#------------------------------------------------------------------------------ #$Date: 2026-06-10 03:21:42 +0100 (Wed, 10 Jun 2026) $ #$Revision: 306539 $ #$URL: svn://www.crystallography.net/cod/cif/7/06/44/7064443.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7064443 loop_ _publ_author_name 'Qu, Ziyi' 'Zhao, Jinjin' 'Ren, Ning' 'Zhang, Jianjun' _publ_section_title ; Synthesis, structures, thermal decomposition mechanism, and luminescence properties of Sm(iii), Pr(iii), Nd(iii), and La(iii) complexes with diverse carboxylate coordination modes ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D5NJ05019G _journal_year 2026 _chemical_formula_moiety 'C88 H82 La2 N4 O16' _chemical_formula_sum 'C88 H82 La2 N4 O16' _chemical_formula_weight 1729.39 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2025-04-15 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _audit_update_record ; 2025-09-22 deposited with the CCDC. 2026-05-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 89.995(4) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 14.5700(15) _cell_length_b 14.7415(16) _cell_length_c 18.4795(18) _cell_measurement_reflns_used 9796 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 25.849 _cell_measurement_theta_min 2.796 _cell_volume 3969.1(7) _computing_cell_refinement 'SAINT V8.40A (Bruker, 2019)' _computing_data_reduction 'SAINT V8.40A (Bruker, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100.0 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_unetI/netI 0.0412 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 60189 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.932 _diffrn_reflns_theta_min 2.602 _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.132 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_correction_T_min 0.6254 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0978 before and 0.0722 after correction. The Ratio of minimum to maximum transmission is 0.8391. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.447 _exptl_crystal_description block _exptl_crystal_F_000 1760 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _refine_diff_density_max 2.197 _refine_diff_density_min -1.256 _refine_diff_density_rms 0.138 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 514 _refine_ls_number_reflns 7653 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.103 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0575 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+28.0157P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1116 _refine_ls_wR_factor_ref 0.1235 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6192 _reflns_number_total 7653 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d5nj05019g2.cif _cod_data_source_block mo_250401e1laa_a _cod_database_code 7064443 _shelx_shelxl_version_number 2019/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.915 _shelx_estimated_absorpt_t_min 0.831 