032(2) 0.018(2) 0.0065(17) 0.0005(19) -0.018(2) C9 0.021(3) 0.014(3) 0.020(3) 0.001(2) -0.004(2) 0.000(2) O10 0.026(2) 0.033(2) 0.019(2) -0.0063(17) -0.0021(16) -0.0091(17) C10 0.015(3) 0.018(3) 0.022(3) 0.001(2) -0.001(2) -0.003(2) O11 0.020(2) 0.028(2) 0.027(2) -0.0032(17) 0.0050(17) -0.0081(16) C11 0.019(3) 0.019(3) 0.028(3) -0.001(2) 0.001(2) -0.007(2) O12 0.037(2) 0.044(3) 0.034(2) -0.014(2) 0.017(2) -0.008(2) C12 0.021(3) 0.027(3) 0.026(3) -0.008(2) -0.001(2) -0.007(2) O13 0.0178(19) 0.024(2) 0.0160(18) 0.0023(15) 0.0025(15) -0.0067(16) C13 0.026(3) 0.021(3) 0.016(3) 0.001(2) 0.003(2) -0.002(2) O14 0.0185(18) 0.020(2) 0.0178(18) 0.0016(15) -0.0056(15) -0.0075(15) C14 0.024(3) 0.026(3) 0.019(3) 0.008(2) -0.002(2) -0.009(2) O15 0.038(2) 0.028(2) 0.0172(19) 0.0028(16) 0.0083(17) -0.0079(18) C15 0.028(3) 0.021(3) 0.023(3) 0.005(2) -0.005(2) -0.010(2) O16 0.0133(18) 0.039(2) 0.019(2) 0.0037(17) -0.0017(16) -0.0107(16) C16 0.045(4) 0.043(4) 0.024(3) -0.013(3) 0.010(3) -0.010(3) O17 0.017(2) 0.045(3) 0.026(2) 0.0120(18) 0.0075(17) -0.0015(18) C17 0.019(3) 0.023(3) 0.018(3) 0.002(2) 0.003(2) -0.003(2) C18 0.019(3) 0.016(3) 0.016(3) -0.003(2) 0.002(2) 0.000(2) O18A 0.052(4) 0.039(3) 0.018(3) -0.001(2) 0.012(3) -0.005(3) O18B 0.045(11) 0.014(9) 0.026(10) 0.000(7) -0.003(8) -0.008(8) O19 0.024(2) 0.048(3) 0.018(2) 0.0016(18) 0.0056(18) -0.029(2) C19 0.018(3) 0.019(3) 0.021(3) 0.001(2) 0.001(2) -0.006(2) O20 0.019(2) 0.038(2) 0.020(2) 0.0076(18) -0.0021(17) -0.0202(18) C20 0.028(3) 0.021(3) 0.025(3) -0.002(2) -0.007(2) -0.005(2) C21 0.038(3) 0.016(3) 0.017(3) -0.001(2) 0.004(2) -0.001(2) O21A 0.031(5) 0.011(5) 0.028(4) 0.009(4) -0.003(3) -0.002(4) O21B 0.011(7) 0.011(7) 0.011(7) -0.0008(11) 0.0000(10) -0.003(2) O22 0.028(2) 0.024(2) 0.025(2) -0.0027(16) 0.0079(16) -0.0113(16) C22 0.029(3) 0.021(3) 0.023(3) 0.001(2) 0.009(2) -0.008(2) O23 0.050(3) 0.041(3) 0.055(3) -0.002(2) 0.007(2) -0.012(2) C23 0.023(3) 0.019(3) 0.023(3) 0.000(2) 0.001(2) -0.005(2) O24 0.044(3) 0.032(2) 0.050(3) -0.012(2) 0.015(2) -0.017(2) C24 0.082(5) 0.047(4) 0.022(3) 0.016(3) -0.011(3) -0.023(4) C25 0.020(3) 0.023(3) 0.016(3) 0.007(2) 0.000(2) -0.006(2) C26 0.019(3) 0.023(3) 0.011(2) 0.005(2) -0.004(2) -0.003(2) C27 0.025(3) 0.027(3) 0.020(3) 0.005(2) -0.003(2) -0.011(2) C28 0.021(3) 0.033(3) 0.024(3) -0.001(3) 0.008(2) -0.007(2) C29 0.028(3) 0.026(3) 0.022(3) 0.001(2) 0.010(2) 0.000(3) C30 0.032(3) 0.029(3) 0.026(3) -0.005(2) 0.001(3) -0.010(3) C31 0.022(3) 0.026(3) 0.020(3) 0.004(2) 0.000(2) -0.007(2) C32 0.037(4) 0.058(5) 0.054(4) -0.018(4) 0.026(3) -0.009(3) C33 0.016(3) 0.017(3) 0.015(3) -0.002(2) 0.001(2) -0.012(2) C34 0.021(3) 0.013(3) 0.016(3) -0.001(2) -0.003(2) -0.008(2) C35 0.021(3) 0.015(3) 0.020(3) 0.003(2) 0.002(2) -0.005(2) C36 0.024(3) 0.019(3) 0.020(3) 0.005(2) -0.002(2) -0.004(2) C37 0.028(3) 0.020(3) 0.011(3) 0.000(2) 0.001(2) -0.012(2) C38 0.023(3) 0.020(3) 0.022(3) -0.007(2) 0.005(2) -0.006(2) C39 0.019(3) 0.021(3) 0.016(3) -0.001(2) -0.001(2) -0.007(2) C40 0.049(4) 0.038(4) 0.018(3) -0.001(3) 0.011(3) -0.016(3) C41 0.022(3) 0.025(3) 0.014(3) 0.000(2) 0.000(2) -0.011(2) C42A 0.019(4) 0.009(5) 0.021(4) -0.001(4) -0.003(3) -0.005(4) C42B 0.004(7) 0.004(7) 0.004(7) -0.0001(11) 0.0001(10) -0.0010(19) C43A 0.035(5) 0.043(5) 0.012(4) -0.009(4) 0.005(4) -0.017(5) C43B 0.024(11) 0.019(10) 0.019(11) 0.001(8) -0.001(8) -0.003(8) C44A 0.041(5) 0.044(5) 0.030(5) -0.007(4) 0.003(4) -0.014(4) C44B 0.024(11) 0.022(11) 0.019(12) 0.000(9) 0.001(9) 0.001(8) C45A 0.034(5) 0.023(6) 0.019(5) 0.002(4) 0.003(4) -0.008(4) C45B 0.020(9) 0.024(10) 0.018(9) 0.006(8) -0.001(8) -0.008(8) C46A 0.037(5) 0.036(5) 0.018(4) 0.007(3) -0.005(4) -0.002(4) C46B 0.016(9) 0.025(9) 0.017(9) 0.006(7) 0.005(7) 0.004(7) C47A 0.024(4) 0.031(5) 0.020(4) 0.006(3) 0.002(3) 0.001(3) C47B 0.013(8) 0.013(9) 0.015(8) 0.000(7) -0.006(7) -0.009(7) C48A 0.109(10) 0.039(6) 0.015(5) -0.007(4) 0.013(5) -0.045(7) C48B 0.067(17) 0.066(17) 0.065(17) -0.004(5) 0.001(5) -0.016(6) C49A 0.047(6) 0.019(5) 0.038(5) 0.005(4) -0.011(5) -0.014(4) C49B 0.034(9) 0.034(9) 0.034(9) -0.0024(12) 0.0003(10) -0.008(2) C50A 0.037(5) 0.039(5) 0.026(5) 0.011(4) 0.006(4) -0.009(4) C50B 0.036(7) 0.035(7) 0.035(7) -0.0023(11) 0.0004(10) -0.009(2) C51 0.102(6) 0.026(4) 0.055(5) 0.004(3) 0.026(4) -0.003(4) C52 0.082(6) 0.060(5) 0.045(4) -0.017(4) 0.000(4) -0.034(4) C53 0.044(4) 0.051(4) 0.044(4) -0.007(3) -0.021(3) -0.005(3) C54 0.035(3) 0.034(4) 0.036(4) -0.009(3) -0.001(3) -0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O10 2.460(3) . ? La1 O1 2.477(3) . ? La1 O14 2.481(3) 1_655 ? La1 O21A 2.490(11) . ? La1 O4 2.537(3) . ? La1 O7 2.537(3) . ? La1 O17 2.543(3) 1_655 ? La1 O19 2.575(4) . ? La1 O21B 2.70(4) . ? O1 C1 1.260(5) . ? C1 O2 1.245(6) . ? C1 C2 1.505(7) . ? S1A O21A 1.534(12) . ? S1A C49A 1.786(9) . ? S1A C50A 1.794(8) . ? S1B O21B 1.46(5) . ? S1B C49B 1.73(3) . ? S1B C50B 1.82(3) . ? La2 O8 2.447(3) . ? La2 O5 2.457(3) . ? La2 O16 2.483(3) . ? La2 O2 2.501(3) . ? La2 O13 2.515(3) . ? La2 O11 2.532(3) . ? La2 O20 2.554(4) . ? La2 O22 2.621(3) . ? S2 O22 1.527(4) . ? S2 C52 1.769(6) . ? S2 C51 1.772(7) . ? C2 C7 1.379(7) . ? C2 C3 1.390(7) . ? S3 O24 1.518(4) . ? S3 C54 1.766(5) . ? S3 C53 1.802(6) . ? O3 C5 1.372(6) . ? O3 C8 1.428(6) . ? C3 C4 1.376(7) . ? C3 H3 0.9500 . ? O4 C9 1.257(6) . ? C4 C5 1.390(7) . ? C4 H4 0.9500 . ? O5 C9 1.266(6) . ? C5 C6 1.396(7) . ? O6 C13 1.372(6) . ? O6 C16 1.424(6) . ? C6 C7 1.397(7) . ? C6 H6 0.9500 . ? O7 C17 1.251(6) . ? C7 H7 0.9500 . ? O8 C17 1.266(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O9 C21 1.384(6) . ? O9 C24 1.433(7) . ? C9 C10 1.495(7) . ? O10 C25 1.257(6) . ? C10 C11 1.389(7) . ? C10 C15 1.395(7) . ? O11 C25 1.254(6) . ? C11 C12 1.385(7) . ? C11 H11 0.9500 . ? O12 C29 1.374(6) . ? O12 C32 1.419(7) . ? C12 C13 1.388(7) . ? C12 H12 0.9500 . ? O13 C33 1.253(5) . ? C13 C14 1.399(7) . ? O14 C33 1.257(6) . ? O14 La1 2.481(3) 1_455 ? C14 C15 1.382(7) . ? C14 H14 0.9500 . ? O15 C37 1.379(6) . ? O15 C40 1.432(6) . ? C15 H15 0.9500 . ? O16 C41 1.253(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O17 C41 1.242(6) . ? O17 La1 2.543(3) 1_455 ? C17 C18 1.507(7) . ? C18 C19 1.388(6) . ? C18 C23 1.393(7) . ? O18A C48A 1.296(12) . ? O18A C45A 1.390(9) . ? O18B C45B 1.40(3) . ? O18B C48B 1.57(5) . ? O19 H1O 0.867(10) . ? O19 H2O 0.866(10) . ? C19 C20 1.399(7) . ? C19 H19 0.9500 . ? O20 H3O 0.866(10) . ? O20 H4O 0.870(10) . ? C20 C21 1.385(7) . ? C20 H20 0.9500 . ? C21 C22 1.399(7) . ? C22 C23 1.375(7) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.496(7) . ? C26 C27 1.373(7) . ? C26 C31 1.397(7) . ? C27 C28 1.404(7) . ? C27 H27 0.9500 . ? C28 C29 1.383(7) . ? C28 H28 0.9500 . ? C29 C30 1.394(7) . ? C30 C31 1.370(7) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.487(6) . ? C34 C35 1.398(7) . ? C34 C39 1.400(7) . ? C35 C36 1.389(7) . ? C35 H35 0.9500 . ? C36 C37 1.379(7) . ? C36 H36 0.9500 . ? C37 C38 1.382(7) . ? C38 C39 1.386(7) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42A 1.505(9) . ? C41 C42B 1.53(3) . ? C42A C47A 1.385(10) . ? C42A C43A 1.388(12) . ? C42B C47B 1.38(3) . ? C42B C43B 1.46(4) . ? C43A C44A 1.380(11) . ? C43A H43A 0.9500 . ? C43B C44B 1.42(4) . ? C43B H43B 0.9500 . ? C44A C45A 1.383(12) . ? C44A H44A 0.9500 . ? C44B C45B 1.42(4) . ? C44B H44B 0.9500 . ? C45A C46A 1.365(12) . ? C45B C46B 1.41(3) . ? C46A C47A 1.388(9) . ? C46A H46A 0.9500 . ? C46B C47B 1.36(3) . ? C46B H46B 0.9500 . ? C47A H47A 0.9500 . ? C47B H47B 0.9500 . ? C48A H48D 0.9800 . ? C48A H48E 0.9800 . ? C48A H48F 0.9800 . ? C48B H48A 0.9800 . ? C48B H48B 0.9800 . ? C48B H48C 0.9800 . ? C49A H49A 0.9800 . ? C49A H49B 0.9800 . ? C49A H49C 0.9800 . ? C49B H49D 0.9800 . ? C49B H49E 0.9800 . ? C49B H49F 0.9800 . ? C50A H50A 0.9800 . ? C50A H50B 0.9800 . ? C50A H50C 0.9800 . ? C50B H50D 0.9800 . ? C50B H50E 0.9800 . ? C50B H50F 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? 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 O10 La1 O1 70.55(11) . . ? O10 La1 O14 146.80(11) . 1_655 ? O1 La1 O14 141.80(11) . 1_655 ? O10 La1 O21A 139.0(3) . . ? O1 La1 O21A 74.1(3) . . ? O14 La1 O21A 68.4(3) 1_655 . ? O10 La1 O4 121.73(11) . . ? O1 La1 O4 85.30(11) . . ? O14 La1 O4 77.80(10) 1_655 . ? O21A La1 O4 74.5(3) . . ? O10 La1 O7 80.28(11) . . ? O1 La1 O7 128.03(11) . . ? O14 La1 O7 80.05(10) 1_655 . ? O21A La1 O7 139.6(3) . . ? O4 La1 O7 74.63(11) . . ? O10 La1 O17 83.37(12) . 1_655 ? O1 La1 O17 80.33(11) . 1_655 ? O14 La1 O17 94.02(11) 1_655 1_655 ? O21A La1 O17 70.6(3) . 1_655 ? O4 La1 O17 144.68(12) . 1_655 ? O7 La1 O17 138.40(11) . 1_655 ? O10 La1 O19 74.94(11) . . ? O1 La1 O19 136.94(11) . . ? O14 La1 O19 73.01(11) 1_655 . ? O21A La1 O19 122.0(3) . . ? O4 La1 O19 135.73(11) . . ? O7 La1 O19 68.17(11) . . ? O17 La1 O19 70.72(12) 1_655 . ? O10 La1 O21B 138.6(9) . . ? O1 La1 O21B 71.3(9) . . ? O14 La1 O21B 70.8(9) 1_655 . ? O21A La1 O21B 5.6(10) . . ? O4 La1 O21B 69.8(9) . . ? O7 La1 O21B 137.6(9) . . ? O17 La1 O21B 75.1(9) 1_655 . ? O19 La1 O21B 127.3(8) . . ? C1 O1 La1 133.5(3) . . ? O2 C1 O1 125.7(5) . . ? O2 C1 C2 117.5(4) . . ? O1 C1 C2 116.8(4) . . ? O21A S1A C49A 104.5(6) . . ? O21A S1A C50A 105.3(5) . . ? C49A S1A C50A 99.0(4) . . ? O21B S1B C49B 104(2) . . ? O21B S1B C50B 103(2) . . ? C49B S1B C50B 99.7(15) . . ? O8 La2 O5 71.28(11) . . ? O8 La2 O16 139.76(12) . . ? O5 La2 O16 147.92(11) . . ? O8 La2 O2 124.17(11) . . ? O5 La2 O2 81.26(11) . . ? O16 La2 O2 83.06(11) . . ? O8 La2 O13 84.98(11) . . ? O5 La2 O13 86.71(11) . . ? O16 La2 O13 88.49(11) . . ? O2 La2 O13 141.66(11) . . ? O8 La2 O11 79.40(11) . . ? O5 La2 O11 122.90(11) . . ? O16 La2 O11 79.70(11) . . ? O2 La2 O11 76.39(11) . . ? O13 La2 O11 138.59(11) . . ? O8 La2 O20 140.33(11) . . ? O5 La2 O20 75.27(11) . . ? O16 La2 O20 73.05(11) . . ? O2 La2 O20 69.48(11) . . ? O13 La2 O20 72.28(11) . . ? O11 La2 O20 138.21(11) . . ? O8 La2 O22 69.92(11) . . ? O5 La2 O22 135.31(11) . . ? O16 La2 O22 70.72(11) . . ? O2 La2 O22 140.14(11) . . ? O13 La2 O22 68.73(11) . . ? O11 La2 O22 69.90(11) . . ? O20 La2 O22 126.46(11) . . ? O22 S2 C52 104.7(3) . . ? O22 S2 C51 105.5(3) . . ? C52 S2 C51 99.9(4) . . ? C1 O2 La2 137.2(3) . . ? C7 C2 C3 118.6(5) . . ? C7 C2 C1 120.6(4) . . ? C3 C2 C1 120.7(4) . . ? O24 S3 C54 106.2(3) . . ? O24 S3 C53 103.4(3) . . ? C54 S3 C53 99.1(3) . . ? C5 O3 C8 116.9(4) . . ? C4 C3 C2 121.3(5) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C9 O4 La1 109.1(3) . . ? C3 C4 C5 119.7(5) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C9 O5 La2 172.1(3) . . ? O3 C5 C4 115.3(5) . . ? O3 C5 C6 124.5(5) . . ? C4 C5 C6 120.2(5) . . ? C13 O6 C16 116.9(4) . . ? C5 C6 C7 118.7(5) . . ? C5 C6 H6 120.7 . . ? C7 C6 H6 120.7 . . ? C17 O7 La1 134.5(3) . . ? C2 C7 C6 121.5(5) . . ? C2 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C17 O8 La2 138.0(3) . . ? O3 C8 H8A 109.5 . . ? O3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C21 O9 C24 116.1(4) . . ? O4 C9 O5 123.5(5) . . ? O4 C9 C10 117.8(4) . . ? O5 C9 C10 118.7(4) . . ? C25 O10 La1 175.8(3) . . ? C11 C10 C15 118.3(5) . . ? C11 C10 C9 120.0(5) . . ? C15 C10 C9 121.6(5) . . ? C25 O11 La2 111.0(3) . . ? C12 C11 C10 122.2(5) . . ? C12 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? C29 O12 C32 117.9(4) . . ? C11 C12 C13 118.8(5) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C33 O13 La2 138.2(3) . . ? O6 C13 C12 124.4(5) . . ? O6 C13 C14 115.5(5) . . ? C12 C13 C14 120.1(5) . . ? C33 O14 La1 145.6(3) . 1_455 ? C15 C14 C13 120.1(5) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C37 O15 C40 116.9(4) . . ? C14 C15 C10 120.6(5) . . ? C14 C15 H15 119.7 . . ? C10 C15 H15 119.7 . . ? C41 O16 La2 152.0(3) . . ? O6 C16 H16A 109.5 . . ? O6 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O6 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C41 O17 La1 134.3(3) . 1_455 ? O7 C17 O8 125.9(5) . . ? O7 C17 C18 118.6(4) . . ? O8 C17 C18 115.5(4) . . ? C19 C18 C23 118.8(5) . . ? C19 C18 C17 121.0(4) . . ? C23 C18 C17 120.2(4) . . ? C48A O18A C45A 121.0(8) . . ? C45B O18B C48B 116(3) . . ? La1 O19 H1O 122(3) . . ? La1 O19 H2O 118(3) . . ? H1O O19 H2O 90(4) . . ? C18 C19 C20 121.0(5) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? La2 O20 H3O 112(3) . . ? La2 O20 H4O 121(3) . . ? H3O O20 H4O 100(4) . . ? C21 C20 C19 119.1(5) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? O9 C21 C20 124.9(5) . . ? O9 C21 C22 114.7(5) . . ? C20 C21 C22 120.4(5) . . ? S1A O21A La1 134.4(7) . . ? S1B O21B La1 140(2) . . ? S2 O22 La2 122.57(18) . . ? C23 C22 C21 119.7(5) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C18 121.1(5) . . ? C22 C23 H23 119.5 . . ? C18 C23 H23 119.5 . . ? O9 C24 H24A 109.5 . . ? O9 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O9 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O11 C25 O10 122.9(5) . . ? O11 C25 C26 118.5(4) . . ? O10 C25 C26 118.6(4) . . ? C27 C26 C31 118.3(5) . . ? C27 C26 C25 121.6(5) . . ? C31 C26 C25 120.1(5) . . ? C26 C27 C28 121.8(5) . . ? C26 C27 H27 119.1 . . ? C28 C27 H27 119.1 . . ? C29 C28 C27 118.3(5) . . ? C29 C28 H28 120.8 . . ? C27 C28 H28 120.8 . . ? O12 C29 C28 124.6(5) . . ? O12 C29 C30 114.8(5) . . ? C28 C29 C30 120.6(5) . . ? C31 C30 C29 119.6(5) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C26 121.3(5) . . ? C30 C31 H31 119.4 . . ? C26 C31 H31 119.4 . . ? O12 C32 H32A 109.5 . . ? O12 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O12 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O13 C33 O14 123.9(4) . . ? O13 C33 C34 117.6(4) . . ? O14 C33 C34 118.4(4) . . ? C35 C34 C39 118.0(5) . . ? C35 C34 C33 121.5(4) . . ? C39 C34 C33 120.5(4) . . ? C36 C35 C34 120.7(5) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C37 C36 C35 120.3(5) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 O15 115.4(4) . . ? C36 C37 C38 120.1(5) . . ? O15 C37 C38 124.5(5) . . ? C37 C38 C39 119.9(5) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C38 C39 C34 121.1(5) . . ? C38 C39 H39 119.5 . . ? C34 C39 H39 119.5 . . ? O15 C40 H40A 109.5 . . ? O15 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O15 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O17 C41 O16 124.4(5) . . ? O17 C41 C42A 121.9(5) . . ? O16 C41 C42A 113.3(5) . . ? O17 C41 C42B 109.8(11) . . ? O16 C41 C42B 124.8(11) . . ? C42A C41 C42B 20.8(9) . . ? C47A C42A C43A 117.3(7) . . ? C47A C42A C41 120.2(7) . . ? C43A C42A C41 122.5(6) . . ? C47B C42B C43B 121(2) . . ? C47B C42B C41 126(2) . . ? C43B C42B C41 112(2) . . ? C44A C43A C42A 121.6(9) . . ? C44A C43A H43A 119.2 . . ? C42A C43A H43A 119.2 . . ? C44B C43B C42B 119(3) . . ? C44B C43B H43B 120.5 . . ? C42B C43B H43B 120.5 . . ? C43A C44A C45A 119.4(9) . . ? C43A C44A H44A 120.3 . . ? C45A C44A H44A 120.3 . . ? C45B C44B C43B 117(3) . . ? C45B C44B H44B 121.7 . . ? C43B C44B H44B 121.7 . . ? C46A C45A C44A 120.5(8) . . ? C46A C45A O18A 125.3(8) . . ? C44A C45A O18A 114.2(7) . . ? O18B C45B C46B 114(2) . . ? O18B C45B C44B 123(3) . . ? C46B C45B C44B 123(2) . . ? C45A C46A C47A 119.4(7) . . ? C45A C46A H46A 120.3 . . ? C47A C46A H46A 120.3 . . ? C47B C46B C45B 119(2) . . ? C47B C46B H46B 120.4 . . ? C45B C46B H46B 120.4 . . ? C42A C47A C46A 121.8(7) . . ? C42A C47A H47A 119.1 . . ? C46A C47A H47A 119.1 . . ? C46B C47B C42B 121(2) . . ? C46B C47B H47B 119.5 . . ? C42B C47B H47B 119.5 . . ? O18A C48A H48D 109.5 . . ? O18A C48A H48E 109.5 . . ? H48D C48A H48E 109.5 . . ? O18A C48A H48F 109.5 . . ? H48D C48A H48F 109.5 . . ? H48E C48A H48F 109.5 . . ? O18B C48B H48A 109.5 . . ? O18B C48B H48B 109.5 . . ? H48A C48B H48B 109.5 . . ? O18B C48B H48C 109.5 . . ? H48A C48B H48C 109.5 . . ? H48B C48B H48C 109.5 . . ? S1A C49A H49A 109.5 . . ? S1A C49A H49B 109.5 . . ? H49A C49A H49B 109.5 . . ? S1A C49A H49C 109.5 . . ? H49A C49A H49C 109.5 . . ? H49B C49A H49C 109.5 . . ? S1A C50A H50A 109.5 . . ? S1A C50A H50B 109.5 . . ? H50A C50A H50B 109.5 . . ? S1A C50A H50C 109.5 . . ? H50A C50A H50C 109.5 . . ? H50B C50A H50C 109.5 . . ? S2 C51 H51A 109.5 . . ? S2 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? S2 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? S2 C52 H52A 109.5 . . ? S2 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? S2 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? S3 C53 H53A 109.5 . . ? S3 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? S3 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? S3 C54 H54A 109.5 . . ? S3 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? S3 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? 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 O19 H1O O16 0.867(10) 2.17(3) 2.838(5) 133(4) 1_655 O19 H1O O22 0.867(10) 2.49(3) 3.232(5) 144(4) 1_655 O19 H2O O23 0.866(10) 1.951(14) 2.808(6) 170(4) . O20 H3O O14 0.866(10) 2.15(3) 2.875(5) 141(4) . O20 H4O O24 0.870(10) 1.934(18) 2.774(5) 162(4) . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.297 _refine_diff_density_min -1.251 _refine_diff_density_rms 0.140 # Attachment '15.CIF' data_hb24dmf _database_code_depnum_ccdc_archive 'CCDC 634370' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(aqua)(dimethylformamide)tris(4-ethoxybenzoato)lanthanum(III)] ; _chemical_name_common ;((aqua)(dimethylformamide)tris(4- ethoxybenzoato)lanthanum(iii)) ; _chemical_melting_point ? _chemical_formula_moiety 'C30 H36 La1 N1 O11, C3 H7 N1 O1' _chemical_formula_sum 'C33 H43 La N2 O12' _chemical_formula_weight 798.60 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' O O 0.0106 0.0060 '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' _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 11.5323(2) _cell_length_b 33.7471(6) _cell_length_c 9.5791(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.326(1) _cell_angle_gamma 90.00 _cell_volume 3612.08(14) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 1.244 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7714 _exptl_absorpt_correction_T_max 0.8451 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 28151 _diffrn_reflns_av_R_equivalents 0.0762 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8123 _reflns_number_gt 5040 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0441P)^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 8123 _refine_ls_number_parameters 448 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0798 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.958 _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 0.044164(14) 0.000066(6) 0.797661(17) 0.01215(7) Uani 1 1 d . . . O1 O 0.21246(19) -0.04559(7) 0.9276(2) 0.0206(6) Uani 1 1 d . . . N1 N 0.3684(2) 0.06546(9) 0.6699(3) 0.0201(7) Uani 1 1 d . . . C1 C 0.1865(3) -0.04940(11) 1.0478(3) 0.0163(8) Uani 1 1 d . . . H1O H -0.172(4) -0.0041(11) 0.5131(10) 0.061(15) Uiso 1 1 d D . . O2 O 0.11939(18) -0.02455(7) 1.0907(2) 0.0171(5) Uani 1 1 d . . . N2 N -0.4660(2) -0.05660(10) 0.8145(3) 0.0256(8) Uani 1 1 d . . . C2 C 0.2342(3) -0.08447(11) 1.1380(3) 0.0147(7) Uani 1 1 d . . . H2O H -0.2179(16) -0.0212(10) 0.613(4) 0.039(12) Uiso 1 1 d D . . O3 O 0.3498(2) -0.18753(8) 1.3686(2) 0.0298(6) Uani 1 1 d . . . C3 C 0.2857(3) -0.11596(11) 1.0808(3) 0.0190(8) Uani 1 1 d . . . H3 H 0.2939 -0.1142 0.9847 0.023 Uiso 1 1 calc R . . O4 O 0.12636(19) 0.05890(7) 0.9467(2) 0.0209(6) Uani 1 1 d . . . C4 C 0.3246(3) -0.14933(12) 1.1590(4) 0.0250(9) Uani 1 1 d . . . H4 H 0.3593 -0.1704 1.1172 0.030 Uiso 1 1 calc R . . O5 O 0.05897(19) 0.06100(7) 1.1476(2) 0.0189(6) Uani 1 1 d . . . C5 C 0.3135(3) -0.15245(11) 1.2999(4) 0.0219(8) Uani 1 1 d . . . O6 O 0.3135(2) 0.22751(8) 1.2056(3) 0.0342(7) Uani 1 1 d . . . C6 C 0.2672(3) -0.12097(11) 1.3617(4) 0.0220(8) Uani 1 1 d . . . H6 H 0.2627 -0.1223 1.4593 0.026 Uiso 1 1 calc R . . O7 O 0.09342(19) -0.04146(7) 0.6050(2) 0.0188(6) Uani 1 1 d . . . C7 C 0.2273(3) -0.08740(11) 1.2799(4) 0.0222(8) Uani 1 1 d . . . H7 H 0.1946 -0.0660 1.3222 0.027 Uiso 1 1 calc R . . O8 O -0.00887(19) -0.05525(7) 0.3801(2) 0.0182(5) Uani 1 1 d . . . C8 C 0.3248(4) -0.19384(14) 1.5062(4) 0.0414(12) Uani 1 1 d . . . H8A H 0.2396 -0.1880 1.5005 0.050 Uiso 1 1 calc R . . H8B H 0.3747 -0.1760 1.5790 0.050 Uiso 1 1 calc R . . O9 O 0.0528(2) -0.22855(8) 0.6444(2) 0.0287(6) Uani 1 1 d . . . C9 C 0.3521(4) -0.23635(15) 1.5487(5) 0.0632(16) Uani 1 1 d . . . H9A H 0.3061 -0.2538 1.4731 0.095 Uiso 1 1 calc R . . H9B H 0.3302 -0.2417 1.6394 0.095 Uiso 1 1 calc R . . H9C H 0.4378 -0.2413 1.5612 0.095 Uiso 1 1 calc R . . O10 O -0.1511(2) -0.00986(8) 0.6055(2) 0.0208(6) Uani 1 1 d D . . C10 C 0.1151(3) 0.07522(11) 1.0614(4) 0.0170(8) Uani 1 1 d . . . O11 O 0.24827(19) 0.02095(8) 0.7431(2) 0.0214(6) Uani 1 1 d . . . C11 C 0.1745(3) 0.11466(10) 1.0997(3) 0.0171(8) Uani 1 1 d . . . O12 O -0.3577(2) -0.04228(9) 0.6525(3) 0.0383(8) Uani 1 1 d . . . C12 C 0.1725(3) 0.13305(11) 1.2292(3) 0.0224(8) Uani 1 1 d . . . H12 H 0.1372 0.1199 1.2961 0.027 Uiso 1 1 calc R . . C13 C 0.2211(3) 0.17012(11) 1.2610(4) 0.0247(9) Uani 1 1 d . . . H13 H 0.2190 0.1823 1.3497 0.030 Uiso 1 1 calc R . . C14 C 0.2732(3) 0.18982(12) 1.1659(4) 0.0254(9) Uani 1 1 d . . . C15 C 0.2814(3) 0.17127(12) 1.0390(4) 0.0276(9) Uani 1 1 d . . . H15 H 0.3206 0.1840 0.9748 0.033 Uiso 1 1 calc R . . C16 C 0.2312(3) 0.13382(12) 1.0075(4) 0.0233(9) Uani 1 1 d . . . H16 H 0.2360 0.1211 0.9206 0.028 Uiso 1 1 calc R . . C17 C 0.3624(3) 0.25001(12) 1.1069(4) 0.0331(10) Uani 1 1 d . . . H17A H 0.3079 0.2491 1.0093 0.040 Uiso 1 1 calc R . . H17B H 0.4409 0.2390 1.1020 0.040 Uiso 1 1 calc R . . C18 C 0.3768(3) 0.29173(12) 1.1611(4) 0.0366(10) Uani 1 1 d . . . H18A H 0.2980 0.3030 1.1587 0.055 Uiso 1 1 calc R . . H18B H 0.4156 0.3076 1.0997 0.055 Uiso 1 1 calc R . . H18C H 0.4263 0.2920 1.2603 0.055 Uiso 1 1 calc R . . C19 C 0.0409(3) -0.06526(11) 0.5071(3) 0.0150(8) Uani 1 1 d . . . C20 C 0.0411(3) -0.10841(11) 0.5435(3) 0.0151(8) Uani 1 1 d . . . C21 C 0.1006(3) -0.12272(11) 0.6803(3) 0.0194(8) Uani 1 1 d . . . H21 H 0.1397 -0.1047 0.7528 0.023 Uiso 1 1 calc R . . C22 C 0.1026(3) -0.16255(11) 0.7100(4) 0.0234(9) Uani 1 1 d . . . H22 H 0.1444 -0.1718 0.8024 0.028 Uiso 1 1 calc R . . C23 C 0.0443(3) -0.18951(11) 0.6066(4) 0.0202(8) Uani 1 1 d . . . C24 C -0.0168(3) -0.17578(11) 0.4708(4) 0.0214(9) Uani 1 1 d . . . H24 H -0.0586 -0.1938 0.3999 0.026 Uiso 1 1 calc R . . C25 C -0.0161(3) -0.13593(11) 0.4407(4) 0.0196(8) Uani 1 1 d . . . H25 H -0.0557 -0.1269 0.3471 0.023 Uiso 1 1 calc R . . C26 C 0.0057(3) -0.25756(12) 0.5339(4) 0.0305(10) Uani 1 1 d . . . H26A H 0.0404 -0.2534 0.4503 0.037 Uiso 1 1 calc R . . H26B H -0.0823 -0.2549 0.5007 0.037 Uiso 1 1 calc R . . C27 C 0.0373(4) -0.29788(13) 0.5953(4) 0.0418(11) Uani 1 1 d . . . H27A H 0.1244 -0.3000 0.6314 0.063 Uiso 1 1 calc R . . H27B H 0.0092 -0.3178 0.5203 0.063 Uiso 1 1 calc R . . H27C H -0.0008 -0.3023 0.6748 0.063 Uiso 1 1 calc R . . C28 C 0.2688(3) 0.05448(11) 0.7018(3) 0.0199(8) Uani 1 1 d . . . H28 H 0.2074 0.0738 0.6925 0.024 Uiso 1 1 calc R . . C29 C 0.4674(3) 0.03807(12) 0.6812(3) 0.0245(9) Uani 1 1 d . . . H29A H 0.4475 0.0127 0.7192 0.037 Uiso 1 1 calc R . . H29B H 0.5394 0.0491 0.7464 0.037 Uiso 1 1 calc R . . H29C H 0.4820 0.0340 0.5858 0.037 Uiso 1 1 calc R . . C30 C 0.3816(3) 0.10507(12) 0.6156(4) 0.0354(10) Uani 1 1 d . . . H30A H 0.3103 0.1208 0.6164 0.053 Uiso 1 1 calc R . . H30B H 0.3909 0.1033 0.5169 0.053 Uiso 1 1 calc R . . H30C H 0.4524 0.1178 0.6771 0.053 Uiso 1 1 calc R . . C31 C -0.3726(3) -0.04129(11) 0.7747(4) 0.0259(9) Uani 1 1 d . . . H31 H -0.3127 -0.0286 0.8470 0.031 Uiso 1 1 calc R . . C32 C -0.5641(4) -0.07565(16) 0.7121(4) 0.0529(15) Uani 1 1 d . . . H32A H -0.5650 -0.1040 0.7343 0.079 Uiso 1 1 calc R . . H32B H -0.5537 -0.0722 0.6144 0.079 Uiso 1 1 calc R . . H32C H -0.6400 -0.0636 0.7185 0.079 Uiso 1 1 calc R . . C33 C -0.4752(3) -0.05548(14) 0.9629(4) 0.0434(13) Uani 1 1 d . . . H33A H -0.4070 -0.0409 1.0217 0.065 Uiso 1 1 calc R . . H33B H -0.4751 -0.0826 0.9996 0.065 Uiso 1 1 calc R . . H33C H -0.5498 -0.0422 0.9674 0.065 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 0.01390(10) 0.01140(10) 0.01085(10) 0.00029(9) 0.00252(7) -0.00171(10) O1 0.0215(13) 0.0221(16) 0.0192(12) 0.0042(11) 0.0072(10) 0.0014(11) N1 0.0182(15) 0.0171(19) 0.0259(16) -0.0004(14) 0.0071(12) -0.0046(13) C1 0.0132(17) 0.014(2) 0.0204(18) -0.0014(16) 0.0013(14) -0.0050(14) O2 0.0184(12) 0.0142(15) 0.0177(12) 0.0008(11) 0.0028(9) 0.0001(11) N2 0.0196(16) 0.031(2) 0.0247(17) 0.0027(15) 0.0024(13) -0.0025(14) C2 0.0117(16) 0.014(2) 0.0189(17) -0.0004(15) 0.0046(13) 0.0003(14) O3 0.0331(15) 0.0240(18) 0.0355(15) 0.0165(13) 0.0145(12) 0.0085(12) C3 0.0184(18) 0.021(2) 0.0166(18) 0.0014(16) 0.0026(14) 0.0004(16) O4 0.0250(13) 0.0175(16) 0.0202(13) -0.0033(11) 0.0054(10) -0.0047(11) C4 0.0233(19) 0.027(3) 0.026(2) -0.0040(18) 0.0074(15) 0.0028(17) O5 0.0216(13) 0.0173(15) 0.0177(12) 0.0020(11) 0.0049(10) -0.0054(10) C5 0.0121(17) 0.020(2) 0.031(2) 0.0095(18) 0.0023(15) 0.0004(15) O6 0.0471(17) 0.0196(17) 0.0410(16) -0.0087(13) 0.0206(13) -0.0167(13) C6 0.0226(19) 0.025(2) 0.0193(18) 0.0064(17) 0.0057(15) 0.0054(16) O7 0.0215(13) 0.0170(16) 0.0182(12) -0.0003(11) 0.0056(10) -0.0005(10) C7 0.0163(17) 0.021(2) 0.030(2) -0.0013(17) 0.0061(15) 0.0035(16) O8 0.0221(13) 0.0163(15) 0.0149(12) 0.0023(11) 0.0019(10) -0.0018(11) C8 0.038(2) 0.046(3) 0.048(3) 0.026(2) 0.025(2) 0.018(2) O9 0.0409(16) 0.0144(16) 0.0300(14) 0.0041(12) 0.0071(12) 0.0021(12) C9 0.077(4) 0.052(4) 0.074(3) 0.044(3) 0.044(3) 0.028(3) O10 0.0181(13) 0.040(2) 0.0028(11) 0.0025(11) 0.0004(9) -0.0034(11) C10 0.0136(17) 0.014(2) 0.0209(18) 0.0024(16) 0.0002(14) 0.0032(14) O11 0.0204(13) 0.0169(17) 0.0276(13) 0.0005(12) 0.0072(10) -0.0014(11) C11 0.0177(17) 0.012(2) 0.0212(18) 0.0025(16) 0.0043(14) 0.0011(14) O12 0.0261(15) 0.061(2) 0.0279(14) 0.0026(14) 0.0079(12) -0.0075(14) C12 0.0249(19) 0.021(2) 0.0227(19) -0.0021(17) 0.0085(15) -0.0069(16) C13 0.031(2) 0.021(2) 0.0238(19) -0.0092(18) 0.0104(16) -0.0090(17) C14 0.027(2) 0.016(2) 0.034(2) -0.0037(18) 0.0088(16) -0.0054(17) C15 0.036(2) 0.024(3) 0.028(2) 0.0012(18) 0.0182(17) -0.0109(18) C16 0.030(2) 0.022(2) 0.0201(19) -0.0061(17) 0.0112(16) -0.0077(17) C17 0.032(2) 0.022(3) 0.047(2) 0.001(2) 0.0143(19) -0.0116(19) C18 0.028(2) 0.016(2) 0.065(3) -0.003(2) 0.009(2) -0.0064(18) C19 0.0125(14) 0.017(2) 0.0165(18) -0.0004(15) 0.0052(14) 0.0007(14) C20 0.0143(15) 0.015(2) 0.0165(16) 0.0036(16) 0.0051(13) 0.0004(15) C21 0.0219(18) 0.014(2) 0.0213(18) -0.0022(16) 0.0035(15) -0.0005(15) C22 0.027(2) 0.022(2) 0.0204(19) 0.0041(17) 0.0040(15) 0.0023(17) C23 0.0229(19) 0.013(2) 0.028(2) 0.0026(17) 0.0109(15) 0.0020(15) C24 0.020(2) 0.015(2) 0.029(2) -0.0017(16) 0.0059(16) -0.0031(15) C25 0.0175(18) 0.021(2) 0.0185(17) 0.0015(17) 0.0005(14) 0.0006(15) C26 0.033(2) 0.017(2) 0.039(2) -0.0006(18) 0.0045(19) 0.0006(18) C27 0.058(3) 0.022(3) 0.044(3) 0.002(2) 0.010(2) 0.008(2) C28 0.0162(17) 0.019(2) 0.0230(19) -0.0061(17) 0.0031(14) -0.0013(15) C29 0.0204(19) 0.028(3) 0.025(2) 0.0014(18) 0.0062(16) 0.0015(17) C30 0.034(2) 0.025(3) 0.050(3) 0.008(2) 0.015(2) -0.0059(19) C31 0.0167(18) 0.024(2) 0.033(2) 0.0018(19) -0.0003(16) 0.0027(16) C32 0.043(3) 0.078(4) 0.041(3) -0.019(3) 0.016(2) -0.036(3) C33 0.034(2) 0.067(4) 0.031(2) 0.002(2) 0.0108(18) 0.001(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 O8 2.488(2) 3_556 ? La1 O4 2.492(2) . ? La1 O7 2.492(2) . ? La1 O5 2.499(2) 3_557 ? La1 O2 2.527(2) 3_557 ? La1 O1 2.548(2) . ? La1 O10 2.553(2) . ? La1 O11 2.630(2) . ? La1 O2 2.849(2) . ? La1 C1 3.045(3) . ? O1 C1 1.266(4) . ? N1 C28 1.313(4) . ? N1 C29 1.451(4) . ? N1 C30 1.456(4) . ? C1 O2 1.276(4) . ? C1 C2 1.489(5) . ? O2 La1 2.527(2) 3_557 ? N2 C31 1.333(4) . ? N2 C32 1.451(4) . ? N2 C33 1.452(4) . ? C2 C7 1.385(4) . ? C2 C3 1.394(5) . ? O3 C5 1.369(4) . ? O3 C8 1.434(4) . ? C3 C4 1.365(5) . ? C3 H3 0.9500 . ? O4 C10 1.264(4) . ? C4 C5 1.391(4) . ? C4 H4 0.9500 . ? O5 C10 1.263(4) . ? O5 La1 2.499(2) 3_557 ? C5 C6 1.386(5) . ? O6 C14 1.375(4) . ? O6 C17 1.432(4) . ? C6 C7 1.390(5) . ? C6 H6 0.9500 . ? O7 C19 1.269(4) . ? C7 H7 0.9500 . ? O8 C19 1.256(3) . ? O8 La1 2.488(2) 3_556 ? C8 C9 1.503(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? O9 C23 1.363(4) . ? O9 C26 1.446(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? O10 H1O 0.880(13) . ? O10 H2O 0.880(20) . ? C10 C11 1.500(5) . ? O11 C28 1.241(4) . ? C11 C16 1.383(4) . ? C11 C12 1.392(4) . ? O12 C31 1.225(4) . ? C12 C13 1.374(5) . ? C12 H12 0.9500 . ? C13 C14 1.380(5) . ? C13 H13 0.9500 . ? C14 C15 1.391(5) . ? C15 C16 1.392(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.496(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.497(5) . ? C20 C25 1.395(5) . ? C20 C21 1.406(4) . ? C21 C22 1.373(5) . ? C21 H21 0.9500 . ? C22 C23 1.390(5) . ? C22 H22 0.9500 . ? C23 C24 1.396(5) . ? C24 C25 1.376(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.492(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? 