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Others Sof(H6)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=1-FVAR(1) Sof(H4)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(1) 3.a Aromatic/amide H refined with riding coordinates: C23(H23), C19(H19), C40(H40), C36(H36), C21(H21), C34(H34), C43(H43), C20(H20), C15(H15), C35(H35), C7(H7), C41(H41), C11(H11), C6(H6), C14(H14), C3(H3), C13(H13), C32(H32), C27(H27), C4(H4), C30(H30), C5(H5), C31(H31) 3.b Idealised Me refined as rotating group: C24(H24A,H24B,H24C), C38(H38A,H38B,H38C), C44(H44A,H44B,H44C), C29(H29A,H29B, H29C), C16(H16A,H16B,H16C), C8A(H8AA,H8AB,H8AC), C8(H8A,H8B,H8C) 3.c Idealised tetrahedral OH refined as rotating group: O2(H2) ; _shelx_res_file ; TITL mo_250401e1Laa_a.res in P2(1)/n mo_250401e1laa_a.res created by SHELXL-2019/3 at 20:04:48 on 15-Apr-2025 REM Old TITL mo_250401e1Laa in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.109, Rweak 0.006, Alpha 0.050, Orientation as input REM Formula found by SHELXT: C44 La N3 O8 CELL 0.71073 14.57 14.7415 18.4795 90 89.9953 90 ZERR 2 0.0015 0.0016 0.0018 0 0.0036 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H La N O UNIT 176 164 4 8 32 L.S. 10 PLAN 4 SIZE 0.08 0.1 0.17 TEMP -173.15 CONF HTAB O2 O4 BOND $H LIST 4 MORE -1 fmap 2 acta REM REM REM WGHT 0.021900 28.015699 FVAR 0.25228 0.46859 LA1 3 0.359858 0.513461 0.508949 11.00000 0.01779 0.02555 = 0.02632 -0.00033 -0.00198 -0.00125 O5 5 0.498628 0.607868 0.515540 11.00000 0.02289 0.02509 = 0.03765 0.00003 -0.00394 -0.00383 O7 5 0.412800 0.516780 0.379853 11.00000 0.01977 0.03418 = 0.02675 0.00320 -0.00073 -0.00176 O3 5 0.292407 0.651643 0.452360 11.00000 0.02268 0.02774 = 0.04019 0.00492 -0.00804 0.00100 O8 5 0.565400 0.540722 0.377425 11.00000 0.02473 0.03379 = 0.03066 0.00397 -0.00280 0.00075 O6 5 0.643492 0.653785 0.522628 11.00000 0.02533 0.03160 = 0.04630 -0.00500 -0.00225 -0.00187 O1 5 0.305238 0.616200 0.610261 11.00000 0.02767 0.03218 = 0.03778 -0.00471 0.00276 0.00123 O2 5 0.162156 0.672781 0.606748 11.00000 0.03042 0.05115 = 0.03823 -0.00399 -0.00030 0.00619 AFIX 147 H2 2 0.172555 0.673238 0.562039 11.00000 -1.50000 AFIX 0 O4 5 0.152315 0.704351 0.477229 11.00000 0.02590 0.04483 = 0.04827 -0.00258 -0.00776 0.00246 N1 4 0.217100 0.436755 0.581606 11.00000 0.02750 0.02555 = 0.03203 -0.00016 -0.00182 -0.00264 N2 4 0.200382 0.470857 0.439026 11.00000 0.02843 0.03095 = 0.02948 -0.00236 -0.00088 0.00120 C18 1 0.527234 0.765223 0.541448 11.00000 0.03184 0.02171 = 0.02863 -0.00288 0.00020 -0.00407 C33 1 0.137480 0.410792 0.550116 11.00000 0.02159 0.02857 = 0.03922 -0.00055 -0.00139 -0.00286 C17 1 0.558360 0.670704 0.526132 11.00000 0.02617 0.02820 = 0.02844 0.00204 -0.00415 0.00163 C9 1 0.487397 0.536525 0.347849 11.00000 0.02487 0.02610 = 0.02674 0.00086 0.00073 0.00532 C23 1 0.435204 0.788772 0.534283 11.00000 0.02854 0.02650 = 0.03149 -0.00013 -0.00188 -0.00413 AFIX 43 H23 2 0.391922 0.743975 0.520101 11.00000 -1.20000 AFIX 