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 O8 La1 O4 76.73(7) 3_556 . ? O8 La1 O7 86.72(7) 3_556 . ? O4 La1 O7 138.44(7) . . ? O8 La1 O5 139.03(7) 3_556 3_557 ? O4 La1 O5 132.08(7) . 3_557 ? O7 La1 O5 84.21(7) . 3_557 ? O8 La1 O2 91.84(7) 3_556 3_557 ? O4 La1 O2 73.43(7) . 3_557 ? O7 La1 O2 145.92(7) . 3_557 ? O5 La1 O2 74.75(8) 3_557 3_557 ? O8 La1 O1 139.70(7) 3_556 . ? O4 La1 O1 93.79(7) . . ? O7 La1 O1 74.70(7) . . ? O5 La1 O1 75.13(7) 3_557 . ? O2 La1 O1 123.30(7) 3_557 . ? O8 La1 O10 68.84(7) 3_556 . ? O4 La1 O10 131.31(8) . . ? O7 La1 O10 73.40(7) . . ? O5 La1 O10 70.27(7) 3_557 . ? O2 La1 O10 74.37(7) 3_557 . ? O1 La1 O10 134.59(8) . . ? O8 La1 O11 70.51(7) 3_556 . ? O4 La1 O11 70.62(7) . . ? O7 La1 O11 67.94(7) . . ? O5 La1 O11 139.32(8) 3_557 . ? O2 La1 O11 142.66(8) 3_557 . ? O1 La1 O11 69.41(7) . . ? O10 La1 O11 124.38(7) . . ? O8 La1 O2 148.31(7) 3_556 . ? O4 La1 O2 71.81(7) . . ? O7 La1 O2 119.73(7) . . ? O5 La1 O2 66.27(7) 3_557 . ? O2 La1 O2 75.84(7) 3_557 . ? O1 La1 O2 48.16(6) . . ? O10 La1 O2 132.16(7) . . ? O11 La1 O2 101.81(6) . . ? O8 La1 C1 156.03(8) 3_556 . ? O4 La1 C1 86.07(8) . . ? O7 La1 C1 95.58(8) . . ? O5 La1 C1 64.83(8) 3_557 . ? O2 La1 C1 99.18(8) 3_557 . ? O1 La1 C1 24.12(7) . . ? O10 La1 C1 134.64(8) . . ? O11 La1 C1 88.21(8) . . ? O2 La1 C1 24.71(7) . . ? C1 O1 La1 100.51(19) . . ? C28 N1 C29 121.3(3) . . ? C28 N1 C30 121.1(3) . . ? C29 N1 C30 117.5(3) . . ? O1 C1 O2 121.7(3) . . ? O1 C1 C2 118.2(3) . . ? O2 C1 C2 120.1(3) . . ? O1 C1 La1 55.37(16) . . ? O2 C1 La1 68.99(17) . . ? C2 C1 La1 160.5(2) . . ? C1 O2 La1 158.0(2) . 3_557 ? C1 O2 La1 86.30(18) . . ? La1 O2 La1 104.16(7) 3_557 . ? C31 N2 C32 121.9(3) . . ? C31 N2 C33 122.0(3) . . ? C32 N2 C33 116.1(3) . . ? C7 C2 C3 117.7(3) . . ? C7 C2 C1 121.6(3) . . ? C3 C2 C1 120.7(3) . . ? C5 O3 C8 117.6(3) . . ? C4 C3 C2 121.8(3) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C10 O4 La1 137.6(2) . . ? C3 C4 C5 119.9(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C10 O5 La1 142.9(2) . 3_557 ? O3 C5 C6 124.2(3) . . ? O3 C5 C4 116.2(3) . . ? C6 C5 C4 119.6(4) . . ? C14 O6 C17 118.0(3) . . ? C5 C6 C7 119.5(3) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C19 O7 La1 138.5(2) . . ? C2 C7 C6 121.3(3) . . ? C2 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C19 O8 La1 145.3(2) . 3_556 ? O3 C8 C9 108.3(3) . . ? O3 C8 H8A 110.0 . . ? C9 C8 H8A 110.0 . . ? O3 C8 H8B 110.0 . . ? C9 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? C23 O9 C26 118.1(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? La1 O10 H1O 132(3) . . ? La1 O10 H2O 129(2) . . ? H1O O10 H2O 99(3) . . ? O5 C10 O4 125.6(3) . . ? O5 C10 C11 117.0(3) . . ? O4 C10 C11 117.4(3) . . ? C28 O11 La1 124.0(2) . . ? C16 C11 C12 118.4(3) . . ? C16 C11 C10 121.2(3) . . ? C12 C11 C10 120.4(3) . . ? C13 C12 C11 120.5(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 120.8(3) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? O6 C14 C13 115.8(3) . . ? O6 C14 C15 124.5(3) . . ? C13 C14 C15 119.7(4) . . ? C14 C15 C16 118.9(3) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? C11 C16 C15 121.6(3) . . ? C11 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? O6 C17 C18 107.4(3) . . ? O6 C17 H17A 110.2 . . ? C18 C17 H17A 110.2 . . ? O6 C17 H17B 110.2 . . ? C18 C17 H17B 110.2 . . ? H17A C17 H17B 108.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O8 C19 O7 124.4(3) . . ? O8 C19 C20 117.5(3) . . ? O7 C19 C20 118.1(3) . . ? C25 C20 C21 117.8(3) . . ? C25 C20 C19 120.7(3) . . ? C21 C20 C19 121.6(3) . . ? C22 C21 C20 120.6(3) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 120.9(3) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? O9 C23 C22 116.9(3) . . ? O9 C23 C24 123.7(3) . . ? C22 C23 C24 119.4(4) . . ? C25 C24 C23 119.5(3) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C24 C25 C20 121.9(3) . . ? C24 C25 H25 119.0 . . ? C20 C25 H25 119.0 . . ? O9 C26 C27 108.5(3) . . ? O9 C26 H26A 110.0 . . ? C27 C26 H26A 110.0 . . ? O9 C26 H26B 110.0 . . ? C27 C26 H26B 110.0 . . ? H26A C26 H26B 108.4 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O11 C28 N1 125.4(3) . . ? O11 C28 H28 117.3 . . ? N1 C28 H28 117.3 . . ? N1 C29 H29A 109.5 . . ? N1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N1 C30 H30A 109.5 . . ? N1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O12 C31 N2 125.2(3) . . ? O12 C31 H31 117.4 . . ? N2 C31 H31 117.4 . . ? N2 C32 H32A 109.5 . . ? N2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N2 C33 H33A 109.5 . . ? N2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? 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 O10 H1O O11 0.880(13) 2.459(18) 3.270(3) 153(3) 3_556 O10 H2O O12 0.880(20) 1.884(6) 2.759(3) 173(3) . C31 H31 O2 0.95 2.81 3.641(4) 147.0 3_557 C31 H31 O4 0.95 2.73 3.433(4) 131.1 3_557 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.020 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.113 # Attachment '2.CIF' data_HB31DMF.CIF _database_code_depnum_ccdc_archive 'CCDC 634371' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((La3(BA)9(DMF)3).DMF)n _chemical_melting_point ? _chemical_formula_moiety 'C75 H73 La3 N4 O22' _chemical_formula_sum 'C75 H73 La3 N4 O22' _chemical_formula_weight 1799.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 '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' _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 20.0604(3) _cell_length_b 17.4169(2) _cell_length_c 23.1887(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.945(1) _cell_angle_gamma 90.00 _cell_volume 7346.10(17) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3592 _exptl_absorpt_coefficient_mu 1.792 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5343 _exptl_absorpt_correction_T_max 0.6629 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 50032 _diffrn_reflns_av_R_equivalents 0.0701 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16819 _reflns_number_gt 12599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^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 16819 _refine_ls_number_parameters 944 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 La1 La 0.287654(12) 0.168264(12) 0.947991(9) 0.01385(6) Uani 1 1 d . . . O1 O 0.31645(14) 0.16815(14) 1.07491(11) 0.0178(6) Uani 1 1 d . . . N1 N 0.46062(19) 0.01834(19) 0.90498(15) 0.0253(8) Uani 1 1 d . . . C1 C 0.3856(2) 0.17027(19) 1.08942(17) 0.0159(8) Uani 1 1 d . . . La2 La 0.235891(12) 0.263772(12) 0.772295(9) 0.01428(6) Uani 1 1 d . . . O2 O 0.40879(14) 0.17675(14) 1.04714(11) 0.0208(6) Uani 1 1 d . . . N2 N 0.1128(3) 0.0970(2) 0.53916(19) 0.0522(12) Uani 1 1 d . A 1 C2 C 0.4389(2) 0.1656(2) 1.15776(17) 0.0180(8) Uani 1 1 d . . . La3 La 0.204459(12) 0.343630(12) 0.596093(9) 0.01391(6) Uani 1 1 d . . . O3 O 0.27486(14) 0.30990(14) 0.97208(11) 0.0213(6) Uani 1 1 d . . . N3 N -0.00414(18) 0.45329(17) 0.60272(14) 0.0192(7) Uani 1 1 d . . . C3 C 0.4190(2) 0.1329(2) 1.20225(18) 0.0288(10) Uani 1 1 d . . . H3 H 0.3711 0.1119 1.1895 0.035 Uiso 1 1 calc R . . O4 O 0.21132(14) 0.28094(13) 0.87053(11) 0.0151(5) Uani 1 1 d . . . N4 N -0.2929(2) 0.0620(2) 0.31874(17) 0.0373(9) Uani 1 1 d . . . C4 C 0.4689(3) 0.1307(3) 1.2657(2) 0.0440(13) Uani 1 1 d . . . H4 H 0.4553 0.1078 1.2963 0.053 Uiso 1 1 calc R . . O5 O 0.36230(14) 0.23926(14) 0.90363(11) 0.0195(6) Uani 1 1 d . . . C5 C 0.5379(3) 0.1613(3) 1.2844(2) 0.0440(13) Uani 1 1 d . . . H5 H 0.5716 0.1603 1.3280 0.053 Uiso 1 1 calc R . . O6 O 0.34880(15) 0.33986(15) 0.84112(12) 0.0259(7) Uani 1 1 d . . . C6 C 0.5582(2) 0.1935(2) 1.2400(2) 0.0359(11) Uani 1 1 d . . . H6 H 0.6062 0.2142 1.2531 0.043 Uiso 1 1 calc R . . O7 O 0.22751(14) 0.13214(14) 0.83240(11) 0.0189(6) Uani 1 1 d . . . C7 C 0.5094(2) 0.1960(2) 1.17647(19) 0.0245(9) Uani 1 1 d . . . H7 H 0.5236 0.2182 1.1459 0.029 Uiso 1 1 calc R . . O8 O 0.18075(16) 0.12809(15) 0.72751(11) 0.0263(7) Uani 1 1 d . . . C8 C 0.2277(2) 0.3274(2) 0.91766(16) 0.0167(8) Uani 1 1 d . . . O9 O 0.34350(15) 0.18446(16) 0.77236(12) 0.0261(6) Uani 1 1 d . . . C9 C 0.1881(2) 0.4023(2) 0.90689(16) 0.0189(8) Uani 1 1 d . . . O10 O 0.28394(14) 0.24427(14) 0.68157(11) 0.0181(6) Uani 1 1 d . . . C10 C 0.2149(2) 0.4598(2) 0.95256(18) 0.0280(10) Uani 1 1 d . . . H10 H 0.2582 0.4512 0.9903 0.034 Uiso 1 1 calc R . . O11 O 0.09339(14) 0.27047(14) 0.72502(11) 0.0211(6) Uani 1 1 d . . . C11 C 0.1789(3) 0.5296(2) 0.9433(2) 0.0373(12) Uani 1 1 d . . . H11 H 0.1978 0.5691 0.9742 0.045 Uiso 1 1 calc R . . O12 O 0.13831(14) 0.27633(14) 0.65291(11) 0.0197(6) Uani 1 1 d . . . C12 C 0.1148(3) 0.5416(2) 0.88863(19) 0.0332(11) Uani 1 1 d . . . H12 H 0.0894 0.5891 0.8826 0.040 Uiso 1 1 calc R . . O13 O 0.20315(15) 0.40263(14) 0.76824(11) 0.0205(6) Uani 1 1 d . . . C13 C 0.0875(2) 0.4841(2) 0.84260(18) 0.0272(10) Uani 1 1 d . . . H13 H 0.0439 0.4928 0.8051 0.033 Uiso 1 1 calc R . . O14 O 0.25919(14) 0.40061(14) 0.70366(11) 0.0205(6) Uani 1 1 d . . . C14 C 0.1239(2) 0.4146(2) 0.85149(17) 0.0220(9) Uani 1 1 d . . . H14 H 0.1054 0.3754 0.8202 0.026 Uiso 1 1 calc R . . O15 O 0.08778(14) 0.34789(15) 0.49706(11) 0.0225(6) Uani 1 1 d . . . C15 C 0.3839(2) 0.3039(2) 0.89178(17) 0.0193(8) Uani 1 1 d . . . O16 O 0.16940(14) 0.32772(14) 0.45794(11) 0.0190(6) Uani 1 1 d . . . C16 C 0.4545(2) 0.3379(2) 0.93942(17) 0.0180(8) Uani 1 1 d . . . O17 O 0.23152(15) 0.47196(14) 0.56156(12) 0.0217(6) Uani 1 1 d . . . C17 C 0.4956(2) 0.3009(2) 0.99691(17) 0.0208(8) Uani 1 1 d . . . H17 H 0.4791 0.2536 1.0065 0.025 Uiso 1 1 calc R . . O18 O 0.26687(15) 0.45870(15) 0.48226(12) 0.0247(6) Uani 1 1 d . . . C18 C 0.5605(2) 0.3334(2) 1.03992(18) 0.0261(9) Uani 1 1 d . . . H18 H 0.5882 0.3081 1.0791 0.031 Uiso 1 1 calc R . . O19 O 0.37338(16) 0.07209(15) 0.92942(12) 0.0267(6) Uani 1 1 d . . . C19 C 0.5855(2) 0.4014(3) 1.02685(19) 0.0327(11) Uani 1 1 d . . . H19 H 0.6305 0.4226 1.0565 0.039 Uiso 1 1 calc R . . O20 O 0.17495(17) 0.21044(15) 0.54932(12) 0.0291(7) Uani 1 1 d . A . C20 C 0.5445(3) 0.4392(3) 0.9700(2) 0.0394(12) Uani 1 1 d . . . H20 H 0.5614 0.4864 0.9605 0.047 Uiso 1 1 calc R . . O21 O 0.11084(15) 0.43409(15) 0.60923(12) 0.0235(6) Uani 1 1 d . . . C21 C 0.4785(2) 0.4075(2) 0.92705(18) 0.0299(10) Uani 1 1 d . . . H21 H 0.4498 0.4340 0.8888 0.036 Uiso 1 1 calc R . . O22 O -0.2137(3) 0.1547(3) 0.3772(2) 0.0931(16) Uani 1 1 d . . . C22 C 0.1951(2) 0.0959(2) 0.77953(18) 0.0204(8) Uani 1 1 d . . . C23 C 0.1740(2) 0.0136(2) 0.78014(18) 0.0229(9) Uani 1 1 d . . . C24 C 0.2098(3) -0.0315(2) 0.8335(2) 0.0318(11) Uani 1 1 d . . . H24 H 0.2455 -0.0095 0.8715 0.038 Uiso 1 1 calc R . . C25 C 0.1933(3) -0.1086(3) 0.8312(2) 0.0441(13) Uani 1 1 d . . . H25 H 0.2189 -0.1397 0.8675 0.053 Uiso 1 1 calc R . . C26 C 0.1403(3) -0.1415(3) 0.7772(3) 0.0478(14) Uani 1 1 d . . . H26 H 0.1300 -0.1948 0.7762 0.057 Uiso 1 1 calc R . . C27 C 0.1027(3) -0.0963(3) 0.7250(2) 0.0454(13) Uani 1 1 d . . . H27 H 0.0650 -0.1180 0.6880 0.054 Uiso 1 1 calc R . . C28 C 0.1197(3) -0.0185(2) 0.7261(2) 0.0332(11) Uani 1 1 d . . . H28 H 0.0940 0.0126 0.6897 0.040 Uiso 1 1 calc R . . C29 C 0.3350(2) 0.1997(2) 0.71661(17) 0.0192(8) Uani 1 1 d . . . C30 C 0.3849(2) 0.1630(2) 0.69159(17) 0.0189(8) Uani 1 1 d . . . C31 C 0.4511(2) 0.1329(2) 0.7346(2) 0.0298(10) Uani 1 1 d . . . H31 H 0.4639 0.1357 0.7789 0.036 Uiso 1 1 calc R . . C32 C 0.4991(3) 0.0984(2) 0.7132(2) 0.0342(11) Uani 1 1 d . . . H32 H 0.5440 0.0767 0.7426 0.041 Uiso 1 1 calc R . . C33 C 0.4807(2) 0.0961(2) 0.6485(2) 0.0317(10) Uani 1 1 d . . . H33 H 0.5139 0.0737 0.6337 0.038 Uiso 1 1 calc R . . C34 C 0.4151(2) 0.1257(2) 0.6054(2) 0.0279(10) Uani 1 1 d . . . H34 H 0.4028 0.1231 0.5611 0.034 Uiso 1 1 calc R . . C35 C 0.3668(2) 0.1594(2) 0.62677(18) 0.0200(8) Uani 1 1 d . . . H35 H 0.3214 0.1800 0.5971 0.024 Uiso 1 1 calc R . . C36 C 0.0841(2) 0.2692(2) 0.66841(18) 0.0199(8) Uani 1 1 d . . . C37 C 0.0082(2) 0.2565(2) 0.61680(17) 0.0214(9) Uani 1 1 d . . . C38 C -0.0526(2) 0.2604(2) 0.6308(2) 0.0261(9) Uani 1 1 d . . . H38 H -0.0460 0.2731 0.6727 0.031 Uiso 1 1 calc R . . C39 C -0.1226(2) 0.2460(2) 0.5845(2) 0.0362(11) Uani 1 1 d . . . H39 H -0.1638 0.2487 0.5946 0.043 Uiso 1 1 calc R . . C40 C -0.1318(3) 0.2278(3) 0.5242(2) 0.0409(13) Uani 1 1 d . . . H40 H -0.1796 0.2167 0.4925 0.049 Uiso 1 1 calc R . . C41 C -0.0731(3) 0.2253(3) 0.5088(2) 0.0461(14) Uani 1 1 d . . . H41 H -0.0805 0.2135 0.4665 0.055 Uiso 1 1 calc R . . C42 C -0.0023(3) 0.2400(3) 0.55518(19) 0.0367(11) Uani 1 1 d . . . H42 H 0.0384 0.2387 0.5445 0.044 Uiso 1 1 calc R . . C43 C 0.2383(2) 0.4356(2) 0.74228(16) 0.0177(8) Uani 1 1 d . . . C44 C 0.2589(2) 0.5180(2) 0.75741(16) 0.0174(8) Uani 1 1 d . . . C45 C 0.2475(2) 0.5532(2) 0.80663(17) 0.0207(9) Uani 1 1 d . . . H45 H 0.2276 0.5245 0.8305 0.025 Uiso 1 1 calc R . . C46 C 0.2652(2) 0.6298(2) 0.82062(18) 0.0242(9) Uani 1 1 d . . . H46 H 0.2569 0.6536 0.8539 0.029 Uiso 1 1 calc R . . C47 C 0.2947(2) 0.6716(2) 0.7866(2) 0.0316(11) Uani 1 1 d . . . H47 H 0.3070 0.7242 0.7965 0.038 Uiso 1 1 calc R . . C48 C 0.3065(3) 0.6371(3) 0.7379(2) 0.0358(11) Uani 1 1 d . . . H48 H 0.3267 0.6660 0.7144 0.043 Uiso 1 1 calc R . . C49 C 0.2887(2) 0.5603(2) 0.72353(19) 0.0284(10) Uani 1 1 d . . . H49 H 0.2971 0.5367 0.6902 0.034 Uiso 1 1 calc R . . C50 C 0.1038(2) 0.3370(2) 0.45070(16) 0.0158(8) Uani 1 1 d . . . C51 C 0.0422(2) 0.33778(19) 0.38515(16) 0.0155(8) Uani 1 1 d . . . C52 C -0.0299(2) 0.3441(2) 0.37807(18) 0.0234(9) Uani 1 1 d . . . H52 H -0.0401 0.3456 0.4145 0.028 Uiso 1 1 calc R . . C53 C -0.0868(2) 0.3483(2) 0.31774(18) 0.0282(10) Uani 1 1 d . . . H53 H -0.1363 0.3517 0.3127 0.034 Uiso 1 1 calc R . . C54 C -0.0717(2) 0.3475(2) 0.26474(18) 0.0245(9) Uani 1 1 d . . . H54 H -0.1108 0.3512 0.2235 0.029 Uiso 1 1 calc R . . C55 C -0.0003(2) 0.3413(2) 0.27145(17) 0.0249(9) Uani 1 1 d . . . H55 H 0.0099 0.3412 0.2350 0.030 Uiso 1 1 calc R . . C56 C 0.0570(2) 0.3354(2) 0.33192(17) 0.0202(8) Uani 1 1 d . . . H56 H 0.1061 0.3298 0.3367 0.024 Uiso 1 1 calc R . . C57 C 0.2585(2) 0.4968(2) 0.52544(17) 0.0177(8) Uani 1 1 d . . . C58 C 0.2840(2) 0.5791(2) 0.53251(18) 0.0245(9) Uani 1 1 d . . . C59 C 0.2734(3) 0.6294(2) 0.57346(18) 0.0310(10) Uani 1 1 d . . . H59 H 0.2461 0.6137 0.5964 0.037 Uiso 1 1 calc R . . C60 C 0.3025(3) 0.7037(3) 0.5816(2) 0.0439(13) Uani 1 1 d . . . H60 H 0.2960 0.7377 0.6108 0.053 Uiso 1 1 calc R . . C61 C 0.3400(3) 0.7276(3) 0.5478(3) 0.0538(15) Uani 1 1 d . . . H61 H 0.3599 0.7780 0.5536 0.065 Uiso 1 1 calc R . . C62 C 0.3491(3) 0.6784(3) 0.5052(3) 0.0576(16) Uani 1 1 d . . . H62 H 0.3744 0.6951 0.4809 0.069 Uiso 1 1 calc R . . C63 C 0.3215(3) 0.6051(3) 0.4979(2) 0.0408(12) Uani 1 1 d . . . H63 H 0.3283 0.5714 0.4685 0.049 Uiso 1 1 calc R . . C64 C 0.4215(2) 0.0780(2) 0.90994(18) 0.0253(9) Uani 1 1 d . . . H64 H 0.4313 0.1274 0.8979 0.030 Uiso 1 1 calc R . . C65 C 0.4461(3) -0.0583(2) 0.9222(2) 0.0348(11) Uani 1 1 d . . . H65A H 0.4390 -0.0555 0.9614 0.052 Uiso 1 1 calc R . . H65B H 0.4880 -0.0918 0.9288 0.052 Uiso 1 1 calc R . . H65C H 0.4017 -0.0790 0.8878 0.052 Uiso 1 1 calc R . . C66 C 0.5204(3) 0.0265(3) 0.8857(2) 0.0408(12) Uani 1 1 d . . . H66A H 0.5064 0.0029 0.8438 0.061 Uiso 1 1 calc R . . H66B H 0.5645 0.0011 0.9169 0.061 Uiso 1 1 calc R . . H66C H 0.5308 0.0812 0.8834 0.061 Uiso 1 1 calc R . . C67 C 0.1632(3) 0.1498(3) 0.5722(2) 0.0479(14) Uani 1 1 d . . . H67 H 0.1919 0.1404 0.6162 0.057 Uiso 1 1 calc R A 1 C68 C 0.0606(3) 0.1109(3) 0.4729(2) 0.0593(16) Uani 1 1 d . A 1 H68A H 0.0714 0.1604 0.4588 0.089 Uiso 1 1 calc R A 1 H68B H 0.0104 0.1115 0.4700 0.089 Uiso 1 1 calc R A 1 H68C H 0.0650 0.0699 0.4458 0.089 Uiso 1 1 calc R A 1 C69 C 0.1054(4) 0.0236(4) 0.5671(3) 0.077(2) Uani 1 1 d . A 1 H69A H 0.1433 0.0200 0.6108 0.116 Uiso 1 1 calc R A 1 H69B H 0.1112 -0.0188 0.5418 0.116 Uiso 1 1 calc R A 1 H69C H 0.0567 0.0207 0.5672 0.116 Uiso 1 1 calc R A 1 C70 C 0.0434(2) 0.4399(2) 0.57882(19) 0.0269(10) Uani 1 1 d . . . H70 H 0.0244 0.4342 0.5340 0.032 Uiso 1 1 calc R . . C71 C 0.0188(2) 0.4588(2) 0.67130(18) 0.0293(10) Uani 1 1 d . . . H71A H 0.0725 0.4553 0.6932 0.044 Uiso 1 1 calc R . . H71B H -0.0032 0.4167 0.6853 0.044 Uiso 1 1 calc R . . H71C H 0.0026 0.5080 0.6814 0.044 Uiso 1 1 calc R . . C72 C -0.0826(2) 0.4574(3) 0.5623(2) 0.0327(10) Uani 1 1 d . . . H72A H -0.0907 0.4571 0.5176 0.049 Uiso 1 1 calc R . . H72B H -0.1026 0.5049 0.5714 0.049 Uiso 1 1 calc R . . H72C H -0.1073 0.4132 0.5708 0.049 Uiso 1 1 calc R . . C73 C -0.2466(3) 0.1205(3) 0.3264(3) 0.0493(13) Uani 1 1 d . . . H73 H -0.2386 0.1365 0.2906 0.059 Uiso 1 1 calc R . . C74 C -0.3092(3) 0.0354(3) 0.3705(2) 0.0590(16) Uani 1 1 d . . . H74A H -0.3440 -0.0075 0.3558 0.089 Uiso 1 1 calc R . . H74B H -0.3309 0.0774 0.3850 0.089 Uiso 1 1 calc R . . H74C H -0.2637 0.0182 0.4057 0.089 Uiso 1 1 calc R . . C75 C -0.3285(3) 0.0243(3) 0.2583(2) 0.0485(13) Uani 1 1 d . . . H75A H -0.3140 0.0490 0.2274 0.073 Uiso 1 1 calc R . . H75B H -0.3820 0.0280 0.2435 0.073 Uiso 1 1 calc R . . H75C H -0.3140 -0.0299 0.2628 0.073 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 0.01498(11) 0.01585(11) 0.01293(10) 0.00104(8) 0.00804(9) 0.00227(9) O1 0.0160(14) 0.0214(14) 0.0175(13) -0.0008(10) 0.0086(11) 0.0004(11) N1 0.0239(19) 0.030(2) 0.0278(18) 0.0030(15) 0.0165(16) 0.0076(15) C1 0.0152(19) 0.0120(18) 0.0221(19) -0.0004(15) 0.0092(16) 0.0023(15) La2 0.01664(11) 0.01596(11) 0.01202(10) -0.00023(8) 0.00777(9) -0.00022(9) O2 0.0164(14) 0.0299(15) 0.0185(13) 0.0031(11) 0.0099(11) 0.0027(12) N2 0.064(3) 0.051(3) 0.044(2) -0.009(2) 0.026(2) -0.016(2) C2 0.0156(19) 0.0187(19) 0.0204(19) -0.0004(15) 0.0083(16) 0.0068(16) La3 0.01387(11) 0.01809(11) 0.01128(10) -0.00009(8) 0.00678(8) -0.00049(9) O3 0.0233(15) 0.0222(14) 0.0127(13) 0.0006(11) 0.0022(11) 0.0057(12) N3 0.0212(18) 0.0171(16) 0.0222(16) -0.0012(13) 0.0119(14) 0.0013(14) C3 0.022(2) 0.041(3) 0.025(2) 0.0102(19) 0.0124(18) 0.0049(19) O4 0.0179(14) 0.0148(13) 0.0145(12) -0.0006(10) 0.0089(11) 0.0029(10) N4 0.042(2) 0.036(2) 0.036(2) -0.0016(17) 0.0177(19) -0.0056(19) C4 0.043(3) 0.068(3) 0.024(2) 0.016(2) 0.016(2) 0.015(3) O5 0.0207(14) 0.0211(14) 0.0210(13) -0.0008(11) 0.0130(12) -0.0023(12) C5 0.040(3) 0.056(3) 0.018(2) 0.001(2) -0.004(2) 0.010(3) O6 0.0216(15) 0.0253(15) 0.0212(14) 0.0043(12) -0.0005(12) -0.0020(12) C6 0.023(2) 0.031(2) 0.035(3) -0.005(2) -0.005(2) -0.002(2) O7 0.0245(15) 0.0162(13) 0.0175(13) -0.0030(11) 0.0102(12) -0.0013(11) C7 0.022(2) 0.020(2) 0.029(2) -0.0002(17) 0.0081(18) 0.0023(17) O8 0.0379(18) 0.0219(15) 0.0156(13) -0.0022(11) 0.0078(13) -0.0048(13) C8 0.021(2) 0.0169(19) 0.0170(18) 0.0032(15) 0.0123(16) 0.0015(16) O9 0.0272(16) 0.0349(16) 0.0191(14) 0.0009(12) 0.0126(12) 0.0106(13) C9 0.027(2) 0.0175(19) 0.0174(18) 0.0006(15) 0.0140(17) 0.0016(17) O10 0.0209(14) 0.0185(13) 0.0184(13) 0.0022(11) 0.0118(11) 0.0067(11) C10 0.033(3) 0.028(2) 0.020(2) -0.0030(17) 0.0087(19) 0.0065(19) O11 0.0213(15) 0.0279(15) 0.0168(13) -0.0014(11) 0.0107(11) -0.0027(12) C11 0.051(3) 0.027(2) 0.032(2) -0.011(2) 0.015(2) 0.004(2) O12 0.0203(15) 0.0253(15) 0.0152(13) -0.0004(11) 0.0092(11) -0.0044(12) C12 0.045(3) 0.025(2) 0.031(2) 0.0067(19) 0.018(2) 0.019(2) O13 0.0239(15) 0.0189(14) 0.0196(13) 0.0012(11) 0.0101(12) -0.0015(12) C13 0.031(2) 0.030(2) 0.021(2) 0.0051(18) 0.0118(18) 0.0097(19) O14 0.0146(14) 0.0285(15) 0.0168(12) -0.0048(11) 0.0049(11) 0.0039(12) C14 0.028(2) 0.023(2) 0.0185(19) -0.0003(16) 0.0138(17) 0.0044(18) O15 0.0190(15) 0.0362(16) 0.0130(12) -0.0005(11) 0.0073(11) 0.0039(12) C15 0.018(2) 0.023(2) 0.0199(19) -0.0028(16) 0.0112(17) -0.0016(17) O16 0.0122(13) 0.0266(15) 0.0182(13) -0.0001(11) 0.0063(11) -0.0018(11) C16 0.016(2) 0.022(2) 0.0185(18) -0.0021(16) 0.0101(16) -0.0017(16) O17 0.0263(16) 0.0212(14) 0.0252(14) 0.0014(11) 0.0183(12) 0.0025(12) C17 0.018(2) 0.026(2) 0.0194(19) 0.0016(16) 0.0084(17) 0.0003(17) O18 0.0320(17) 0.0224(15) 0.0279(15) -0.0004(12) 0.0206(14) -0.0013(12) C18 0.022(2) 0.035(2) 0.0170(19) 0.0039(17) 0.0041(17) 0.0068(19) O19 0.0288(17) 0.0286(16) 0.0302(15) 0.0006(12) 0.0197(14) 0.0075(13) C19 0.026(2) 0.041(3) 0.026(2) -0.0066(19) 0.0054(19) -0.011(2) O20 0.049(2) 0.0180(14) 0.0208(14) -0.0003(12) 0.0148(14) -0.0086(14) C20 0.044(3) 0.034(3) 0.030(2) 0.001(2) 0.007(2) -0.020(2) O21 0.0172(15) 0.0312(16) 0.0220(14) 0.0017(12) 0.0081(12) 0.0059(12) C21 0.036(3) 0.028(2) 0.018(2) 0.0027(17) 0.0043(19) -0.009(2) O22 0.085(4) 0.091(3) 0.106(4) -0.053(3) 0.042(3) -0.035(3) C22 0.019(2) 0.019(2) 0.026(2) -0.0015(16) 0.0127(17) -0.0010(17) C23 0.028(2) 0.023(2) 0.026(2) -0.0055(17) 0.0189(18) -0.0034(18) C24 0.049(3) 0.023(2) 0.029(2) -0.0060(18) 0.021(2) -0.010(2) C25 0.075(4) 0.025(2) 0.043(3) 0.003(2) 0.035(3) -0.006(3) C26 0.076(4) 0.024(3) 0.060(3) -0.008(2) 0.046(3) -0.015(3) C27 0.054(3) 0.040(3) 0.052(3) -0.022(2) 0.032(3) -0.023(3) C28 0.038(3) 0.026(2) 0.038(2) -0.0079(19) 0.017(2) -0.006(2) C29 0.020(2) 0.019(2) 0.0180(19) -0.0059(16) 0.0081(17) -0.0076(17) C30 0.021(2) 0.0150(19) 0.025(2) -0.0026(16) 0.0138(17) -0.0005(16) C31 0.031(3) 0.034(2) 0.030(2) 0.0061(19) 0.018(2) 0.010(2) C32 0.030(3) 0.035(3) 0.040(3) 0.004(2) 0.018(2) 0.010(2) C33 0.036(3) 0.024(2) 0.047(3) -0.005(2) 0.030(2) 0.004(2) C34 0.039(3) 0.022(2) 0.032(2) -0.0039(18) 0.024(2) -0.001(2) C35 0.024(2) 0.0157(19) 0.026(2) 0.0006(16) 0.0159(18) -0.0004(17) C36 0.023(2) 0.0152(19) 0.024(2) 0.0028(16) 0.0119(17) 0.0005(16) C37 0.023(2) 0.018(2) 0.0186(19) 0.0041(16) 0.0046(17) -0.0083(17) C38 0.021(2) 0.018(2) 0.036(2) 0.0010(17) 0.0087(19) -0.0010(17) C39 0.019(2) 0.028(2) 0.055(3) -0.002(2) 0.009(2) -0.0021(19) C40 0.027(3) 0.032(3) 0.047(3) 0.010(2) -0.001(2) -0.008(2) C41 0.051(3) 0.058(3) 0.020(2) 0.002(2) 0.006(2) -0.022(3) C42 0.034(3) 0.048(3) 0.026(2) -0.001(2) 0.010(2) -0.019(2) C43 0.0133(19) 0.019(2) 0.0161(18) -0.0012(15) 0.0012(16) 0.0039(16) C44 0.016(2) 0.0175(19) 0.0185(18) -0.0003(15) 0.0067(16) -0.0010(16) C45 0.021(2) 0.021(2) 0.0205(19) 0.0001(16) 0.0091(17) 0.0016(17) C46 0.020(2) 0.024(2) 0.023(2) -0.0083(17) 0.0037(17) 0.0033(17) C47 0.031(3) 0.023(2) 0.031(2) -0.0028(18) 0.004(2) -0.0078(19) C48 0.041(3) 0.031(2) 0.037(2) -0.001(2) 0.018(2) -0.016(2) C49 0.031(3) 0.033(2) 0.028(2) -0.0066(18) 0.019(2) -0.008(2) C50 0.0151(19) 0.0191(19) 0.0142(17) -0.0006(15) 0.0070(15) -0.0024(16) C51 0.0163(19) 0.0145(18) 0.0150(17) -0.0008(14) 0.0061(15) 0.0002(15) C52 0.018(2) 0.034(2) 0.0195(19) -0.0005(17) 0.0094(17) 0.0006(18) C53 0.014(2) 0.041(3) 0.024(2) -0.0004(18) 0.0029(17) 0.0007(19) C54 0.024(2) 0.026(2) 0.0149(18) -0.0013(16) -0.0003(17) 0.0047(18) C55 0.028(2) 0.032(2) 0.0151(18) -0.0033(17) 0.0086(17) 0.0073(19) C56 0.019(2) 0.025(2) 0.0183(19) 0.0010(16) 0.0087(16) 0.0038(17) C57 0.015(2) 0.021(2) 0.0194(19) 0.0009(16) 0.0096(16) 0.0013(16) C58 0.025(2) 0.022(2) 0.024(2) 0.0006(17) 0.0087(18) -0.0019(18) C59 0.041(3) 0.023(2) 0.023(2) 0.0015(18) 0.008(2) 0.005(2) C60 0.065(4) 0.023(2) 0.034(3) -0.007(2) 0.011(3) -0.001(2) C61 0.067(4) 0.034(3) 0.052(3) -0.002(3) 0.016(3) -0.017(3) C62 0.069(4) 0.049(3) 0.061(4) -0.006(3) 0.033(3) -0.031(3) C63 0.044(3) 0.038(3) 0.044(3) -0.007(2) 0.021(2) -0.015(2) C64 0.029(2) 0.024(2) 0.024(2) 0.0034(17) 0.0122(19) 0.0080(19) C65 0.036(3) 0.034(3) 0.043(3) 0.000(2) 0.025(2) 0.010(2) C66 0.034(3) 0.044(3) 0.054(3) 0.005(2) 0.028(2) 0.011(2) C67 0.044(3) 0.063(4) 0.038(3) -0.017(3) 0.019(3) -0.008(3) C68 0.062(4) 0.069(4) 0.042(3) -0.006(3) 0.017(3) -0.005(3) C69 0.091(5) 0.075(4) 0.069(4) 0.023(3) 0.036(4) -0.017(4) C70 0.034(3) 0.026(2) 0.023(2) 0.0005(17) 0.014(2) 0.0048(19) C71 0.038(3) 0.028(2) 0.028(2) -0.0039(18) 0.020(2) 0.001(2) C72 0.022(2) 0.032(2) 0.041(3) 0.001(2) 0.011(2) 0.0019(19) C73 0.045(3) 0.045(3) 0.064(4) -0.010(3) 0.029(3) -0.009(3) C74 0.072(4) 0.069(4) 0.048(3) 0.007(3) 0.035(3) 0.000(3) C75 0.055(4) 0.049(3) 0.045(3) -0.009(2) 0.026(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O18 2.444(3) 4_566 ? La1 O5 2.476(3) . ? La1 O16 2.479(3) 4_566 ? La1 O7 2.512(2) . ? La1 O2 2.549(2) . ? La1 O19 2.564(3) . ? La1 O3 2.566(3) . ? La1 O4 2.665(2) . ? La1 O1 2.750(2) . ? La1 C1 3.030(4) . ? La1 La2 4.1080(3) . ? O1 C1 1.282(4) . ? O1 La3 2.502(3) 4_566 ? N1 C64 1.336(5) . ? N1 C66 1.453(5) . ? N1 C65 1.457(5) . ? C1 O2 1.256(4) . ? C1 C2 1.494(5) . ? La2 O13 2.497(2) . ? La2 O6 2.527(3) . ? La2 O4 2.543(2) . ? La2 O9 2.562(3) . ? La2 O11 2.597(3) . ? La2 O8 2.630(3) . ? La2 O12 2.641(2) . ? La2 O10 2.680(2) . ? La2 O7 2.725(2) . ? La2 O14 3.010(3) . ? La2 O5 3.062(2) . ? La2 La3 4.1053(3) . ? N2 C67 1.342(6) . ? N2 C68 1.468(6) . ? N2 C69 1.468(7) . ? C2 C3 1.378(5) . ? C2 C7 1.395(5) . ? La3 O14 2.470(2) . ? La3 O15 2.495(2) . ? La3 O1 2.502(3) 4_565 ? La3 O17 2.510(3) . ? La3 O12 2.519(3) . ? La3 O20 2.523(3) . ? La3 O21 2.566(3) . ? La3 O10 2.608(2) . ? La3 O16 2.989(2) . ? La3 C50 3.117(3) . ? La3 La1 4.4110(3) 4_565 ? O3 C8 1.254(4) . ? N3 C70 1.310(5) . ? N3 C72 1.454(5) . ? N3 C71 1.460(5) . ? C3 C4 1.388(6) . ? C3 H3 0.9500 . ? O4 C8 1.286(4) . ? N4 C73 1.338(6) . ? N4 C75 1.436(6) . ? N4 C74 1.447(6) . ? C4 C5 1.370(7) . ? C4 H4 0.9500 . ? O5 C15 1.277(4) . ? C5 C6 1.377(7) . ? C5 H5 0.9500 . ? O6 C15 1.253(4) . ? C6 C7 1.384(5) . ? C6 H6 0.9500 . ? O7 C22 1.286(4) . ? C7 H7 0.9500 . ? O8 C22 1.249(4) . ? C8 C9 1.494(5) . ? O9 C29 1.259(4) . ? C9 C10 1.391(5) . ? C9 C14 1.399(5) . ? O10 C29 1.268(4) . ? C10 C11 1.384(6) . ? C10 H10 0.9500 . ? O11 C36 1.246(4) . ? C11 C12 1.389(6) . ? C11 H11 0.9500 . ? O12 C36 1.288(4) . ? C12 C13 1.395(6) . ? C12 H12 0.9500 . ? O13 C43 1.245(4) . ? C13 C14 1.385(5) . ? C13 H13 0.9500 . ? O14 C43 1.291(4) . ? C14 H14 0.9500 . ? O15 C50 1.259(4) . ? C15 C16 1.503(5) . ? O16 C50 1.265(4) . ? O16 La1 2.479(3) 4_565 ? C16 C21 1.378(5) . ? C16 C17 1.395(5) . ? O17 C57 1.251(4) . ? C17 C18 1.383(5) . ? C17 H17 0.9500 . ? O18 C57 1.269(4) . ? O18 La1 2.444(3) 4_565 ? C18 C19 1.368(6) . ? C18 H18 0.9500 . ? O19 C64 1.231(5) . ? C19 C20 1.391(6) . ? C19 H19 0.9500 . ? O20 C67 1.248(6) . ? C20 C21 1.391(6) . ? C20 H20 0.9500 . ? O21 C70 1.238(5) . ? C21 H21 0.9500 . ? O22 C73 1.235(6) . ? C22 C23 1.495(5) . ? C23 C24 1.384(6) . ? C23 C28 1.385(5) . ? C24 C25 1.379(6) . ? C24 H24 0.9500 . ? C25 C26 1.378(7) . ? C25 H25 0.9500 . ? C26 C27 1.373(7) . ? C26 H26 0.9500 . ? C27 C28 1.395(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.495(5) . ? C30 C31 1.385(5) . ? C30 C35 1.391(5) . ? C31 C32 1.391(6) . ? C31 H31 0.9500 . ? C32 C33 1.387(6) . ? C32 H32 0.9500 . ? C33 C34 1.373(6) . ? C33 H33 0.9500 . ? C34 C35 1.392(5) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.503(5) . ? C37 C42 1.383(5) . ? C37 C38 1.390(6) . ? C38 C39 1.384(6) . ? C38 H38 0.9500 . ? C39 C40 1.370(7) . ? C39 H39 0.9500 . ? C40 C41 1.366(7) . ? C40 H40 0.9500 . ? C41 C42 1.397(6) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.492(5) . ? C44 C49 1.384(5) . ? C44 C45 1.397(5) . ? C45 C46 1.382(5) . ? C45 H45 0.9500 . ? C46 C47 1.380(6) . ? C46 H46 0.9500 . ? C47 C48 1.383(6) . ? C47 H47 0.9500 . ? C48 C49 1.388(6) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? C50 C51 1.501(5) . ? C51 C56 1.386(5) . ? C51 C52 1.390(5) . ? C52 C53 1.385(5) . ? C52 H52 0.9500 . ? C53 C54 1.385(6) . ? C53 H53 0.9500 . ? C54 C55 1.379(6) . ? C54 H54 0.9500 . ? C55 C56 1.391(5) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C58 1.507(5) . ? C58 C59 1.373(6) . ? C58 C63 1.389(6) . ? C59 C60 1.400(6) . ? C59 H59 0.9500 . ? C60 C61 1.360(7) . ? C60 H60 0.9500 . ? C61 C62 1.377(7) . ? C61 H61 0.9500 . ? C62 C63 1.374(6) . ? C62 H62 0.9500 . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67 0.9500 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70 0.9500 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73 0.9500 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? 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 O18 La1 O5 143.41(9) 4_566 . ? O18 La1 O16 72.19(9) 4_566 4_566 ? O5 La1 O16 142.63(8) . 4_566 ? O18 La1 O7 92.83(8) 4_566 . ? O5 La1 O7 77.53(8) . . ? O16 La1 O7 93.35(8) 4_566 . ? O18 La1 O2 89.29(8) 4_566 . ? O5 La1 O2 80.35(8) . . ? O16 La1 O2 120.00(8) 4_566 . ? O7 La1 O2 145.39(8) . . ? O18 La1 O19 71.46(9) 4_566 . ? O5 La1 O19 71.97(9) . . ? O16 La1 O19 140.35(9) 4_566 . ? O7 La1 O19 73.23(8) . . ? O2 La1 O19 74.79(8) . . ? O18 La1 O3 138.81(8) 4_566 . ? O5 La1 O3 75.15(8) . . ? O16 La1 O3 76.42(8) 4_566 . ? O7 La1 O3 115.21(8) . . ? O2 La1 O3 83.84(8) . . ? O19 La1 O3 143.17(9) . . ? O18 La1 O4 139.20(8) 4_566 . ? O5 La1 O4 68.19(8) . . ? O16 La1 O4 75.03(8) 4_566 . ? O7 La1 O4 65.44(7) . . ? O2 La1 O4 128.56(8) . . ? O19 La1 O4 127.11(8) . . ? O3 La1 O4 49.98(7) . . ? O18 La1 O1 68.84(8) 4_566 . ? O5 La1 O1 123.66(8) . . ? O16 La1 O1 71.20(8) 4_566 . ? O7 La1 O1 158.68(8) . . ? O2 La1 O1 49.07(8) . . ? O19 La1 O1 109.04(8) . . ? O3 La1 O1 76.29(7) . . ? O4 La1 O1 121.57(7) . . ? O18 La1 C1 77.30(9) 4_566 . ? O5 La1 C1 102.39(9) . . ? O16 La1 C1 96.19(9) 4_566 . ? O7 La1 C1 163.40(9) . . ? O2 La1 C1 24.09(9) . . ? O19 La1 C1 90.85(9) . . ? O3 La1 C1 80.33(8) . . ? O4 La1 C1 130.31(8) . . ? O1 La1 C1 25.03(8) . . ? O18 La1 La2 133.03(6) 4_566 . ? O5 La1 La2 47.92(6) . . ? O16 La1 La2 103.25(5) 4_566 . ? O7 La1 La2 40.21(6) . . ? O2 La1 La2 128.10(6) . . ? O19 La1 La2 90.28(6) . . ? O3 La1 La2 79.62(5) . . ? O4 La1 La2 36.90(5) . . ? O1 La1 La2 155.91(5) . . ? C1 La1 La2 147.79(7) . . ? C1 O1 La3 155.8(2) . 4_566 ? C1 O1 La1 89.8(2) . . ? La3 O1 La1 114.17(9) 4_566 . ? C64 N1 C66 122.8(4) . . ? C64 N1 C65 119.8(4) . . ? C66 N1 C65 117.4(3) . . ? O2 C1 O1 120.9(3) . . ? O2 C1 C2 119.8(3) . . ? O1 C1 C2 119.3(3) . . ? O2 C1 La1 55.98(18) . . ? O1 C1 La1 65.17(18) . . ? C2 C1 La1 174.1(2) . . ? O13 La2 O6 70.57(8) . . ? O13 La2 O4 76.86(8) . . ? O6 La2 O4 80.40(9) . . ? O13 La2 O9 136.90(9) . . ? O6 La2 O9 75.63(9) . . ? O4 La2 O9 122.98(8) . . ? O13 La2 O11 73.46(8) . . ? O6 La2 O11 140.99(8) . . ? O4 La2 O11 77.18(8) . . ? O9 La2 O11 143.28(8) . . ? O13 La2 O8 142.66(9) . . ? O6 La2 O8 146.75(9) . . ? O4 La2 O8 104.55(8) . . ? O9 La2 O8 74.32(9) . . ? O11 La2 O8 70.66(9) . . ? O13 La2 O12 79.25(8) . . ? O6 La2 O12 133.59(8) . . ? O4 La2 O12 126.25(8) . . ? O9 La2 O12 107.28(8) . . ? O11 La2 O12 49.94(8) . . ? O8 La2 O12 70.01(8) . . ? O13 La2 O10 105.62(8) . . ? O6 La2 O10 92.23(8) . . ? O4 La2 O10 171.05(8) . . ? O9 La2 O10 49.47(8) . . ? O11 La2 O10 111.76(8) . . ? O8 La2 O10 78.86(8) . . ? O12 La2 O10 62.64(8) . . ? O13 La2 O7 139.65(8) . . ? O6 La2 O7 110.52(8) . . ? O4 La2 O7 64.13(7) . . ? O9 La2 O7 77.28(8) . . ? O11 La2 O7 87.67(8) . . ? O8 La2 O7 48.66(7) . . ? O12 La2 O7 115.31(7) . . ? O10 La2 O7 114.53(7) . . ? O13 La2 O14 46.39(8) . . ? O6 La2 O14 67.73(7) . . ? O4 La2 O14 120.83(7) . . ? O9 La2 O14 96.23(8) . . ? O11 La2 O14 97.47(7) . . ? O8 La2 O14 129.49(7) . . ? O12 La2 O14 65.91(7) . . ? O10 La2 O14 59.85(7) . . ? O7 La2 O14 173.49(7) . . ? O13 La2 O5 105.48(7) . . ? O6 La2 O5 45.50(7) . . ? O4 La2 O5 61.15(7) . . ? O9 La2 O5 65.17(7) . . ? O11 La2 O5 136.77(7) . . ? O8 La2 O5 107.54(7) . . ? O12 La2 O5 172.40(7) . . ? O10 La2 O5 110.00(7) . . ? O7 La2 O5 65.03(7) . . ? O14 La2 O5 112.84(7) . . ? O13 La2 La3 72.96(6) . . ? O6 La2 La3 99.87(6) . . ? O4 La2 La3 147.69(5) . . ? O9 La2 La3 87.65(6) . . ? O11 La2 La3 83.40(5) . . ? O8 La2 La3 92.81(5) . . ? O12 La2 La3 36.26(6) . . ? O10 La2 La3 38.44(5) . . ? O7 La2 La3 141.02(5) . . ? O14 La2 La3 36.71(5) . . ? O5 La2 La3 138.80(5) . . ? C1 O2 La1 99.9(2) . . ? C67 N2 C68 121.2(5) . . ? C67 N2 C69 122.4(5) . . ? C68 N2 C69 116.3(4) . . ? C3 C2 C7 120.0(4) . . ? C3 C2 C1 120.8(4) . . ? C7 C2 C1 119.2(3) . . ? O14 La3 O15 139.68(8) . . ? O14 La3 O1 100.23(8) . 4_565 ? O15 La3 O1 113.16(8) . 4_565 ? O14 La3 O17 84.29(8) . . ? O15 La3 O17 85.70(9) . . ? O1 La3 O17 71.18(8) 4_565 . ? O14 La3 O12 76.51(8) . . ? O15 La3 O12 89.92(8) . . ? O1 La3 O12 141.18(8) 4_565 . ? O17 La3 O12 144.47(8) . . ? O14 La3 O20 136.65(8) . . ? O15 La3 O20 70.90(9) . . ? O1 La3 O20 84.70(9) 4_565 . ? O17 La3 O20 136.45(8) . . ? O12 La3 O20 73.57(9) . . ? O14 La3 O21 70.69(8) . . ? O15 La3 O21 68.99(8) . . ? O1 La3 O21 146.75(8) 4_565 . ? O17 La3 O21 76.03(8) . . ? O12 La3 O21 69.53(8) . . ? O20 La3 O21 124.39(9) . . ? O14 La3 O10 68.30(8) . . ? O15 La3 O10 139.02(8) . . ? O1 La3 O10 77.47(8) 4_565 . ? O17 La3 O10 133.50(8) . . ? O12 La3 O10 65.27(8) . . ? O20 La3 O10 70.97(8) . . ? O21 La3 O10 124.11(8) . . ? O14 La3 O16 157.36(8) . . ? O15 La3 O16 46.44(8) . . ? O1 La3 O16 66.85(7) 4_565 . ? O17 La3 O16 74.06(7) . . ? O12 La3 O16 125.43(7) . . ? O20 La3 O16 63.10(8) . . ? O21 La3 O16 109.33(7) . . ? O10 La3 O16 123.04(7) . . ? O14 La3 C50 156.39(9) . . ? O15 La3 C50 22.65(9) . . ? O1 La3 C50 90.59(9) 4_565 . ? O17 La3 C50 79.42(9) . . ? O12 La3 C50 107.74(9) . . ? O20 La3 C50 64.76(9) . . ? O21 La3 C50 88.76(9) . . ? O10 La3 C50 135.01(8) . . ? O16 La3 C50 23.79(8) . . ? O14 La3 La2 46.75(6) . . ? O15 La3 La2 128.09(6) . . ? O1 La3 La2 113.19(5) 4_565 . ? O17 La3 La2 131.01(6) . . ? O12 La3 La2 38.32(6) . . ? O20 La3 La2 91.49(6) . . ? O21 La3 La2 84.42(6) . . ? O10 La3 La2 39.70(5) . . ? O16 La3 La2 154.59(5) . . ? C50 La3 La2 145.24(7) . . ? O14 La3 La1 130.70(6) . 4_565 ? O15 La3 La1 78.51(6) . 4_565 ? O1 La3 La1 34.66(5) 4_565 4_565 ? O17 La3 La1 65.77(6) . 4_565 ? O12 La3 La1 147.26(6) . 4_565 ? O20 La3 La1 73.70(7) . 4_565 ? O21 La3 La1 131.10(6) . 4_565 ? O10 La3 La1 104.47(5) . 4_565 ? O16 La3 La1 32.48(5) . 4_565 ? C50 La3 La1 56.04(7) . 4_565 ? La2 La3 La1 144.022(7) . 4_565 ? C8 O3 La1 96.7(2) . . ? C70 N3 C72 121.3(3) . . ? C70 N3 C71 121.4(3) . . ? C72 N3 C71 117.2(3) . . ? C2 C3 C4 119.8(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C8 O4 La2 139.3(2) . . ? C8 O4 La1 91.26(19) . . ? La2 O4 La1 104.11(8) . . ? C73 N4 C75 120.6(4) . . ? C73 N4 C74 121.4(4) . . ? C75 N4 C74 118.0(4) . . ? C5 C4 C3 120.4(4) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C15 O5 La1 148.2(2) . . ? C15 O5 La2 82.9(2) . . ? La1 O5 La2 95.20(8) . . ? C4 C5 C6 119.9(4) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C15 O6 La2 109.2(2) . . ? C5 C6 C7 120.6(4) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C22 O7 La1 164.4(2) . . ? C22 O7 La2 92.4(2) . . ? La1 O7 La2 103.27(8) . . ? C6 C7 C2 119.2(4) . . ? C6 C7 H7 120.4 . . ? C2 C7 H7 120.4 . . ? C22 O8 La2 97.8(2) . . ? O3 C8 O4 121.1(3) . . ? O3 C8 C9 120.2(3) . . ? O4 C8 C9 118.7(3) . . ? C29 O9 La2 97.8(2) . . ? C10 C9 C14 120.0(3) . . ? C10 C9 C8 119.6(3) . . ? C14 C9 C8 120.4(3) . . ? C29 O10 La3 164.2(2) . . ? C29 O10 La2 92.0(2) . . ? La3 O10 La2 101.86(8) . . ? C11 C10 C9 120.4(4) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C36 O11 La2 95.4(2) . . ? C10 C11 C12 119.7(4) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C36 O12 La3 152.2(2) . . ? C36 O12 La2 92.3(2) . . ? La3 O12 La2 105.41(9) . . ? C11 C12 C13 120.3(4) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C43 O13 La2 105.8(2) . . ? C14 C13 C12 120.1(4) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C43 O14 La3 139.0(2) . . ? C43 O14 La2 80.8(2) . . ? La3 O14 La2 96.53(8) . . ? C13 C14 C9 119.6(4) . . ? C13 C14 H14 120.2 . . ? C9 C14 H14 120.2 . . ? C50 O15 La3 107.7(2) . . ? O6 C15 O5 122.3(3) . . ? O6 C15 C16 118.3(3) . . ? O5 C15 C16 119.3(3) . . ? C50 O16 La1 165.2(2) . 4_565 ? C50 O16 La3 83.78(19) . . ? La1 O16 La3 107.17(8) 4_565 . ? C21 C16 C17 119.2(4) . . ? C21 C16 C15 119.8(3) . . ? C17 C16 C15 121.0(3) . . ? C57 O17 La3 137.3(2) . . ? C18 C17 C16 119.9(4) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C57 O18 La1 145.7(2) . 4_565 ? C19 C18 C17 121.0(4) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C64 O19 La1 133.8(3) . . ? C18 C19 C20 119.7(4) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C67 O20 La3 130.3(3) . . ? C19 C20 C21 119.6(4) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C70 O21 La3 131.4(3) . . ? C16 C21 C20 120.7(4) . . ? C16 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? O8 C22 O7 121.2(3) . . ? O8 C22 C23 119.3(3) . . ? O7 C22 C23 119.6(3) . . ? C24 C23 C28 119.6(4) . . ? C24 C23 C22 120.6(4) . . ? C28 C23 C22 119.7(4) . . ? C25 C24 C23 119.5(4) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C26 C25 C24 121.4(5) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C27 C26 C25 119.2(4) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 120.2(5) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C23 C28 C27 120.1(4) . . ? C23 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? O9 C29 O10 120.7(3) . . ? O9 C29 C30 119.0(3) . . ? O10 C29 C30 120.3(3) . . ? C31 C30 C35 119.6(4) . . ? C31 C30 C29 118.6(3) . . ? C35 C30 C29 121.8(3) . . ? C30 C31 C32 120.4(4) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C33 C32 C31 119.4(4) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C34 C33 C32 120.7(4) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 119.9(4) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C30 C35 C34 120.0(4) . . ? C30 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? O11 C36 O12 121.5(3) . . ? O11 C36 C37 119.6(4) . . ? O12 C36 C37 118.8(3) . . ? C42 C37 C38 118.9(4) . . ? C42 C37 C36 121.1(4) . . ? C38 C37 C36 120.0(3) . . ? C39 C38 C37 120.9(4) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C40 C39 C38 119.3(5) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? C41 C40 C39 121.0(4) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C40 C41 C42 120.0(4) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C37 C42 C41 119.8(4) . . ? C37 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? O13 C43 O14 122.2(3) . . ? O13 C43 C44 119.1(3) . . ? O14 C43 C44 118.6(3) . . ? C49 C44 C45 119.2(3) . . ? C49 C44 C43 121.4(3) . . ? C45 C44 C43 119.3(3) . . ? C46 C45 C44 120.1(4) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C47 C46 C45 120.3(4) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C46 C47 C48 119.9(4) . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C47 C48 C49 120.0(4) . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C44 C49 C48 120.4(4) . . ? C44 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? O15 C50 O16 122.1(3) . . ? O15 C50 C51 117.8(3) . . ? O16 C50 C51 120.1(3) . . ? O15 C50 La3 49.70(17) . . ? O16 C50 La3 72.42(19) . . ? C51 C50 La3 167.5(3) . . ? C56 C51 C52 120.0(3) . . ? C56 C51 C50 120.6(3) . . ? C52 C51 C50 119.4(3) . . ? C53 C52 C51 119.8(4) . . ? C53 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C54 C53 C52 120.0(4) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C55 C54 C53 120.5(4) . . ? C55 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? C54 C55 C56 119.7(4) . . ? C54 C55 H55 120.1 . . ? C56 C55 H55 120.1 . . ? C51 C56 C55 120.0(4) . . ? C51 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? O17 C57 O18 125.9(3) . . ? O17 C57 C58 118.6(3) . . ? O18 C57 C58 115.5(3) . . ? C59 C58 C63 118.1(4) . . ? C59 C58 C57 122.6(4) . . ? C63 C58 C57 119.3(4) . . ? C58 C59 C60 120.4(4) . . ? C58 C59 H59 119.8 . . ? C60 C59 H59 119.8 . . ? C61 C60 C59 120.4(5) . . ? C61 C60 H60 119.8 . . ? C59 C60 H60 119.8 . . ? C60 C61 C62 119.7(5) . . ? C60 C61 H61 120.1 . . ? C62 C61 H61 120.1 . . ? C63 C62 C61 119.9(5) . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? C62 C63 C58 121.4(5) . . ? C62 C63 H63 119.3 . . ? C58 C63 H63 119.3 . . ? O19 C64 N1 123.1(4) . . ? O19 C64 H64 118.4 . . ? N1 C64 H64 118.4 . . ? N1 C65 H65A 109.5 . . ? N1 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? N1 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N1 C66 H66A 109.5 . . ? N1 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? N1 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O20 C67 N2 124.6(5) . . ? O20 C67 H67 117.7 . . ? N2 C67 H67 117.7 . . ? O21 C70 N3 126.1(4) . . ? O21 C70 H70 117.0 . . ? N3 C70 H70 117.0 . . ? N3 C71 H71A 109.5 . . ? N3 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? N3 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N3 C72 H72A 109.5 . . ? N3 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? N3 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? O22 C73 N4 123.8(5) . . ? O22 C73 H73 118.1 . . ? N4 C73 H73 118.1 . . ? N4 C74 H74A 109.5 . . ? N4 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? N4 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? N4 C75 H75A 109.5 . . ? N4 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? N4 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? 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 C40 H40 O22 0.95 2.69 3.348(7) 126.8 . C41 H41 O22 0.95 2.79 3.393(6) 121.9 . C64 H64 O5 0.95 2.43 3.029(5) 121.1 . C67 H67 O8 0.95 2.69 3.488(6) 141.7 . C67 H67 O10 0.95 2.57 3.134(5) 118.1 . C71 H71A O13 0.98 2.62 3.559(5) 159.6 . C70 H70 O15 0.95 2.35 2.895(5) 115.9 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.600 _refine_diff_density_min -0.932 _refine_diff_density_rms 0.125 # Attachment '3.CIF' data_hb11dmf _database_code_depnum_ccdc_archive 'CCDC 634372' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (La3(2-MeBA)9(DMF)2)n _chemical_melting_point ? _chemical_formula_moiety 'C78 H74 La3 N2 O20' _chemical_formula_sum 'C78 H74 La3 N2 O20' _chemical_formula_weight 1779.15 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.4745(1) _cell_length_b 21.8201(2) _cell_length_c 22.9482(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.962(1) _cell_angle_gamma 90.00 _cell_volume 7411.50(11) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3560 _exptl_absorpt_coefficient_mu 1.772 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5375 _exptl_absorpt_correction_T_max 0.7769 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 43039 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16965 _reflns_number_gt 13926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0000P)^2^+23.0052P] 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 16965 _refine_ls_number_parameters 1167 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.010 _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 0.267534(17) 0.813056(11) 1.157710(10) 0.02107(6) Uani 1 1 d . . . O1 O 0.1302(3) 0.88396(16) 1.12988(16) 0.0454(10) Uani 1 1 d . . . N1 N 0.4303(3) 0.99294(18) 1.2236(2) 0.0406(11) Uani 1 1 d . . . C1 C 0.0849(3) 0.85586(19) 1.15796(19) 0.0292(11) Uani 1 1 d . . . La2 La 0.243205(15) 0.749811(11) 0.987356(10) 0.01591(6) Uani 1 1 d . . . O2 O 0.1240(2) 0.81913(13) 1.20129(12) 0.0227(6) Uani 1 1 d . . . N2 N 0.0616(4) 0.49578(18) 0.78679(18) 0.0413(11) Uani 1 1 d . . . C2 C -0.0159(4) 0.8636(2) 1.1397(2) 0.0362(12) Uani 1 1 d . . . La3 La 0.179891(17) 0.694250(10) 0.814435(10) 0.01935(6) Uani 1 1 d . . . O3 O 0.4353(2) 0.79110(17) 1.17143(15) 0.0390(8) Uani 1 1 d . . . C3 C -0.0613(4) 0.8449(2) 1.1806(2) 0.0403(12) Uani 1 1 d . . . H3 H -0.0284 0.8264 1.2180 0.048 Uiso 1 1 calc R . . O4 O 0.34441(18) 0.74110(13) 1.09501(12) 0.0216(6) Uani 1 1 d . . . C4 C -0.1539(4) 0.8527(3) 1.1679(3) 0.0608(18) Uani 1 1 d . . . H4 H -0.1835 0.8408 1.1970 0.073 Uiso 1 1 calc R . . O5 O 0.2550(2) 0.85342(13) 1.05052(13) 0.0247(7) Uani 1 1 d . . . C5 C -0.2021(5) 0.8773(4) 1.1137(4) 0.082(2) Uani 1 1 d . . . H5 H -0.2654 0.8834 1.1050 0.099 Uiso 1 1 calc R . . O6 O 0.3093(2) 0.85486(15) 0.97258(15) 0.0382(9) Uani 1 1 d . . . C6 C -0.1583(6) 0.8933(4) 1.0716(4) 0.087(3) Uani 1 1 d . . . H6 H -0.1930 0.9092 1.0335 0.105 Uiso 1 1 calc R . . O7 O 0.15999(19) 0.75150(13) 1.07715(13) 0.0252(6) Uani 1 1 d . . . C7 C -0.0643(5) 0.8870(3) 1.0826(3) 0.0592(18) Uani 1 1 d . . . O8 O 0.0760(2) 0.73726(16) 0.98344(13) 0.0336(8) Uani 1 1 d . . . C8 C -0.0217(6) 0.9044(3) 1.0333(3) 0.079(2) Uani 1 1 d . . . H8A H 0.0163 0.9408 1.0461 0.119 Uiso 1 1 calc R . . H8B H -0.0693 0.9134 0.9955 0.119 Uiso 1 1 calc R . . H8C H 0.0154 0.8703 1.0264 0.119 Uiso 1 1 calc R . . C9 C 0.4218(3) 0.7481(2) 1.13343(19) 0.0261(9) Uani 1 1 d . . . O9B O 0.2471(3) 0.63495(14) 1.01035(14) 0.0391(8) Uani 1 1 d . . . O10 O 0.1699(2) 0.65628(13) 0.91543(12) 0.0243(6) Uani 1 1 d . . . C10 C 0.4936(3) 0.7025(2) 1.1332(2) 0.0323(11) Uani 1 1 d . . . O11 O 0.14186(18) 0.78191(13) 0.88521(12) 0.0200(6) Uani 1 1 d . . . C11 C 0.4666(4) 0.6466(2) 1.1044(2) 0.0382(12) Uani 1 1 d . . . H11 H 0.4041 0.6389 1.0859 0.046 Uiso 1 1 calc R . . O12 O 0.02982(19) 0.74366(14) 0.81149(13) 0.0279(7) Uani 1 1 d . . . C12 C 0.5297(5) 0.6018(3) 1.1024(3) 0.0630(19) Uani 1 1 d . . . H12 H 0.5105 0.5636 1.0830 0.076 Uiso 1 1 calc R . . O13 O 0.4072(2) 0.73502(16) 0.98634(14) 0.0350(8) Uani 1 1 d . . . C13 C 0.6206(5) 0.6134(4) 1.1288(3) 0.077(3) Uani 1 1 d . . . H13 H 0.6643 0.5835 1.1268 0.093 Uiso 1 1 calc R . . O14 O 0.31334(19) 0.73636(14) 0.89412(13) 0.0245(6) Uani 1 1 d . . . C14 C 0.6471(4) 0.6675(4) 1.1575(3) 0.071(2) Uani 1 1 d . . . H14 H 0.7098 0.6744 1.1759 0.085 Uiso 1 1 calc R . . O15 O 0.2927(2) 0.60751(14) 0.83661(15) 0.0366(8) Uani 1 1 d . . . C15 C 0.5858(3) 0.7140(3) 1.1611(2) 0.0487(16) Uani 1 1 d . . . O16 O 0.3236(2) 0.67190(13) 0.77201(12) 0.0227(6) Uani 1 1 d . . . C16 C 0.6210(4) 0.7730(3) 1.1930(3) 0.074(2) Uani 1 1 d . . . H16A H 0.6023 0.7765 1.2302 0.111 Uiso 1 1 calc R . . H16B H 0.5965 0.8076 1.1660 0.111 Uiso 1 1 calc R . . H16C H 0.6871 0.7735 1.2037 0.111 Uiso 1 1 calc R . . O17 O 0.1985(2) 0.79317(13) 0.77003(13) 0.0280(7) Uani 1 1 d . . . C17 C 0.3023(3) 0.8787(2) 1.0201(2) 0.0274(10) Uani 1 1 d . . . O18 O 0.2761(2) 0.79079(14) 0.70218(13) 0.0282(7) Uani 1 1 d . . . C18 C 0.3475(4) 0.9388(2) 1.0414(2) 0.0387(13) Uani 1 1 d . . . O19 O 0.3401(3) 0.91470(15) 1.18038(15) 0.0455(10) Uani 1 1 d . . . C19 C 0.2934(5) 0.9869(2) 1.0534(2) 0.0574(19) Uani 1 1 d . . . H19 H 0.2309 0.9811 1.0488 0.069 Uiso 1 1 calc R . . O20 O 0.0892(3) 0.59791(14) 0.79045(15) 0.0388(9) Uani 1 1 d . . . C20 C 0.3360(7) 1.0435(3) 1.0723(3) 0.079(3) Uani 1 1 d . . . H20 H 0.3013 1.0772 1.0791 0.095 Uiso 1 1 calc R . . C21 C 0.4272(8) 1.0507(4) 1.0811(3) 0.094(3) Uani 1 1 d . . . H21 H 0.4551 1.0890 1.0944 0.112 Uiso 1 1 calc R . . C22 C 0.4784(6) 1.0026(4) 1.0708(3) 0.083(3) Uani 1 1 d . . . H22 H 0.5415 1.0081 1.0778 0.100 Uiso 1 1 calc R . . C23 C 0.4394(4) 0.9456(3) 1.0502(3) 0.0513(16) Uani 1 1 d . . . C24 C 0.4960(5) 0.8960(4) 1.0424(3) 0.078(2) Uani 1 1 d . . . H24A H 0.4917 0.8620 1.0694 0.118 Uiso 1 1 calc R . . H24B H 0.5588 0.9100 1.0525 0.118 Uiso 1 1 calc R . . H24C H 0.4762 0.8820 1.0000 0.118 Uiso 1 1 calc R . . C25 C 0.0840(3) 0.73915(19) 1.03907(19) 0.0219(9) Uani 1 1 d . . . C26 C 0.0055(3) 0.7262(2) 1.0628(2) 0.0286(10) Uani 1 1 d . . . C27 C 0.0255(3) 0.70827(19) 1.1239(2) 0.0304(10) Uani 1 1 d . . . H27 H 0.0867 0.7040 1.1476 0.036 Uiso 1 1 calc R . . C28 C -0.0423(5) 0.6968(2) 1.1500(3) 0.0492(16) Uani 1 1 d . . . H28 H -0.0283 0.6858 1.1918 0.059 Uiso 1 1 calc R . . C29 C -0.1316(5) 0.7014(4) 1.1143(4) 0.082(3) Uani 1 1 d . . . H29 H -0.1792 0.6926 1.1315 0.098 Uiso 1 1 calc R . . C30 C -0.1511(5) 0.7185(4) 1.0550(4) 0.099(3) Uani 1 1 d . . . H30 H -0.2126 0.7222 1.0317 0.119 Uiso 1 1 calc R . . C31 C -0.0839(4) 0.7308(3) 1.0269(3) 0.0617(19) Uani 1 1 d . . . C32 C -0.1112(4) 0.7495(5) 0.9602(3) 0.099(3) Uani 1 1 d . . . H32A H -0.0945 0.7924 0.9569 0.149 Uiso 1 1 calc R . . H32B H -0.1767 0.7448 0.9428 0.149 Uiso 1 1 calc R . . H32C H -0.0800 0.7235 0.9380 0.149 Uiso 1 1 calc R . . C33A C 0.1922(3) 0.6201(2) 0.9619(2) 0.0280(10) Uani 1 1 d . . . C34A C 0.1334(9) 0.5611(7) 0.9551(7) 0.019(4) Uani 0.50 1 d PU A 1 C34B C 0.1617(8) 0.5555(6) 0.9566(5) 0.019(3) Uani 0.50 1 d P A 2 C35A C 0.191(2) 0.5123(16) 0.9813(16) 0.042(7) Uani 0.50 1 d P A 1 H35A H 0.2529 0.5192 1.0013 0.050 Uiso 0.50 1 calc PR A 1 C35B C 0.2183(18) 0.5050(17) 0.9777(14) 0.032(5) Uani 0.50 1 d P A 2 H35B H 0.2812 0.5125 0.9946 0.039 Uiso 0.50 1 calc PR A 2 C36A C 0.1532(11) 0.4516(7) 0.9770(8) 0.041(4) Uani 0.50 1 d PU A 1 H36A H 0.1903 0.4168 0.9907 0.050 Uiso 0.50 1 calc PR A 1 C36B C 0.1897(10) 0.4476(5) 0.9755(5) 0.035(3) Uani 0.50 1 d P A 2 H36B H 0.2312 0.4147 0.9882 0.042 Uiso 0.50 1 calc PR A 2 C37A C 0.0589(13) 0.4462(8) 0.9517(6) 0.046(5) Uani 0.50 1 d P A 1 H37A H 0.0326 0.4067 0.9508 0.055 Uiso 0.50 1 calc PR A 1 C37B C 0.0958(11) 0.4367(9) 0.9537(9) 0.041(5) Uani 0.50 1 d PU A 2 H37B H 0.0724 0.3964 0.9540 0.049 Uiso 0.50 1 calc PR A 2 C38A C 0.0064(19) 0.492(2) 0.9297(18) 0.049(8) Uani 0.50 1 d P A 1 H38A H -0.0565 0.4845 0.9126 0.059 Uiso 0.50 1 calc PR A 1 C38B C 0.0370(17) 0.487(3) 0.9313(19) 0.045(7) Uani 0.50 1 d P A 2 H38B H -0.0261 0.4797 0.9154 0.053 Uiso 0.50 1 calc PR A 2 C39A C 0.0421(8) 0.5559(5) 0.9304(5) 0.025(3) Uani 0.50 1 d PU A 1 C39B C 0.0691(8) 0.5434(5) 0.9322(5) 0.023(3) Uani 0.50 1 d PU A 2 C40A C -0.0180(9) 0.6101(6) 0.9071(7) 0.036(3) Uani 0.50 1 d P A 1 H40D H -0.0117 0.6398 0.9402 0.054 Uiso 0.50 1 calc PR A 1 H40E H -0.0810 0.5964 0.8924 0.054 Uiso 0.50 1 calc PR A 1 H40F H -0.0007 0.6294 0.8736 0.054 Uiso 0.50 1 calc PR A 1 C40B C -0.0007(11) 0.5922(6) 0.9103(8) 0.032(4) Uani 0.50 1 d PU A 2 H40A H -0.0605 0.5755 0.9078 0.048 Uiso 0.50 1 calc PR A 2 H40B H 0.0002 0.6063 0.8699 0.048 Uiso 0.50 1 calc PR A 2 H40C H 0.0125 0.6267 0.9388 0.048 Uiso 0.50 1 calc PR A 2 C41 C 0.0605(3) 0.78396(19) 0.85108(18) 0.0212(9) Uani 1 1 d . . . C42 C 0.0050(3) 0.8388(2) 0.8567(2) 0.0336(11) Uani 1 1 d . D . C43 C 0.0521(5) 0.8914(2) 0.8841(2) 0.0489(15) Uani 1 1 d . . . H43 H 0.1159 0.8898 0.9010 0.059 Uiso 1 1 calc R D . C44 C 0.0066(7) 0.9453(3) 0.8865(3) 0.078(2) Uani 1 1 d . D . H44 H 0.0389 0.9813 0.9032 0.093 Uiso 1 1 calc R . . C45 C -0.0865(7) 0.9459(4) 0.8644(3) 0.092(3) Uani 1 1 d . . . H45 H -0.1184 0.9826 0.8667 0.110 Uiso 1 1 calc R D . C46 C -0.1338(5) 0.8944(4) 0.8392(3) 0.080(3) Uani 1 1 d . D . H46 H -0.1980 0.8958 0.8253 0.096 Uiso 1 1 calc R . . C47 C -0.0889(4) 0.8395(3) 0.8336(2) 0.0515(16) Uani 1 1 d . . . C48 C -0.1435(4) 0.7856(4) 0.8045(3) 0.070(2) Uani 1 1 d . D . H48A H -0.1347 0.7783 0.7645 0.105 Uiso 1 1 calc R . . H48B H -0.2076 0.7937 0.7996 0.105 Uiso 1 1 calc R . . H48C H -0.1243 0.7495 0.8304 0.105 Uiso 1 1 calc R . . C49 C 0.3933(3) 0.74333(19) 0.93083(18) 0.0219(9) Uani 1 1 d . . . C50 C 0.4674(3) 0.7628(2) 0.9048(2) 0.0288(10) Uani 1 1 d . A . C51 C 0.4433(3) 0.7835(2) 0.8452(2) 0.0270(10) Uani 1 1 d . . . H51 H 0.3811 0.7853 0.8228 0.032 Uiso 1 1 calc R A . C52 C 0.5076(4) 0.8018(2) 0.8175(2) 0.0388(12) Uani 1 1 d . A . H52 H 0.4901 0.8147 0.7762 0.047 Uiso 1 1 calc R . . C53 C 0.5969(4) 0.8008(3) 0.8509(3) 0.0600(18) Uani 1 1 d . . . H53 H 0.6418 0.8130 0.8326 0.072 Uiso 1 1 calc R A . C54 C 0.6218(4) 0.7823(4) 0.9106(4) 0.089(3) Uani 1 1 d . A . H54 H 0.6840 0.7828 0.9330 0.106 Uiso 1 1 calc R . . C55 C 0.5587(4) 0.7628(4) 0.9396(3) 0.068(2) Uani 1 1 d . . . C56 C 0.5918(4) 0.7419(6) 1.0058(4) 0.132(5) Uani 1 1 d . A . H56A H 0.6558 0.7524 1.0228 0.197 Uiso 1 1 calc R . . H56B H 0.5842 0.6975 1.0078 0.197 Uiso 1 1 calc R . . H56C H 0.5566 0.7625 1.0293 0.197 Uiso 1 1 calc R . . C57 C 0.3500(3) 0.6320(2) 0.8151(2) 0.0290(10) Uani 1 1 d . . . C58A C 0.4567(14) 0.6226(8) 0.8421(5) 0.019(3) Uani 0.63(5) 1 d P B 1 C58B C 0.4321(17) 0.6123(9) 0.8393(9) 0.012(4) Uani 0.37(5) 1 d PU B 2 C59A C 0.512(2) 0.6439(16) 0.8100(14) 0.029(6) Uani 0.63(5) 1 d P B 1 H59A H 0.4873 0.6641 0.7721 0.034 Uiso 0.63(5) 1 calc PR B 1 C59B C 0.498(4) 0.633(3) 0.811(2) 0.029(11) Uani 0.37(5) 1 d P B 2 H59B H 0.4798 0.6605 0.7780 0.035 Uiso 0.37(5) 1 calc PR B 2 C60A C 0.6046(11) 0.6362(12) 0.8323(5) 0.038(3) Uani 0.63(5) 1 d P B 1 H60A H 0.6438 0.6520 0.8108 0.045 Uiso 0.63(5) 1 calc PR B 1 C60B C 0.5885(14) 0.6147(14) 0.8299(8) 0.024(5) Uani 0.37(5) 1 d PU B 2 H60B H 0.6281 0.6258 0.8068 0.029 Uiso 0.37(5) 1 calc PR B 2 C61A C 0.6396(17) 0.6044(13) 0.8878(10) 0.049(5) Uani 0.63(5) 1 d P B 1 H61A H 0.7030 0.5986 0.9035 0.059 Uiso 0.63(5) 1 calc PR B 1 C61B C 0.619(2) 0.5811(17) 0.8810(15) 0.036(6) Uani 0.37(5) 1 d P B 2 H61B H 0.6798 0.5681 0.8956 0.043 Uiso 0.37(5) 1 calc PR B 2 C62A C 0.5852(18) 0.5819(10) 0.9188(8) 0.041(5) Uani 0.63(5) 1 d P B 1 H62A