0 C25 1 0.220826 0.692953 0.434307 11.00000 0.03411 0.02598 = 0.04127 -0.00537 -0.00458 -0.00713 C39 1 0.128100 0.429859 0.472503 11.00000 0.02978 0.02980 = 0.03585 0.00498 -0.00437 -0.00302 C19 1 0.591217 0.830422 0.562750 11.00000 0.02544 0.03390 = 0.02397 -0.00233 0.00114 -0.00248 AFIX 43 H19 2 0.654259 0.815074 0.567475 11.00000 -1.20000 AFIX 0 C40 1 0.048999 0.409661 0.434345 11.00000 0.02810 0.05621 = 0.03780 0.00842 -0.00717 -0.01572 AFIX 43 H40 2 -0.000913 0.380358 0.457752 11.00000 -1.20000 AFIX 0 C1 1 0.233855 0.643798 0.640586 11.00000 0.02879 0.02725 = 0.04087 -0.00260 -0.00338 -0.00415 C10 1 0.483082 0.558335 0.267973 11.00000 0.02963 0.03043 = 0.02532 -0.00074 -0.00306 0.00139 C36 1 0.226770 0.423142 0.652819 11.00000 0.02162 0.03725 = 0.03463 0.00086 -0.00266 -0.00310 AFIX 43 H36 2 0.283398 0.440258 0.674332 11.00000 -1.20000 AFIX 0 C21 1 0.469452 0.940892 0.569996 11.00000 0.03925 0.02236 = 0.02917 -0.00090 0.00205 0.00097 AFIX 43 H21 2 0.450098 1.000946 0.580719 11.00000 -1.20000 AFIX 0 C34 1 0.068319 0.369349 0.591367 11.00000 0.02667 0.04878 = 0.04350 0.00947 -0.00371 -0.01175 AFIX 43 H34 2 0.013333 0.349557 0.568700 11.00000 -1.20000 AFIX 0 C43 1 0.193712 0.491750 0.369334 11.00000 0.02085 0.03271 = 0.03069 0.00210 -0.00289 -0.00569 AFIX 43 H43 2 0.245043 0.519543 0.346673 11.00000 -1.20000 AFIX 0 C20 1 0.561325 0.917997 0.576920 11.00000 0.03768 0.02493 = 0.03352 -0.00066 0.00086 -0.00886 AFIX 43 H20 2 0.604337 0.962823 0.591546 11.00000 -1.20000 AFIX 0 C22 1 0.405539 0.877211 0.547620 11.00000 0.03111 0.02970 = 0.02752 0.00282 -0.00098 0.00054 C15 1 0.553534 0.607395 0.234574 11.00000 0.03474 0.04614 = 0.03765 0.00425 -0.00475 -0.01067 AFIX 43 H15 2 0.604274 0.627789 0.262457 11.00000 -1.20000 AFIX 0 C26 1 0.214772 0.728782 0.357984 11.00000 0.05223 0.02577 = 0.04151 0.00628 -0.02108 -0.00616 C37 1 0.160214 0.385891 0.697521 11.00000 0.03052 0.03303 = 0.03457 0.00275 0.00315 -0.00054 C35 1 0.080148 0.357322 0.664893 11.00000 0.03195 0.05096 = 0.03858 0.01365 0.00487 -0.01073 AFIX 43 H35 2 0.033292 0.329464 0.692898 11.00000 -1.20000 AFIX 0 C7 1 0.147957 0.677484 0.755729 11.00000 0.03753 0.04015 = 0.04390 -0.00087 0.00867 -0.00295 AFIX 43 H7 2 0.096684 0.695643 0.727470 11.00000 -1.20000 AFIX 0 C24 1 0.305259 0.901935 0.536814 11.00000 0.03516 0.03311 = 0.04218 -0.00620 -0.00326 0.00658 AFIX 137 H24A 2 0.290348 0.899697 0.485134 11.00000 -1.50000 H24B 2 0.294246 0.963316 0.555238 11.00000 -1.50000 H24C 2 0.266489 0.858743 0.563100 11.00000 -1.50000 AFIX 0 C41 1 0.043120 0.432322 0.362223 11.00000 0.02812 0.05621 = 0.04832 0.00760 -0.01445 -0.01773 AFIX 43 H41 2 -0.011081 0.418521 0.335856 11.00000 -1.20000 AFIX 0 C11 1 0.409411 0.528394 0.226431 11.00000 0.03547 0.05182 = 0.02466 0.00083 -0.00376 -0.00043 AFIX 43 H11 2 0.361189 0.495284 0.248787 11.00000 -1.20000 AFIX 0 C42 1 0.116199 0.475416 0.327566 11.00000 0.03031 0.04058 = 0.03442 -0.00025 -0.00779 -0.00341 C2 1 0.227311 