H 0.6105 0.5596 0.9553 0.050 Uiso 0.63(5) 1 calc PR B 1 C62B C 0.553(2) 0.5661(17) 0.9121(14) 0.042(7) Uani 0.37(5) 1 d P B 2 H62B H 0.5760 0.5468 0.9507 0.051 Uiso 0.37(5) 1 calc PR B 2 C63A C 0.4904(17) 0.5912(9) 0.8977(8) 0.025(4) Uani 0.63(5) 1 d P B 1 C63B C 0.464(2) 0.5760(17) 0.8930(16) 0.025(5) Uani 0.37(5) 1 d P B 2 C64A C 0.4341(18) 0.5667(12) 0.9376(12) 0.043(5) Uani 0.63(5) 1 d P B 1 H64D H 0.4016 0.6007 0.9496 0.064 Uiso 0.63(5) 1 calc PR B 1 H64E H 0.4741 0.5474 0.9740 0.064 Uiso 0.63(5) 1 calc PR B 1 H64F H 0.3906 0.5365 0.9145 0.064 Uiso 0.63(5) 1 calc PR B 1 C64B C 0.403(3) 0.558(2) 0.930(2) 0.045(8) Uani 0.37(5) 1 d P B 2 H64A H 0.4359 0.5319 0.9640 0.067 Uiso 0.37(5) 1 calc PR B 2 H64B H 0.3503 0.5362 0.9047 0.067 Uiso 0.37(5) 1 calc PR B 2 H64C H 0.3826 0.5953 0.9468 0.067 Uiso 0.37(5) 1 calc PR B 2 C65 C 0.2398(3) 0.81873(19) 0.73694(18) 0.0227(9) Uani 1 1 d . . . C66A C 0.2475(6) 0.8869(4) 0.7500(5) 0.019(2) Uani 0.544(10) 1 d P C 2 C66B C 0.2442(9) 0.8870(6) 0.7252(6) 0.023(3) Uani 0.456(10) 1 d PU C 1 C67A C 0.2548(10) 0.9083(7) 0.8099(6) 0.031(3) Uani 0.544(10) 1 d P C 2 H67A H 0.2552 0.8794 0.8410 0.037 Uiso 0.544(10) 1 calc PR C 2 C67B C 0.2368(8) 0.9084(6) 0.6664(6) 0.023(3) Uani 0.456(10) 1 d P C 1 H67B H 0.2370 0.8799 0.6351 0.028 Uiso 0.456(10) 1 calc PR C 1 C68A C 0.2613(6) 0.9692(4) 0.8238(5) 0.042(3) Uani 0.544(10) 1 d P C 2 H68A H 0.2671 0.9827 0.8641 0.050 Uiso 0.544(10) 1 calc PR C 2 C68B C 0.2292(8) 0.9702(5) 0.6530(5) 0.040(3) Uani 0.456(10) 1 d P C 1 H68B H 0.2197 0.9841 0.6124 0.048 Uiso 0.456(10) 1 calc PR C 1 C69A C 0.2593(12) 1.0108(6) 0.7785(8) 0.049(4) Uani 0.544(10) 1 d P C 2 H69A H 0.2635 1.0534 0.7874 0.059 Uiso 0.544(10) 1 calc PR C 2 C69B C 0.2356(12) 1.0104(7) 0.6988(9) 0.035(4) Uani 0.456(10) 1 d P C 1 H69B H 0.2331 1.0531 0.6902 0.042 Uiso 0.456(10) 1 calc PR C 1 C70A C 0.2512(12) 0.9911(7) 0.7203(8) 0.044(4) Uani 0.544(10) 1 d P C 2 H70A H 0.2486 1.0209 0.6896 0.053 Uiso 0.544(10) 1 calc PR C 2 C70B C 0.2457(12) 0.9913(7) 0.7566(9) 0.037(4) Uani 0.456(10) 1 d P C 1 H70B H 0.2499 1.0212 0.7875 0.045 Uiso 0.456(10) 1 calc PR C 1 C71A C 0.2466(6) 0.9296(4) 0.7044(5) 0.026(2) Uani 0.544(10) 1 d P C 2 C71B C 0.2501(7) 0.9285(5) 0.7726(6) 0.029(3) Uani 0.456(10) 1 d P C 1 C72A C 0.2374(10) 0.9099(6) 0.6393(5) 0.037(3) Uani 0.544(10) 1 d P C 2 H72A H 0.2918 0.8876 0.6381 0.056 Uiso 0.544(10) 1 calc PR C 2 H72B H 0.2300 0.9462 0.6132 0.056 Uiso 0.544(10) 1 calc PR C 2 H72C H 0.1845 0.8833 0.6247 0.056 Uiso 0.544(10) 1 calc PR C 2 C72B C 0.2622(16) 0.9100(10) 0.8372(8) 0.046(5) Uani 0.456(10) 1 d P C 1 H72D H 0.2055 0.8929 0.8409 0.069 Uiso 0.456(10) 1 calc PR C 1 H72E H 0.2790 0.9460 0.8637 0.069 Uiso 0.456(10) 1 calc PR C 1 H72F H 0.3100 0.8791 0.8493 0.069 Uiso 0.456(10) 1 calc PR C 1 C73 C 0.4149(4) 0.9408(2) 1.1943(2) 0.0371(12) Uani 1 1 d . . . H73 H 0.4630 0.9220 1.1831 0.045 Uiso 1 1 calc R . . C74 C 0.3608(5) 1.0221(3) 1.2433(3) 0.072(2) Uani 1 1 d . . . H74A H 0.3020 1.0047 1.2212 0.107 Uiso 1 1 calc R . . H74B H 0.3608 1.0662 1.2352 0.107 Uiso 1 1 calc R . . H74C H 0.3720 1.0154 1.2871 0.107 Uiso 1 1 calc R . . C75 C 0.5198(5) 1.0209(3) 1.2418(4) 0.082(3) Uani 1 1 d . . . H75A H 0.5429 1.0217 1.2864 0.124 Uiso 1 1 calc R . . H75B H 0.5159 1.0629 1.2260 0.124 Uiso 1 1 calc R . . H75C H 0.5608 0.9969 1.2253 0.124 Uiso 1 1 calc R . . C76A C 0.0302(5) 0.5548(3) 0.7788(3) 0.0304(18) Uani 0.679(8) 1 d P D 2 H76A H -0.0326 0.5634 0.7652 0.036 Uiso 0.679(8) 1 calc PR D 2 C76B C 0.1316(11) 0.5422(6) 0.7995(6) 0.030(4) Uani 0.321(8) 1 d P D 1 H76B H 0.1950 0.5352 0.8117 0.035 Uiso 0.321(8) 1 calc PR D 1 C77A C -0.0139(6) 0.4483(3) 0.7734(4) 0.041(2) Uani 0.679(8) 1 d P D 2 H77A H -0.0718 0.4684 0.7539 0.061 Uiso 0.679(8) 1 calc PR D 2 H77B H -0.0161 0.4292 0.8116 0.061 Uiso 0.679(8) 1 calc PR D 2 H77C H -0.0024 0.4169 0.7461 0.061 Uiso 0.679(8) 1 calc PR D 2 C77B C -0.0154(13) 0.4976(8) 0.7615(8) 0.047(5) Uani 0.321(8) 1 d P D 1 H77D H -0.0270 0.4784 0.7214 0.070 Uiso 0.321(8) 1 calc PR D 1 H77E H -0.0354 0.5404 0.7565 0.070 Uiso 0.321(8) 1 calc PR D 1 H77F H -0.0487 0.4756 0.7854 0.070 Uiso 0.321(8) 1 calc PR D 1 C78A C 0.1470(6) 0.4786(4) 0.8127(4) 0.043(2) Uani 0.679(8) 1 d P D 2 H78A H 0.1515 0.4579 0.8514 0.064 Uiso 0.679(8) 1 calc PR D 2 H78B H 0.1861 0.5148 0.8203 0.064 Uiso 0.679(8) 1 calc PR D 2 H78C H 0.1660 0.4505 0.7855 0.064 Uiso 0.679(8) 1 calc PR D 2 C78B C 0.1193(14) 0.4319(6) 0.8006(8) 0.050(5) Uani 0.321(8) 1 d P D 1 H78D H 0.1091 0.4117 0.8361 0.075 Uiso 0.321(8) 1 calc PR D 1 H78E H 0.1838 0.4410 0.8088 0.075 Uiso 0.321(8) 1 calc PR D 1 H78F H 0.0997 0.4048 0.7651 0.075 Uiso 0.321(8) 1 calc PR D 1 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 0.03259(14) 0.02058(12) 0.01093(11) -0.00201(9) 0.00775(10) -0.00420(11) O1 0.062(2) 0.040(2) 0.045(2) 0.0253(17) 0.032(2) 0.0249(18) N1 0.046(3) 0.029(2) 0.038(3) 0.0006(19) -0.002(2) -0.012(2) C1 0.055(3) 0.020(2) 0.015(2) -0.0014(17) 0.015(2) 0.012(2) La2 0.01607(11) 0.02159(11) 0.01031(10) -0.00208(9) 0.00421(8) -0.00319(10) O2 0.0338(17) 0.0230(15) 0.0119(14) 0.0038(12) 0.0075(12) 0.0028(13) N2 0.073(4) 0.023(2) 0.020(2) -0.0019(17) 0.002(2) -0.016(2) C2 0.051(3) 0.026(2) 0.030(3) 0.001(2) 0.010(2) 0.021(2) La3 0.03037(13) 0.01763(11) 0.01042(11) -0.00021(9) 0.00655(9) 0.00169(10) O3 0.0320(19) 0.057(2) 0.0280(18) -0.0168(16) 0.0091(15) -0.0188(17) C3 0.042(3) 0.041(3) 0.037(3) -0.001(2) 0.010(2) 0.012(2) O4 0.0204(14) 0.0307(16) 0.0128(14) -0.0018(12) 0.0034(11) 0.0012(13) C4 0.041(3) 0.070(4) 0.070(5) -0.005(4) 0.015(3) 0.022(3) O5 0.0341(17) 0.0249(15) 0.0164(15) 0.0008(12) 0.0091(13) -0.0044(13) C5 0.056(5) 0.093(6) 0.085(6) 0.004(5) 0.003(4) 0.045(4) O6 0.061(2) 0.0334(18) 0.0285(18) -0.0081(15) 0.0261(17) -0.0187(17) C6 0.091(6) 0.090(6) 0.061(5) 0.013(4) -0.010(4) 0.059(5) O7 0.0260(15) 0.0301(16) 0.0197(15) -0.0010(13) 0.0071(12) -0.0048(14) C7 0.085(5) 0.054(4) 0.034(3) 0.010(3) 0.009(3) 0.041(3) O8 0.0237(16) 0.060(2) 0.0173(16) -0.0008(15) 0.0065(13) -0.0066(16) C8 0.129(7) 0.076(5) 0.030(3) 0.024(3) 0.018(4) 0.052(5) C9 0.019(2) 0.042(3) 0.018(2) 0.004(2) 0.0055(16) -0.011(2) O9B 0.061(2) 0.0275(17) 0.0209(17) 0.0013(14) -0.0004(16) -0.0084(17) O10 0.0358(17) 0.0236(15) 0.0145(14) 0.0016(12) 0.0087(13) -0.0045(13) C10 0.020(2) 0.058(3) 0.018(2) 0.015(2) 0.0035(18) 0.005(2) O11 0.0212(15) 0.0253(15) 0.0144(14) -0.0007(12) 0.0065(12) -0.0006(12) C11 0.034(3) 0.054(3) 0.026(3) 0.010(2) 0.008(2) 0.018(2) O12 0.0245(16) 0.0339(17) 0.0231(16) -0.0034(14) 0.0032(13) -0.0038(14) C12 0.077(5) 0.073(4) 0.040(3) 0.016(3) 0.019(3) 0.047(4) O13 0.0243(17) 0.062(2) 0.0200(16) 0.0095(15) 0.0084(13) 0.0040(16) C13 0.062(5) 0.125(7) 0.049(4) 0.037(5) 0.023(4) 0.058(5) O14 0.0188(15) 0.0359(17) 0.0196(15) -0.0037(13) 0.0071(12) -0.0036(13) C14 0.024(3) 0.139(7) 0.053(4) 0.050(5) 0.015(3) 0.027(4) O15 0.049(2) 0.0307(17) 0.037(2) 0.0125(15) 0.0241(17) 0.0122(16) C15 0.023(3) 0.089(4) 0.032(3) 0.030(3) 0.004(2) 0.000(3) O16 0.0305(16) 0.0243(15) 0.0120(14) 0.0039(12) 0.0041(12) 0.0089(13) C16 0.026(3) 0.108(6) 0.075(5) 0.027(4) -0.006(3) -0.026(3) O17 0.0424(19) 0.0255(16) 0.0194(16) 0.0043(13) 0.0143(14) 0.0024(14) C17 0.034(3) 0.026(2) 0.020(2) 0.0024(18) 0.0032(19) -0.004(2) O18 0.0372(18) 0.0321(17) 0.0165(15) 0.0003(13) 0.0098(14) 0.0019(14) C18 0.065(4) 0.033(3) 0.017(2) 0.001(2) 0.011(2) -0.022(3) O19 0.077(3) 0.0328(18) 0.0193(17) 0.0013(14) 0.0020(18) -0.0236(19) C19 0.130(6) 0.023(3) 0.014(2) 0.000(2) 0.012(3) -0.009(3) O20 0.065(2) 0.0204(16) 0.0258(18) -0.0013(13) 0.0054(17) -0.0133(16) C20 0.176(9) 0.033(3) 0.029(3) -0.004(3) 0.031(5) -0.017(4) C21 0.176(10) 0.068(5) 0.038(4) -0.014(4) 0.033(5) -0.074(6) C22 0.115(7) 0.092(6) 0.039(4) -0.002(4) 0.018(4) -0.071(5) C23 0.063(4) 0.058(4) 0.033(3) 0.003(3) 0.015(3) -0.030(3) C24 0.056(4) 0.105(6) 0.075(5) 0.015(5) 0.020(4) -0.028(4) C25 0.021(2) 0.023(2) 0.022(2) 0.0013(17) 0.0071(17) 0.0015(17) C26 0.029(2) 0.032(2) 0.030(3) 0.004(2) 0.016(2) 0.005(2) C27 0.043(3) 0.023(2) 0.031(3) -0.0036(19) 0.019(2) -0.006(2) C28 0.088(5) 0.031(3) 0.048(3) 0.001(2) 0.050(3) -0.005(3) C29 0.062(5) 0.099(6) 0.112(7) 0.030(5) 0.068(5) 0.008(4) C30 0.036(4) 0.162(8) 0.115(7) 0.067(6) 0.046(4) 0.027(4) C31 0.028(3) 0.096(5) 0.068(4) 0.036(4) 0.024(3) 0.013(3) C32 0.021(3) 0.188(9) 0.083(5) 0.076(6) 0.007(3) 0.017(4) C33A 0.036(3) 0.024(2) 0.028(2) 0.0064(19) 0.015(2) -0.005(2) C34A 0.019(4) 0.019(4) 0.019(4) -0.0002(10) 0.0056(14) -0.0003(10) C34B 0.010(6) 0.035(7) 0.009(4) -0.004(4) -0.002(4) -0.005(5) C35A 0.08(2) 0.019(9) 0.025(7) -0.010(6) 0.013(13) -0.001(13) C35B 0.047(11) 0.029(11) 0.014(8) -0.001(6) -0.002(7) 0.008(8) C36A 0.042(4) 0.041(4) 0.041(4) 0.0004(10) 0.0116(16) -0.0002(10) C36B 0.044(8) 0.032(6) 0.028(6) -0.003(4) 0.007(6) -0.002(6) C37A 0.085(15) 0.030(7) 0.026(6) 0.002(5) 0.021(8) -0.031(9) C37B 0.041(5) 0.040(5) 0.041(5) 0.0006(10) 0.0117(17) -0.0006(10) C38A 0.071(18) 0.059(14) 0.021(7) -0.014(8) 0.021(14) -0.053(19) C38B 0.041(13) 0.068(13) 0.030(8) -0.013(8) 0.019(11) -0.043(14) C39A 0.025(3) 0.025(3) 0.025(3) -0.0003(10) 0.0074(12) -0.0003(10) C39B 0.023(3) 0.023(3) 0.023(3) 0.0001(10) 0.0066(12) 0.0003(10) C40A 0.025(7) 0.029(7) 0.048(8) -0.005(6) 0.002(5) -0.006(6) C40B 0.032(4) 0.032(4) 0.032(4) -0.0002(10) 0.0092(15) -0.0002(10) C41 0.023(2) 0.027(2) 0.016(2) 0.0042(17) 0.0103(17) 0.0012(18) C42 0.046(3) 0.039(3) 0.020(2) 0.010(2) 0.015(2) 0.018(2) C43 0.085(5) 0.032(3) 0.036(3) 0.003(2) 0.027(3) 0.020(3) C44 0.142(8) 0.047(4) 0.052(4) 0.003(3) 0.039(5) 0.036(4) C45 0.142(9) 0.095(6) 0.044(4) 0.010(4) 0.037(5) 0.082(6) C46 0.082(5) 0.125(7) 0.037(4) 0.022(4) 0.023(4) 0.076(5) C47 0.049(4) 0.081(4) 0.027(3) 0.015(3) 0.016(3) 0.032(3) C48 0.028(3) 0.128(7) 0.050(4) -0.002(4) 0.006(3) 0.014(4) C49 0.023(2) 0.027(2) 0.019(2) 0.0018(18) 0.0099(17) 0.0019(18) C50 0.027(2) 0.035(3) 0.030(2) 0.008(2) 0.017(2) 0.006(2) C51 0.032(3) 0.027(2) 0.025(2) -0.0001(19) 0.012(2) -0.0019(19) C52 0.059(4) 0.032(3) 0.035(3) 0.001(2) 0.029(3) -0.005(2) C53 0.048(4) 0.077(4) 0.073(5) 0.022(4) 0.046(4) 0.006(3) C54 0.026(3) 0.158(8) 0.089(6) 0.066(5) 0.027(3) 0.017(4) C55 0.022(3) 0.124(6) 0.060(4) 0.055(4) 0.016(3) 0.022(3) C56 0.016(3) 0.279(13) 0.091(6) 0.115(8) 0.004(3) 0.022(5) C57 0.050(3) 0.023(2) 0.020(2) -0.0013(18) 0.019(2) 0.011(2) C58A 0.016(6) 0.023(5) 0.020(4) -0.001(4) 0.007(4) 0.005(5) C58B 0.012(5) 0.012(4) 0.012(4) -0.0003(10) 0.0036(16) 0.0000(10) C59A 0.038(13) 0.030(11) 0.022(7) 0.001(6) 0.015(7) 0.013(10) C59B 0.024(14) 0.034(19) 0.020(13) 0.007(10) -0.009(11) -0.002(11) C60A 0.037(6) 0.035(8) 0.040(5) 0.002(5) 0.009(4) 0.009(6) C60B 0.024(5) 0.024(5) 0.024(5) -0.0001(10) 0.0072(17) 0.0000(10) C61A 0.045(10) 0.055(12) 0.041(8) 0.002(8) 0.001(7) 0.025(8) C61B 0.028(12) 0.040(15) 0.033(10) -0.006(11) -0.001(9) 0.016(10) C62A 0.029(10) 0.062(10) 0.030(6) 0.013(6) 0.004(7) 0.032(8) C62B 0.009(11) 0.082(18) 0.029(10) 0.018(9) -0.004(9) -0.005(11) C63A 0.032(11) 0.023(7) 0.022(5) 0.005(5) 0.009(7) 0.012(6) C63B 0.018(12) 0.031(14) 0.028(10) 0.008(9) 0.010(9) -0.002(8) C64A 0.048(12) 0.051(9) 0.035(8) 0.021(7) 0.021(9) 0.039(9) C64B 0.037(18) 0.076(17) 0.024(11) 0.033(10) 0.012(13) 0.025(15) C65 0.025(2) 0.022(2) 0.0147(19) 0.0014(17) -0.0038(17) 0.0007(18) C66A 0.016(4) 0.022(5) 0.021(5) -0.003(4) 0.007(4) 0.003(3) C66B 0.023(3) 0.023(4) 0.023(4) 0.0001(10) 0.0068(14) 0.0001(10) C67A 0.040(6) 0.031(6) 0.030(8) -0.001(7) 0.023(7) -0.004(4) C67B 0.023(5) 0.026(6) 0.025(8) -0.004(7) 0.014(6) -0.009(4) C68A 0.040(6) 0.041(6) 0.045(6) -0.026(5) 0.016(5) -0.011(4) C68B 0.039(7) 0.041(7) 0.038(7) 0.018(5) 0.008(5) 0.000(5) C69A 0.068(10) 0.021(7) 0.072(11) -0.013(6) 0.043(9) -0.009(6) C69B 0.041(8) 0.013(7) 0.056(11) 0.002(6) 0.021(8) -0.002(6) C70A 0.060(9) 0.027(8) 0.055(11) 0.015(7) 0.033(9) -0.003(6) C70B 0.047(8) 0.019(8) 0.050(12) -0.005(8) 0.019(9) -0.009(7) C71A 0.035(5) 0.014(4) 0.033(6) 0.000(4) 0.016(4) -0.003(3) C71B 0.032(6) 0.026(6) 0.036(7) -0.002(6) 0.019(5) -0.005(5) C72A 0.059(7) 0.031(6) 0.030(7) 0.008(6) 0.027(7) 0.005(5) C72B 0.068(11) 0.035(8) 0.051(12) 0.007(10) 0.044(12) -0.006(7) C73 0.060(4) 0.028(2) 0.026(3) 0.005(2) 0.018(2) -0.005(2) C74 0.085(5) 0.047(4) 0.072(5) -0.015(3) 0.006(4) 0.019(4) C75 0.058(4) 0.069(5) 0.095(6) 0.014(4) -0.018(4) -0.042(4) C76A 0.040(4) 0.029(4) 0.022(4) -0.003(3) 0.007(3) -0.004(3) C76B 0.051(10) 0.020(7) 0.016(7) -0.004(5) 0.007(6) -0.011(6) C77A 0.058(5) 0.025(4) 0.037(4) -0.006(3) 0.011(4) -0.015(4) C77B 0.061(13) 0.033(10) 0.040(10) -0.015(8) 0.005(9) -0.027(9) C78A 0.059(6) 0.033(4) 0.036(4) -0.001(3) 0.015(4) -0.002(4) C78B 0.100(16) 0.012(7) 0.042(10) 0.000(7) 0.026(10) -0.004(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O19 2.472(3) . ? La1 O18 2.473(3) 4_576 ? La1 O7 2.489(3) . ? La1 O16 2.532(3) 4_576 ? La1 O1 2.554(3) . ? La1 O5 2.566(3) . ? La1 O3 2.567(3) . ? La1 O4 2.636(3) . ? La1 O2 2.693(3) . ? La1 C9 2.965(4) . ? La1 C1 2.978(5) . ? La1 La2 4.0584(3) . ? O1 C1 1.244(6) . ? N1 C73 1.307(6) . ? N1 C74 1.434(8) . ? N1 C75 1.458(7) . ? C1 O2 1.283(5) . ? C1 C2 1.502(7) . ? La2 O11 2.510(3) . ? La2 O4 2.517(3) . ? La2 O9B 2.558(3) . ? La2 O13 2.564(3) . ? La2 O6 2.572(3) . ? La2 O8 2.577(3) . ? La2 O10 2.662(3) . ? La2 O5 2.663(3) . ? La2 O14 2.683(3) . ? La2 O7 2.730(3) . ? La2 C33A 2.951(4) . ? La2 C49 2.976(4) . ? O2 La3 2.503(3) 4_576 ? N2 C77B 1.165(19) . ? N2 C78A 1.335(9) . ? N2 C76A 1.369(8) . ? N2 C76B 1.448(14) . ? N2 C77A 1.524(8) . ? N2 C78B 1.635(17) . ? C2 C3 1.388(7) . ? C2 C7 1.402(7) . ? La3 O17 2.440(3) . ? La3 O20 2.498(3) . ? La3 O14 2.500(3) . ? La3 O2 2.503(3) 4_575 ? La3 O10 2.508(3) . ? La3 O15 2.524(3) . ? La3 O12 2.543(3) . ? La3 O11 2.683(3) . ? La3 O16 2.719(3) . ? La3 C57 2.958(5) . ? La3 C41 2.976(4) . ? O3 C9 1.256(5) . ? C3 C4 1.386(8) . ? C3 H3 0.9500 . ? O4 C9 1.272(5) . ? C4 C5 1.360(9) . ? C4 H4 0.9500 . ? O5 C17 1.274(5) . ? C5 C6 1.378(11) . ? C5 H5 0.9500 . ? O6 C17 1.242(5) . ? C6 C7 1.408(10) . ? C6 H6 0.9500 . ? O7 C25 1.272(5) . ? C7 C8 1.514(9) . ? O8 C25 1.247(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.493(7) . ? O9B C33A 1.229(5) . ? O10 C33A 1.291(5) . ? C10 C11 1.392(7) . ? C10 C15 1.406(7) . ? O11 C41 1.274(5) . ? C11 C12 1.393(7) . ? C11 H11 0.9500 . ? O12 C41 1.254(5) . ? C12 C13 1.383(10) . ? C12 H12 0.9500 . ? O13 C49 1.242(5) . ? C13 C14 1.356(11) . ? C13 H13 0.9500 . ? O14 C49 1.287(5) . ? C14 C15 1.408(9) . ? C14 H14 0.9500 . ? O15 C57 1.253(5) . ? C15 C16 1.503(9) . ? O16 C57 1.291(5) . ? O16 La1 2.532(3) 4_575 ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O17 C65 1.257(5) . ? C17 C18 1.499(6) . ? O18 C65 1.258(5) . ? O18 La1 2.473(3) 4_575 ? C18 C23 1.384(8) . ? C18 C19 1.418(8) . ? O19 C73 1.245(6) . ? C19 C20 1.408(8) . ? C19 H19 0.9500 . ? O20 C76A 1.284(7) . ? O20 C76B 1.369(15) . ? C20 C21 1.375(12) . ? C20 H20 0.9500 . ? C21 C22 1.375(12) . ? C21 H21 0.9500 . ? C22 C23 1.404(9) . ? C22 H22 0.9500 . ? C23 C24 1.436(10) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.497(6) . ? C26 C31 1.391(7) . ? C26 C27 1.401(6) . ? C27 C28 1.375(7) . ? C27 H27 0.9500 . ? C28 C29 1.390(10) . ? C28 H28 0.9500 . ? C29 C30 1.359(10) . ? C29 H29 0.9500 . ? C30 C31 1.401(8) . ? C30 H30 0.9500 . ? C31 C32 1.520(9) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33A C34B 1.479(13) . ? C33A C34A 1.558(15) . ? C34A C39A 1.364(17) . ? C34A C35A 1.40(3) . ? C34B C39B 1.403(16) . ? C34B C35B 1.40(3) . ? C35A C36A 1.44(4) . ? C35A H35A 0.9500 . ? C35B C36B 1.33(4) . ? C35B H35B 0.9500 . ? C36A C37A 1.41(2) . ? C36A H36A 0.9500 . ? C36B C37B 1.41(2) . ? C36B H36B 0.9500 . ? C37A C38A 1.29(6) . ? C37A H37A 0.9500 . ? C37B C38B 1.42(6) . ? C37B H37B 0.9500 . ? C38A C39A 1.51(5) . ? C38A H38A 0.9500 . ? C38B C39B 1.33(5) . ? C38B H38B 0.9500 . ? C39A C40A 1.502(17) . ? C39B C40B 1.494(16) . ? C40A H40D 0.9800 . ? C40A H40E 0.9800 . ? C40A H40F 0.9800 . ? C40B H40A 0.9800 . ? C40B H40B 0.9800 . ? C40B H40C 0.9800 . ? C41 C42 1.501(6) . ? C42 C47 1.393(8) . ? C42 C43 1.405(8) . ? C43 C44 1.380(8) . ? C43 H43 0.9500 . ? C44 C45 1.382(12) . ? C44 H44 0.9500 . ? C45 C46 1.374(12) . ? C45 H45 0.9500 . ? C46 C47 1.409(9) . ? C46 H46 0.9500 . ? C47 C48 1.488(9) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.501(6) . ? C50 C51 1.385(6) . ? C50 C55 1.404(7) . ? C51 C52 1.386(6) . ? C51 H51 0.9500 . ? C52 C53 1.371(8) . ? C52 H52 0.9500 . ? C53 C54 1.371(9) . ? C53 H53 0.9500 . ? C54 C55 1.398(8) . ? C54 H54 0.9500 . ? C55 C56 1.524(8) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58B 1.30(2) . ? C57 C58A 1.60(2) . ? C58A C59A 1.37(4) . ? C58A C63A 1.41(2) . ? C58B C63B 1.43(4) . ? C58B C59B 1.43(6) . ? C59A C60A 1.38(3) . ? C59A H59A 0.9500 . ? C59B C60B 1.39(6) . ? C59B H59B 0.9500 . ? C60A C61A 1.41(2) . ? C60A H60A 0.9500 . ? C60B C61B 1.35(4) . ? C60B H60B 0.9500 . ? C61A C62A 1.34(3) . ? C61A H61A 0.9500 . ? C61B C62B 1.44(4) . ? C61B H61B 0.9500 . ? C62A C63A 1.419(17) . ? C62A H62A 0.9500 . ? C62B C63B 1.35(3) . ? C62B H62B 0.9500 . ? C63A C64A 1.53(3) . ? C63B C64B 1.49(4) . ? C64A H64D 0.9800 . ? C64A H64E 0.9800 . ? C64A H64F 0.9800 . ? C64B H64A 0.9800 . ? C64B H64B 0.9800 . ? C64B H64C 0.9800 . ? C65 C66A 1.515(10) . ? C65 C66B 1.518(14) . ? C66A C71A 1.398(13) . ? C66A C67A 1.427(15) . ? C66B C71B 1.398(16) . ? C66B C67B 1.403(18) . ? C67A C68A 1.364(18) . ? C67A H67A 0.9500 . ? C67B C68B 1.379(18) . ? C67B H67B 0.9500 . ? C68A C69A 1.374(19) . ? C68A H68A 0.9500 . ? C68B C69B 1.35(2) . ? C68B H68B 0.9500 . ? C69A C70A 1.37(2) . ? C69A H69A 0.9500 . ? C69B C70B 1.36(2) . ? C69B H69B 0.9500 . ? C70A C71A 1.388(18) . ? C70A H70A 0.9500 . ? C70B C71B 1.42(2) . ? C70B H70B 0.9500 . ? C71A C72A 1.519(13) . ? C71B C72B 1.494(17) . ? C72A H72A 0.9800 . ? C72A H72B 0.9800 . ? C72A H72C 0.9800 . ? C72B H72D 0.9800 . ? C72B H72E 0.9800 . ? C72B H72F 0.9800 . ? C73 H73 0.9500 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76A H76A 0.9500 . ? C76B H76B 0.9500 . ? C77A H77A 0.9800 . ? C77A H77B 0.9800 . ? C77A H77C 0.9800 . ? C77B H77D 0.9800 . ? C77B H77E 0.9800 . ? C77B H77F 0.9800 . ? C78A H78A 0.9800 . ? C78A H78B 0.9800 . ? C78A H78C 0.9800 . ? C78B H78D 0.9800 . ? C78B H78E 0.9800 . ? C78B H78F 0.9800 . ? 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 O19 La1 O18 140.27(11) . 4_576 ? O19 La1 O7 143.59(10) . . ? O18 La1 O7 75.86(10) 4_576 . ? O19 La1 O16 70.63(10) . 4_576 ? O18 La1 O16 74.36(9) 4_576 4_576 ? O7 La1 O16 142.37(9) . 4_576 ? O19 La1 O1 78.64(13) . . ? O18 La1 O1 126.77(11) 4_576 . ? O7 La1 O1 79.28(12) . . ? O16 La1 O1 100.90(11) 4_576 . ? O19 La1 O5 78.25(10) . . ? O18 La1 O5 133.64(9) 4_576 . ? O7 La1 O5 68.04(9) . . ? O16 La1 O5 148.83(9) 4_576 . ? O1 La1 O5 74.20(10) . . ? O19 La1 O3 76.14(13) . . ? O18 La1 O3 81.25(11) 4_576 . ? O7 La1 O3 115.05(10) . . ? O16 La1 O3 82.44(10) 4_576 . ? O1 La1 O3 151.81(12) . . ? O5 La1 O3 88.44(10) . . ? O19 La1 O4 113.55(11) . . ? O18 La1 O4 72.61(9) 4_576 . ? O7 La1 O4 65.40(9) . . ? O16 La1 O4 124.73(9) 4_576 . ? O1 La1 O4 134.36(10) . . ? O5 La1 O4 66.50(9) . . ? O3 La1 O4 49.80(9) . . ? O19 La1 O2 104.55(11) . . ? O18 La1 O2 80.93(9) 4_576 . ? O7 La1 O2 81.78(9) . . ? O16 La1 O2 71.30(9) 4_576 . ? O1 La1 O2 49.21(9) . . ? O5 La1 O2 119.95(9) . . ? O3 La1 O2 151.40(9) . . ? O4 La1 O2 141.69(9) . . ? O19 La1 C9 97.30(13) . . ? O18 La1 C9 71.98(11) 4_576 . ? O7 La1 C9 90.17(11) . . ? O16 La1 C9 101.84(11) 4_576 . ? O1 La1 C9 154.03(11) . . ? O5 La1 C9 79.86(10) . . ? O3 La1 C9 24.94(10) . . ? O4 La1 C9 25.39(10) . . ? O2 La1 C9 152.87(10) . . ? O19 La1 C1 95.25(13) . . ? O18 La1 C1 102.89(11) 4_576 . ? O7 La1 C1 75.02(11) . . ? O16 La1 C1 89.77(11) 4_576 . ? O1 La1 C1 24.48(11) . . ? O5 La1 C1 95.04(11) . . ? O3 La1 C1 169.90(11) . . ? O4 La1 C1 140.13(10) . . ? O2 La1 C1 25.51(10) . . ? C9 La1 C1 165.16(12) . . ? O19 La1 La2 114.62(8) . . ? O18 La1 La2 93.71(7) 4_576 . ? O7 La1 La2 41.16(6) . . ? O16 La1 La2 161.68(7) 4_576 . ? O1 La1 La2 97.38(8) . . ? O5 La1 La2 39.96(6) . . ? O3 La1 La2 82.01(7) . . ? O4 La1 La2 37.02(6) . . ? O2 La1 La2 121.32(6) . . ? C9 La1 La2 60.66(8) . . ? C1 La1 La2 106.68(8) . . ? C1 O1 La1 97.2(3) . . ? C73 N1 C74 120.5(5) . . ? C73 N1 C75 121.9(6) . . ? C74 N1 C75 117.4(5) . . ? O1 C1 O2 120.0(5) . . ? O1 C1 C2 119.8(4) . . ? O2 C1 C2 120.2(4) . . ? O1 C1 La1 58.3(2) . . ? O2 C1 La1 64.7(2) . . ? C2 C1 La1 160.7(3) . . ? O11 La2 O4 167.99(9) . . ? O11 La2 O9B 115.89(10) . . ? O4 La2 O9B 75.71(10) . . ? O11 La2 O13 112.14(9) . . ? O4 La2 O13 70.46(9) . . ? O9B La2 O13 85.12(12) . . ? O11 La2 O6 78.02(10) . . ? O4 La2 O6 92.25(10) . . ? O9B La2 O6 156.05(12) . . ? O13 La2 O6 71.25(11) . . ? O11 La2 O8 69.49(9) . . ? O4 La2 O8 110.92(9) . . ? O9B La2 O8 82.29(12) . . ? O13 La2 O8 166.45(11) . . ? O6 La2 O8 121.59(11) . . ? O11 La2 O10 66.27(9) . . ? O4 La2 O10 125.55(9) . . ? O9B La2 O10 49.97(9) . . ? O13 La2 O10 98.16(10) . . ? O6 La2 O10 135.68(9) . . ? O8 La2 O10 69.81(10) . . ? O11 La2 O5 101.32(9) . . ? O4 La2 O5 66.77(9) . . ? O9B La2 O5 136.52(9) . . ? O13 La2 O5 101.60(10) . . ? O6 La2 O5 49.35(9) . . ? O8 La2 O5 91.02(10) . . ? O10 La2 O5 159.65(9) . . ? O11 La2 O14 64.76(9) . . ? O4 La2 O14 119.60(9) . . ? O9B La2 O14 93.83(10) . . ? O13 La2 O14 49.26(9) . . ? O6 La2 O14 73.94(9) . . ? O8 La2 O14 126.60(9) . . ? O10 La2 O14 67.67(9) . . ? O5 La2 O14 123.20(9) . . ? O11 La2 O7 113.41(9) . . ? O4 La2 O7 63.61(9) . . ? O9B La2 O7 81.10(10) . . ? O13 La2 O7 133.97(9) . . ? O6 La2 O7 112.38(9) . . ? O8 La2 O7 48.54(9) . . ? O10 La2 O7 105.58(9) . . ? O5 La2 O7 63.27(9) . . ? O14 La2 O7 173.25(9) . . ? O11 La2 C33A 91.41(11) . . ? O4 La2 C33A 100.12(11) . . ? O9B La2 C33A 24.48(11) . . ? O13 La2 C33A 94.93(12) . . ? O6 La2 C33A 157.28(11) . . ? O8 La2 C33A 71.52(12) . . ? O10 La2 C33A 25.94(10) . . ? O5 La2 C33A 153.37(11) . . ? O14 La2 C33A 83.37(11) . . ? O7 La2 C33A 90.24(11) . . ? O11 La2 C49 87.75(10) . . ? O4 La2 C49 94.76(10) . . ? O9B La2 C49 93.97(12) . . ? O13 La2 C49 24.49(10) . . ? O6 La2 C49 66.04(11) . . ? O8 La2 C49 152.02(11) . . ? O10 La2 C49 86.51(10) . . ? O5 La2 C49 109.84(10) . . ? O14 La2 C49 25.62(10) . . ? O7 La2 C49 158.38(10) . . ? C33A La2 C49 93.79(12) . . ? C1 O2 La3 145.0(3) . 4_576 ? C1 O2 La1 89.8(3) . . ? La3 O2 La1 107.84(10) 4_576 . ? C77B N2 C78A 165.5(10) . . ? C77B N2 C76A 68.2(9) . . ? C78A N2 C76A 126.1(6) . . ? C77B N2 C76B 132.3(11) . . ? C78A N2 C76B 61.4(7) . . ? C76A N2 C76B 65.5(7) . . ? C77B N2 C77A 46.3(9) . . ? C78A N2 C77A 120.0(5) . . ? C76A N2 C77A 113.0(6) . . ? C76B N2 C77A 178.5(8) . . ? C77B N2 C78B 123.2(11) . . ? C78A N2 C78B 42.4(7) . . ? C76A N2 C78B 168.3(9) . . ? C76B N2 C78B 102.8(10) . . ? C77A N2 C78B 78.7(8) . . ? C3 C2 C7 120.1(5) . . ? C3 C2 C1 117.9(4) . . ? C7 C2 C1 122.0(5) . . ? O17 La3 O20 141.24(11) . . ? O17 La3 O14 78.88(10) . . ? O20 La3 O14 139.60(10) . . ? O17 La3 O2 73.57(9) . 4_575 ? O20 La3 O2 70.81(10) . 4_575 ? O14 La3 O2 139.78(9) . 4_575 ? O17 La3 O10 136.46(9) . . ? O20 La3 O10 75.13(10) . . ? O14 La3 O10 72.91(9) . . ? O2 La3 O10 145.50(9) 4_575 . ? O17 La3 O15 126.05(11) . . ? O20 La3 O15 74.01(12) . . ? O14 La3 O15 75.69(11) . . ? O2 La3 O15 97.54(10) 4_575 . ? O10 La3 O15 77.97(10) . . ? O17 La3 O12 80.34(10) . . ? O20 La3 O12 84.32(11) . . ? O14 La3 O12 114.62(9) . . ? O2 La3 O12 89.15(9) 4_575 . ? O10 La3 O12 82.09(10) . . ? O15 La3 O12 153.60(10) . . ? O17 La3 O11 72.29(9) . . ? O20 La3 O11 121.66(10) . . ? O14 La3 O11 64.88(9) . . ? O2 La3 O11 129.83(9) 4_575 . ? O10 La3 O11 65.96(9) . . ? O15 La3 O11 132.33(10) . . ? O12 La3 O11 49.77(9) . . ? O17 La3 O16 78.48(9) . . ? O20 La3 O16 103.63(11) . . ? O14 La3 O16 74.96(9) . . ? O2 La3 O16 71.28(9) 4_575 . ? O10 La3 O16 123.30(9) . . ? O15 La3 O16 49.30(9) . . ? O12 La3 O16 154.46(9) . . ? O11 La3 O16 133.73(9) . . ? O17 La3 C57 101.23(12) . . ? O20 La3 C57 93.24(13) . . ? O14 La3 C57 67.74(11) . . ? O2 La3 C57 89.40(11) 4_575 . ? O10 La3 C57 97.96(11) . . ? O15 La3 C57 24.85(11) . . ? O12 La3 C57 177.47(11) . . ? O11 La3 C57 132.55(11) . . ? O16 La3 C57 25.84(10) . . ? O17 La3 C41 72.23(10) . . ? O20 La3 C41 105.12(12) . . ? O14 La3 C41 89.99(11) . . ? O2 La3 C41 108.33(10) 4_575 . ? O10 La3 C41 75.25(10) . . ? O15 La3 C41 152.38(11) . . ? O12 La3 C41 24.71(10) . . ? O11 La3 C41 25.35(10) . . ? O16 La3 C41 149.19(10) . . ? C57 La3 C41 157.71(12) . . ? O17 La3 La2 97.01(7) . . ? O20 La3 La2 115.73(7) . . ? O14 La3 La2 41.39(6) . . ? O2 La3 La2 167.90(6) 4_575 . ? O10 La3 La2 40.94(6) . . ? O15 La3 La2 94.16(8) . . ? O12 La3 La2 81.66(7) . . ? O11 La3 La2 38.25(6) . . ? O16 La3 La2 114.93(6) . . ? C57 La3 La2 100.06(9) . . ? C41 La3 La2 60.76(8) . . ? C9 O3 La1 95.6(3) . . ? C4 C3 C2 121.2(5) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C9 O4 La2 149.5(3) . . ? C9 O4 La1 91.9(2) . . ? La2 O4 La1 103.89(10) . . ? C5 C4 C3 119.9(7) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C17 O5 La1 141.1(3) . . ? C17 O5 La2 91.6(2) . . ? La1 O5 La2 101.80(9) . . ? C4 C5 C6 119.3(7) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C17 O6 La2 96.7(3) . . ? C5 C6 C7 123.0(6) . . ? C5 C6 H6 118.5 . . ? C7 C6 H6 118.5 . . ? C25 O7 La1 155.2(3) . . ? C25 O7 La2 91.3(2) . . ? La1 O7 La2 101.97(10) . . ? C2 C7 C6 116.4(6) . . ? C2 C7 C8 124.0(6) . . ? C6 C7 C8 119.6(6) . . ? C25 O8 La2 99.3(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C9 O4 120.2(4) . . ? O3 C9 C10 121.8(4) . . ? O4 C9 C10 117.9(4) . . ? O3 C9 La1 59.5(2) . . ? O4 C9 La1 62.7(2) . . ? C10 C9 La1 163.7(3) . . ? C33A O9B La2 95.9(3) . . ? C33A O10 La3 153.1(3) . . ? C33A O10 La2 89.6(2) . . ? La3 O10 La2 100.93(9) . . ? C11 C10 C15 119.9(5) . . ? C11 C10 C9 117.7(4) . . ? C15 C10 C9 122.4(5) . . ? C41 O11 La2 145.1(2) . . ? C41 O11 La3 90.3(2) . . ? La2 O11 La3 100.30(9) . . ? C10 C11 C12 120.9(6) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C41 O12 La3 97.3(2) . . ? C13 C12 C11 119.4(7) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C49 O13 La2 96.6(2) . . ? C14 C13 C12 119.8(6) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C49 O14 La3 162.5(3) . . ? C49 O14 La2 90.0(2) . . ? La3 O14 La2 100.58(9) . . ? C13 C14 C15 122.8(6) . . ? C13 C14 H14 118.6 . . ? C15 C14 H14 118.6 . . ? C57 O15 La3 97.4(3) . . ? C10 C15 C14 117.1(6) . . ? C10 C15 C16 123.4(5) . . ? C14 C15 C16 119.4(6) . . ? C57 O16 La1 144.8(3) . 4_575 ? C57 O16 La3 87.5(2) . . ? La1 O16 La3 106.18(10) 4_575 . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C65 O17 La3 142.0(3) . . ? O6 C17 O5 120.7(4) . . ? O6 C17 C18 120.0(4) . . ? O5 C17 C18 119.2(4) . . ? O6 C17 La2 58.9(2) . . ? O5 C17 La2 63.1(2) . . ? C18 C17 La2 170.2(4) . . ? C65 O18 La1 136.5(3) . 4_575 ? C23 C18 C19 122.1(5) . . ? C23 C18 C17 120.2(5) . . ? C19 C18 C17 117.7(5) . . ? C73 O19 La1 142.8(4) . . ? C20 C19 C18 117.4(7) . . ? C20 C19 H19 121.3 . . ? C18 C19 H19 121.3 . . ? C76A O20 C76B 70.1(7) . . ? C76A O20 La3 169.3(4) . . ? C76B O20 La3 120.1(7) . . ? C21 C20 C19 120.9(8) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C22 C21 C20 120.4(7) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 121.4(8) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C18 C23 C22 117.8(7) . . ? C18 C23 C24 122.6(5) . . ? C22 C23 C24 119.5(7) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O8 C25 O7 120.4(4) . . ? O8 C25 C26 121.1(4) . . ? O7 C25 C26 118.4(4) . . ? O8 C25 La2 56.8(2) . . ? O7 C25 La2 63.9(2) . . ? C26 C25 La2 173.4(3) . . ? C31 C26 C27 120.3(4) . . ? C31 C26 C25 122.9(4) . . ? C27 C26 C25 116.8(4) . . ? C28 C27 C26 120.9(5) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 118.9(5) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C30 C29 C28 120.1(6) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C31 122.5(7) . . ? C29 C30 H30 118.7 . . ? C31 C30 H30 118.7 . . ? C26 C31 C30 117.1(6) . . ? C26 C31 C32 123.6(5) . . ? C30 C31 C32 119.3(6) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O9B C33A O10 122.3(4) . . ? O9B C33A C34B 116.4(6) . . ? O10 C33A C34B 120.8(6) . . ? O9B C33A C34A 122.5(6) . . ? O10 C33A C34A 114.5(6) . . ? C34B C33A C34A 16.6(6) . . ? O9B C33A La2 59.6(2) . . ? O10 C33A La2 64.4(2) . . ? C34B C33A La2 172.0(5) . . ? C34A C33A La2 158.0(5) . . ? C39A C34A C35A 124.3(19) . . ? C39A C34A C33A 127.8(11) . . ? C35A C34A C33A 107.9(17) . . ? C39B C34B C35B 116.9(17) . . ? C39B C34B C33A 118.4(11) . . ? C35B C34B C33A 124.6(17) . . ? C34A C35A C36A 119(2) . . ? C34A C35A H35A 120.7 . . ? C36A C35A H35A 120.7 . . ? C36B C35B C34B 124(2) . . ? C36B C35B H35B 117.9 . . ? C34B C35B H35B 117.9 . . ? C37A C36A C35A 117.1(17) . . ? C37A C36A H36A 121.5 . . ? C35A C36A H36A 121.5 . . ? C35B C36B C37B 118.1(17) . . ? C35B C36B H36B 121.0 . . ? C37B C36B H36B 121.0 . . ? C38A C37A C36A 123.7(18) . . ? C38A C37A H37A 118.2 . . ? C36A C37A H37A 118.2 . . ? C36B C37B C38B 119(2) . . ? C36B C37B H37B 120.6 . . ? C38B C37B H37B 120.5 . . ? C37A C38A C39A 122(2) . . ? C37A C38A H38A 119.1 . . ? C39A C38A H38A 119.1 . . ? C39B C38B C37B 121(2) . . ? C39B C38B H38B 119.6 . . ? C37B C38B H38B 119.6 . . ? C34A C39A C40A 122.8(11) . . ? C34A C39A C38A 114.4(18) . . ? C40A C39A C38A 122.8(17) . . ? C38B C39B C34B 121.0(19) . . ? C38B C39B C40B 115.3(19) . . ? C34B C39B C40B 123.6(11) . . ? C39B C40B H40A 109.5 . . ? C39B C40B H40B 109.5 . . ? H40A C40B H40B 109.5 . . ? C39B C40B H40C 109.5 . . ? H40A C40B H40C 109.5 . . ? H40B C40B H40C 109.5 . . ? O12 C41 O11 121.2(4) . . ? O12 C41 C42 121.1(4) . . ? O11 C41 C42 117.6(4) . . ? O12 C41 La3 58.0(2) . . ? O11 C41 La3 64.4(2) . . ? C42 C41 La3 165.3(3) . . ? C47 C42 C43 120.5(5) . . ? C47 C42 C41 122.4(5) . . ? C43 C42 C41 117.0(5) . . ? C44 C43 C42 120.7(7) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C43 C44 C45 118.9(8) . . ? C43 C44 H44 120.5 . . ? C45 C44 H44 120.5 . . ? C46 C45 C44 121.1(7) . . ? C46 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? C45 C46 C47 121.1(7) . . ? C45 C46 H46 119.4 . . ? C47 C46 H46 119.4 . . ? C42 C47 C46 117.6(7) . . ? C42 C47 C48 123.7(5) . . ? C46 C47 C48 118.8(6) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O13 C49 O14 120.0(4) . . ? O13 C49 C50 121.7(4) . . ? O14 C49 C50 118.3(4) . . ? O13 C49 La2 58.9(2) . . ? O14 C49 La2 64.4(2) . . ? C50 C49 La2 160.8(3) . . ? C51 C50 C55 119.9(4) . . ? C51 C50 C49 117.9(4) . . ? C55 C50 C49 122.2(4) . . ? C50 C51 C52 121.6(5) . . ? C50 C51 H51 119.2 . . ? C52 C51 H51 119.2 . . ? C53 C52 C51 118.7(5) . . ? C53 C52 H52 120.7 . . ? C51 C52 H52 120.7 . . ? C52 C53 C54 120.5(5) . . ? C52 C53 H53 119.8 . . ? C54 C53 H53 119.8 . . ? C53 C54 C55 122.2(6) . . ? C53 C54 H54 118.9 . . ? C55 C54 H54 118.9 . . ? C54 C55 C50 117.1(5) . . ? C54 C55 C56 119.1(5) . . ? C50 C55 C56 123.8(5) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O15 C57 O16 119.2(4) . . ? O15 C57 C58B 113.9(11) . . ? O16 C57 C58B 126.9(11) . . ? O15 C57 C58A 124.2(7) . . ? O16 C57 C58A 116.3(7) . . ? C58B C57 C58A 12.4(9) . . ? O15 C57 La3 57.8(2) . . ? O16 C57 La3 66.7(2) . . ? C58B C57 La3 155.4(9) . . ? C58A C57 La3 151.4(5) . . ? C59A C58A C63A 122.0(17) . . ? C59A C58A C57 119.2(15) . . ? C63A C58A C57 118.8(10) . . ? C57 C58B C63B 126.6(19) . . ? C57 C58B C59B 116(3) . . ? C63B C58B C59B 117(3) . . ? C58A C59A C60A 120(3) . . ? C58A C59A H59A 119.8 . . ? C60A C59A H59A 119.9 . . ? C60B C59B C58B 124(4) . . ? C60B C59B H59B 118.0 . . ? C58B C59B H59B 118.1 . . ? C59A C60A C61A 118.5(19) . . ? C59A C60A H60A 120.7 . . ? C61A C60A H60A 120.7 . . ? C61B C60B C59B 119(3) . . ? C61B C60B H60B 120.5 . . ? C59B C60B H60B 120.5 . . ? C62A C61A C60A 121.5(16) . . ? C62A C61A H61A 119.3 . . ? C60A C61A H61A 119.3 . . ? C60B C61B C62B 116(2) . . ? C60B C61B H61B 121.9 . . ? C62B C61B H61B 121.9 . . ? C61A C62A C63A 120.8(15) . . ? C61A C62A H62A 119.6 . . ? C63A C62A H62A 119.6 . . ? C63B C62B C61B 128(3) . . ? C63B C62B H62B 116.2 . . ? C61B C62B H62B 116.2 . . ? C58A C63A C62A 116.8(13) . . ? C58A C63A C64A 125.9(14) . . ? C62A C63A C64A 117.3(15) . . ? C62B C63B C58B 115(2) . . ? C62B C63B C64B 122(3) . . ? C58B C63B C64B 122(3) . . ? C63B C64B H64A 109.5 . . ? C63B C64B H64B 109.5 . . ? H64A C64B H64B 109.5 . . ? C63B C64B H64C 109.5 . . ? H64A C64B H64C 109.5 . . ? H64B C64B H64C 109.5 . . ? O17 C65 O18 124.6(4) . . ? O17 C65 C66A 110.0(5) . . ? O18 C65 C66A 125.2(5) . . ? O17 C65 C66B 126.8(6) . . ? O18 C65 C66B 108.2(6) . . ? C66A C65 C66B 21.1(4) . . ? C71A C66A C67A 119.0(10) . . ? C71A C66A C65 121.6(9) . . ? C67A C66A C65 119.4(9) . . ? C71B C66B C67B 120.0(12) . . ? C71B C66B C65 119.7(10) . . ? C67B C66B C65 120.2(11) . . ? C68A C67A C66A 121.6(12) . . ? C68A C67A H67A 119.2 . . ? C66A C67A H67A 119.2 . . ? C68B C67B C66B 121.2(13) . . ? C68B C67B H67B 119.4 . . ? C66B C67B H67B 119.4 . . ? C67A C68A C69A 118.9(11) . . ? C67A C68A H68A 120.6 . . ? C69A C68A H68A 120.6 . . ? C69B C68B C67B 118.7(12) . . ? C69B C68B H68B 120.7 . . ? C67B C68B H68B 120.7 . . ? C70A C69A C68A 120.4(13) . . ? C70A C69A H69A 119.8 . . ? C68A C69A H69A 119.8 . . ? C68B C69B C70B 121.6(15) . . ? C68B C69B H69B 119.2 . . ? C70B C69B H69B 119.2 . . ? C69A C70A C71A 122.7(14) . . ? C69A C70A H70A 118.6 . . ? C71A C70A H70A 118.6 . . ? C69B C70B C71B 122.2(16) . . ? C69B C70B H70B 118.9 . . ? C71B C70B H70B 118.9 . . ? C70A C71A C66A 117.3(11) . . ? C70A C71A C72A 121.0(11) . . ? C66A C71A C72A 121.7(9) . . ? C66B C71B C70B 116.1(14) . . ? C66B C71B C72B 123.8(12) . . ? C70B C71B C72B 120.0(15) . . ? C71A C72A H72A 109.5 . . ? C71A C72A H72B 109.5 . . ? H72A C72A H72B 109.5 . . ? C71A C72A H72C 109.5 . . ? H72A C72A H72C 109.5 . . ? H72B C72A H72C 109.5 . . ? O19 C73 N1 123.2(5) . . ? O19 C73 H73 118.4 . . ? N1 C73 H73 118.4 . . ? N1 C74 H74A 109.5 . . ? N1 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? N1 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? N1 C75 H75A 109.5 . . ? N1 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? N1 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? O20 C76A N2 117.3(6) . . ? O20 C76A H76A 121.3 . . ? N2 C76A H76A 121.3 . . ? O20 C76B N2 107.0(11) . . ? O20 C76B H76B 126.5 . . ? N2 C76B H76B 126.5 . . ? N2 C77A H77A 109.5 . . ? N2 C77A H77B 109.5 . . ? H77A C77A H77B 109.5 . . ? N2 C77A H77C 109.5 . . ? H77A C77A H77C 109.5 . . ? H77B C77A H77C 109.5 . . ? N2 C77B H77D 109.5 . . ? N2 C77B H77E 109.5 . . ? N2 C77B H77F 109.5 . . ? N2 C78A H78A 109.5 . . ? N2 C78A H78B 109.5 . . ? H78A C78A H78B 109.5 . . ? N2 C78A H78C 109.5 . . ? H78A C78A H78C 109.5 . . ? H78B C78A H78C 109.5 . . ? N2 C78B H78D 109.5 . . ? N2 C78B H78E 109.5 . . ? N2 C78B H78F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.428 _refine_diff_density_min -1.106 _refine_diff_density_rms 0.111 # Attachment '4.CIF' data_HB9DMSO _database_code_depnum_ccdc_archive 'CCDC 634373' _audit_creation_method SHELXL-97 _chemical_name_systematic ; poly[(aqua)(dimethylsulphoxide)tris(3-methylbenzoato)lanthanum(III)] water solvate ; _chemical_name_common ; poly((aqua)(dimethylsulphoxide)tris(3- methylbenzoato)lanthanum(iii)) water solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C26 H29 La1 O8 S1, H2 O1' _chemical_formula_sum 'C26 H31 La1 O9 S1' _chemical_formula_weight 658.48 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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6022(2) _cell_length_b 9.9801(2) _cell_length_c 16.1375(3) _cell_angle_alpha 106.171(1) _cell_angle_beta 94.743(1) _cell_angle_gamma 101.490(1) _cell_volume 1439.75(5) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 1.603 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6995 _exptl_absorpt_correction_T_max 0.8309 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 13733 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6554 _reflns_number_gt 5565 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^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_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6554 _refine_ls_number_parameters 345 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0774 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 2.505 _refine_ls_shift/su_max 0.011 _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 0.78499(4) 0.51119(4) 0.51150(3) 0.02746(16) Uani 1 1 d . . . S1 S 0.8358(2) 0.9067(2) 0.54729(18) 0.0557(6) Uani 1 1 d . . . O1 O 0.8253(5) 0.3963(6) 0.6323(4) 0.0443(13) Uani 1 1 d . . . C1 C 0.9557(7) 0.3910(7) 0.6350(5) 0.0324(15) Uani 1 1 d . . . O2 O 1.0300(5) 0.4240(5) 0.5799(3) 0.0349(11) Uani 1 1 d . . . C2 C 1.0206(8) 0.3415(8) 0.7048(5) 0.0367(17) Uani 1 1 d . . . O3 O 0.9580(5) 0.7049(5) 0.6333(4) 0.0440(13) Uani 1 1 d . . . C3 C 0.9534(9) 0.3393(9) 0.7771(6) 0.051(2) Uani 1 1 d . . . H3 H 0.8681 0.3736 0.7826 0.061 Uiso 1 1 calc R . . O4 O 1.1700(5) 0.7093(5) 0.5858(4) 0.0425(13) Uani 1 1 d . . . C4 C 1.0070(12) 0.2884(12) 0.8417(7) 0.069(3) Uani 1 1 d . . . O5 O 0.6179(5) 0.5982(6) 0.6103(3) 0.0416(12) Uani 1 1 d . . . C5 C 1.1311(12) 0.2378(12) 0.8309(8) 0.076(3) Uani 1 1 d . . . H5 H 1.1690 0.1996 0.8732 0.092 Uiso 1 1 calc R . . O6 O 0.3874(5) 0.5258(6) 0.6187(3) 0.0417(13) Uani 1 1 d . . . C6 C 1.1993(12) 0.2420(12) 0.7607(8) 0.075(3) Uani 1 1 d . . . H6 H 1.2845 0.2076 0.7548 0.090 Uiso 1 1 calc R . . O7 O 0.5684(6) 0.2909(6) 0.5000(5) 0.0478(15) Uani 1 1 d . . . C7 C 1.1464(9) 0.2952(10) 0.6989(6) 0.055(2) Uani 1 1 d . . . H7 H 1.1967 0.3003 0.6511 0.066 Uiso 1 1 calc R . . H7A H 0.552(12) 0.280(12) 0.555(8) 0.09(4) Uiso 1 1 d . . . H7B H 0.501(10) 0.297(10) 0.480(7) 0.06(3) Uiso 1 1 d . . . H9A H 0.5010 0.2574 0.7073 1.254 Uiso 1 1 d D . . H9B H 0.6671 0.2924 0.6995 1.465 Uiso 1 1 d D . . O8 O 0.7516(5) 0.7551(5) 0.5018(4) 0.0436(13) Uani 1 1 d . . . C8 C 0.9306(16) 0.286(2) 0.9198(9) 0.126(6) Uani 1 1 d . . . H8A H 0.9877 0.3586 0.9719 0.189 Uiso 1 1 calc R . . H8B H 0.9185 0.1910 0.9281 0.189 Uiso 1 1 calc R . . H8C H 0.8361 0.3067 0.9098 0.189 Uiso 1 1 calc R . . O9 O 0.57541(14) 0.2547(8) 0.67893(17) 0.119(3) Uani 1 1 d D . . C9 C 1.0938(8) 0.7403(7) 0.6442(5) 0.0357(17) Uani 1 1 d . . . C10 C 1.1695(8) 0.8254(8) 0.7345(5) 0.0400(18) Uani 1 1 d . . . C11 C 1.3167(9) 0.8817(8) 0.7471(6) 0.051(2) Uani 1 1 d . . . H11 H 1.3673 0.8690 0.6984 0.061 Uiso 1 1 calc R . . C12 C 1.3912(10) 0.9566(10) 0.8304(7) 0.065(3) Uani 1 1 d . . . C13 C 1.3170(13) 0.9738(11) 0.8992(7) 0.072(3) Uani 1 1 d . . . H13 H 1.3674 1.0243 0.9560 0.087 Uiso 1 1 calc R . . C14 C 1.1722(14) 0.9208(12) 0.8892(7) 0.077(3) Uani 1 1 d . . . H14 H 1.1228 0.9350 0.9384 0.092 Uiso 1 1 calc R . . C15 C 1.0970(10) 0.8455(10) 0.8057(6) 0.059(2) Uani 1 1 d . . . H15 H 0.9962 0.8082 0.7981 0.071 Uiso 1 1 calc R . . C16 C 1.5523(13) 1.0162(15) 0.8427(10) 0.112(5) Uani 1 1 d . . . H16A H 1.5858 1.0740 0.9036 0.169 Uiso 1 1 calc R . . H16B H 1.5743 1.0762 0.8045 0.169 Uiso 1 1 calc R . . H16C H 1.6007 0.9368 0.8279 0.169 Uiso 1 1 calc R . . C17 C 0.5165(7) 0.5731(7) 0.6526(5) 0.0314(15) Uani 1 1 d . . . C18 C 0.5517(8) 0.6034(8) 0.7494(5) 0.0380(17) Uani 1 1 d . . . C19 C 0.4432(9) 0.5987(8) 0.8003(5) 0.0443(19) Uani 1 1 d . . . H19 H 0.3461 0.5765 0.7735 0.053 Uiso 1 1 calc R . . C20 C 0.4731(12) 0.6256(10) 0.8899(6) 0.061(2) Uani 1 1 d . . . C21 C 0.6169(15) 0.6563(12) 0.9264(7) 0.083(3) Uani 1 1 d . . . H21 H 0.6403 0.6750 0.9875 0.099 Uiso 1 1 calc R . . C22 C 0.7252(13) 0.6602(14) 0.8763(7) 0.089(4) Uani 1 1 d . . . H22 H 0.8221 0.6804 0.9029 0.107 Uiso 1 1 calc R . . C23 C 0.6946(9) 0.6353(11) 0.7879(6) 0.063(3) Uani 1 1 d . . . H23 H 0.7700 0.6396 0.7534 0.075 Uiso 1 1 calc R . . C24 C 0.3549(15) 0.6232(13) 0.9452(8) 0.093(4) Uani 1 1 d . . . H24A H 0.3376 0.7197 0.9661 0.139 Uiso 1 1 calc R . . H24B H 0.3831 0.5918 0.9952 0.139 Uiso 1 1 calc R . . H24C H 0.2669 0.5566 0.9105 0.139 Uiso 1 1 calc R . . C25 C 0.7560(14) 1.0129(10) 0.4941(9) 0.090(4) Uani 1 1 d . . . H25A H 0.7825 0.9977 0.4354 0.135 Uiso 1 1 calc R . . H25B H 0.7903 1.1144 0.5277 0.135 Uiso 1 1 calc R . . H25C H 0.6513 0.9850 0.4899 0.135 Uiso 1 1 calc R . . C26 C 0.7735(14) 0.9572(11) 0.6489(8) 0.089(4) Uani 1 1 d . . . H26A H 0.8111 0.9080 0.6873 0.134 Uiso 1 1 calc R . . H26B H 0.6682 0.9305 0.6400 0.134 Uiso 1 1 calc R . . H26C H 0.8065 1.0612 0.6757 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 0.0234(2) 0.0325(2) 0.0271(2) 0.00883(16) 0.00338(15) 0.00822(16) S1 0.0449(11) 0.0386(11) 0.0833(19) 0.0196(11) 0.0119(11) 0.0065(9) O1 0.032(3) 0.061(3) 0.048(3) 0.028(3) 0.007(2) 0.014(2) C1 0.036(4) 0.032(4) 0.030(4) 0.011(3) 0.005(3) 0.008(3) O2 0.035(3) 0.039(3) 0.035(3) 0.017(2) 0.009(2) 0.011(2) C2 0.037(4) 0.038(4) 0.035(4) 0.017(3) -0.002(3) 0.002(3) O3 0.032(3) 0.043(3) 0.047(3) -0.001(3) -0.003(2) 0.010(2) C3 0.050(5) 0.065(5) 0.042(5) 0.027(4) 0.004(4) 0.007(4) O4 0.043(3) 0.036(3) 0.042(3) 0.001(2) 0.008(3) 0.010(2) C4 0.074(7) 0.087(7) 0.045(6) 0.039(5) -0.006(5) -0.006(6) O5 0.031(3) 0.060(3) 0.035(3) 0.013(3) 0.011(2) 0.014(2) C5 0.079(7) 0.083(7) 0.074(8) 0.055(6) -0.021(6) 0.005(6) O6 0.029(3) 0.058(3) 0.035(3) 0.017(3) -0.003(2) 0.003(2) C6 0.071(6) 0.086(7) 0.089(9) 0.052(7) 0.003(6) 0.033(6) O7 0.030(3) 0.051(3) 0.065(5) 0.023(3) 0.003(3) 0.008(3) C7 0.055(5) 0.063(6) 0.059(6) 0.033(5) 0.008(4) 0.022(4) O8 0.049(3) 0.036(3) 0.049(4) 0.013(3) 0.011(3) 0.016(2) C8 0.119(11) 0.208(17) 0.070(9) 0.086(11) 0.021(8) 0.017(11) O9 0.108(7) 0.112(7) 0.156(10) 0.074(7) 0.038(7) 0.017(6) C9 0.037(4) 0.028(3) 0.039(4) 0.006(3) -0.001(3) 0.008(3) C10 0.044(4) 0.033(4) 0.039(5) 0.006(3) -0.001(3) 0.011(3) C11 0.048(5) 0.045(4) 0.049(5) 0.001(4) -0.006(4) 0.010(4) C12 0.059(6) 0.056(5) 0.062(7) 0.002(5) -0.020(5) 0.006(4) C13 0.092(8) 0.063(6) 0.045(6) 0.002(5) -0.022(6) 0.012(6) C14 0.108(9) 0.082(7) 0.037(6) 0.011(5) 0.015(6) 0.023(7) C15 0.059(6) 0.061(5) 0.049(6) 0.008(5) 0.006(5) 0.007(4) C16 0.067(8) 0.122(11) 0.107(11) 0.000(9) -0.032(7) -0.004(7) C17 0.033(4) 0.030(3) 0.032(4) 0.007(3) 0.005(3) 0.012(3) C18 0.042(4) 0.042(4) 0.028(4) 0.008(3) 0.000(3) 0.014(3) C19 0.052(5) 0.046(4) 0.037(5) 0.013(4) 0.012(4) 0.014(4) C20 0.096(7) 0.052(5) 0.038(5) 0.016(4) 0.016(5) 0.018(5) C21 0.122(10) 0.088(8) 0.030(5) 0.009(5) -0.008(6) 0.029(7) C22 0.078(8) 0.123(10) 0.049(7) 0.004(7) -0.026(6) 0.028(7) C23 0.047(5) 0.088(7) 0.042(5) 0.006(5) -0.009(4) 0.017(5) C24 0.146(12) 0.093(8) 0.047(7) 0.025(6) 0.049(7) 0.024(8) C25 0.106(8) 0.049(6) 0.126(12) 0.043(7) 0.009(8) 0.026(6) C26 0.124(10) 0.053(6) 0.077(8) -0.006(6) 0.018(7) 0.023(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 O6 2.458(5) 2_666 ? La1 O4 2.462(5) 2_766 ? La1 O5 2.466(5) . ? La1 O2 2.501(5) 2_766 ? La1 O3 2.534(5) . ? La1 O1 2.562(5) . ? La1 O8 2.563(5) . ? La1 O7 2.661(6) . ? La1 O2 2.903(5) . ? La1 C1 3.110(7) . ? La1 La1 4.2204(7) 2_766 ? S1 O8 1.510(5) . ? S1 C26 1.767(12) . ? S1 C25 1.780(10) . ? O1 C1 1.261(8) . ? C1 O2 1.259(8) . ? C1 C2 1.489(10) . ? O2 La1 2.501(5) 2_766 ? C2 C7 1.378(11) . ? C2 C3 1.383(11) . ? O3 C9 1.265(8) . ? C3 C4 1.386(12) . ? C3 H3 0.9500 . ? O4 C9 1.249(9) . ? O4 La1 2.462(5) 2_766 ? C4 C5 1.390(16) . ? C4 C8 1.512(16) . ? O5 C17 1.259(9) . ? C5 C6 1.361(16) . ? C5 H5 0.9500 . ? O6 C17 1.252(8) . ? O6 La1 2.458(5) 2_666 ? C6 C7 1.362(13) . ? C6 H6 0.9500 . ? O7 H7A 0.94(13) . ? O7 H7B 0.72(10) . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O9 H9A 0.8813 . ? O9 H9B 0.8817 . ? C9 C10 1.505(10) . ? C10 C15 1.380(12) . ? C10 C11 1.388(11) . ? C11 C12 1.394(12) . ? C11 H11 0.9500 . ? C12 C13 1.358(15) . ? C12 C16 1.517(15) . ? C13 C14 1.364(16) . ? C13 H13 0.9500 . ? C14 C15 1.400(14) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.502(10) . ? C18 C19 1.381(11) . ? C18 C23 1.395(11) . ? C19 C20 1.388(12) . ? C19 H19 0.9500 . ? C20 C21 1.394(15) . ? C20 C24 1.501(15) . ? C21 C22 1.370(17) . ? C21 H21 0.9500 . ? C22 C23 1.373(14) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 La1 O4 79.38(18) 2_666 2_766 ? O6 La1 O5 92.21(17) 2_666 . ? O4 La1 O5 142.19(18) 2_766 . ? O6 La1 O2 84.44(16) 2_666 2_766 ? O4 La1 O2 70.60(17) 2_766 2_766 ? O5 La1 O2 145.80(17) . 2_766 ? O6 La1 O3 142.52(17) 2_666 . ? O4 La1 O3 128.28(16) 2_766 . ? O5 La1 O3 79.06(17) . . ? O2 La1 O3 83.12(17) 2_766 . ? O6 La1 O1 139.67(17) 2_666 . ? O4 La1 O1 84.81(18) 2_766 . ? O5 La1 O1 78.10(17) . . ? O2 La1 O1 124.55(15) 2_766 . ? O3 La1 O1 74.49(18) . . ? O6 La1 O8 70.79(17) 2_666 . ? O4 La1 O8 137.68(18) 2_766 . ? O5 La1 O8 69.71(18) . . ? O2 La1 O8 77.12(16) 2_766 . ? O3 La1 O8 72.00(17) . . ? O1 La1 O8 136.95(18) . . ? O6 La1 O7 71.5(2) 2_666 . ? O4 La1 O7 70.67(19) 2_766 . ? O5 La1 O7 71.69(19) . . ? O2 La1 O7 137.35(19) 2_766 . ? O3 La1 O7 136.3(2) . . ? O1 La1 O7 68.3(2) . . ? O8 La1 O7 123.75(18) . . ? O6 La1 O2 144.93(17) 2_666 . ? O4 La1 O2 66.36(16) 2_766 . ? O5 La1 O2 119.29(16) . . ? O2 La1 O2 77.57(16) 2_766 . ? O3 La1 O2 64.88(15) . . ? O1 La1 O2 46.98(14) . . ? O8 La1 O2 131.90(15) . . ? O7 La1 O2 102.39(17) . . ? O6 La1 C1 150.81(18) 2_666 . ? O4 La1 C1 75.82(18) 2_766 . ? O5 La1 C1 97.96(18) . . ? O2 La1 C1 101.38(17) 2_766 . ? O3 La1 C1 66.59(17) . . ? O1 La1 C1 23.21(17) . . ? O8 La1 C1 138.39(18) . . ? O7 La1 C1 85.8(2) . . ? O2 La1 C1 23.85(16) . . ? O6 La1 La1 120.38(12) 2_666 2_766 ? O4 La1 La1 61.79(12) 2_766 2_766 ? O5 La1 La1 145.77(12) . 2_766 ? O2 La1 La1 42.21(11) 2_766 2_766 ? O3 La1 La1 68.71(11) . 2_766 ? O1 La1 La1 82.34(11) . 2_766 ? O8 La1 La1 109.11(12) . 2_766 ? O7 La1 La1 125.70(13) . 2_766 ? O2 La1 La1 35.36(10) . 2_766 ? C1 La1 La1 59.19(13) . 2_766 ? O8 S1 C26 105.5(4) . . ? O8 S1 C25 104.3(5) . . ? C26 S1 C25 99.4(6) . . ? C1 O1 La1 103.6(4) . . ? O2 C1 O1 121.8(7) . . ? O2 C1 C2 120.0(6) . . ? O1 C1 C2 118.3(7) . . ? O2 C1 La1 68.8(4) . . ? O1 C1 La1 53.2(4) . . ? C2 C1 La1 170.3(5) . . ? C1 O2 La1 169.8(5) . 2_766 ? C1 O2 La1 87.3(4) . . ? La1 O2 La1 102.43(16) 2_766 . ? C7 C2 C3 118.4(8) . . ? C7 C2 C1 121.6(7) . . ? C3 C2 C1 119.9(7) . . ? C9 O3 La1 129.8(5) . . ? C2 C3 C4 121.8(9) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C9 O4 La1 136.7(5) . 2_766 ? C3 C4 C5 117.4(10) . . ? C3 C4 C8 120.8(11) . . ? C5 C4 C8 121.9(11) . . ? C17 O5 La1 149.9(5) . . ? C6 C5 C4 121.1(9) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C17 O6 La1 144.5(5) . 2_666 ? C5 C6 C7 120.5(10) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? La1 O7 H7A 113(7) . . ? La1 O7 H7B 113(8) . . ? H7A O7 H7B 107(10) . . ? C6 C7 C2 120.7(9) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? S1 O8 La1 132.4(3) . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? H9A O9 H9B 128.4 . . ? O4 C9 O3 125.1(7) . . ? O4 C9 C10 117.4(6) . . ? O3 C9 C10 117.5(7) . . ? C15 C10 C11 119.1(8) . . ? C15 C10 C9 121.6(7) . . ? C11 C10 C9 119.3(8) . . ? C10 C11 C12 120.9(9) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C13 C12 C11 118.7(9) . . ? C13 C12 C16 121.3(10) . . ? C11 C12 C16 119.9(11) . . ? C12 C13 C14 122.1(9) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C13 C14 C15 119.4(10) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C10 C15 C14 119.9(9) . . ? C10 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O6 C17 O5 123.8(7) . . ? O6 C17 C18 118.0(6) . . ? O5 C17 C18 118.2(6) . . ? C19 C18 C23 119.9(8) . . ? C19 C18 C17 120.3(7) . . ? C23 C18 C17 119.8(7) . . ? C18 C19 C20 121.3(8) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C19 C20 C21 117.4(9) . . ? C19 C20 C24 121.1(10) . . ? C21 C20 C24 121.4(10) . . ? C22 C21 C20 121.6(10) . . ? C22 C21 H21 119.2 . . ? C20 C21 H21 119.2 . . ? C21 C22 C23 120.5(10) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C22 C23 C18 119.2(10) . . ? C22 C23 H23 120.4 . . ? C18 C23 H23 120.4 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? S1 C25 H25A 109.5 . . ? S1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? S1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? S1 C26 H26A 109.5 . . ? S1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? S1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? 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 O7 H7A O9 0.94(13) 2.09(13) 3.005(9) 164(10) . O7 H7B O5 0.72(10) 2.35(10) 2.992(9) 148(10) 2_666 O7 H7B O8 0.72(10) 2.44(10) 3.011(8) 137(10) 2_666 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.945 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.093 # Attachment '5.CIF' data_HB9DMF _database_code_depnum_ccdc_archive 'CCDC 634374' _audit_creation_method SHELXL-97 _chemical_name_systematic ; poly[tris(3-methylbenzoato)(3-methylbenzoic acid)lanthanum(III)] 3- methylbenzoic acid solvate ; _chemical_name_common ; poly(tris(3-methylbenzoato)(3-methylbenzoic acid)lanthanum(iii)) 3-methylbenzoic acid solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C28 H25 La1 O7, C8 H8 O2' _chemical_formula_sum 'C36 H33 La1 O9' _chemical_formula_weight 748.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2424(3) _cell_length_b 12.3545(6) _cell_length_c 16.3741(9) _cell_angle_alpha 79.625(3) _cell_angle_beta 87.983(3) _cell_angle_gamma 82.373(3) _cell_volume 1625.51(13) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 1.369 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7714 _exptl_absorpt_correction_T_max 0.7907 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 12030 _diffrn_reflns_av_R_equivalents 0.1243 _diffrn_reflns_av_sigmaI/netI 0.1310 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5560 _reflns_number_gt 4146 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^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_extinction_expression ? _refine_ls_number_reflns 5560 _refine_ls_number_parameters 465 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1288 _refine_ls_R_factor_gt 0.0959 _refine_ls_wR_factor_ref 0.2566 _refine_ls_wR_factor_gt 0.2267 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _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 0.24670(7) 0.48377(5) 0.02537(3) 0.0199(3) Uani 1 1 d . . . O1 O 0.2477(9) 0.6430(6) -0.1000(4) 0.0264(18) Uani 1 1 d . . . O6 O -0.1832(9) 0.5813(7) 0.0998(4) 0.0266(18) Uani 1 1 d . . . O4 O 0.3822(9) 0.2849(6) 0.0396(4) 0.0248(17) Uani 1 1 d . . . O8 O 0.5999(9) 0.3981(8) 0.2399(5) 0.037(2) Uani 1 1 d . . . H8 H 0.6448 0.3963 0.1932 0.044 Uiso 1 1 calc R . . C1 C 0.0941(13) 0.6738(8) -0.1057(6) 0.020(2) Uani 1 1 d . . . O7 O 0.3739(9) 0.4113(7) 0.1672(5) 0.0312(19) Uani 1 1 d . . . C17 C -0.0686(12) 0.5993(9) 0.1426(6) 0.021(2) Uani 1 1 d . . . C25 C 0.4418(14) 0.4084(10) 0.2325(7) 0.028(3) Uani 1 1 d . . . C18 C -0.1216(14) 0.6538(11) 0.2161(7) 0.032(3) Uani 1 1 d . . . C9 C 0.5045(13) 0.3017(9) -0.0058(6) 0.022(2) Uani 1 1 d . . . C3 C -0.1258(15) 0.8031(9) -0.1838(7) 0.027(3) Uani 1 1 d . . . H3 H -0.2017 0.7577 -0.1553 0.032 Uiso 1 1 calc R . . C26 C 0.3498(14) 0.4125(10) 0.3117(7) 0.027(3) Uani 1 1 d . . . C11 C 0.6244(13) 0.1026(10) 0.0315(7) 0.025(2) Uani 1 1 d . . . H11 H 0.5561 0.0978 0.0797 0.030 Uiso 1 1 calc R . . C23 C -0.0043(15) 0.6824(11) 0.2649(7) 0.035(3) Uani 1 1 d . . . H23 H 0.1091 0.6655 0.2534 0.042 Uiso 1 1 calc R . . C2 C 0.0375(14) 0.7742(9) -0.1694(6) 0.022(2) Uani 1 1 d . . . C10 C 0.6200(13) 0.2033(9) -0.0238(7) 0.027(3) Uani 1 1 d . . . C19 C -0.2879(16) 0.6774(10) 0.2349(7) 0.032(3) Uani 1 1 d . . . H19 H -0.3673 0.6570 0.2018 0.038 Uiso 1 1 calc R . . C27 C 0.1832(14) 0.4077(11) 0.3125(7) 0.033(3) Uani 1 1 d . . . H27 H 0.1312 0.4045 0.2623 0.040 Uiso 1 1 calc R . . C15 C 0.7176(13) 0.2140(10) -0.0952(7) 0.029(3) Uani 1 1 d . . . H15 H 0.7179 0.2833 -0.1314 0.035 Uiso 1 1 calc R . . C14 C 0.8158(15) 0.1180(11) -0.1113(8) 0.037(3) Uani 1 1 d . . . H14 H 0.8789 0.1211 -0.1612 0.045 Uiso 1 1 calc R . . C6 C 0.0947(17) 0.9364(11) -0.2672(8) 0.041(3) Uani 1 1 d . . . H6 H 0.1703 0.9829 -0.2946 0.050 Uiso 1 1 calc R . . C12 C 0.7272(15) 0.0097(11) 0.0169(8) 0.034(3) Uani 1 1 d . . . C30 C 0.3338(16) 0.4230(12) 0.4571(8) 0.040(3) Uani 1 1 d . . . H30 H 0.3843 0.4314 0.5065 0.048 Uiso 1 1 calc R . . C4 C -0.1846(15) 0.9012(10) -0.2417(7) 0.034(3) Uani 1 1 d . . . C13 C 0.8220(16) 0.0198(11) -0.0563(8) 0.036(3) Uani 1 1 d . . . H13 H 0.8924 -0.0430 -0.0680 0.043 Uiso 1 1 calc R . . C5 C -0.0669(18) 0.9611(11) -0.2828(7) 0.041(3) Uani 1 1 d . . . H5 H -0.1017 1.0231 -0.3245 0.049 Uiso 1 1 calc R . . C31 C 0.4289(16) 0.4191(10) 0.3843(7) 0.033(3) Uani 1 1 d . . . H31 H 0.5437 0.4209 0.3846 0.040 Uiso 1 1 calc R . . C7 C 0.1480(15) 0.8424(10) -0.2106(7) 0.031(3) Uani 1 1 d . . . H7 H 0.2616 0.8239 -0.1994 0.037 Uiso 1 1 calc R . . C20 C -0.3388(17) 0.7299(11) 0.3010(7) 0.039(3) Uani 1 1 d . . . C16 C 0.7358(17) -0.0971(11) 0.0794(9) 0.043(3) Uani 1 1 d . . . H16A H 0.8149 -0.0958 0.1225 0.065 Uiso 1 1 calc R . . H16B H 0.7705 -0.1601 0.0514 0.065 Uiso 1 1 calc R . . H16C H 0.6276 -0.1045 0.1050 0.065 Uiso 1 1 calc R . . C22 C -0.0570(18) 0.7370(13) 0.3317(8) 0.047(4) Uani 1 1 d . . . H22 H 0.0208 0.7593 0.3646 0.057 Uiso 1 1 calc R . . C29 C 0.1705(16) 0.4148(14) 0.4579(7) 0.048(4) Uani 1 1 d . . . H29 H 0.1106 0.4142 0.5086 0.058 Uiso 1 1 calc R . . C24 C -0.5211(19) 0.7511(13) 0.3212(10) 0.055(4) Uani 1 1 d . . . H24A H -0.5388 0.8030 0.3604 0.083 Uiso 1 1 calc R . . H24B H -0.5604 0.6809 0.3460 0.083 Uiso 1 1 calc R . . H24C H -0.5812 0.7830 0.2700 0.083 Uiso 1 1 calc R . . C28 C 0.0883(16) 0.4073(15) 0.3860(9) 0.053(4) Uani 1 1 d . . . C21 C -0.2207(17) 0.7574(11) 0.3486(8) 0.041(3) Uani 1 1 d . . . H21 H -0.2545 0.7918 0.3949 0.050 Uiso 1 1 calc R . . C8 C -0.3638(19) 0.9294(15) -0.2571(10) 0.063(5) Uani 1 1 d . . . H8A H -0.4124 0.9772 -0.2185 0.094 Uiso 1 1 calc R . . H8B H -0.4154 0.8611 -0.2485 0.094 Uiso 1 1 calc R . . H8C H -0.3815 0.9685 -0.3143 0.094 Uiso 1 1 calc R . . O2 O -0.0038(9) 0.6227(6) -0.0609(4) 0.0228(17) Uani 1 1 d . . . O3 O 0.5321(9) 0.4010(6) -0.0392(5) 0.0230(17) Uani 1 1 d . . . O5 O 0.0794(9) 0.5773(7) 0.1274(5) 0.0278(18) Uani 1 1 d . . . C32 C -0.0933(18) 0.401(2) 0.3834(10) 0.091(8) Uani 1 1 d . . . H7A H -0.1297 0.3619 0.4369 0.136 Uiso 1 1 calc R . . H7B H -0.1156 0.3615 0.3392 0.136 Uiso 1 1 calc R . . H7C H -0.1525 0.4765 0.3725 0.136 Uiso 1 1 calc R . . O9 O 0.851(3) -0.0838(17) 0.5038(12) 0.044(5) Uani 0.50 1 d P . . O10 O 0.835(3) 0.098(2) 0.4873(14) 0.055(6) Uani 0.50 1 d P . . C33 C 0.763(6) 0.008(3) 0.491(3) 0.049(11) Uani 0.50 1 d P . . C35 C 0.509(5) -0.070(3) 0.509(2) 0.042(8) Uani 0.50 1 d PU . . H35 H 0.5690 -0.1406 0.5281 0.051 Uiso 0.50 1 calc PR . . C38 C 0.331(4) 0.134(2) 0.4505(16) 0.040(7) Uani 0.50 1 d P . . H38 H 0.2717 0.2045 0.4315 0.048 Uiso 0.50 1 calc PR . . C34 C 0.590(4) 0.020(3) 0.4882(14) 0.033(7) Uani 0.50 1 d P . . C37 C 0.249(5) 0.039(4) 0.472(2) 0.052(11) Uani 0.50 1 d P . . H37 H 0.1341 0.0451 0.4651 0.063 Uiso 0.50 1 calc PR . . C39 C 0.497(4) 0.122(3) 0.457(2) 0.048(8) Uani 0.50 1 d P . . H39 H 0.5524 0.1855 0.4398 0.057 Uiso 0.50 1 calc PR . . C36 C 0.335(6) -0.059(3) 0.5032(18) 0.043(8) Uani 0.50 1 d P . . C40 C 0.246(4) -0.163(3) 0.530(2) 0.052(8) Uani 0.50 1 d P . . H40A H 0.1373 -0.1494 0.5049 0.078 Uiso 0.50 1 calc PR . . H40B H 0.2342 -0.1775 0.5907 0.078 Uiso 0.50 1 calc PR . . H40C H 0.3097 -0.2270 0.5117 0.078 Uiso 0.50 1 calc PR . . 