0.647004 0.721435 11.00000 0.03778 0.02404 = 0.04207 -0.00094 0.00356 -0.00382 C38 1 0.175422 0.377984 0.777970 11.00000 0.03915 0.04170 = 0.03738 0.00646 0.00809 -0.00409 AFIX 137 H38A 2 0.162626 0.436480 0.801060 11.00000 -1.50000 H38B 2 0.239267 0.360650 0.787306 11.00000 -1.50000 H38C 2 0.134258 0.331681 0.797840 11.00000 -1.50000 AFIX 0 C44 1 0.114110 0.501145 0.248760 11.00000 0.03726 0.06634 = 0.03431 0.00594 -0.01093 -0.01486 AFIX 137 H44A 2 0.139543 0.451492 0.219753 11.00000 -1.50000 H44B 2 0.150834 0.556047 0.241288 11.00000 -1.50000 H44C 2 0.050590 0.512647 0.233930 11.00000 -1.50000 AFIX 0 C6 1 0.142841 0.681659 0.830484 11.00000 0.05949 0.05555 = 0.04821 0.00296 0.02122 0.00406 PART 2 AFIX 43 H6 2 0.088322 0.702034 0.853529 -21.00000 -1.20000 AFIX 0 PART 0 C14 1 0.550001 0.626508 0.161248 11.00000 0.04952 0.07142 = 0.03455 0.01391 -0.00084 -0.01891 AFIX 43 H14 2 0.597825 0.660118 0.138835 11.00000 -1.20000 AFIX 0 C3 1 0.301225 0.618356 0.762809 11.00000 0.04045 0.03492 = 0.04234 0.00230 0.00059 0.00153 AFIX 43 H3 2 0.354443 0.594756 0.739832 11.00000 -1.20000 AFIX 0 C13 1 0.476477 0.596295 0.121205 11.00000 0.05369 0.09470 = 0.02678 0.01372 -0.00408 -0.01418 AFIX 43 H13 2 0.473755 0.609638 0.070957 11.00000 -1.20000 AFIX 0 C12 1 0.405498 0.546158 0.153260 11.00000 0.03340 0.08420 = 0.03327 0.00790 -0.00990 -0.00770 C32 1 0.290013 0.723169 0.312223 11.00000 0.08004 0.03660 = 0.04544 0.00260 0.01506 0.00052 AFIX 43 H32 2 0.345239 0.697959 0.330726 11.00000 -1.20000 AFIX 0 C27 1 0.133932 0.762896 0.332237 11.00000 0.04745 0.05268 = 0.07127 0.03177 -0.02578 -0.02196 AFIX 43 H27 2 0.081872 0.769250 0.362774 11.00000 -1.20000 AFIX 0 C4 1 0.297583 0.624140 0.838349 11.00000 0.05423 0.05046 = 0.04298 0.01050 0.00224 -0.00263 PART 1 AFIX 43 H4 2 0.348878 0.606621 0.866840 21.00000 -1.20000 AFIX 0 PART 0 C28 1 0.130422 0.789006 0.256805 11.00000 0.06993 0.06236 = 0.07149 0.02757 -0.05250 -0.01921 C30 1 0.208735 0.783673 0.215972 11.00000 0.11972 0.06613 = 0.05778 0.01458 -0.00743 -0.05611 AFIX 43 H30 2 0.205630 0.803409 0.167096 11.00000 -1.20000 AFIX 0 C5 1 0.217996 0.655828 0.871131 11.00000 0.06948 0.06465 = 0.03927 0.00985 0.01389 0.00493 AFIX 43 H5 2 0.215203 0.659804 0.922394 11.00000 -1.20000 AFIX 0 C31 1 0.288919 0.752685 0.240187 11.00000 0.11290 0.03371 = 0.06200 0.00564 -0.01203 -0.01013 AFIX 43 H31 2 0.342069 0.750724 0.210446 11.00000 -1.20000 AFIX 0 C29 1 0.043712 0.810595 0.221750 11.00000 0.08218 0.07504 = 0.08388 0.02184 -0.00779 0.00614 AFIX 137 H29A 2 0.017844 0.755480 0.200226 11.00000 -1.50000 H29B 2 0.054122 0.855853 0.183782 11.00000 -1.50000 H29C 2 0.000771 0.834992 0.257632 11.00000 -1.50000 AFIX 0 C16 1 0.326731 0.509806 0.108118 11.00000 0.05528 0.17437 = 0.03982 0.01655 -0.02088 -0.04355 AFIX 137 H16A 2 0.296585 0.460125 0.134135 11.00000 -1.50000 H16B 2 0.350397 0.487338 0.061825 11.00000 -1.50000 H16C 2 0.282313 0.558467 0.099226 11.00000 -1.50000 AFIX 0 PART 