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 0.0228(4) 0.0165(4) 0.0213(4) -0.0018(2) 0.0019(2) -0.0089(3) O1 0.036(5) 0.017(4) 0.028(4) -0.002(3) 0.008(3) -0.017(3) O6 0.029(4) 0.035(5) 0.019(4) -0.007(3) 0.001(3) -0.011(4) O4 0.027(4) 0.023(5) 0.024(4) -0.001(3) 0.004(3) -0.008(3) O8 0.020(4) 0.074(7) 0.017(4) -0.004(4) 0.001(3) -0.009(4) C1 0.033(6) 0.007(5) 0.021(5) -0.004(4) -0.009(5) -0.002(4) O7 0.034(4) 0.038(5) 0.022(4) 0.000(3) 0.000(3) -0.012(4) C17 0.022(6) 0.024(6) 0.018(5) -0.011(4) 0.008(4) -0.005(5) C25 0.030(6) 0.023(7) 0.032(6) -0.002(5) -0.008(5) -0.007(5) C18 0.032(6) 0.035(8) 0.033(6) -0.015(5) 0.008(5) -0.012(5) C9 0.028(6) 0.023(6) 0.017(5) -0.009(4) -0.005(4) -0.003(5) C3 0.043(7) 0.015(6) 0.024(6) -0.003(4) 0.004(5) -0.009(5) C26 0.033(6) 0.025(7) 0.023(6) 0.000(5) 0.002(5) -0.009(5) C11 0.027(6) 0.027(7) 0.022(6) 0.000(5) -0.001(4) -0.016(5) C23 0.037(7) 0.046(8) 0.028(6) -0.016(6) 0.002(5) -0.014(6) C2 0.038(6) 0.014(6) 0.015(5) 0.003(4) 0.008(4) -0.012(5) C10 0.022(6) 0.018(6) 0.044(7) -0.008(5) -0.007(5) -0.006(5) C19 0.050(8) 0.019(7) 0.024(6) -0.001(5) -0.001(5) 0.003(6) C27 0.027(6) 0.046(8) 0.025(6) 0.004(5) 0.002(5) -0.014(6) C15 0.027(6) 0.029(7) 0.030(6) 0.004(5) 0.001(5) -0.009(5) C14 0.032(7) 0.039(8) 0.044(7) -0.021(6) 0.011(6) 0.000(6) C6 0.050(8) 0.032(8) 0.038(7) 0.013(6) 0.005(6) -0.016(6) C12 0.036(7) 0.035(8) 0.041(7) -0.023(6) -0.009(6) -0.013(6) C30 0.040(7) 0.053(9) 0.025(6) -0.006(6) -0.003(5) 0.001(6) C4 0.044(7) 0.028(7) 0.027(6) 0.015(5) -0.012(5) -0.013(6) C13 0.039(7) 0.019(7) 0.048(7) -0.009(6) -0.010(6) 0.007(5) C5 0.078(10) 0.025(7) 0.016(6) 0.014(5) -0.004(6) -0.017(7) C31 0.039(7) 0.032(8) 0.030(6) -0.006(5) -0.005(5) -0.010(6) C7 0.039(7) 0.030(7) 0.023(6) 0.000(5) 0.006(5) -0.008(6) C20 0.057(8) 0.028(7) 0.026(6) -0.003(5) 0.010(6) 0.006(6) C16 0.040(8) 0.029(8) 0.058(9) 0.002(6) -0.011(6) -0.008(6) C22 0.062(9) 0.051(10) 0.039(8) -0.020(7) 0.007(7) -0.029(8) C29 0.039(8) 0.085(12) 0.018(6) -0.004(6) 0.011(5) -0.007(7) C24 0.067(10) 0.043(10) 0.055(9) -0.011(7) 0.006(8) 0.000(8) C28 0.031(7) 0.083(13) 0.042(8) -0.002(8) 0.001(6) -0.014(7) C21 0.061(9) 0.041(9) 0.029(7) -0.017(6) 0.012(6) -0.019(7) C8 0.056(10) 0.068(12) 0.060(10) 0.010(9) -0.015(8) -0.019(9) O2 0.026(4) 0.020(4) 0.023(4) 0.002(3) 0.010(3) -0.018(3) O3 0.022(4) 0.013(4) 0.037(4) -0.004(3) 0.001(3) -0.013(3) O5 0.028(4) 0.030(5) 0.029(4) -0.015(4) 0.004(3) -0.003(3) C32 0.042(9) 0.19(3) 0.033(9) 0.000(11) 0.015(7) -0.032(12) O9 0.049(12) 0.035(12) 0.052(12) -0.015(9) -0.018(10) -0.005(10) O10 0.070(17) 0.036(15) 0.061(14) -0.009(11) 0.014(12) -0.017(12) C33 0.07(3) 0.02(2) 0.06(3) -0.018(17) -0.01(2) 0.02(2) C35 0.049(11) 0.037(12) 0.041(11) -0.010(8) 0.001(9) -0.004(9) C38 0.07(2) 0.014(14) 0.040(15) -0.011(11) -0.013(13) 0.002(13) C34 0.032(17) 0.06(2) 0.022(12) -0.024(13) 0.003(11) -0.030(18) C37 0.04(2) 0.06(3) 0.05(3) -0.02(2) -0.03(2) 0.02(2) C39 0.05(2) 0.04(2) 0.06(2) -0.011(16) 0.002(15) -0.007(15) C36 0.06(2) 0.04(2) 0.041(17) -0.021(14) 0.007(16) -0.02(2) C40 0.05(2) 0.06(3) 0.06(2) -0.020(18) 0.008(16) -0.033(18) _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 O6 2.429(7) 2_565 ? La1 O5 2.477(7) . ? La1 O3 2.497(7) 2_665 ? La1 O2 2.533(6) 2_565 ? La1 O4 2.535(8) . ? La1 O7 2.543(8) . ? La1 O1 2.575(7) . ? La1 O3 2.698(7) . ? La1 O2 2.756(8) . ? La1 La1 4.1322(12) 2_565 ? La1 La1 4.2857(11) 2_665 ? O1 C1 1.274(13) . ? O6 C17 1.261(12) . ? O6 La1 2.429(7) 2_565 ? O4 C9 1.249(13) . ? O8 C25 1.301(13) . ? O8 H8 0.8400 . ? C1 O2 1.231(13) . ? C1 C2 1.503(14) . ? O7 C25 1.216(13) . ? C17 O5 1.241(12) . ? C17 C18 1.507(14) . ? C25 C26 1.486(16) . ? C18 C23 1.395(16) . ? C18 C19 1.399(17) . ? C9 O3 1.296(13) . ? C9 C10 1.507(15) . ? C3 C2 1.363(16) . ? C3 C4 1.437(16) . ? C3 H3 0.9500 . ? C26 C27 1.381(16) . ? C26 C31 1.396(16) . ? C11 C12 1.386(17) . ? C11 C10 1.398(16) . ? C11 H11 0.9500 . ? C23 C22 1.411(17) . ? C23 H23 0.9500 . ? C2 C7 1.396(15) . ? C10 C15 1.392(16) . ? C19 C20 1.386(16) . ? C19 H19 0.9500 . ? C27 C28 1.412(17) . ? C27 H27 0.9500 . ? C15 C14 1.406(17) . ? C15 H15 0.9500 . ? C14 C13 1.370(18) . ? C14 H14 0.9500 . ? C6 C5 1.349(19) . ? C6 C7 1.381(17) . ? C6 H6 0.9500 . ? C12 C13 1.403(19) . ? C12 C16 1.512(18) . ? C30 C29 1.363(18) . ? C30 C31 1.408(17) . ? C30 H30 0.9500 . ? C4 C5 1.381(17) . ? C4 C8 1.491(19) . ? C13 H13 0.9500 . ? C5 H5 0.9500 . ? C31 H31 0.9500 . ? C7 H7 0.9500 . ? C20 C21 1.381(19) . ? C20 C24 1.52(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C22 C21 1.37(2) . ? C22 H22 0.9500 . ? C29 C28 1.402(19) . ? C29 H29 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C28 C32 1.511(19) . ? C21 H21 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O2 La1 2.533(6) 2_565 ? O3 La1 2.497(7) 2_665 ? C32 H7A 0.9800 . ? C32 H7B 0.9800 . ? C32 H7C 0.9800 . ? O9 C33 1.26(5) . ? O10 C33 1.32(5) . ? O10 C37 1.92(5) 2_656 ? C33 C34 1.41(5) . ? C35 C34 1.36(4) . ? C35 C36 1.43(5) . ? C35 H35 0.9500 . ? C38 C39 1.36(4) . ? C38 C37 1.41(5) . ? C38 H38 0.9500 . ? C34 C39 1.40(5) . ? C34 C39 2.04(4) 2_656 ? C37 C36 1.35(6) . ? C37 O10 1.92(5) 2_656 ? C37 H37 0.9500 . ? C39 C34 2.04(4) 2_656 ? C39 H39 0.9500 . ? C36 C40 1.54(5) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? 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 La1 O5 133.8(3) 2_565 . ? O6 La1 O3 125.8(2) 2_565 2_665 ? O5 La1 O3 89.1(2) . 2_665 ? O6 La1 O2 73.4(2) 2_565 2_565 ? O5 La1 O2 74.1(2) . 2_565 ? O3 La1 O2 160.7(2) 2_665 2_565 ? O6 La1 O4 73.5(3) 2_565 . ? O5 La1 O4 129.6(2) . . ? O3 La1 O4 106.6(2) 2_665 . ? O2 La1 O4 78.4(2) 2_565 . ? O6 La1 O7 140.4(3) 2_565 . ? O5 La1 O7 72.6(3) . . ? O3 La1 O7 73.0(2) 2_665 . ? O2 La1 O7 92.7(2) 2_565 . ? O4 La1 O7 67.4(3) . . ? O6 La1 O1 70.5(2) 2_565 . ? O5 La1 O1 101.4(2) . . ? O3 La1 O1 69.5(2) 2_665 . ? O2 La1 O1 122.3(2) 2_565 . ? O4 La1 O1 129.0(2) . . ? O7 La1 O1 142.1(2) . . ? O6 La1 O3 72.6(2) 2_565 . ? O5 La1 O3 153.6(2) . . ? O3 La1 O3 68.9(3) 2_665 . ? O2 La1 O3 124.3(2) 2_565 . ? O4 La1 O3 50.2(2) . . ? O7 La1 O3 86.7(2) . . ? O1 La1 O3 84.8(2) . . ? O6 La1 O2 68.6(2) 2_565 . ? O5 La1 O2 72.9(2) . . ? O3 La1 O2 107.0(2) 2_665 . ? O2 La1 O2 77.3(2) 2_565 . ? O4 La1 O2 139.4(2) . . ? O7 La1 O2 145.4(2) . . ? O1 La1 O2 48.2(2) . . ? O3 La1 O2 126.4(2) . . ? O6 La1 La1 65.29(17) 2_565 2_565 ? O5 La1 La1 68.60(18) . 2_565 ? O3 La1 La1 140.69(17) 2_665 2_565 ? O2 La1 La1 40.60(17) 2_565 2_565 ? O4 La1 La1 112.55(17) . 2_565 ? O7 La1 La1 125.32(17) . 2_565 ? O1 La1 La1 83.25(17) . 2_565 ? O3 La1 La1 137.84(15) . 2_565 ? O2 La1 La1 36.74(13) . 2_565 ? O6 La1 La1 98.79(17) 2_565 2_665 ? O5 La1 La1 123.65(18) . 2_665 ? O3 La1 La1 35.96(17) 2_665 2_665 ? O2 La1 La1 154.77(18) 2_565 2_665 ? O4 La1 La1 76.33(16) . 2_665 ? O7 La1 La1 78.02(17) . 2_665 ? O1 La1 La1 74.90(17) . 2_665 ? O3 La1 La1 32.93(14) . 2_665 ? O2 La1 La1 122.96(13) . 2_665 ? La1 La1 La1 156.56(3) 2_565 2_665 ? C1 O1 La1 99.1(6) . . ? C17 O6 La1 144.4(6) . 2_565 ? C9 O4 La1 98.4(7) . . ? C25 O8 H8 109.5 . . ? O2 C1 O1 121.1(10) . . ? O2 C1 C2 121.4(10) . . ? O1 C1 C2 117.5(9) . . ? C25 O7 La1 161.2(8) . . ? O5 C17 O6 125.0(9) . . ? O5 C17 C18 119.6(10) . . ? O6 C17 C18 115.4(9) . . ? O7 C25 O8 123.6(11) . . ? O7 C25 C26 122.4(10) . . ? O8 C25 C26 114.0(10) . . ? C23 C18 C19 119.9(11) . . ? C23 C18 C17 119.9(10) . . ? C19 C18 C17 120.3(10) . . ? O4 C9 O3 121.7(10) . . ? O4 C9 C10 118.8(10) . . ? O3 C9 C10 119.4(9) . . ? C2 C3 C4 120.9(10) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C27 C26 C31 120.4(11) . . ? C27 C26 C25 118.3(10) . . ? C31 C26 C25 121.3(10) . . ? C12 C11 C10 120.7(11) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C18 C23 C22 118.8(12) . . ? C18 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C3 C2 C7 119.2(10) . . ? C3 C2 C1 119.4(9) . . ? C7 C2 C1 121.3(10) . . ? C15 C10 C11 121.6(11) . . ? C15 C10 C9 119.6(10) . . ? C11 C10 C9 118.8(10) . . ? C20 C19 C18 121.0(12) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C26 C27 C28 121.7(11) . . ? C26 C27 H27 119.1 . . ? C28 C27 H27 119.1 . . ? C10 C15 C14 117.2(11) . . ? C10 C15 H15 121.4 . . ? C14 C15 H15 121.4 . . ? C13 C14 C15 121.0(11) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C5 C6 C7 118.8(11) . . ? C5 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? C11 C12 C13 117.6(12) . . ? C11 C12 C16 119.9(11) . . ? C13 C12 C16 122.5(12) . . ? C29 C30 C31 121.1(12) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C5 C4 C3 116.3(11) . . ? C5 C4 C8 124.1(12) . . ? C3 C4 C8 119.5(11) . . ? C14 C13 C12 121.8(12) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C6 C5 C4 123.7(11) . . ? C6 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? C26 C31 C30 118.2(11) . . ? C26 C31 H31 120.9 . . ? C30 C31 H31 120.9 . . ? C6 C7 C2 121.0(12) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? C21 C20 C19 118.2(12) . . ? C21 C20 C24 122.3(12) . . ? C19 C20 C24 119.5(13) . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C21 C22 C23 119.5(13) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C30 C29 C28 121.8(11) . . ? C30 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C29 C28 C27 116.8(12) . . ? C29 C28 C32 123.7(13) . . ? C27 C28 C32 119.5(13) . . ? C22 C21 C20 122.5(12) . . ? C22 C21 H21 118.7 . . ? C20 C21 H21 118.7 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C1 O2 La1 157.1(7) . 2_565 ? C1 O2 La1 91.5(6) . . ? La1 O2 La1 102.7(2) 2_565 . ? C9 O3 La1 134.1(7) . 2_665 ? C9 O3 La1 89.6(6) . . ? La1 O3 La1 111.1(3) 2_665 . ? C17 O5 La1 136.4(7) . . ? C28 C32 H7A 109.5 . . ? C28 C32 H7B 109.5 . . ? H7A C32 H7B 109.5 . . ? C28 C32 H7C 109.5 . . ? H7A C32 H7C 109.5 . . ? H7B C32 H7C 109.5 . . ? C33 O10 C37 18(2) . 2_656 ? O9 C33 O10 118(4) . . ? O9 C33 C34 124(4) . . ? O10 C33 C34 118(4) . . ? C34 C35 C36 121(4) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C39 C38 C37 119(3) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C35 C34 C39 117(4) . . ? C35 C34 C33 120(4) . . ? C39 C34 C33 122(3) . . ? C35 C34 C39 13.3(19) . 2_656 ? C39 C34 C39 127(2) . 2_656 ? C33 C34 C39 111(3) . 2_656 ? C36 C37 C38 119(4) . . ? C36 C37 O10 53(3) . 2_656 ? C38 C37 O10 171(3) . 2_656 ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? O10 C37 H37 67.9 2_656 . ? C38 C39 C34 122(3) . . ? C38 C39 C34 70(2) . 2_656 ? C34 C39 C34 53(2) . 2_656 ? C38 C39 H39 118.8 . . ? C34 C39 H39 118.8 . . ? C34 C39 H39 169.2 2_656 . ? C37 C36 C35 120(4) . . ? C37 C36 C40 120(4) . . ? C35 C36 C40 120(3) . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? 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 O8 H8 O1 0.84 1.85 2.671(10) 166.5 2_665 _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 3.206 _refine_diff_density_min -3.232 _refine_diff_density_rms 0.264 # Attachment '6.CIF' data_HB28DMSO _database_code_depnum_ccdc_archive 'CCDC 634375' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis[bis(dimethylsulphoxide)tris(2,4,6-trimethylbenzoato)lanthanum (III)] ; _chemical_name_common ;bis(bis(dimethylsulphoxide)tris(2,4,6- trimethylbenzoato)lanthanum (iii)) ; _chemical_melting_point ? _chemical_formula_moiety 'C68 H90 La2 O16 S4' _chemical_formula_sum 'C68 H90 La2 O16 S4' _chemical_formula_weight 1569.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.5545(2) _cell_length_b 19.5508(2) _cell_length_c 16.9228(2) _cell_angle_alpha 90.00 _cell_angle_beta 118.495(1) _cell_angle_gamma 90.00 _cell_volume 7430.58(13) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3216 _exptl_absorpt_coefficient_mu 1.307 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6951 _exptl_absorpt_correction_T_max 0.7800 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 30729 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8497 _reflns_number_gt 5616 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^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_extinction_expression ? _refine_ls_number_reflns 8497 _refine_ls_number_parameters 519 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0870 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1136 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.038 _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 La1 La 0.069548(9) 0.330238(10) 0.389163(14) 0.04094(10) Uani 1 1 d . . . O1 O 0.10911(14) 0.38444(14) 0.54900(18) 0.0670(8) Uani 1 1 d . C . C1 C 0.12488(19) 0.3280(2) 0.5887(3) 0.0533(10) Uani 1 1 d . . . S1 S 0.23424(6) 0.35235(8) 0.48106(9) 0.0765(4) Uani 1 1 d D A 1 C31 C 0.2717(3) 0.4297(3) 0.4850(5) 0.144(3) Uani 1 1 d D A 1 H31A H 0.2510 0.4528 0.4267 0.216 Uiso 1 1 calc R A 1 H31B H 0.3127 0.4195 0.4986 0.216 Uiso 1 1 calc R A 1 H31C H 0.2721 0.4594 0.5319 0.216 Uiso 1 1 calc R A 1 C32 C 0.2535(3) 0.3062(3) 0.4098(4) 0.118(2) Uani 1 1 d D A 1 H32A H 0.2253 0.2684 0.3822 0.177 Uiso 1 1 calc R A 1 H32B H 0.2938 0.2879 0.4447 0.177 Uiso 1 1 calc R A 1 H32C H 0.2519 0.3365 0.3626 0.177 Uiso 1 1 calc R A 1 S2A S 0.05560(10) 0.50924(9) 0.4401(2) 0.1019(12) Uani 0.775(6) 1 d PD B 1 C33A C 0.0229(4) 0.5853(4) 0.3792(9) 0.210(13) Uani 0.775(6) 1 d PD B 1 H33A H -0.0205 0.5803 0.3471 0.315 Uiso 0.775(6) 1 calc PR B 1 H33B H 0.0374 0.5935 0.3358 0.315 Uiso 0.775(6) 1 calc PR B 1 H33C H 0.0339 0.6239 0.4209 0.315 Uiso 0.775(6) 1 calc PR B 1 C34A C 0.1304(2) 0.5347(3) 0.4887(5) 0.175(8) Uani 0.775(6) 1 d PD B 1 H34A H 0.1559 0.4977 0.5265 0.262 Uiso 0.775(6) 1 calc PR B 1 H34B H 0.1363 0.5756 0.5256 0.262 Uiso 0.775(6) 1 calc PR B 1 H34C H 0.1407 0.5451 0.4411 0.262 Uiso 0.775(6) 1 calc PR B 1 O2 O 0.11973(14) 0.27396(14) 0.54703(19) 0.0662(8) Uani 1 1 d . C . C2A C 0.1582(5) 0.3312(8) 0.6937(6) 0.050(3) Uani 0.598(18) 1 d PD C 1 C3A C 0.1275(6) 0.3022(6) 0.7382(8) 0.066(4) Uani 0.598(18) 1 d PD C 1 C4A C 0.1558(9) 0.3096(11) 0.8311(11) 0.087(5) Uani 0.598(18) 1 d PD C 1 H4A H 0.1367 0.2916 0.8629 0.105 Uiso 0.598(18) 1 calc PR C 1 C5A C 0.2108(7) 0.3419(8) 0.8802(7) 0.085(5) Uani 0.598(18) 1 d PD C 1 C6A C 0.2366(5) 0.3683(6) 0.8360(6) 0.070(3) Uani 0.598(18) 1 d PD C 1 H6A H 0.2736 0.3909 0.8698 0.084 Uiso 0.598(18) 1 calc PR C 1 C7A C 0.2127(6) 0.3653(7) 0.7415(5) 0.050(3) Uani 0.598(18) 1 d PD C 1 C8A C 0.0678(8) 0.2684(10) 0.6816(11) 0.092(6) Uani 0.598(18) 1 d PD C 1 H8A1 H 0.0739 0.2227 0.6637 0.138 Uiso 0.598(18) 1 calc PR C 1 H8A2 H 0.0443 0.2961 0.6278 0.138 Uiso 0.598(18) 1 calc PR C 1 H8A3 H 0.0465 0.2646 0.7166 0.138 Uiso 0.598(18) 1 calc PR C 1 C9A C 0.2383(8) 0.3460(8) 0.9827(5) 0.125(6) Uani 0.598(18) 1 d PD C 1 H9A1 H 0.2260 0.3060 1.0048 0.188 Uiso 0.598(18) 1 calc PR C 1 H9A2 H 0.2247 0.3878 0.9993 0.188 Uiso 0.598(18) 1 calc PR C 1 H9A3 H 0.2818 0.3467 1.0097 0.188 Uiso 0.598(18) 1 calc PR C 1 C10A C 0.2461(6) 0.3914(11) 0.6939(10) 0.075(4) Uani 0.598(18) 1 d PD C 1 H10A H 0.2640 0.3528 0.6787 0.113 Uiso 0.598(18) 1 calc PR C 1 H10B H 0.2774 0.4231 0.7334 0.113 Uiso 0.598(18) 1 calc PR C 1 H10C H 0.2183 0.4153 0.6387 0.113 Uiso 0.598(18) 1 calc PR C 1 C2B C 0.1354(9) 0.3216(11) 0.6805(7) 0.046(4) Uani 0.402(18) 1 d PD C 2 C3B C 0.0950(10) 0.2883(11) 0.7052(13) 0.099(17) Uani 0.402(18) 1 d PD C 2 C4B C 0.1125(11) 0.2880(10) 0.7966(14) 0.109(9) Uani 0.402(18) 1 d PD C 2 H4B H 0.0852 0.2717 0.8152 0.130 Uiso 0.402(18) 1 calc PR C 2 C5B C 0.1683(12) 0.3104(16) 0.8625(10) 0.108(18) Uani 0.402(18) 1 d PD C 2 C6B C 0.2046(10) 0.3376(11) 0.8363(7) 0.094(10) Uani 0.402(18) 1 d PD C 2 H6B H 0.2418 0.3545 0.8814 0.113 Uiso 0.402(18) 1 calc PR C 2 C7B C 0.1920(9) 0.3433(8) 0.7455(8) 0.054(5) Uani 0.402(18) 1 d PD C 2 C8B C 0.0365(10) 0.2616(11) 0.6314(15) 0.100(7) Uani 0.402(18) 1 d PD C 2 H8B1 H 0.0309 0.2141 0.6445 0.150 Uiso 0.402(18) 1 calc PR C 2 H8B2 H 0.0370 0.2634 0.5739 0.150 Uiso 0.402(18) 1 calc PR C 2 H8B3 H 0.0038 0.2898 0.6278 0.150 Uiso 0.402(18) 1 calc PR C 2 C9B C 0.1835(15) 0.3059(13) 0.9615(9) 0.188(19) Uani 0.402(18) 1 d PD C 2 H9B1 H 0.2070 0.2646 0.9884 0.282 Uiso 0.402(18) 1 calc PR C 2 H9B2 H 0.1466 0.3039 0.9658 0.282 Uiso 0.402(18) 1 calc PR C 2 H9B3 H 0.2065 0.3463 0.9937 0.282 Uiso 0.402(18) 1 calc PR C 2 C10B C 0.2342(7) 0.3766(11) 0.7180(10) 0.062(7) Uani 0.402(18) 1 d PD C 2 H10D H 0.2459 0.3433 0.6861 0.093 Uiso 0.402(18) 1 calc PR C 2 H10E H 0.2697 0.3927 0.7717 0.093 Uiso 0.402(18) 1 calc PR C 2 H10F H 0.2144 0.4155 0.6784 0.093 Uiso 0.402(18) 1 calc PR C 2 O3 O -0.04909(11) 0.34317(12) 0.27166(17) 0.0450(6) Uani 1 1 d . . . O4 O -0.02010(12) 0.34513(14) 0.41632(18) 0.0556(7) Uani 1 1 d . . . O5 O 0.11563(12) 0.21361(13) 0.37803(19) 0.0546(7) Uani 1 1 d . . . O6 O 0.02490(12) 0.21237(13) 0.3615(2) 0.0586(7) Uani 1 1 d . . . O7 O 0.05061(14) 0.45742(14) 0.3681(2) 0.0674(9) Uani 1 1 d . . . O8 O 0.17034(12) 0.36890(16) 0.4268(2) 0.0728(9) Uani 1 1 d . . . C11 C -0.06060(17) 0.34840(17) 0.3362(3) 0.0421(9) Uani 1 1 d . . . C12 C -0.12327(16) 0.35929(19) 0.3186(2) 0.0432(9) Uani 1 1 d . . . C13 C -0.15180(18) 0.3066(2) 0.3409(3) 0.0489(9) Uani 1 1 d . . . C14 C -0.2095(2) 0.3171(2) 0.3257(3) 0.0586(11) Uani 1 1 d . . . H14 H -0.2292 0.2814 0.3391 0.070 Uiso 1 1 calc R . . C15 C -0.23912(18) 0.3779(3) 0.2916(3) 0.0617(12) Uani 1 1 d . . . C16 C -0.20980(19) 0.4294(2) 0.2726(3) 0.0572(11) Uani 1 1 d . . . H16 H -0.2296 0.4718 0.2502 0.069 Uiso 1 1 calc R . . C17 C -0.15188(17) 0.42109(19) 0.2854(3) 0.0474(9) Uani 1 1 d . . . C18 C -0.1207(2) 0.2399(2) 0.3805(4) 0.0789(15) Uani 1 1 d . . . H18A H -0.0936 0.2458 0.4449 0.118 Uiso 1 1 calc R . . H18B H -0.0978 0.2257 0.3504 0.118 Uiso 1 1 calc R . . H18C H -0.1503 0.2048 0.3719 0.118 Uiso 1 1 calc R . . C19 C -0.1220(2) 0.4799(2) 0.2650(3) 0.0676(12) Uani 1 1 d . . . H19A H -0.1239 0.5209 0.2969 0.101 Uiso 1 1 calc R . . H19B H -0.1424 0.4887 0.2001 0.101 Uiso 1 1 calc R . . H19C H -0.0802 0.4683 0.2848 0.101 Uiso 1 1 calc R . . C20 C -0.3031(2) 0.3879(4) 0.2743(4) 0.103(2) Uani 1 1 d . . . H20A H -0.3168 0.4339 0.2503 0.154 Uiso 0.50 1 calc PR . . H20B H -0.3045 0.3824 0.3308 0.154 Uiso 0.50 1 calc PR . . H20C H -0.3290 0.3538 0.2307 0.154 Uiso 0.50 1 calc PR . . H20D H -0.3168 0.3462 0.2909 0.154 Uiso 0.50 1 calc PR . . H20E H -0.3290 0.3977 0.2104 0.154 Uiso 0.50 1 calc PR . . H20F H -0.3045 0.4263 0.3105 0.154 Uiso 0.50 1 calc PR . . C21 C 0.07067(17) 0.18154(19) 0.3711(3) 0.0471(10) Uani 1 1 d . . . C22 C 0.07177(16) 0.10506(19) 0.3766(3) 0.0510(11) Uani 1 1 d . . . C23 C 0.06368(19) 0.0732(2) 0.4444(3) 0.0652(12) Uani 1 1 d . . . C24 C 0.0660(2) 0.0014(2) 0.4489(4) 0.0802(15) Uani 1 1 d . . . H24 H 0.0616 -0.0205 0.4956 0.096 Uiso 1 1 calc R . . C25 C 0.0742(2) -0.0384(3) 0.3895(4) 0.0876(18) Uani 1 1 d . . . C26 C 0.0816(2) -0.0058(2) 0.3226(4) 0.0758(15) Uani 1 1 d . . . H26 H 0.0870 -0.0328 0.2804 0.091 Uiso 1 1 calc R . . C27 C 0.08132(17) 0.0658(2) 0.3152(3) 0.0562(11) Uani 1 1 d . . . C28 C 0.0538(3) 0.1129(3) 0.5116(4) 0.0855(16) Uani 1 1 d . . . H28A H 0.0818 0.1513 0.5338 0.128 Uiso 1 1 calc R . . H28B H 0.0602 0.0830 0.5619 0.128 Uiso 1 1 calc R . . H28C H 0.0129 0.1303 0.4830 0.128 Uiso 1 1 calc R . . C29 C 0.0903(2) 0.0985(2) 0.2425(3) 0.0706(13) Uani 1 1 d . . . H29A H 0.1281 0.1236 0.2695 0.106 Uiso 1 1 calc R . . H29B H 0.0575 0.1303 0.2082 0.106 Uiso 1 1 calc R . . H29C H 0.0912 0.0631 0.2022 0.106 Uiso 1 1 calc R . . C30 C 0.0749(2) -0.1189(2) 0.3997(3) 0.146(3) Uani 1 1 d . . . H30A H 0.0812 -0.1404 0.3526 0.219 Uiso 0.50 1 calc PR . . H30B H 0.0367 -0.1342 0.3940 0.219 Uiso 0.50 1 calc PR . . H30C H 0.1071 -0.1321 0.4589 0.219 Uiso 0.50 1 calc PR . . H30D H 0.0688 -0.1308 0.4511 0.219 Uiso 0.50 1 calc PR . . H30E H 0.1133 -0.1369 0.4096 0.219 Uiso 0.50 1 calc PR . . H30F H 0.0429 -0.1390 0.3448 0.219 Uiso 0.50 1 calc PR . . S2B S 0.0646(2) 0.5323(2) 0.3896(3) 0.079(3) Uani 0.225(6) 1 d PR B 2 C33B C 0.0229(4) 0.5853(4) 0.3792(9) 0.23(3) Uani 0.225(6) 1 d P B 2 H33D H -0.0128 0.5803 0.3207 0.343 Uiso 0.225(6) 1 calc PR B 2 H33E H 0.0411 0.6300 0.3824 0.343 Uiso 0.225(6) 1 calc PR B 2 H33F H 0.0121 0.5816 0.4272 0.343 Uiso 0.225(6) 1 calc PR B 2 C34B C 0.1304(2) 0.5347(3) 0.4887(5) 0.125(11) Uani 0.225(6) 1 d P B 2 H34D H 0.1560 0.4969 0.4900 0.187 Uiso 0.225(6) 1 calc PR B 2 H34E H 0.1222 0.5303 0.5394 0.187 Uiso 0.225(6) 1 calc PR B 2 H34F H 0.1505 0.5783 0.4932 0.187 Uiso 0.225(6) 1 calc PR B 2 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 0.03450(14) 0.04090(14) 0.04133(14) 0.00001(9) 0.01316(10) -0.00136(9) O1 0.079(2) 0.0539(17) 0.0478(17) 0.0014(13) 0.0136(15) 0.0044(15) C1 0.050(2) 0.059(3) 0.049(2) 0.005(2) 0.022(2) 0.0117(19) S1 0.0554(7) 0.1093(10) 0.0601(7) 0.0131(7) 0.0236(6) 0.0112(7) C31 0.064(4) 0.175(7) 0.151(7) -0.014(5) 0.017(4) -0.061(4) C32 0.133(6) 0.155(6) 0.084(4) 0.047(4) 0.066(4) 0.083(5) S2A 0.1102(17) 0.0524(11) 0.135(2) -0.0081(12) 0.0515(15) 0.0066(10) C33A 0.153(11) 0.083(8) 0.35(2) 0.100(14) 0.079(19) 0.043(11) C34A 0.156(11) 0.094(7) 0.143(11) -0.066(10) -0.035(11) -0.059(10) O2 0.083(2) 0.0526(16) 0.0563(18) 0.0010(14) 0.0276(17) 0.0133(15) C2A 0.034(7) 0.062(7) 0.048(7) 0.006(5) 0.015(5) 0.019(6) C3A 0.078(9) 0.062(5) 0.054(9) 0.015(6) 0.029(7) 0.032(6) C4A 0.120(14) 0.087(11) 0.057(15) 0.023(9) 0.043(11) 0.042(11) C5A 0.107(10) 0.090(9) 0.052(7) -0.006(6) 0.033(7) 0.037(7) C6A 0.069(7) 0.075(8) 0.042(5) -0.010(4) 0.006(5) 0.025(5) C7A 0.052(9) 0.048(7) 0.044(7) -0.002(5) 0.017(5) 0.011(6) C8A 0.083(17) 0.122(13) 0.074(16) 0.012(12) 0.041(13) 0.016(12) C9A 0.175(15) 0.130(11) 0.042(5) 0.011(5) 0.028(7) 0.052(10) C10A 0.051(6) 0.108(11) 0.069(7) -0.019(7) 0.031(5) 0.000(5) C2B 0.042(11) 0.054(8) 0.047(8) 0.008(6) 0.025(7) 0.016(8) C3B 0.10(3) 0.13(3) 0.033(12) -0.005(14) 0.006(17) 0.07(3) C4B 0.17(2) 0.100(14) 0.106(17) 0.042(13) 0.106(18) 0.066(15) C5B 0.18(4) 0.13(2) 0.045(18) 0.046(15) 0.08(2) 0.11(3) C6B 0.14(3) 0.081(15) 0.037(11) -0.015(11) 0.017(13) 0.047(15) C7B 0.074(15) 0.036(9) 0.048(9) 0.006(7) 0.027(9) 0.017(8) C8B 0.093(17) 0.124(14) 0.103(16) -0.012(14) 0.063(14) -0.014(12) C9B 0.34(5) 0.17(2) 0.063(12) 0.055(13) 0.11(2) 0.16(3) C10B 0.046(13) 0.078(14) 0.051(14) -0.035(12) 0.013(8) -0.006(9) O3 0.0437(15) 0.0473(14) 0.0470(15) -0.0008(11) 0.0240(13) 0.0049(11) O4 0.0440(16) 0.0754(19) 0.0406(16) -0.0017(13) 0.0148(14) 0.0039(13) O5 0.0457(16) 0.0473(15) 0.0737(19) -0.0006(13) 0.0309(14) -0.0004(12) O6 0.0396(15) 0.0439(15) 0.085(2) -0.0024(13) 0.0240(14) -0.0002(12) O7 0.078(2) 0.0409(15) 0.0632(18) -0.0038(13) 0.0179(16) -0.0026(14) O8 0.0419(17) 0.081(2) 0.088(2) -0.0060(17) 0.0249(16) -0.0135(15) C11 0.045(2) 0.0345(18) 0.047(2) -0.0016(15) 0.022(2) 0.0026(15) C12 0.038(2) 0.050(2) 0.039(2) -0.0080(16) 0.0164(17) -0.0008(17) C13 0.050(2) 0.054(2) 0.049(2) -0.0051(18) 0.028(2) -0.0019(18) C14 0.058(3) 0.077(3) 0.052(3) -0.013(2) 0.035(2) -0.017(2) C15 0.039(2) 0.096(3) 0.051(3) -0.014(2) 0.022(2) 0.001(2) C16 0.049(2) 0.064(3) 0.052(2) -0.0071(19) 0.019(2) 0.013(2) C17 0.045(2) 0.047(2) 0.048(2) -0.0048(16) 0.0199(19) 0.0041(17) C18 0.087(4) 0.064(3) 0.098(4) 0.013(3) 0.054(3) -0.002(3) C19 0.061(3) 0.053(2) 0.088(3) 0.007(2) 0.035(3) 0.007(2) C20 0.047(3) 0.163(6) 0.103(5) -0.002(4) 0.038(3) 0.009(3) C21 0.040(2) 0.042(2) 0.053(2) 0.0030(16) 0.017(2) 0.0014(17) C22 0.036(2) 0.042(2) 0.069(3) 0.0026(18) 0.020(2) 0.0023(16) C23 0.047(3) 0.064(3) 0.086(3) 0.010(2) 0.033(2) 0.000(2) C24 0.077(3) 0.052(3) 0.111(4) 0.022(3) 0.044(3) 0.000(2) C25 0.078(4) 0.045(3) 0.141(6) 0.015(3) 0.052(4) 0.003(2) C26 0.056(3) 0.051(3) 0.117(4) -0.009(3) 0.038(3) 0.004(2) C27 0.038(2) 0.048(2) 0.076(3) 0.001(2) 0.022(2) 0.0062(17) C28 0.093(4) 0.084(3) 0.089(4) 0.012(3) 0.051(3) -0.003(3) C29 0.059(3) 0.068(3) 0.081(3) -0.007(2) 0.031(3) 0.008(2) C30 0.163(7) 0.049(3) 0.248(10) 0.020(4) 0.115(7) 0.011(4) S2B 0.152(7) 0.040(3) 0.064(4) -0.002(2) 0.067(4) -0.016(3) C33B 0.228(18) 0.23(2) 0.23(3) 0.00(7) 0.11(7) 0.00(8) C34B 0.125(9) 0.125(11) 0.125(14) 0.00(3) 0.06(2) 0.00(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O8 2.459(3) . ? La1 O6 2.514(2) . ? La1 O7 2.526(3) . ? La1 O3 2.527(3) 2 ? La1 O4 2.559(3) . ? La1 O2 2.593(3) . ? La1 O5 2.614(3) . ? La1 O1 2.618(3) . ? La1 O3 2.731(2) . ? La1 La1 4.3410(4) 2 ? O1 C1 1.255(5) . ? C1 O2 1.242(5) . ? C1 C2B 1.450(9) . ? C1 C2A 1.562(9) . ? S1 O8 1.478(3) . ? S1 C32 1.754(5) . ? S1 C31 1.774(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? S2A O7 1.542(4) . ? S2A C34A 1.754(5) . ? S2A C33A 1.774(5) . ? C33A H33A 0.9800 . ? C33A H33B 0.9800 . ? C33A H33C 0.9800 . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? C2A C7A 1.401(13) . ? C2A C3A 1.441(16) . ? C3A C4A 1.39(2) . ? C3A C8A 1.511(19) . ? C4A C5A 1.40(2) . ? C4A H4A 0.9500 . ? C5A C6A 1.316(18) . ? C5A C9A 1.531(13) . ? C6A C7A 1.416(11) . ? C6A H6A 0.9500 . ? C7A C10A 1.512(12) . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C2B C7B 1.402(13) . ? C2B C3B 1.441(16) . ? C3B C4B 1.39(2) . ? C3B C8B 1.511(19) . ? C4B C5B 1.40(2) . ? C4B H4B 0.9500 . ? C5B C6B 1.316(19) . ? C5B C9B 1.532(13) . ? C6B C7B 1.416(11) . ? C6B H6B 0.9500 . ? C7B C10B 1.512(12) . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? C8B H8B3 0.9800 . ? C9B H9B1 0.9800 . ? C9B H9B2 0.9800 . ? C9B H9B3 0.9800 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? O3 C11 1.264(4) . ? O3 La1 2.527(3) 2 ? O4 C11 1.255(4) . ? O5 C21 1.264(4) . ? O6 C21 1.256(4) . ? O7 S2B 1.510(5) . ? C11 C12 1.498(5) . ? C12 C17 1.385(5) . ? C12 C13 1.413(6) . ? C13 C14 1.385(6) . ? C13 C18 1.509(6) . ? C14 C15 1.380(6) . ? C14 H14 0.9500 . ? C15 C16 1.381(6) . ? C15 C20 1.530(6) . ? C16 C17 1.399(6) . ? C16 H16 0.9500 . ? C17 C19 1.509(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C20 H20D 0.9800 . ? C20 H20E 0.9800 . ? C20 H20F 0.9800 . ? C21 C22 1.498(5) . ? C22 C27 1.404(6) . ? C22 C23 1.405(6) . ? C23 C24 1.405(6) . ? C23 C28 1.493(7) . ? C24 C25 1.365(8) . ? C24 H24 0.9500 . ? C25 C26 1.389(7) . ? C25 C30 1.583(6) . ? C26 C27 1.405(6) . ? C26 H26 0.9500 . ? C27 C29 1.499(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C30 H30D 0.9800 . ? C30 H30E 0.9800 . ? C30 H30F 0.9800 . ? 