2 C8A 1 0.381099 0.601142 0.887578 -21.00000 0.04803 0.06604 = 0.03678 0.00979 -0.00647 -0.00421 AFIX 137 H8AA 2 0.431174 0.577029 0.857850 -21.00000 -1.50000 H8AB 2 0.362890 0.555685 0.923514 -21.00000 -1.50000 H8AC 2 0.401809 0.656235 0.912361 -21.00000 -1.50000 AFIX 0 PART 1 C8 1 0.051390 0.705299 0.862057 21.00000 0.08635 0.04632 = 0.03961 -0.00265 0.02818 0.00839 AFIX 137 H8A 2 0.053037 0.767514 0.880697 21.00000 -1.50000 H8B 2 0.037098 0.663358 0.901630 21.00000 -1.50000 H8C 2 0.004117 0.700514 0.824529 21.00000 -1.50000 AFIX 0 HKLF 4 REM mo_250401e1Laa_a.res in P2(1)/n REM wR2 = 0.1235, GooF = S = 1.103, Restrained GooF = 1.103 for all data REM R1 = 0.0575 for 6192 Fo > 4sig(Fo) and 0.0777 for all 7653 data REM 514 parameters refined using 0 restraints END WGHT 0.0218 28.0363 REM Highest difference peak 2.197, deepest hole -1.256, 1-sigma level 0.138 Q1 1 0.0807 0.4839 0.5281 11.00000 0.05 2.20 Q2 1 0.3595 0.4570 0.5091 11.00000 0.05 1.78 Q3 1 0.3205 0.7448 0.1772 11.00000 0.05 1.66 Q4 1 0.0896 0.8234 0.2887 11.00000 0.05 1.00 ; _shelx_res_checksum 88403 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.35986(2) 0.51346(2) 0.50895(2) 0.02322(10) Uani 1 1 d . . . . . O5 O 0.4986(2) 0.6079(2) 0.5155(2) 0.0285(9) Uani 1 1 d . . . . . O7 O 0.4128(2) 0.5168(3) 0.37985(19) 0.0269(8) Uani 1 1 d . . . . . O3 O 0.2924(2) 0.6516(3) 0.4524(2) 0.0302(9) Uani 1 1 d . . . . . O8 O 0.5654(2) 0.5407(3) 0.3774(2) 0.0297(9) Uani 1 1 d . . . . . O6 O 0.6435(3) 0.6538(3) 0.5226(2) 0.0344(9) Uani 1 1 d . . . . . O1 O 0.3052(3) 0.6162(3) 0.6103(2) 0.0325(9) Uani 1 1 d . . . . . O2 O 0.1622(3) 0.6728(3) 0.6067(2) 0.0399(10) Uani 1 1 d . . . . . H2 H 0.172555 0.673238 0.562039 0.060 Uiso 1 1 calc R U . . . O4 O 0.1523(3) 0.7044(3) 0.4772(2) 0.0397(10) Uani 1 1 d . . . . . N1 N 0.2171(3) 0.4368(3) 0.5816(2) 0.0284(10) Uani 1 1 d . . . . . N2 N 0.2004(3) 0.4709(3) 0.4390(2) 0.0296(10) Uani 1 1 d . . . . . C18 C 0.5272(4) 0.7652(4) 0.5414(3) 0.0274(12) Uani 1 1 d . . . . . C33 C 0.1375(4) 0.4108(4) 0.5501(3) 0.0298(12) Uani 1 1 d . . . . . C17 C 0.5584(4) 0.6707(4) 0.5261(3) 0.0276(12) Uani 1 1 d . . . . . C9 C 0.4874(4) 0.5365(4) 0.3478(3) 0.0259(11) Uani 1 1 d . . . . . C23 C 0.4352(4) 0.7888(4) 0.5343(3) 0.0288(12) Uani 1 1 d . . . . . H23 H 0.391922 0.743975 0.520101 0.035 Uiso 1 1 calc R U . . . C25 C 0.2208(4) 0.6930(4) 0.4343(3) 0.0338(13) Uani 1 1 d . . . . . C39 C 0.1281(4) 0.4299(4) 0.4725(3) 0.0318(13) Uani 1 1 d . . . . . C19 C 0.5912(4) 0.8304(4) 0.5628(3) 0.0278(12) Uani 1 1 d . . . . . H19 H 0.654259 0.815074 0.567475 0.033 Uiso 1 1 calc R U . . . C40 C 0.0490(4) 0.4097(5) 0.4343(3) 0.0407(15) Uani 1 1 d . . . . . H40 H -0.000913 0.380358 0.457752 0.049 Uiso 1 1 calc R U . . . C1 C 0.2339(4) 0.6438(4) 0.6406(3) 0.0323(13) Uani 1 1 d . . . . . C10 C 0.4831(4) 0.5583(4) 0.2680(3) 0.0285(12) Uani 1 1 d . . . . . C36 C 0.2268(4) 0.4231(4) 0.6528(3) 0.0312(13) Uani 1 1 d . . . . . H36 H 0.283398 