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 O8 La1 O6 131.02(10) . . ? O8 La1 O7 80.82(11) . . ? O6 La1 O7 146.79(10) . . ? O8 La1 O3 84.32(10) . 2 ? O6 La1 O3 92.81(9) . 2 ? O7 La1 O3 79.78(9) . 2 ? O8 La1 O4 146.66(10) . . ? O6 La1 O4 76.82(9) . . ? O7 La1 O4 77.61(10) . . ? O3 La1 O4 116.04(8) 2 . ? O8 La1 O2 85.50(11) . . ? O6 La1 O2 76.13(9) . . ? O7 La1 O2 122.02(9) . . ? O3 La1 O2 153.97(9) 2 . ? O4 La1 O2 84.74(9) . . ? O8 La1 O5 80.48(9) . . ? O6 La1 O5 50.75(8) . . ? O7 La1 O5 155.68(10) . . ? O3 La1 O5 83.02(8) 2 . ? O4 La1 O5 125.79(9) . . ? O2 La1 O5 71.69(9) . . ? O8 La1 O1 76.55(11) . . ? O6 La1 O1 118.72(10) . . ? O7 La1 O1 72.58(9) . . ? O3 La1 O1 148.41(8) 2 . ? O4 La1 O1 72.90(9) . . ? O2 La1 O1 49.44(9) . . ? O5 La1 O1 117.54(9) . . ? O8 La1 O3 145.28(9) . . ? O6 La1 O3 72.65(8) . . ? O7 La1 O3 74.62(8) . . ? O3 La1 O3 67.61(10) 2 . ? O4 La1 O3 48.87(8) . . ? O2 La1 O3 128.40(9) . . ? O5 La1 O3 114.21(8) . . ? O1 La1 O3 117.54(9) . . ? O8 La1 La1 119.69(8) . 2 ? O6 La1 La1 74.58(7) . 2 ? O7 La1 La1 81.05(7) . 2 ? O3 La1 La1 35.90(6) 2 2 ? O4 La1 La1 81.67(6) . 2 ? O2 La1 La1 149.81(7) . 2 ? O5 La1 La1 94.91(6) . 2 ? O1 La1 La1 146.49(7) . 2 ? O3 La1 La1 32.86(6) . 2 ? C1 O1 La1 93.7(2) . . ? O2 C1 O1 121.6(4) . . ? O2 C1 C2B 116.8(9) . . ? O1 C1 C2B 119.9(9) . . ? O2 C1 C2A 122.2(7) . . ? O1 C1 C2A 115.8(7) . . ? C2B C1 C2A 20.6(5) . . ? O8 S1 C32 105.9(3) . . ? O8 S1 C31 104.7(3) . . ? C32 S1 C31 98.1(3) . . ? O7 S2A C34A 102.6(3) . . ? O7 S2A C33A 104.6(5) . . ? C34A S2A C33A 98.0(3) . . ? S2A C33A H33A 109.5 . . ? S2A C33A H33B 109.5 . . ? H33A C33A H33B 109.5 . . ? S2A C33A H33C 109.5 . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 109.5 . . ? S2A C34A H34A 109.5 . . ? S2A C34A H34B 109.5 . . ? H34A C34A H34B 109.5 . . ? S2A C34A H34C 109.5 . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? C1 O2 La1 95.2(2) . . ? C7A C2A C3A 121.7(9) . . ? C7A C2A C1 121.9(8) . . ? C3A C2A C1 116.2(9) . . ? C4A C3A C2A 115.6(12) . . ? C4A C3A C8A 125.9(16) . . ? C2A C3A C8A 118.5(12) . . ? C3A C4A C5A 123.7(13) . . ? C3A C4A H4A 118.2 . . ? C5A C4A H4A 118.2 . . ? C6A C5A C4A 118.2(11) . . ? C6A C5A C9A 122.7(12) . . ? C4A C5A C9A 119.1(13) . . ? C5A C6A C7A 124.4(10) . . ? C5A C6A H6A 117.8 . . ? C7A C6A H6A 117.8 . . ? C2A C7A C6A 116.4(11) . . ? C2A C7A C10A 120.6(9) . . ? C6A C7A C10A 122.7(11) . . ? C7B C2B C3B 121.5(9) . . ? C7B C2B C1 114.1(9) . . ? C3B C2B C1 123.9(11) . . ? C4B C3B C2B 115.4(12) . . ? C4B C3B C8B 125.9(16) . . ? C2B C3B C8B 118.5(12) . . ? C3B C4B C5B 123.6(13) . . ? C3B C4B H4B 118.2 . . ? C5B C4B H4B 118.2 . . ? C6B C5B C4B 118.2(11) . . ? C6B C5B C9B 122.7(12) . . ? C4B C5B C9B 119.0(13) . . ? C5B C6B C7B 124.4(10) . . ? C5B C6B H6B 117.8 . . ? C7B C6B H6B 117.8 . . ? C2B C7B C6B 116.4(10) . . ? C2B C7B C10B 120.7(9) . . ? C6B C7B C10B 122.7(11) . . ? C3B C8B H8B1 109.5 . . ? C3B C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C3B C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C5B C9B H9B1 109.5 . . ? C5B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C5B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C7B C10B H10D 109.5 . . ? C7B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C7B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C11 O3 La1 157.7(2) . 2 ? C11 O3 La1 90.8(2) . . ? La1 O3 La1 111.24(9) 2 . ? C11 O4 La1 99.2(2) . . ? C21 O5 La1 91.1(2) . . ? C21 O6 La1 96.0(2) . . ? S2B O7 S2A 41.58(19) . . ? S2B O7 La1 156.0(3) . . ? S2A O7 La1 126.68(19) . . ? S1 O8 La1 143.5(2) . . ? O4 C11 O3 121.2(4) . . ? O4 C11 C12 118.3(3) . . ? O3 C11 C12 120.5(3) . . ? C17 C12 C13 120.3(4) . . ? C17 C12 C11 120.8(3) . . ? C13 C12 C11 118.8(3) . . ? C14 C13 C12 118.8(4) . . ? C14 C13 C18 120.0(4) . . ? C12 C13 C18 121.2(4) . . ? C15 C14 C13 121.9(4) . . ? C15 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C14 C15 C16 118.3(4) . . ? C14 C15 C20 120.9(5) . . ? C16 C15 C20 120.8(5) . . ? C15 C16 C17 122.0(4) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C12 C17 C16 118.6(4) . . ? C12 C17 C19 122.0(4) . . ? C16 C17 C19 119.3(4) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C15 C20 H20D 109.5 . . ? H20A C20 H20D 141.1 . . ? H20B C20 H20D 56.3 . . ? H20C C20 H20D 56.3 . . ? C15 C20 H20E 109.5 . . ? H20A C20 H20E 56.3 . . ? H20B C20 H20E 141.1 . . ? H20C C20 H20E 56.3 . . ? H20D C20 H20E 109.5 . . ? C15 C20 H20F 109.5 . . ? H20A C20 H20F 56.3 . . ? H20B C20 H20F 56.3 . . ? H20C C20 H20F 141.1 . . ? H20D C20 H20F 109.5 . . ? H20E C20 H20F 109.5 . . ? O6 C21 O5 121.6(3) . . ? O6 C21 C22 118.4(3) . . ? O5 C21 C22 120.0(3) . . ? C27 C22 C23 120.5(4) . . ? C27 C22 C21 120.3(4) . . ? C23 C22 C21 119.2(4) . . ? C24 C23 C22 117.9(5) . . ? C24 C23 C28 119.7(5) . . ? C22 C23 C28 122.3(4) . . ? C25 C24 C23 123.1(5) . . ? C25 C24 H24 118.4 . . ? C23 C24 H24 118.4 . . ? C24 C25 C26 117.9(5) . . ? C24 C25 C30 118.9(5) . . ? C26 C25 C30 123.2(5) . . ? C25 C26 C27 122.2(5) . . ? C25 C26 H26 118.9 . . ? C27 C26 H26 118.9 . . ? C26 C27 C22 118.3(4) . . ? C26 C27 C29 120.2(4) . . ? C22 C27 C29 121.6(4) . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C25 C30 H30D 109.5 . . ? H30A C30 H30D 141.1 . . ? H30B C30 H30D 56.3 . . ? H30C C30 H30D 56.3 . . ? C25 C30 H30E 109.5 . . ? H30A C30 H30E 56.3 . . ? H30B C30 H30E 141.1 . . ? H30C C30 H30E 56.3 . . ? H30D C30 H30E 109.5 . . ? C25 C30 H30F 109.5 . . ? H30A C30 H30F 56.3 . . ? H30B C30 H30F 56.3 . . ? H30C C30 H30F 141.1 . . ? H30D C30 H30F 109.5 . . ? H30E C30 H30F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.258 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.084 # Attachment '7.CIF' data_hb27dmso _database_code_depnum_ccdc_archive 'CCDC 634376' _audit_creation_method SHELXL-97 _chemical_name_systematic ; poly[(dimethylsulphoxide)tris(4-tert-butylbenzoato)lanthanum(III)] ; _chemical_name_common ;poly((dimethylsulphoxide)tris(4-tert- butylbenzoato)lanthanum(iii)) ; _chemical_melting_point ? _chemical_formula_moiety 'C35 H45 La1 O7 S1' _chemical_formula_sum 'C35 H45 La1 O7 S1' _chemical_formula_weight 748.68 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' 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 22.1543(18) _cell_length_b 16.1425(13) _cell_length_c 9.6019(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.077(3) _cell_angle_gamma 90.00 _cell_volume 3428.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 1.352 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8333 _exptl_absorpt_correction_T_max 0.8546 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _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 44313 _diffrn_reflns_av_R_equivalents 0.0941 _diffrn_reflns_av_sigmaI/netI 0.0687 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5964 _reflns_number_gt 5665 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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. Data shows signs of twinning (large Fc2 vs Fo2) ; _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^)+(0.0000P)^2^+606.8138P] 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 5964 _refine_ls_number_parameters 408 _refine_ls_number_restraints 276 _refine_ls_R_factor_all 0.1913 _refine_ls_R_factor_gt 0.1868 _refine_ls_wR_factor_ref 0.4040 _refine_ls_wR_factor_gt 0.4019 _refine_ls_goodness_of_fit_ref 1.272 _refine_ls_restrained_S_all 1.245 _refine_ls_shift/su_max 0.000 _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 0.42158(6) 0.22752(8) 0.30587(13) 0.0033(4) Uani 1 1 d . . . S1 S 0.5083(3) 0.0351(4) 0.2577(7) 0.0161(13) Uani 1 1 d U . . O1 O 0.5043(8) 0.3267(11) 0.2506(17) 0.017(4) Uani 1 1 d U . . C1 C 0.5141(10) 0.3019(16) 0.128(2) 0.013(5) Uani 1 1 d U . . O2 O 0.4740(6) 0.2582(9) 0.0566(15) 0.005(3) Uani 1 1 d U . . C2 C 0.5786(9) 0.3118(13) 0.076(2) 0.002(4) Uani 1 1 d U . . O3 O 0.3966(7) 0.1126(10) 0.1427(17) 0.013(4) Uani 1 1 d U . . C3 C 0.5952(11) 0.2578(14) -0.034(2) 0.011(5) Uani 1 1 d U . . H3 H 0.5693 0.2158 -0.0729 0.013 Uiso 1 1 calc R . . O4 O 0.3869(8) 0.1443(11) -0.0836(17) 0.014(4) Uani 1 1 d U . . C4 C 0.6525(11) 0.2728(17) -0.079(3) 0.016(5) Uani 1 1 d U . . H4 H 0.6670 0.2366 -0.1481 0.020 Uiso 1 1 calc R . . O5 O 0.3375(7) 0.2779(11) 0.1546(17) 0.013(3) Uani 1 1 d U . . C5 C 0.6909(11) 0.3374(17) -0.031(3) 0.017(5) Uani 1 1 d U . . O6 O 0.3423(8) 0.3317(11) -0.0561(17) 0.014(4) Uani 1 1 d U . . C6 C 0.6724(11) 0.3841(16) 0.078(3) 0.015(5) Uani 1 1 d U . . H6 H 0.6980 0.4266 0.1154 0.018 Uiso 1 1 calc R . . O7 O 0.4952(8) 0.1126(11) 0.3389(19) 0.016(4) Uani 1 1 d U . . C7 C 0.6160(11) 0.3701(15) 0.134(2) 0.012(5) Uani 1 1 d U . . H7 H 0.6042 0.4014 0.2120 0.014 Uiso 1 1 calc R . . C8 C 0.7504(12) 0.3472(17) -0.106(3) 0.021(6) Uani 1 1 d U . . C9 C 0.7358(18) 0.363(3) -0.265(4) 0.050(10) Uani 1 1 d U . . H9A H 0.7736 0.3650 -0.3134 0.075 Uiso 1 1 calc R . . H9B H 0.7143 0.4157 -0.2772 0.075 Uiso 1 1 calc R . . H9C H 0.7104 0.3179 -0.3034 0.075 Uiso 1 1 calc R . . C10 C 0.7901(19) 0.271(3) -0.089(5) 0.063(11) Uani 1 1 d U . . H10A H 0.8307 0.2841 -0.1182 0.094 Uiso 1 1 calc R . . H10B H 0.7728 0.2262 -0.1474 0.094 Uiso 1 1 calc R . . H10C H 0.7924 0.2536 0.0087 0.094 Uiso 1 1 calc R . . C11 C 0.7837(16) 0.422(2) -0.046(4) 0.041(8) Uani 1 1 d U . . H11A H 0.8033 0.4084 0.0449 0.061 Uiso 1 1 calc R . . H11B H 0.7550 0.4678 -0.0348 0.061 Uiso 1 1 calc R . . H11C H 0.8145 0.4398 -0.1097 0.061 Uiso 1 1 calc R . . C12 C 0.3684(11) 0.1124(15) 0.026(3) 0.013(5) Uani 1 1 d U . . C13 C 0.3057(11) 0.0725(15) 0.018(3) 0.011(5) Uani 1 1 d U . . C14 C 0.2898(12) 0.0253(16) 0.125(3) 0.018(5) Uani 1 1 d U . . H14 H 0.3181 0.0148 0.2010 0.021 Uiso 1 1 calc R . . C15 C 0.2300(12) -0.0093(17) 0.125(3) 0.021(6) Uani 1 1 d U . . H15 H 0.2187 -0.0428 0.2005 0.025 Uiso 1 1 calc R . . C16 C 0.1889(11) 0.0061(15) 0.014(2) 0.012(5) Uani 1 1 d U . . C17 C 0.2085(13) 0.0568(17) -0.096(3) 0.024(6) Uani 1 1 d U . . H17 H 0.1810 0.0696 -0.1725 0.028 Uiso 1 1 calc R . . C18 C 0.2657(13) 0.0873(17) -0.094(3) 0.022(6) Uani 1 1 d U . . H18 H 0.2783 0.1191 -0.1705 0.027 Uiso 1 1 calc R . . C19 C 0.1241(13) -0.0208(19) 0.017(3) 0.026(6) Uani 1 1 d U . . C20 C 0.1093(11) -0.0722(16) 0.141(3) 0.015(5) Uani 1 1 d U . . H20A H 0.1383 -0.1179 0.1522 0.022 Uiso 1 1 calc R . . H20B H 0.0683 -0.0947 0.1266 0.022 Uiso 1 1 calc R . . H20C H 0.1116 -0.0377 0.2251 0.022 Uiso 1 1 calc R . . C21 C 0.0835(12) 0.0591(17) 0.018(3) 0.021(6) Uani 1 1 d U . . H21A H 0.0409 0.0430 0.0189 0.031 Uiso 1 1 calc R . . H21B H 0.0898 0.0918 -0.0665 0.031 Uiso 1 1 calc R . . H21C H 0.0946 0.0924 0.1004 0.031 Uiso 1 1 calc R . . C22 C 0.1049(12) -0.0698(17) -0.114(3) 0.021(6) Uani 1 1 d U . . H22A H 0.1263 -0.1230 -0.1126 0.032 Uiso 1 1 calc R . . H22B H 0.1149 -0.0382 -0.1964 0.032 Uiso 1 1 calc R . . H22C H 0.0612 -0.0797 -0.1158 0.032 Uiso 1 1 calc R . . C23 C 0.3139(11) 0.3063(16) 0.042(3) 0.017(5) Uani 1 1 d U . . C24 C 0.2464(10) 0.3148(14) 0.033(2) 0.008(4) Uani 1 1 d U . . C25 C 0.2105(11) 0.2778(16) 0.131(3) 0.018(5) Uani 1 1 d U . . H25 H 0.2292 0.2474 0.2059 0.021 Uiso 1 1 calc R . . C26 C 0.1464(11) 0.2849(16) 0.120(3) 0.017(5) Uani 1 1 d U . . H26 H 0.1223 0.2577 0.1847 0.020 Uiso 1 1 calc R . . C27 C 0.1193(12) 0.3323(16) 0.012(3) 0.016(5) Uani 1 1 d U . . C28 C 0.1536(11) 0.3648(15) -0.090(3) 0.013(5) Uani 1 1 d U . . H28 H 0.1346 0.3901 -0.1698 0.016 Uiso 1 1 calc R . . C29 C 0.2183(13) 0.3604(18) -0.075(3) 0.023(6) Uani 1 1 d U . . H29 H 0.2421 0.3888 -0.1388 0.028 Uiso 1 1 calc R . . C30 C 0.0484(10) 0.3424(15) 0.006(2) 0.011(5) Uani 1 1 d U . . C31 C 0.0309(19) 0.388(3) 0.134(4) 0.056(11) Uani 1 1 d U . . H31A H 0.0477 0.4438 0.1333 0.084 Uiso 1 1 calc R . . H31B H 0.0468 0.3580 0.2169 0.084 Uiso 1 1 calc R . . H31C H -0.0133 0.3906 0.1343 0.084 Uiso 1 1 calc R . . C32 C 0.0181(15) 0.255(2) 0.009(4) 0.042(8) Uani 1 1 d U . . H32A H 0.0328 0.2254 0.0931 0.063 Uiso 1 1 calc R . . H32B H 0.0282 0.2237 -0.0738 0.063 Uiso 1 1 calc R . . H32C H -0.0259 0.2616 0.0099 0.063 Uiso 1 1 calc R . . C33 C 0.026(2) 0.387(3) -0.127(4) 0.060(11) Uani 1 1 d U . . H33A H -0.0125 0.4149 -0.1110 0.090 Uiso 1 1 calc R . . H33B H 0.0195 0.3465 -0.2026 0.090 Uiso 1 1 calc R . . H33C H 0.0558 0.4279 -0.1530 0.090 Uiso 1 1 calc R . . C34 C 0.5728(11) -0.0086(16) 0.350(3) 0.017(5) Uani 1 1 d U . . H34A H 0.5978 -0.0375 0.2848 0.025 Uiso 1 1 calc R . . H34B H 0.5594 -0.0479 0.4202 0.025 Uiso 1 1 calc R . . H34C H 0.5964 0.0357 0.3971 0.025 Uiso 1 1 calc R . . C35 C 0.5464(13) 0.0714(18) 0.109(3) 0.024(6) Uani 1 1 d U . . H35A H 0.5225 0.1154 0.0622 0.036 Uiso 1 1 calc R . . H35B H 0.5512 0.0254 0.0435 0.036 Uiso 1 1 calc R . . H35C H 0.5863 0.0930 0.1391 0.036 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 0.0045(6) 0.0030(6) 0.0025(6) 0.0013(5) -0.0003(4) 0.0000(5) S1 0.019(3) 0.004(3) 0.024(3) -0.004(2) -0.005(3) -0.006(2) O1 0.019(7) 0.023(7) 0.009(6) 0.003(6) -0.002(6) -0.006(6) C1 0.009(8) 0.017(9) 0.011(8) 0.000(7) -0.001(7) 0.001(7) O2 0.005(3) 0.005(3) 0.005(3) 0.0000(10) 0.0001(10) 0.0000(10) C2 0.003(4) 0.002(4) 0.002(4) 0.0000(10) 0.0000(10) 0.0000(10) O3 0.013(4) 0.013(4) 0.013(4) 0.0000(10) 0.0006(10) -0.0002(10) C3 0.014(8) 0.006(8) 0.012(8) 0.004(7) -0.002(7) -0.001(7) O4 0.016(7) 0.015(7) 0.011(7) 0.003(6) 0.000(6) -0.008(6) C4 0.014(8) 0.015(9) 0.020(9) 0.003(8) -0.001(7) 0.005(7) O5 0.008(6) 0.016(7) 0.016(7) -0.003(6) -0.002(5) 0.008(6) C5 0.013(8) 0.019(9) 0.018(9) -0.002(7) 0.000(7) 0.002(7) O6 0.015(7) 0.014(7) 0.012(7) 0.000(6) 0.002(6) 0.007(6) C6 0.016(8) 0.014(9) 0.015(8) -0.001(7) 0.004(7) -0.002(7) O7 0.012(7) 0.011(7) 0.024(7) -0.006(6) -0.004(6) 0.009(6) C7 0.015(8) 0.013(8) 0.008(8) 0.002(7) -0.001(7) -0.003(7) C8 0.022(9) 0.020(9) 0.022(9) -0.002(8) 0.003(8) -0.006(8) C9 0.045(12) 0.051(12) 0.054(12) -0.001(9) 0.003(9) -0.006(9) C10 0.058(13) 0.060(14) 0.069(14) 0.002(9) 0.003(9) 0.001(9) C11 0.042(11) 0.043(11) 0.038(11) -0.006(9) 0.005(9) -0.005(9) C12 0.015(8) 0.011(8) 0.012(8) 0.000(7) -0.002(7) -0.001(7) C13 0.011(8) 0.008(8) 0.016(8) -0.001(7) -0.002(7) 0.001(7) C14 0.017(9) 0.018(9) 0.017(9) 0.000(7) -0.009(7) -0.005(7) C15 0.020(9) 0.019(9) 0.023(9) 0.001(8) 0.004(8) -0.004(7) C16 0.010(8) 0.014(8) 0.012(8) 0.003(7) 0.000(7) 0.000(7) C17 0.025(9) 0.019(9) 0.027(9) 0.000(8) 0.002(8) -0.003(8) C18 0.025(9) 0.020(9) 0.022(9) 0.004(8) 0.001(8) 0.001(8) C19 0.023(9) 0.027(10) 0.029(10) -0.007(8) 0.000(8) -0.002(8) C20 0.014(8) 0.015(9) 0.014(8) 0.000(7) 0.001(7) 0.001(7) C21 0.019(9) 0.022(9) 0.022(9) -0.005(8) 0.000(7) 0.000(8) C22 0.019(9) 0.021(9) 0.024(9) -0.004(8) 0.006(8) 0.001(8) C23 0.017(9) 0.012(8) 0.022(9) -0.002(7) 0.002(7) 0.000(7) C24 0.011(8) 0.005(8) 0.007(8) -0.003(7) -0.003(7) -0.001(7) C25 0.018(8) 0.015(9) 0.021(9) 0.002(7) -0.001(7) 0.003(7) C26 0.014(8) 0.017(9) 0.018(9) -0.005(7) -0.007(7) -0.004(7) C27 0.018(9) 0.014(9) 0.015(8) 0.001(7) -0.003(7) 0.004(7) C28 0.013(8) 0.014(8) 0.012(8) 0.004(7) -0.003(7) 0.004(7) C29 0.022(9) 0.021(9) 0.027(9) -0.002(8) 0.007(8) 0.003(8) C30 0.009(8) 0.015(8) 0.011(8) 0.000(7) 0.003(7) 0.002(7) C31 0.052(13) 0.061(13) 0.055(13) -0.009(9) -0.001(9) 0.004(9) C32 0.035(11) 0.039(12) 0.052(12) 0.000(9) -0.002(9) 0.000(8) C33 0.056(13) 0.065(14) 0.058(14) 0.008(9) 0.003(9) 0.004(9) C34 0.020(9) 0.010(8) 0.021(9) -0.002(7) 0.001(7) -0.003(7) C35 0.025(9) 0.022(9) 0.026(9) 0.003(8) 0.001(8) 0.001(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O5 2.439(15) . ? La1 O6 2.451(16) 4_566 ? La1 O4 2.467(16) 4_566 ? La1 O3 2.472(17) . ? La1 O7 2.478(16) . ? La1 O1 2.512(17) . ? La1 O2 2.626(14) 4_566 ? La1 O2 2.762(14) . ? La1 C1 2.99(2) . ? S1 O7 1.511(17) . ? S1 C34 1.79(3) . ? S1 C35 1.80(3) . ? O1 C1 1.27(3) . ? C1 O2 1.30(3) . ? C1 C2 1.55(3) . ? O2 La1 2.626(14) 4_565 ? C2 C7 1.35(3) . ? C2 C3 1.44(3) . ? O3 C12 1.26(3) . ? C3 C4 1.38(3) . ? C3 H3 0.9500 . ? O4 C12 1.26(3) . ? O4 La1 2.467(16) 4_565 ? C4 C5 1.41(4) . ? C4 H4 0.9500 . ? O5 C23 1.26(3) . ? C5 C6 1.37(4) . ? C5 C8 1.54(4) . ? O6 C23 1.23(3) . ? O6 La1 2.451(16) 4_565 ? C6 C7 1.41(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C10 1.51(5) . ? C8 C11 1.52(4) . ? C8 C9 1.57(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.53(3) . ? C13 C14 1.34(4) . ? C13 C18 1.38(4) . ? C14 C15 1.44(4) . ? C14 H14 0.9500 . ? C15 C16 1.38(4) . ? C15 H15 0.9500 . ? C16 C17 1.42(4) . ? C16 C19 1.50(4) . ? C17 C18 1.36(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.50(4) . ? C19 C22 1.53(4) . ? C19 C21 1.57(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.50(3) . ? C24 C29 1.39(4) . ? C24 C25 1.40(3) . ? C25 C26 1.42(3) . ? C25 H25 0.9500 . ? C26 C27 1.40(4) . ? C26 H26 0.9500 . ? C27 C28 1.37(4) . ? C27 C30 1.58(3) . ? C28 C29 1.43(4) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.50(4) . ? C30 C33 1.53(5) . ? C30 C32 1.56(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? 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 O5 La1 O6 84.6(6) . 4_566 ? O5 La1 O4 74.4(6) . 4_566 ? O6 La1 O4 81.1(6) 4_566 4_566 ? O5 La1 O3 74.6(6) . . ? O6 La1 O3 84.7(5) 4_566 . ? O4 La1 O3 146.9(6) 4_566 . ? O5 La1 O7 143.3(6) . . ? O6 La1 O7 97.1(6) 4_566 . ? O4 La1 O7 142.3(6) 4_566 . ? O3 La1 O7 69.0(6) . . ? O5 La1 O1 101.8(6) . . ? O6 La1 O1 156.2(6) 4_566 . ? O4 La1 O1 78.7(6) 4_566 . ? O3 La1 O1 119.0(6) . . ? O7 La1 O1 91.2(6) . . ? O5 La1 O2 143.4(5) . 4_566 ? O6 La1 O2 80.4(5) 4_566 4_566 ? O4 La1 O2 70.4(5) 4_566 4_566 ? O3 La1 O2 136.0(5) . 4_566 ? O7 La1 O2 72.1(5) . 4_566 ? O1 La1 O2 81.1(5) . 4_566 ? O5 La1 O2 76.5(5) . . ? O6 La1 O2 152.4(5) 4_566 . ? O4 La1 O2 112.2(5) 4_566 . ? O3 La1 O2 71.1(5) . . ? O7 La1 O2 86.6(5) . . ? O1 La1 O2 49.9(5) . . ? O2 La1 O2 126.4(5) 4_566 . ? O5 La1 C1 92.9(6) . . ? O6 La1 C1 177.5(6) 4_566 . ? O4 La1 C1 98.5(6) 4_566 . ? O3 La1 C1 94.3(6) . . ? O7 La1 C1 84.7(6) . . ? O1 La1 C1 24.9(6) . . ? O2 La1 C1 101.9(5) 4_566 . ? O2 La1 C1 25.7(5) . . ? O7 S1 C34 104.0(11) . . ? O7 S1 C35 104.6(12) . . ? C34 S1 C35 97.3(13) . . ? C1 O1 La1 99.0(15) . . ? O1 C1 O2 121(2) . . ? O1 C1 C2 118(2) . . ? O2 C1 C2 120(2) . . ? O1 C1 La1 56.1(12) . . ? O2 C1 La1 67.3(12) . . ? C2 C1 La1 154.0(15) . . ? C1 O2 La1 133.8(14) . 4_565 ? C1 O2 La1 87.0(12) . . ? La1 O2 La1 128.6(5) 4_565 . ? C7 C2 C3 123(2) . . ? C7 C2 C1 120(2) . . ? C3 C2 C1 116.8(19) . . ? C12 O3 La1 130.7(15) . . ? C4 C3 C2 114(2) . . ? C4 C3 H3 123.2 . . ? C2 C3 H3 123.2 . . ? C12 O4 La1 145.6(16) . 4_565 ? C3 C4 C5 125(2) . . ? C3 C4 H4 117.5 . . ? C5 C4 H4 117.5 . . ? C23 O5 La1 154.2(16) . . ? C6 C5 C4 117(2) . . ? C6 C5 C8 127(2) . . ? C4 C5 C8 116(2) . . ? C23 O6 La1 134.0(16) . 4_565 ? C5 C6 C7 121(2) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? S1 O7 La1 134.3(10) . . ? C2 C7 C6 119(2) . . ? C2 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C10 C8 C11 110(3) . . ? C10 C8 C5 112(3) . . ? C11 C8 C5 109(2) . . ? C10 C8 C9 109(3) . . ? C11 C8 C9 108(3) . . ? C5 C8 C9 109(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O4 C12 O3 125(2) . . ? O4 C12 C13 118(2) . . ? O3 C12 C13 117(2) . . ? C14 C13 C18 121(2) . . ? C14 C13 C12 118(2) . . ? C18 C13 C12 121(2) . . ? C13 C14 C15 120(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120(2) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 117(2) . . ? C15 C16 C19 122(2) . . ? C17 C16 C19 121(2) . . ? C18 C17 C16 121(3) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C13 121(3) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? C20 C19 C16 115(2) . . ? C20 C19 C22 108(2) . . ? C16 C19 C22 111(2) . . ? C20 C19 C21 108(2) . . ? C16 C19 C21 108(2) . . ? C22 C19 C21 107(2) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O6 C23 O5 125(2) . . ? O6 C23 C24 118(2) . . ? O5 C23 C24 117(2) . . ? C29 C24 C25 119(2) . . ? C29 C24 C23 120(2) . . ? C25 C24 C23 122(2) . . ? C24 C25 C26 121(2) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C27 C26 C25 119(2) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C28 C27 C26 120(2) . . ? C28 C27 C30 122(2) . . ? C26 C27 C30 118(2) . . ? C27 C28 C29 120(2) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C24 C29 C28 120(2) . . ? C24 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C33 112(3) . . ? C31 C30 C32 107(3) . . ? C33 C30 C32 109(3) . . ? C31 C30 C27 109(2) . . ? C33 C30 C27 111(2) . . ? C32 C30 C27 110(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? S1 C34 H34A 109.5 . . ? S1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? S1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? S1 C35 H35A 109.5 . . ? S1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? S1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 9.596 _refine_diff_density_min -10.993 _refine_diff_density_rms 0.433 # Attachment '8.CIF' data_HB12DMF _database_code_depnum_ccdc_archive 'CCDC 634377' _audit_creation_method SHELXL-97 _chemical_name_systematic ; poly[(dimethylformamide)tris(2-aminomethylbenzoato)lanthanum(III)] DMF solvate ; _chemical_name_common ;poly((dimethylformamide)tris(2- aminomethylbenzoato)lanthanum(iii)) DMF solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C27 H31 La1 N4 O7, C3 H7 N1 O1' _chemical_formula_sum 'C30 H38 La N5 O8' _chemical_formula_weight 735.56 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 24.9553(11) _cell_length_b 8.0474(3) _cell_length_c 30.6790(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6161.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _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 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 1.445 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8690 _exptl_absorpt_correction_T_max 0.8932 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD' _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 28375 _diffrn_reflns_av_R_equivalents 0.1335 _diffrn_reflns_av_sigmaI/netI 0.0976 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5416 _reflns_number_gt 4708 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0000P)^2^+205.9680P] 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 SHELXL _refine_ls_extinction_coef 0.0044(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5416 _refine_ls_number_parameters 405 _refine_ls_number_restraints 258 _refine_ls_R_factor_all 0.1490 _refine_ls_R_factor_gt 0.1324 _refine_ls_wR_factor_ref 0.2389 _refine_ls_wR_factor_gt 0.2328 _refine_ls_goodness_of_fit_ref 1.468 _refine_ls_restrained_S_all 1.432 _refine_ls_shift/su_max 0.000 _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 0.27562(3) 0.42946(10) 0.11156(3) 0.0063(3) Uani 1 1 d . . . O1 O 0.3324(4) 0.6164(12) 0.1671(3) 0.008(2) Uani 1 1 d U . . N1 N 0.4202(6) 0.7210(17) 0.2096(4) 0.019(3) Uani 1 1 d U . . H1 H 0.3945 0.6459 0.2088 0.023 Uiso 1 1 calc R . . C1 C 0.3409(5) 0.7233(16) 0.1391(4) 0.003(3) Uani 1 1 d U . . O2 O 0.3063(3) 0.7464(11) 0.1061(3) 0.0029(19) Uani 1 1 d U . . N2 N 0.2311(5) 0.4643(15) -0.0555(4) 0.016(3) Uani 1 1 d U . . H2 H 0.2533 0.4335 -0.0348 0.019 Uiso 1 1 calc R . . C2 C 0.3914(6) 0.8247(17) 0.1379(5) 0.007(3) Uani 1 1 d U . . O3 O 0.2509(4) 0.4708(11) 0.0311(3) 0.006(2) Uani 1 1 d U . . N3 N 0.1970(5) 0.3340(16) 0.2526(5) 0.016(3) Uani 1 1 d U . . H3 H 0.2105 0.3247 0.2262 0.019 Uiso 1 1 calc R . . C3 C 0.4292(6) 0.815(2) 0.1727(5) 0.016(3) Uani 1 1 d U . . O4 O 0.2086(4) 0.6480(12) 0.0719(3) 0.008(2) Uani 1 1 d U . . N4 N 0.4601(5) 0.4450(16) 0.1249(4) 0.012(3) Uani 1 1 d U . . C4 C 0.4771(6) 0.9055(19) 0.1691(5) 0.015(3) Uani 1 1 d U . . H4 H 0.5029 0.9018 0.1918 0.018 Uiso 1 1 calc R . . O5 O 0.2179(4) 0.4809(11) 0.1760(3) 0.008(2) Uani 1 1 d U . . N5 N 0.1079(5) 0.2862(17) 0.4669(4) 0.015(3) Uani 1 1 d U . . C5 C 0.4865(7) 1.002(2) 0.1318(6) 0.022(4) Uani 1 1 d U . . H5 H 0.5192 1.0617 0.1295 0.026 Uiso 1 1 calc R . . O6 O 0.1929(4) 0.7373(13) 0.1668(3) 0.011(2) Uani 1 1 d U . . C6 C 0.4497(6) 1.0109(19) 0.0985(5) 0.013(3) Uani 1 1 d U . . H6 H 0.4569 1.0760 0.0733 0.016 Uiso 1 1 calc R . . O7 O 0.3764(4) 0.4208(13) 0.0983(3) 0.006(2) Uani 1 1 d U . . C7 C 0.4016(6) 0.924(2) 0.1022(5) 0.014(3) Uani 1 1 d U . . H7 H 0.3755 0.9324 0.0798 0.017 Uiso 1 1 calc R . . O8 O 0.0987(5) 0.2820(16) 0.3937(4) 0.034(3) Uani 1 1 d U . . C8 C 0.4503(8) 0.739(3) 0.2489(6) 0.033(5) Uani 1 1 d U . . H8A H 0.4847 0.6818 0.2459 0.050 Uiso 1 1 calc R . . H8B H 0.4302 0.6910 0.2732 0.050 Uiso 1 1 calc R . . H8C H 0.4566 0.8575 0.2545 0.050 Uiso 1 1 calc R . . C9 C 0.2152(5) 0.5794(19) 0.0359(4) 0.010(3) Uani 1 1 d U . . C10 C 0.1797(6) 0.6192(16) -0.0010(4) 0.006(3) Uani 1 1 d U . . C11 C 0.1879(6) 0.560(2) -0.0448(5) 0.016(3) Uani 1 1 d U . . C12 C 0.1506(6) 0.6067(17) -0.0768(5) 0.007(3) Uani 1 1 d U . . H12 H 0.1559 0.5714 -0.1061 0.009 Uiso 1 1 calc R . . C13 C 0.1061(6) 0.704(2) -0.0666(5) 0.017(3) Uani 1 1 d U . . H13 H 0.0809 0.7305 -0.0887 0.020 Uiso 1 1 calc R . . C14 C 0.0982(6) 0.762(2) -0.0248(5) 0.015(3) Uani 1 1 d U . . H14 H 0.0683 0.8306 -0.0182 0.018 Uiso 1 1 calc R . . C15 C 0.1347(6) 0.7196(19) 0.0074(5) 0.010(3) Uani 1 1 d U . . H15 H 0.1291 0.7595 0.0362 0.012 Uiso 1 1 calc R . . C16 C 0.2416(6) 0.412(2) -0.0997(5) 0.020(4) Uani 1 1 d U . . H16A H 0.2122 0.3415 -0.1100 0.029 Uiso 1 1 calc R . . H16B H 0.2752 0.3485 -0.1005 0.029 Uiso 1 1 calc R . . H16C H 0.2448 0.5095 -0.1185 0.029 Uiso 1 1 calc R . . C17 C 0.1968(6) 0.6128(18) 0.1890(5) 0.009(3) Uani 1 1 d U . . C18 C 0.1716(7) 0.614(2) 0.2347(5) 0.017(4) Uani 1 1 d U . . C19 C 0.1729(6) 0.4780(17) 0.2634(5) 0.009(3) Uani 1 1 d U . . C20 C 0.1496(7) 0.498(2) 0.3042(6) 0.021(4) Uani 1 1 d U . . H20 H 0.1494 0.4081 0.3242 0.025 Uiso 1 1 calc R . . C21 C 0.1271(7) 0.646(2) 0.3156(6) 0.027(4) Uani 1 1 d U . . H21 H 0.1130 0.6566 0.3442 0.033 Uiso 1 1 calc R . . C22 C 0.1235(7) 0.780(2) 0.2879(6) 0.021(4) Uani 1 1 d U . . H22 H 0.1059 0.8794 0.2965 0.026 Uiso 1 1 calc R . . C23 C 0.1473(6) 0.763(2) 0.2462(5) 0.015(3) Uani 1 1 d U . . H23 H 0.1467 0.8535 0.2262 0.018 Uiso 1 1 calc R . . C24 C 0.2019(8) 0.192(3) 0.2822(7) 0.039(5) Uani 1 1 d U . . H24A H 0.2283 0.2172 0.3049 0.058 Uiso 1 1 calc R . . H24B H 0.2136 0.0940 0.2657 0.058 Uiso 1 1 calc R . . H24C H 0.1671 0.1691 0.2957 0.058 Uiso 1 1 calc R . . C25 C 0.4103(5) 0.3969(15) 0.1258(4) 0.001(3) Uani 1 1 d U . . H25 H 0.3993 0.3362 0.1508 0.001 Uiso 1 1 calc R . . C26 C 0.4807(7) 0.530(2) 0.0865(5) 0.018(4) Uani 1 1 d U . . H26A H 0.4582 0.5030 0.0613 0.026 Uiso 1 1 calc R . . H26B H 0.5175 0.4940 0.0809 0.026 Uiso 1 1 calc R . . H26C H 0.4801 0.6503 0.0914 0.026 Uiso 1 1 calc R . . C27 C 0.4957(6) 0.419(2) 0.1625(5) 0.020(3) Uani 1 1 d U . . H27A H 0.4769 0.3543 0.1848 0.031 Uiso 1 1 calc R . . H27B H 0.5063 0.5268 0.1746 0.031 Uiso 1 1 calc R . . H27C H 0.5277 0.3584 0.1530 0.031 Uiso 1 1 calc R . . C28 C 0.1243(7) 0.323(2) 0.4270(5) 0.020(4) Uani 1 1 d U . . H28 H 0.1568 0.3834 0.4235 0.024 Uiso 1 1 calc R . . C29 C 0.0607(7) 0.186(2) 0.4754(6) 