0.440258 0.674332 0.037 Uiso 1 1 calc R U . . . C21 C 0.4695(4) 0.9409(4) 0.5700(3) 0.0303(12) Uani 1 1 d . . . . . H21 H 0.450098 1.000946 0.580719 0.036 Uiso 1 1 calc R U . . . C34 C 0.0683(4) 0.3693(4) 0.5914(3) 0.0396(15) Uani 1 1 d . . . . . H34 H 0.013333 0.349557 0.568700 0.048 Uiso 1 1 calc R U . . . C43 C 0.1937(3) 0.4918(4) 0.3693(3) 0.0281(12) Uani 1 1 d . . . . . H43 H 0.245043 0.519543 0.346673 0.034 Uiso 1 1 calc R U . . . C20 C 0.5613(4) 0.9180(4) 0.5769(3) 0.0320(13) Uani 1 1 d . . . . . H20 H 0.604337 0.962823 0.591546 0.038 Uiso 1 1 calc R U . . . C22 C 0.4055(4) 0.8772(4) 0.5476(3) 0.0294(12) Uani 1 1 d . . . . . C15 C 0.5535(4) 0.6074(4) 0.2346(3) 0.0395(15) Uani 1 1 d . . . . . H15 H 0.604274 0.627789 0.262457 0.047 Uiso 1 1 calc R U . . . C26 C 0.2148(5) 0.7288(4) 0.3580(3) 0.0398(15) Uani 1 1 d . . . . . C37 C 0.1602(4) 0.3859(4) 0.6975(3) 0.0327(13) Uani 1 1 d . . . . . C35 C 0.0801(4) 0.3573(5) 0.6649(3) 0.0405(15) Uani 1 1 d . . . . . H35 H 0.033292 0.329464 0.692898 0.049 Uiso 1 1 calc R U . . . C7 C 0.1480(4) 0.6775(4) 0.7557(4) 0.0405(15) Uani 1 1 d . . . . . H7 H 0.096684 0.695643 0.727470 0.049 Uiso 1 1 calc R U . . . C24 C 0.3053(4) 0.9019(4) 0.5368(3) 0.0368(14) Uani 1 1 d . . . . . H24A H 0.290348 0.899697 0.485134 0.055 Uiso 1 1 calc R U . . . H24B H 0.294246 0.963316 0.555238 0.055 Uiso 1 1 calc R U . . . H24C H 0.266489 0.858743 0.563100 0.055 Uiso 1 1 calc R U . . . C41 C 0.0431(4) 0.4323(5) 0.3622(4) 0.0442(16) Uani 1 1 d . . . . . H41 H -0.011081 0.418521 0.335856 0.053 Uiso 1 1 calc R U . . . C11 C 0.4094(4) 0.5284(4) 0.2264(3) 0.0373(14) Uani 1 1 d . . . . . H11 H 0.361189 0.495284 0.248787 0.045 Uiso 1 1 calc R U . . . C42 C 0.1162(4) 0.4754(4) 0.3276(3) 0.0351(13) Uani 1 1 d . . . . . C2 C 0.2273(4) 0.6470(4) 0.7214(3) 0.0346(13) Uani 1 1 d . . . . . C38 C 0.1754(4) 0.3780(4) 0.7780(3) 0.0394(15) Uani 1 1 d . . . . . H38A H 0.162626 0.436480 0.801060 0.059 Uiso 1 1 calc R U . . . H38B H 0.239267 0.360650 0.787306 0.059 Uiso 1 1 calc R U . . . H38C H 0.134258 0.331681 0.797840 0.059 Uiso 1 1 calc R U . . . C44 C 0.1141(4) 0.5011(5) 0.2488(3) 0.0460(17) Uani 1 1 d . . . . . H44A H 0.139543 0.451492 0.219753 0.069 Uiso 1 1 calc R U . . . H44B H 0.150834 0.556047 0.241288 0.069 Uiso 1 1 calc R U . . . H44C H 0.050590 0.512647 0.233930 0.069 Uiso 1 1 calc R U . . . C6 C 0.1428(5) 0.6817(5) 0.8305(4) 0.0544(19) Uani 1 1 d . . . . . H6 H 0.088322 0.702034 0.853529 0.065 Uiso 0.531(14) 1 calc R U P A 2 C14 C 0.5500(5) 0.6265(5) 0.1612(4) 0.0518(19) Uani 1 1 d . . . . . H14 H 0.597825 0.660118 0.138835 0.062 Uiso 1 1 calc R U . . . C3 C 0.3012(4) 0.6184(4) 0.7628(3) 0.0392(14) Uani 1 1 d . . . . . H3 H 0.354443 0.594756 0.739832 0.047 Uiso 1 1 calc R U . . . C13 C 0.4765(5) 0.5963(6) 0.1212(4) 0.058(2) Uani 1 1 d . . . . . H13 H 0.473755 0.609638 0.070957 0.070 Uiso 1 1 calc R U . . . C12 C 0.4055(4) 0.5462(6) 0.1533(4) 0.0503(18) Uani 1 1 d . . . . . C32 C 0.2900(6) 0.7232(5) 0.3122(4) 0.0540(19) Uani 1 1 d . . . . . H32 H 0.345239 0.697959 0.330726 0.065 Uiso 1 1 calc R U . . . C27 C 0.1339(5) 0.7629(5) 0.3322(4) 0.057(2) Uani 1 1 d . . . . . H27 H 0.081872 0.769250 0.362774 0.069 Uiso 1 1 calc R U . . . C4 C 0.2976(5) 0.6241(5) 0.8383(4) 0.0492(17) Uani 1 1 d . . . . . H4 H 0.348878 0.606621 0.866840 0.059 Uiso 0.469(14) 1 calc R U P A 1 C28 C 0.1304(6) 0.7890(6) 0.2568(5) 0.068(3) Uani 1 1 d . . . . . C30 C 0.2087(8) 0.7837(6) 0.2160(5) 0.081(3) Uani 1 1 d . . . . . H30 H 0.205630 0.803409 0.167096 0.097 Uiso 1 1 calc R U . . . C5 C 0.2180(6) 0.6558(5) 0.8711(4) 0.058(2) Uani 1 1 d . . . . . H5 H 0.215203 0.659804 0.922394 0.069 Uiso 1 1 calc R U . . . C31 C 0.2889(8) 0.7527(5) 0.2402(5) 0.070(2) Uani 1 1 d . . . . . H31 H 0.342069 0.750724 0.210446 0.083 Uiso 1 1 calc R U . . . C29 C 0.0437(6) 0.8106(7) 0.2217(5) 0.080(3) Uani 1 1 d . . . . . H29A H 0.017844 0.755480 0.200226 0.121 Uiso 1 1 calc R U . . . H29B H 0.054122 0.855853 0.183782 0.121 Uiso 1 1 calc R U . . . H29C H 0.000771 0.834992 0.257632 0.121 Uiso 1 1 calc R U . . . C16 C 0.3267(6) 0.5098(8) 0.1081(4) 0.090(4) Uani 1 1 d . . . . . H16A H 0.296585 0.460125 0.134135 0.135 Uiso 1 1 calc R U . . . H16B H 0.350397 0.487338 0.061825 0.135 Uiso 1 1 calc R U . . . H16C H 0.282313 0.558467 0.099226 0.135 Uiso 1 1 calc R U . . . C8A C 0.3811(9) 0.6011(10) 0.8876(7) 0.050(4) Uani 0.531(14) 1 d . . P A 2 H8AA H 0.431174 0.577029 0.857850 0.075 Uiso 0.531(14) 1 calc R U P A 2 H8AB H 0.362890 0.555685 0.923514 0.075 Uiso 0.531(14) 1 calc R U P A 2 H8AC H 0.401809 0.656235 0.912361 0.075 Uiso 0.531(14) 1 calc R U P A 2 C8 C 0.0514(12) 0.7053(11) 0.8621(8) 0.057(5) Uani 0.469(14) 1 d . . P A 1 H8A H 0.053037 0.767514 0.880697 0.086 Uiso 0.469(14) 1 calc R U P A 1 H8B H 0.037098 0.663358 0.901630 0.086 Uiso 0.469(14) 1 calc R U P A 1 H8C H 0.004117 0.700514 0.824529 0.086 Uiso 0.469(14) 1 calc R U P A 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 0.01779(15) 0.02555(17) 0.02632(17) -0.00033(13) -0.00198(11) -0.00125(12) O5 0.0229(18) 0.025(2) 0.038(2) 0.0000(17) -0.0039(17) -0.0038(15) O7 0.0198(18) 0.034(2) 0.0268(19) 0.0032(16) -0.0007(15) -0.0018(16) O3 0.0227(19) 0.028(2) 0.040(2) 0.0049(17) -0.0080(17) 0.0010(16) O8 0.0247(19) 0.034(2) 0.031(2) 0.0040(17) -0.0028(16) 0.0007(16) O6 0.025(2) 0.032(2) 0.046(2) -0.0050(19) -0.0022(18) -0.0019(17) O1 0.028(2) 0.032(2) 0.038(2) -0.0047(18) 0.0028(17) 0.0012(17) O2 0.030(2) 0.051(3) 0.038(2) -0.004(2) -0.0003(19) 0.0062(19) O4 0.026(2) 0.045(3) 0.048(3) -0.003(2) -0.0078(19) 0.0025(18) N1 0.027(2) 0.026(2) 0.032(3) 0.000(2) -0.002(2) -0.0026(19) N2 0.028(2) 0.031(3) 0.029(3) -0.002(2) -0.0009(19) 0.001(2) C18 0.032(3) 0.022(3) 0.029(3) -0.003(2) 0.000(2) -0.004(2) C33 0.022(3) 0.029(3) 0.039(3) -0.001(2) -0.001(2) -0.003(2) C17 0.026(3) 0.028(3) 0.028(3) 0.002(2) -0.004(2) 0.002(2) C9 0.025(3) 0.026(3) 0.027(3) 0.001(2) 0.001(2) 0.005(2) C23 