0.023(4) Uani 1 1 d U . . H29A H 0.0380 0.2427 0.4970 0.035 Uiso 1 1 calc R . . H29B H 0.0715 0.0776 0.4868 0.035 Uiso 1 1 calc R . . H29C H 0.0405 0.1713 0.4483 0.035 Uiso 1 1 calc R . . C30 C 0.1438(7) 0.328(2) 0.5029(6) 0.025(4) Uani 1 1 d U . . H30A H 0.1600 0.2264 0.5144 0.037 Uiso 1 1 calc R . . H30B H 0.1234 0.3835 0.5260 0.037 Uiso 1 1 calc R . . H30C H 0.1720 0.4028 0.4924 0.037 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 0.0058(4) 0.0060(4) 0.0070(4) 0.0011(3) -0.0001(3) -0.0004(4) O1 0.008(2) 0.008(2) 0.008(2) 0.0001(10) 0.0001(10) 0.0001(10) N1 0.019(3) 0.019(3) 0.019(3) 0.0000(10) -0.0003(10) -0.0002(10) C1 0.003(3) 0.003(3) 0.003(3) -0.0001(10) 0.0003(10) -0.0001(10) O2 0.002(2) 0.003(2) 0.003(2) 0.0000(10) 0.0003(10) -0.0002(10) N2 0.016(3) 0.016(3) 0.016(3) -0.0003(10) 0.0000(10) 0.0002(10) C2 0.007(3) 0.007(3) 0.007(3) -0.0005(10) 0.0000(10) -0.0001(10) O3 0.006(2) 0.006(2) 0.006(2) 0.0001(10) 0.0000(10) -0.0001(10) N3 0.016(3) 0.016(3) 0.015(3) 0.0002(10) 0.0000(10) -0.0001(10) C3 0.016(3) 0.015(3) 0.016(3) -0.0001(10) -0.0002(10) 0.0001(10) O4 0.008(2) 0.008(2) 0.008(2) 0.0003(10) -0.0001(10) 0.0000(10) N4 0.012(3) 0.012(3) 0.012(3) -0.0002(10) -0.0003(10) 0.0002(10) C4 0.015(3) 0.015(3) 0.015(3) -0.0001(10) -0.0001(10) 0.0001(10) O5 0.008(2) 0.008(2) 0.008(2) 0.0006(10) 0.0004(10) -0.0003(10) N5 0.015(3) 0.015(3) 0.015(3) 0.0002(10) 0.0000(10) 0.0001(10) C5 0.021(4) 0.022(4) 0.022(4) -0.0002(10) -0.0001(10) 0.0001(10) O6 0.011(2) 0.011(2) 0.011(2) 0.0003(10) -0.0003(10) 0.0000(10) C6 0.013(3) 0.013(3) 0.013(3) 0.0002(10) 0.0000(10) 0.0000(10) O7 0.006(2) 0.006(2) 0.007(2) 0.0004(10) 0.0000(10) 0.0003(10) C7 0.014(3) 0.014(3) 0.014(3) -0.0002(10) -0.0002(10) 0.0001(10) O8 0.034(3) 0.034(3) 0.034(3) 0.0003(10) -0.0001(10) 0.0001(10) C8 0.033(5) 0.033(5) 0.033(5) 0.0000(10) 0.0000(10) 0.0000(10) C9 0.010(3) 0.010(3) 0.010(3) 0.0000(10) 0.0001(10) 0.0001(10) C10 0.006(3) 0.006(3) 0.006(3) -0.0001(10) -0.0003(10) -0.0001(10) C11 0.016(3) 0.016(3) 0.016(3) 0.0000(10) 0.0000(10) 0.0000(10) C12 0.008(3) 0.007(3) 0.007(3) 0.0000(10) 0.0000(10) 0.0001(10) C13 0.017(4) 0.017(4) 0.017(4) 0.0002(10) -0.0001(10) -0.0003(10) C14 0.015(3) 0.015(3) 0.015(3) 0.0001(10) 0.0000(10) -0.0001(10) C15 0.010(3) 0.010(3) 0.010(3) 0.0000(10) 0.0000(10) 0.0001(10) C16 0.020(4) 0.020(4) 0.019(4) -0.0001(10) 0.0002(10) -0.0001(10) C17 0.009(3) 0.009(3) 0.010(3) 0.0003(10) -0.0001(10) -0.0002(10) C18 0.017(4) 0.017(4) 0.017(4) -0.0002(10) 0.0001(10) -0.0002(10) C19 0.010(3) 0.009(3) 0.009(3) 0.0002(10) 0.0000(10) -0.0001(10) C20 0.021(4) 0.021(4) 0.021(4) 0.0002(10) 0.0002(10) -0.0002(10) C21 0.027(4) 0.027(4) 0.027(4) -0.0003(10) 0.0003(10) -0.0002(10) C22 0.021(4) 0.021(4) 0.021(4) -0.0001(10) 0.0003(10) -0.0001(10) C23 0.015(3) 0.015(3) 0.015(3) -0.0001(10) 0.0001(10) -0.0001(10) C24 0.039(5) 0.039(5) 0.039(5) 0.0001(10) 0.0000(10) 0.0000(10) C25 0.001(3) 0.001(3) 0.001(3) 0.0001(10) 0.0000(10) 0.0001(10) C26 0.018(4) 0.018(4) 0.018(4) 0.0002(10) -0.0001(10) 0.0000(10) C27 0.020(4) 0.020(4) 0.021(4) -0.0001(10) -0.0002(10) 0.0002(10) C28 0.020(4) 0.020(4) 0.020(4) 0.0000(10) 0.0000(10) 0.0001(10) C29 0.023(4) 0.024(4) 0.023(4) 0.0000(10) -0.0001(10) 0.0000(10) C30 0.025(4) 0.025(4) 0.025(4) 0.0001(10) -0.0001(10) 0.0001(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O6 2.424(10) 7_655 ? La1 O5 2.481(9) . ? La1 O2 2.526(9) 7_655 ? La1 O7 2.549(9) . ? La1 O3 2.566(9) . ? La1 O4 2.601(10) 7_655 ? La1 O2 2.668(9) . ? La1 O1 2.679(10) . ? La1 O4 2.715(10) . ? La1 C1 2.993(13) . ? La1 C9 3.019(14) . ? La1 La1 4.2220(5) 7_655 ? O1 C1 1.234(16) . ? N1 C3 1.38(2) . ? N1 C8 1.43(2) . ? N1 H1 0.8800 . ? C1 O2 1.342(16) . ? C1 C2 1.503(19) . ? O2 La1 2.526(9) 7_665 ? N2 C11 1.36(2) . ? N2 C16 1.444(19) . ? N2 H2 0.8800 . ? C2 C7 1.38(2) . ? C2 C3 1.43(2) . ? O3 C9 1.258(17) . ? N3 C19 1.345(19) . ? N3 C24 1.47(2) . ? N3 H3 0.8800 . ? C3 C4 1.40(2) . ? O4 C9 1.244(17) . ? O4 La1 2.601(10) 7_665 ? N4 C25 1.303(17) . ? N4 C26 1.457(19) . ? N4 C27 1.469(19) . ? C4 C5 1.40(2) . ? C4 H4 0.9500 . ? O5 C17 1.250(17) . ? N5 C28 1.33(2) . ? N5 C29 1.45(2) . ? N5 C30 1.46(2) . ? C5 C6 1.38(2) . ? C5 H5 0.9500 . ? O6 C17 1.215(17) . ? O6 La1 2.424(10) 7_665 ? C6 C7 1.40(2) . ? C6 H6 0.9500 . ? O7 C25 1.209(15) . ? C7 H7 0.9500 . ? O8 C28 1.25(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.472(19) . ? C10 C15 1.41(2) . ? C10 C11 1.44(2) . ? C11 C12 1.40(2) . ? C12 C13 1.39(2) . ? C12 H12 0.9500 . ? C13 C14 1.38(2) . ? C13 H13 0.9500 . ? C14 C15 1.39(2) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.54(2) . ? C18 C23 1.39(2) . ? C18 C19 1.40(2) . ? C19 C20 1.39(2) . ? C20 C21 1.36(2) . ? C20 H20 0.9500 . ? C21 C22 1.38(2) . ? C21 H21 0.9500 . ? C22 C23 1.42(2) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? 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 La1 O5 74.8(3) 7_655 . ? O6 La1 O2 86.4(3) 7_655 7_655 ? O5 La1 O2 71.4(3) . 7_655 ? O6 La1 O7 77.0(3) 7_655 . ? O5 La1 O7 134.8(3) . . ? O2 La1 O7 140.6(3) 7_655 . ? O6 La1 O3 146.4(3) 7_655 . ? O5 La1 O3 127.3(3) . . ? O2 La1 O3 79.5(3) 7_655 . ? O7 La1 O3 95.0(3) . . ? O6 La1 O4 73.9(3) 7_655 7_655 ? O5 La1 O4 127.3(3) . 7_655 ? O2 La1 O4 65.4(3) 7_655 7_655 ? O7 La1 O4 75.7(3) . 7_655 ? O3 La1 O4 72.5(3) . 7_655 ? O6 La1 O2 124.1(3) 7_655 . ? O5 La1 O2 93.3(3) . . ? O2 La1 O2 141.8(2) 7_655 . ? O7 La1 O2 74.5(3) . . ? O3 La1 O2 83.4(3) . . ? O4 La1 O2 139.4(3) 7_655 . ? O6 La1 O1 75.1(3) 7_655 . ? O5 La1 O1 72.9(3) . . ? O2 La1 O1 143.0(3) 7_655 . ? O7 La1 O1 66.1(3) . . ? O3 La1 O1 131.8(3) . . ? O4 La1 O1 135.0(3) 7_655 . ? O2 La1 O1 49.5(3) . . ? O6 La1 O4 157.8(3) 7_655 . ? O5 La1 O4 83.8(3) . . ? O2 La1 O4 81.3(3) 7_655 . ? O7 La1 O4 123.6(3) . . ? O3 La1 O4 48.5(3) . . ? O4 La1 O4 116.6(3) 7_655 . ? O2 La1 O4 61.9(3) . . ? O1 La1 O4 104.3(3) . . ? O6 La1 C1 97.5(4) 7_655 . ? O5 La1 C1 87.7(3) . . ? O2 La1 C1 156.9(3) 7_655 . ? O7 La1 C1 61.9(3) . . ? O3 La1 C1 107.4(3) . . ? O4 La1 C1 137.5(3) 7_655 . ? O2 La1 C1 26.6(3) . . ? O1 La1 C1 24.3(3) . . ? O4 La1 C1 87.1(3) . . ? O6 La1 C9 162.5(4) 7_655 . ? O5 La1 C9 104.8(3) . . ? O2 La1 C9 77.2(3) 7_655 . ? O7 La1 C9 112.4(3) . . ? O3 La1 C9 24.3(3) . . ? O4 La1 C9 93.7(4) 7_655 . ? O2 La1 C9 73.3(3) . . ? O1 La1 C9 121.9(3) . . ? O4 La1 C9 24.3(3) . . ? C1 La1 C9 99.9(4) . . ? O6 La1 La1 59.4(2) 7_655 7_655 ? O5 La1 La1 89.0(2) . 7_655 ? O2 La1 La1 36.8(2) 7_655 7_655 ? O7 La1 La1 105.8(2) . 7_655 ? O3 La1 La1 92.9(2) . 7_655 ? O4 La1 La1 38.4(2) 7_655 7_655 ? O2 La1 La1 176.3(2) . 7_655 ? O1 La1 La1 134.1(2) . 7_655 ? O4 La1 La1 115.5(2) . 7_655 ? C1 La1 La1 156.6(3) . 7_655 ? C9 La1 La1 103.3(3) . 7_655 ? C1 O1 La1 92.2(8) . . ? C3 N1 C8 123.3(15) . . ? C3 N1 H1 118.3 . . ? C8 N1 H1 118.3 . . ? O1 C1 O2 120.8(12) . . ? O1 C1 C2 122.5(12) . . ? O2 C1 C2 116.6(11) . . ? O1 C1 La1 63.4(7) . . ? O2 C1 La1 63.1(6) . . ? C2 C1 La1 151.6(9) . . ? C1 O2 La1 123.5(8) . 7_665 ? C1 O2 La1 90.3(7) . . ? La1 O2 La1 108.7(3) 7_665 . ? C11 N2 C16 122.4(13) . . ? C11 N2 H2 118.8 . . ? C16 N2 H2 118.8 . . ? C7 C2 C3 120.3(13) . . ? C7 C2 C1 119.1(13) . . ? C3 C2 C1 120.5(13) . . ? C9 O3 La1 98.4(8) . . ? C19 N3 C24 123.9(15) . . ? C19 N3 H3 118.0 . . ? C24 N3 H3 118.0 . . ? N1 C3 C4 119.2(14) . . ? N1 C3 C2 122.4(14) . . ? C4 C3 C2 118.4(14) . . ? C9 O4 La1 141.4(9) . 7_665 ? C9 O4 La1 91.7(8) . . ? La1 O4 La1 105.1(3) 7_665 . ? C25 N4 C26 119.5(12) . . ? C25 N4 C27 121.3(12) . . ? C26 N4 C27 119.2(12) . . ? C5 C4 C3 119.5(15) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C17 O5 La1 129.8(9) . . ? C28 N5 C29 122.8(14) . . ? C28 N5 C30 117.2(14) . . ? C29 N5 C30 119.3(13) . . ? C6 C5 C4 121.7(16) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C17 O6 La1 153.1(10) . 7_665 ? C5 C6 C7 119.1(15) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C25 O7 La1 125.6(8) . . ? C2 C7 C6 120.9(14) . . ? C2 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O4 C9 O3 120.4(13) . . ? O4 C9 C10 120.4(13) . . ? O3 C9 C10 119.1(12) . . ? O4 C9 La1 64.0(7) . . ? O3 C9 La1 57.2(7) . . ? C10 C9 La1 168.0(10) . . ? C15 C10 C11 118.3(13) . . ? C15 C10 C9 117.6(12) . . ? C11 C10 C9 124.1(13) . . ? N2 C11 C12 120.3(14) . . ? N2 C11 C10 121.6(13) . . ? C12 C11 C10 118.0(14) . . ? C13 C12 C11 121.4(14) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C13 C12 120.9(15) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 119.0(15) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C14 C15 C10 122.3(14) . . ? C14 C15 H15 118.8 . . ? C10 C15 H15 118.8 . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O6 C17 O5 123.7(14) . . ? O6 C17 C18 118.4(13) . . ? O5 C17 C18 117.8(13) . . ? C23 C18 C19 121.6(15) . . ? C23 C18 C17 114.4(14) . . ? C19 C18 C17 124.0(14) . . ? N3 C19 C20 120.5(14) . . ? N3 C19 C18 121.8(14) . . ? C20 C19 C18 117.7(14) . . ? C21 C20 C19 120.4(16) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 123.7(18) . . ? C20 C21 H21 118.2 . . ? C22 C21 H21 118.2 . . ? C21 C22 C23 117.1(17) . . ? C21 C22 H22 121.5 . . ? C23 C22 H22 121.5 . . ? C18 C23 C22 119.5(15) . . ? C18 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? N3 C24 H24A 109.5 . . ? N3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O7 C25 N4 127.2(13) . . ? O7 C25 H25 116.4 . . ? N4 C25 H25 116.4 . . ? N4 C26 H26A 109.5 . . ? N4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N4 C27 H27A 109.5 . . ? N4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O8 C28 N5 122.5(16) . . ? O8 C28 H28 118.8 . . ? N5 C28 H28 118.8 . . ? N5 C29 H29A 109.5 . . ? N5 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N5 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N5 C30 H30A 109.5 . . ? N5 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N5 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? 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 N1 H1 O1 0.88 2.02 2.683(17) 130.8 . N2 H2 O3 0.88 2.04 2.704(16) 131.0 . N3 H3 O5 0.88 2.00 2.682(16) 133.7 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.428 _refine_diff_density_min -3.600 _refine_diff_density_rms 0.214 # Attachment '9.CIF' data_HB16DMSO _database_code_depnum_ccdc_archive 'CCDC 634378' _audit_creation_method SHELXL-97 _chemical_name_systematic ; poly[(aqua)(dimethylsulphoxide)tris(3-nitrobenzoato)lanthanum(III)] bis DMSO solvate ; _chemical_name_common ; poly((aqua)(dimethylsulphoxide)tris(3- nitrobenzoato)lanthanum(iii)) bis DMSO solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C23 H20 La1 N3 O14 S1, 2(C2 H6 O1 S1)' _chemical_formula_sum 'C27 H32 La1 N3 O16 S3' _chemical_formula_weight 889.65 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9777(1) _cell_length_b 13.9145(2) _cell_length_c 13.9532(2) _cell_angle_alpha 70.295(1) _cell_angle_beta 82.314(1) _cell_angle_gamma 75.908(1) _cell_volume 1766.03(4) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 1.461 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7205 _exptl_absorpt_correction_T_max 0.8676 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 21090 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8069 _reflns_number_gt 6990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^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_extinction_expression ? _refine_ls_number_reflns 8069 _refine_ls_number_parameters 469 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0593 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.032 _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 0.243162(12) 0.498292(10) 0.482860(10) 0.02091(5) Uani 1 1 d . . . S1 S 0.38700(6) 0.37146(6) 0.28421(5) 0.03868(16) Uani 1 1 d . . . O1 O 0.10993(18) 0.48173(15) 0.64906(13) 0.0395(4) Uani 1 1 d . . . N1 N 0.2403(3) 0.3825(3) 1.0151(2) 0.0610(8) Uani 1 1 d . . . C1 C -0.0012(2) 0.46785(19) 0.69860(18) 0.0278(5) Uani 1 1 d . . . H1O H 0.270(3) 0.639(3) 0.6162(18) 0.071(12) Uiso 1 1 d D . . S2 S 0.05007(8) 0.78598(7) 0.69227(7) 0.0512(2) Uani 1 1 d . . . O2 O -0.11574(18) 0.48510(16) 0.66293(14) 0.0436(5) Uani 1 1 d . . . N2 N -0.0978(3) 0.0352(3) 0.8905(2) 0.0630(8) Uani 1 1 d . . . C2 C 0.0041(2) 0.42460(19) 0.81341(18) 0.0288(5) Uani 1 1 d . . . H2O H 0.3994(15) 0.621(3) 0.570(3) 0.092(13) Uiso 1 1 d D . . O3 O 0.3180(3) 0.4377(3) 0.9685(2) 0.0929(10) Uani 1 1 d . . . N3 N 0.4452(3) 0.8271(2) -0.03160(18) 0.0505(7) Uani 1 1 d . . . C3 C 0.1155(2) 0.4278(2) 0.86055(18) 0.0310(5) Uani 1 1 d . . . H3 H 0.1861 0.4597 0.8229 0.037 Uiso 1 1 calc R . . S3A S 0.40312(10) -0.01185(8) 0.36931(8) 0.0540(4) Uani 0.888(3) 1 d P A 1 S3B S 0.2828(17) -0.0271(11) 0.3810(10) 0.124(7) Uani 0.112(3) 1 d PD A 2 O4 O 0.2587(3) 0.3223(3) 1.10160(19) 0.1032(11) Uani 1 1 d . . . C4 C 0.1194(3) 0.3826(2) 0.9646(2) 0.0426(7) Uani 1 1 d . . . O5 O -0.06375(18) 0.33795(14) 0.55526(14) 0.0438(5) Uani 1 1 d . . . C5 C 0.0169(4) 0.3362(3) 1.0230(2) 0.0729(12) Uani 1 1 d . . . H5 H 0.0227 0.3062 1.0932 0.088 Uiso 1 1 calc R . . O6 O 0.16454(18) 0.32691(14) 0.54051(14) 0.0385(4) Uani 1 1 d . . . C6 C -0.0946(4) 0.3350(4) 0.9758(3) 0.0846(14) Uani 1 1 d . . . H6 H -0.1657 0.3042 1.0142 0.102 Uiso 1 1 calc R . . O7 O -0.1921(3) 0.1039(3) 0.9015(2) 0.1052(12) Uani 1 1 d . . . C7 C -0.1011(3) 0.3792(3) 0.8718(2) 0.0562(9) Uani 1 1 d . . . H7 H -0.1772 0.3785 0.8403 0.067 Uiso 1 1 calc R . . O8 O -0.0825(3) -0.0544(2) 0.9471(2) 0.0959(10) Uani 1 1 d . . . C8 C 0.0577(2) 0.29196(19) 0.57639(18) 0.0289(5) Uani 1 1 d . . . O9 O 0.37109(17) 0.61622(14) 0.34002(13) 0.0364(4) Uani 1 1 d . . . C9 C 0.0777(2) 0.18330(19) 0.65326(18) 0.0269(5) Uani 1 1 d . . . O10 O 0.55961(16) 0.60722(14) 0.41346(12) 0.0349(4) Uani 1 1 d . . . C10 C -0.0199(2) 0.1590(2) 0.73278(19) 0.0340(6) Uani 1 1 d . . . H10 H -0.1003 0.2079 0.7383 0.041 Uiso 1 1 calc R . . O11 O 0.3719(3) 0.7705(2) -0.03418(17) 0.0729(7) Uani 1 1 d . . . C11 C 0.0050(3) 0.0601(2) 0.8042(2) 0.0390(6) Uani 1 1 d . . . O12 O 0.4660(3) 0.9013(2) -0.10352(17) 0.0852(9) Uani 1 1 d . . . C12 C 0.1203(3) -0.0148(2) 0.7981(2) 0.0493(8) Uani 1 1 d . . . H12 H 0.1344 -0.0804 0.8473 0.059 Uiso 1 1 calc R . . O13 O 0.31420(18) 0.61622(18) 0.56641(17) 0.0456(5) Uani 1 1 d D . . C13 C 0.2149(3) 0.0092(2) 0.7171(3) 0.0503(8) Uani 1 1 d . . . H13 H 0.2931 -0.0411 0.7106 0.060 Uiso 1 1 calc R . . O14 O 0.40988(17) 0.38581(15) 0.38408(13) 0.0364(4) Uani 1 1 d . . . C14 C 0.1949(3) 0.1073(2) 0.6455(2) 0.0372(6) Uani 1 1 d . . . H14 H 0.2602 0.1229 0.5916 0.045 Uiso 1 1 calc R . . C15 C 0.4855(2) 0.63850(18) 0.33860(17) 0.0240(5) Uani 1 1 d . . . O16 O 0.3013(3) 0.0418(2) 0.4330(2) 0.0885(9) Uani 1 1 d . . . C16 C 0.5363(2) 0.71016(18) 0.24020(17) 0.0242(5) Uani 1 1 d . . . C17 C 0.4678(2) 0.73595(19) 0.15179(18) 0.0292(5) Uani 1 1 d . . . H17 H 0.3914 0.7085 0.1524 0.035 Uiso 1 1 calc R . . C18 C 0.5147(3) 0.8029(2) 0.06299(18) 0.0344(6) Uani 1 1 d . . . C19 C 0.6253(3) 0.8477(2) 0.0590(2) 0.0425(7) Uani 1 1 d . . . H19 H 0.6529 0.8946 -0.0012 0.051 Uiso 1 1 calc R . . C20 C 0.6941(3) 0.8208(2) 0.1473(2) 0.0423(7) Uani 1 1 d . . . H20 H 0.7698 0.8490 0.1464 0.051 Uiso 1 1 calc R . . C21 C 0.6505(2) 0.7521(2) 0.23663(19) 0.0321(6) Uani 1 1 d . . . H21 H 0.6983 0.7337 0.2952 0.038 Uiso 1 1 calc R . . C22 C 0.4884(4) 0.2470(3) 0.2876(3) 0.0624(9) Uani 1 1 d . . . H22A H 0.4470 0.1938 0.3370 0.094 Uiso 1 1 calc R . . H22B H 0.5801 0.2409 0.3061 0.094 Uiso 1 1 calc R . . H22C H 0.4930 0.2387 0.2216 0.094 Uiso 1 1 calc R . . C23 C 0.4903(4) 0.4466(3) 0.1891(2) 0.0655(10) Uani 1 1 d . . . H23A H 0.4501 0.5196 0.1763 0.098 Uiso 1 1 calc R . . H23B H 0.4949 0.4295 0.1274 0.098 Uiso 1 1 calc R . . H23C H 0.5819 0.4316 0.2120 0.098 Uiso 1 1 calc R . . O24 O 0.1830(2) 0.7073(2) 0.71143(18) 0.0683(7) Uani 1 1 d . . . C24 C -0.0741(3) 0.7227(3) 0.6739(3) 0.0534(8) Uani 1 1 d . . . H24A H -0.0971 0.6736 0.7376 0.080 Uiso 1 1 calc R . . H24B H -0.0365 0.6864 0.6255 0.080 Uiso 1 1 calc R . . H24C H -0.1560 0.7737 0.6486 0.080 Uiso 1 1 calc R . . C25 C 0.0643(4) 0.8656(3) 0.5643(3) 0.0836(13) Uani 1 1 d . . . H25A H 0.1298 0.9082 0.5575 0.125 Uiso 1 1 calc R . . H25B H -0.0243 0.9096 0.5444 0.125 Uiso 1 1 calc R . . H25C H 0.0952 0.8224 0.5212 0.125 Uiso 1 1 calc R . . C26A C 0.4359(6) -0.1455(3) 0.4393(4) 0.117(2) Uani 0.888(3) 1 d P A 1 H26A H 0.4866 -0.1573 0.4975 0.175 Uiso 0.888(3) 1 calc PR A 1 H26B H 0.4892 -0.1847 0.3970 0.175 Uiso 0.888(3) 1 calc PR A 1 H26C H 0.3497 -0.1674 0.4617 0.175 Uiso 0.888(3) 1 calc PR A 1 C26B C 0.4359(6) -0.1455(3) 0.4393(4) 0.117(2) Uani 0.11 1 d PD A 2 H26D H 0.4496 -0.1474 0.5068 0.175 Uiso 0.112(3) 1 calc PR A 2 H26E H 0.5192 -0.1368 0.3972 0.175 Uiso 0.112(3) 1 calc PR A 2 H26F H 0.4132 -0.2096 0.4424 0.175 Uiso 0.112(3) 1 calc PR A 2 C27A C 0.3134(6) -0.0152(5) 0.2715(4) 0.123(2) Uani 0.888(3) 1 d P A 1 H27A H 0.2873 0.0541 0.2249 0.184 Uiso 0.888(3) 1 calc PR A 1 H27B H 0.2318 -0.0421 0.3001 0.184 Uiso 0.888(3) 1 calc PR A 1 H27C H 0.3717 -0.0595 0.2359 0.184 Uiso 0.888(3) 1 calc PR A 1 C27B C 0.3134(6) -0.0152(5) 0.2715(4) 0.123(2) Uani 0.11 1 d PD A 2 H27D H 0.2616 0.0508 0.2316 0.184 Uiso 0.112(3) 1 calc PR A 2 H27E H 0.2879 -0.0707 0.2567 0.184 Uiso 0.112(3) 1 calc PR A 2 H27F H 0.4105 -0.0179 0.2552 0.184 Uiso 0.112(3) 1 calc PR A 2 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 0.01415(6) 0.02622(8) 0.01862(7) -0.00161(5) -0.00084(4) -0.00531(5) S1 0.0296(3) 0.0531(4) 0.0406(4) -0.0239(3) -0.0019(3) -0.0092(3) O1 0.0360(10) 0.0509(12) 0.0244(9) -0.0082(8) 0.0068(7) -0.0062(8) N1 0.0528(16) 0.098(2) 0.0343(15) -0.0227(15) -0.0135(13) -0.0108(16) C1 0.0313(12) 0.0283(13) 0.0229(12) -0.0070(10) -0.0044(10) -0.0049(10) S2 0.0434(4) 0.0584(5) 0.0625(5) -0.0335(4) 0.0064(4) -0.0150(4) O2 0.0391(10) 0.0535(12) 0.0382(11) -0.0084(9) -0.0184(8) -0.0101(9) N2 0.0498(16) 0.077(2) 0.0441(16) 0.0164(15) -0.0044(13) -0.0294(15) C2 0.0260(11) 0.0338(14) 0.0242(12) -0.0054(10) -0.0015(9) -0.0074(10) O3 0.0701(17) 0.158(3) 0.0623(17) -0.0215(19) -0.0184(14) -0.057(2) N3 0.0527(15) 0.0670(18) 0.0275(13) -0.0034(12) -0.0062(11) -0.0194(14) C3 0.0273(12) 0.0409(15) 0.0229(12) -0.0090(11) 0.0022(10) -0.0075(11) S3A 0.0534(7) 0.0472(6) 0.0621(6) -0.0205(5) 0.0103(5) -0.0148(4) S3B 0.138(14) 0.094(10) 0.095(9) 0.001(7) 0.043(8) -0.014(8) O4 0.091(2) 0.169(3) 0.0377(14) -0.0077(17) -0.0336(14) -0.025(2) C4 0.0398(14) 0.0590(19) 0.0277(14) -0.0108(13) -0.0073(11) -0.0095(13) O5 0.0335(9) 0.0367(11) 0.0445(11) -0.0004(9) -0.0044(8) 0.0068(8) C5 0.079(2) 0.108(3) 0.0227(15) 0.0066(17) -0.0052(16) -0.042(2) O6 0.0409(10) 0.0370(10) 0.0370(10) -0.0029(8) -0.0018(8) -0.0200(8) C6 0.079(3) 0.134(4) 0.0391(19) 0.008(2) 0.0033(18) -0.074(3) O7 0.0614(16) 0.123(3) 0.0703(19) 0.0172(17) 0.0280(14) 0.0075(18) C7 0.0453(16) 0.085(3) 0.0392(17) -0.0033(16) -0.0034(13) -0.0387(17) O8 0.094(2) 0.085(2) 0.0780(19) 0.0275(16) 0.0092(15) -0.0466(17) C8 0.0306(12) 0.0282(13) 0.0274(12) -0.0093(10) -0.0012(10) -0.0050(10) O9 0.0336(9) 0.0466(11) 0.0293(9) -0.0024(8) 0.0014(7) -0.0244(8) C9 0.0234(11) 0.0282(13) 0.0300(13) -0.0080(10) -0.0044(9) -0.0070(9) O10 0.0262(8) 0.0425(11) 0.0256(9) 0.0014(8) -0.0055(7) -0.0034(8) C10 0.0245(12) 0.0359(14) 0.0357(14) -0.0040(11) -0.0040(10) -0.0048(10) O11 0.0768(16) 0.107(2) 0.0446(14) -0.0125(14) -0.0184(12) -0.0460(16) C11 0.0354(14) 0.0410(16) 0.0355(15) 0.0021(12) -0.0046(11) -0.0177(12) O12 0.109(2) 0.098(2) 0.0345(13) 0.0203(13) -0.0245(13) -0.0431(17) C12 0.0512(17) 0.0309(15) 0.0545(19) 0.0084(13) -0.0160(15) -0.0124(13) O13 0.0242(9) 0.0666(14) 0.0618(14) -0.0394(12) 0.0040(9) -0.0148(9) C13 0.0427(16) 0.0311(16) 0.065(2) -0.0086(14) -0.0087(15) 0.0068(13) O14 0.0300(9) 0.0490(12) 0.0348(10) -0.0208(9) 0.0019(7) -0.0081(8) C14 0.0295(13) 0.0343(15) 0.0439(16) -0.0103(12) 0.0007(11) -0.0042(11) C15 0.0216(11) 0.0229(12) 0.0239(12) -0.0046(9) 0.0006(9) -0.0035(9) O16 0.102(2) 0.0677(18) 0.098(2) -0.0495(17) 0.0163(17) -0.0018(16) C16 0.0199(10) 0.0247(12) 0.0245(12) -0.0033(9) 0.0005(9) -0.0058(9) C17 0.0257(11) 0.0322(13) 0.0286(12) -0.0045(10) -0.0021(10) -0.0114(10) C18 0.0373(13) 0.0401(15) 0.0234(12) -0.0035(11) -0.0036(10) -0.0123(11) C19 0.0499(16) 0.0452(17) 0.0292(14) -0.0004(12) 0.0051(12) -0.0241(13) C20 0.0401(14) 0.0509(18) 0.0391(15) -0.0049(13) 0.0017(12) -0.0310(13) C21 0.0282(12) 0.0391(15) 0.0295(13) -0.0060(11) -0.0047(10) -0.0136(11) C22 0.075(2) 0.052(2) 0.070(2) -0.0340(18) -0.0024(18) -0.0093(17) C23 0.096(3) 0.064(2) 0.0389(18) -0.0121(16) 0.0039(18) -0.031(2) O24 0.0482(13) 0.0928(19) 0.0662(16) -0.0358(14) -0.0129(11) 0.0013(13) C24 0.0500(17) 0.053(2) 0.062(2) -0.0211(16) 0.0060(15) -0.0222(15) C25 0.074(3) 0.069(3) 0.097(3) 0.000(2) -0.005(2) -0.032(2) C26A 0.148(5) 0.058(3) 0.104(4) -0.010(3) 0.032(3) 0.011(3) C26B 0.148(5) 0.058(3) 0.104(4) -0.010(3) 0.032(3) 0.011(3) C27A 0.109(4) 0.183(6) 0.090(4) -0.057(4) -0.019(3) -0.029(4) C27B 0.109(4) 0.183(6) 0.090(4) -0.057(4) -0.019(3) -0.029(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O2 2.4576(17) 2_566 ? La1 O10 2.4583(15) 2_666 ? La1 O5 2.4760(17) 2_566 ? La1 O1 2.4824(17) . ? La1 O6 2.5294(18) . ? La1 O9 2.5354(17) . ? La1 O13 2.575(2) . ? La1 O14 2.5866(17) . ? S1 O14 1.5259(18) . ? S1 C22 1.769(3) . ? S1 C23 1.772(3) . ? O1 C1 1.247(3) . ? N1 O3 1.197(4) . ? N1 O4 1.222(4) . ? N1 C4 1.476(4) . ? C1 O2 1.245(3) . ? C1 C2 1.513(3) . ? S2 O24 1.490(2) . ? S2 C25 1.764(4) . ? S2 C24 1.774(3) . ? O2 La1 2.4576(17) 2_566 ? N2 O7 1.202(4) . ? N2 O8 1.215(4) . ? N2 C11 1.478(4) . ? C2 C3 1.382(3) . ? C2 C7 1.383(4) . ? N3 O12 1.210(3) . ? N3 O11 1.211(3) . ? N3 C18 1.472(3) . ? C3 C4 1.376(3) . ? C3 H3 0.9300 . ? S3A O16 1.488(3) . ? S3A C27A 1.748(5) . ? S3A C26A 1.756(4) . ? S3B O16 1.439(18) . ? C4 C5 1.367(4) . ? O5 C8 1.248(3) . ? O5 La1 2.4760(16) 2_566 ? C5 C6 1.373(5) . ? C5 H5 0.9300 . ? O6 C8 1.252(3) . ? C6 C7 1.376(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.514(3) . ? O9 C15 1.250(3) . ? C9 C10 1.382(3) . ? C9 C14 1.392(3) . ? O10 C15 1.253(3) . ? O10 La1 2.4583(15) 2_666 ? C10 C11 1.387(3) . ? C10 H10 0.9300 . ? C11 C12 1.366(4) . ? C12 C13 1.376(4) . ? C12 H12 0.9300 . ? O13 H1O 0.880(5) . ? O13 H2O 0.879(5) . ? C13 C14 1.379(4) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.508(3) . ? C16 C17 1.388(3) . ? C16 C21 1.389(3) . ? C17 C18 1.379(3) . ? C17 H17 0.9300 . ? C18 C19 1.380(4) . ? C19 C20 1.384(4) . ? C19 H19 0.9300 . ? C20 C21 1.382(3) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26A H26A 0.9600 . ? C26A H26B 0.9600 . ? C26A H26C 0.9600 . ? C27A H27A 0.9600 . ? C27A H27B 0.9600 . ? C27A H27C 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 O2 La1 O10 143.89(6) 2_566 2_666 ? O2 La1 O5 70.30(7) 2_566 2_566 ? O10 La1 O5 145.52(7) 2_666 2_566 ? O2 La1 O1 117.09(6) 2_566 . ? O10 La1 O1 84.97(6) 2_666 . ? O5 La1 O1 77.35(6) 2_566 . ? O2 La1 O6 78.13(6) 2_566 . ? O10 La1 O6 83.00(6) 2_666 . ? O5 La1 O6 118.04(6) 2_566 . ? O1 La1 O6 71.81(6) . . ? O2 La1 O9 79.97(6) 2_566 . ? O10 La1 O9 98.69(6) 2_666 . ? O5 La1 O9 80.20(6) 2_566 . ? O1 La1 O9 144.31(7) . . ? O6 La1 O9 143.85(6) . . ? O2 La1 O13 139.15(7) 2_566 . ? O10 La1 O13 72.79(7) 2_666 . ? O5 La1 O13 73.60(7) 2_566 . ? O1 La1 O13 71.60(7) . . ? O6 La1 O13 137.40(7) . . ? O9 La1 O13 75.64(6) . . ? O2 La1 O14 74.92(6) 2_566 . ? O10 La1 O14 70.61(6) 2_666 . ? O5 La1 O14 138.18(6) 2_566 . ? O1 La1 O14 140.99(6) . . ? O6 La1 O14 75.31(6) . . ? O9 La1 O14 71.41(6) . . ? O13 La1 O14 125.32(6) . . ? O14 S1 C22 105.39(14) . . ? O14 S1 C23 105.96(14) . . ? C22 S1 C23 97.15(18) . . ? C1 O1 La1 146.31(16) . . ? O3 N1 O4 123.4(3) . . ? O3 N1 C4 118.8(3) . . ? O4 N1 C4 117.8(3) . . ? O2 C1 O1 126.5(2) . . ? O2 C1 C2 116.8(2) . . ? O1 C1 C2 116.7(2) . . ? O24 S2 C25 106.23(17) . . ? O24 S2 C24 107.08(16) . . ? C25 S2 C24 96.11(18) . . ? C1 O2 La1 147.30(17) . 2_566 ? O7 N2 O8 123.1(3) . . ? O7 N2 C11 118.9(3) . . ? O8 N2 C11 118.0(3) . . ? C3 C2 C7 119.5(2) . . ? C3 C2 C1 120.4(2) . . ? C7 C2 C1 120.1(2) . . ? O12 N3 O11 123.1(3) . . ? O12 N3 C18 118.7(3) . . ? O11 N3 C18 118.2(2) . . ? C4 C3 C2 118.3(2) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? O16 S3A C27A 107.1(2) . . ? O16 S3A C26A 106.4(2) . . ? C27A S3A C26A 98.9(3) . . ? C5 C4 C3 122.7(3) . . ? C5 C4 N1 118.6(3) . . ? C3 C4 N1 118.7(3) . . ? C8 O5 La1 149.04(18) . 2_566 ? C4 C5 C6 118.6(3) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C8 O6 La1 139.49(16) . . ? C5 C6 C7 120.0(3) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C2 120.8(3) . . ? C6 C7 H7 119.6 . . ? C2 C7 H7 119.6 . . ? O5 C8 O6 126.4(2) . . ? O5 C8 C9 116.7(2) . . ? O6 C8 C9 116.9(2) . . ? C15 O9 La1 129.86(15) . . ? C10 C9 C14 119.3(2) . . ? C10 C9 C8 120.1(2) . . ? C14 C9 C8 120.5(2) . . ? C15 O10 La1 156.30(16) . 2_666 ? C9 C10 C11 118.4(2) . . ? C9 C10 H10 120.8 . . ? C11 C10 H10 120.8 . . ? C12 C11 C10 122.8(3) . . ? C12 C11 N2 118.8(3) . . ? C10 C11 N2 118.4(3) . . ? C11 C12 C13 118.3(3) . . ? C11 C12 H12 120.9 . . ? C13 C12 H12 120.9 . . ? La1 O13 H1O 128(2) . . ? La1 O13 H2O 126(3) . . ? H1O O13 H2O 102(3) . . ? C12 C13 C14 120.6(3) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? S1 O14 La1 127.81(9) . . ? C13 C14 C9 120.5(3) . . ? C13 C14 H14 119.7 . . ? C9 C14 H14 119.7 . . ? O9 C15 O10 124.7(2) . . ? O9 C15 C16 117.47(19) . . ? O10 C15 C16 117.8(2) . . ? S3B O16 S3A 50.5(6) . . ? C17 C16 C21 119.1(2) . . ? C17 C16 C15 120.0(2) . . ? C21 C16 C15 120.9(2) . . ? C18 C17 C16 119.0(2) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C17 C18 C19 122.5(2) . . ? C17 C18 N3 119.0(2) . . ? C19 C18 N3 118.5(2) . . ? C18 C19 C20 118.2(2) . . ? C18 C19 H19 120.9 . . ? C20 C19 H19 120.9 . . ? C21 C20 C19 120.2(2) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C16 121.0(2) . . ? C20 C21 H21 119.5 . . ? C16 C21 H21 119.5 . . ? S1 C22 H22A 109.5 . . ? S1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? S1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? S1 C23 H23A 109.5 . . ? S1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? S1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? S2 C24 H24A 109.5 . . ? S2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? S2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? S2 C25 H25A 109.5 . . ? S2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? S2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? S3A C26A H26A 109.5 . . ? S3A C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? S3A C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? S3A C27A H27A 109.5 . . ? S3A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? S3A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? 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 O13 H1O O24 0.880(5) 1.889(8) 2.762(3) 171(4) . O13 H2O O14 0.879(5) 2.059(11) 2.918(2) 165(4) 2_666 C14 H14 O16 0.93 2.75 3.356(4) 123.8 . C22 H22A O16 0.96 2.73 3.664(5) 164.9 . C6 H6 O11 0.93 2.47 3.323(4) 153.1 2_566 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.766 _refine_diff_density_min -0.669 _refine_diff_density_rms 0.076