0.029(3) 0.027(3) 0.031(3) 0.000(2) -0.002(2) -0.004(2) C25 0.034(3) 0.026(3) 0.041(4) -0.005(3) -0.005(3) -0.007(2) C39 0.030(3) 0.030(3) 0.036(3) 0.005(2) -0.004(2) -0.003(2) C19 0.025(3) 0.034(3) 0.024(3) -0.002(2) 0.001(2) -0.002(2) C40 0.028(3) 0.056(4) 0.038(4) 0.008(3) -0.007(3) -0.016(3) C1 0.029(3) 0.027(3) 0.041(3) -0.003(3) -0.003(3) -0.004(2) C10 0.030(3) 0.030(3) 0.025(3) -0.001(2) -0.003(2) 0.001(2) C36 0.022(3) 0.037(3) 0.035(3) 0.001(3) -0.003(2) -0.003(2) C21 0.039(3) 0.022(3) 0.029(3) -0.001(2) 0.002(2) 0.001(2) C34 0.027(3) 0.049(4) 0.043(4) 0.009(3) -0.004(3) -0.012(3) C43 0.021(3) 0.033(3) 0.031(3) 0.002(2) -0.003(2) -0.006(2) C20 0.038(3) 0.025(3) 0.034(3) -0.001(2) 0.001(3) -0.009(2) C22 0.031(3) 0.030(3) 0.028(3) 0.003(2) -0.001(2) 0.001(2) C15 0.035(3) 0.046(4) 0.038(4) 0.004(3) -0.005(3) -0.011(3) C26 0.052(4) 0.026(3) 0.042(4) 0.006(3) -0.021(3) -0.006(3) C37 0.031(3) 0.033(3) 0.035(3) 0.003(3) 0.003(2) -0.001(2) C35 0.032(3) 0.051(4) 0.039(4) 0.014(3) 0.005(3) -0.011(3) C7 0.038(3) 0.040(4) 0.044(4) -0.001(3) 0.009(3) -0.003(3) C24 0.035(3) 0.033(3) 0.042(4) -0.006(3) -0.003(3) 0.007(3) C41 0.028(3) 0.056(4) 0.048(4) 0.008(3) -0.014(3) -0.018(3) C11 0.035(3) 0.052(4) 0.025(3) 0.001(3) -0.004(2) 0.000(3) C42 0.030(3) 0.041(3) 0.034(3) 0.000(3) -0.008(2) -0.003(3) C2 0.038(3) 0.024(3) 0.042(4) -0.001(3) 0.004(3) -0.004(2) C38 0.039(3) 0.042(4) 0.037(4) 0.006(3) 0.008(3) -0.004(3) C44 0.037(3) 0.066(5) 0.034(3) 0.006(3) -0.011(3) -0.015(3) C6 0.059(5) 0.056(5) 0.048(4) 0.003(4) 0.021(4) 0.004(4) C14 0.050(4) 0.071(5) 0.035(4) 0.014(3) -0.001(3) -0.019(4) C3 0.040(4) 0.035(3) 0.042(4) 0.002(3) 0.001(3) 0.002(3) C13 0.054(4) 0.095(6) 0.027(3) 0.014(4) -0.004(3) -0.014(4) C12 0.033(3) 0.084(5) 0.033(4) 0.008(4) -0.010(3) -0.008(3) C32 0.080(5) 0.037(4) 0.045(4) 0.003(3) 0.015(4) 0.001(4) C27 0.047(4) 0.053(4) 0.071(5) 0.032(4) -0.026(4) -0.022(3) C4 0.054(4) 0.050(4) 0.043(4) 0.010(3) 0.002(3) -0.003(3) C28 0.070(6) 0.062(5) 0.071(6) 0.028(4) -0.052(5) -0.019(4) C30 0.120(9) 0.066(6) 0.058(6) 0.015(5) -0.007(6) -0.056(6) C5 0.069(5) 0.065(5) 0.039(4) 0.010(4) 0.014(4) 0.005(4) C31 0.113(8) 0.034(4) 0.062(5) 0.006(4) -0.012(5) -0.010(4) C29 0.082(6) 0.075(6) 0.084(7) 0.022(5) -0.008(5) 0.006(5) C16 0.055(5) 0.174(11) 0.040(4) 0.017(6) -0.021(4) -0.044(6) C8A 0.048(8) 0.066(9) 0.037(7) 0.010(6) -0.006(6) -0.004(7) C8 0.086(13) 0.046(9) 0.040(9) -0.003(7) 0.028(8) 0.008(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 La1 40.74(9) . 3_666 ? O5 La1 La1 35.43(7) 3_666 3_666 ? O5 La1 O5 76.18(13) . 3_666 ? O5 La1 O7 77.47(12) . . ? O5 La1 O3 83.24(12) . . ? O5 La1 O8 77.32(12) . 3_666 ? O5 La1 O6 125.33(12) . 3_666 ? O5 La1 O1 83.30(12) . . ? O5 La1 N1 147.09(13) . . ? O5 La1 N2 148.58(13) . . ? O5 La1 C17 101.19(13) . 3_666 ? O5 La1 C17 25.07(12) 3_666 3_666 ? O7 La1 La1 67.69(8) . 3_666 ? O7 La1 O5 68.15(11) . 3_666 ? O7 La1 O6 78.81(13) . 3_666 ? O7 La1 O1 141.92(13) . . ? O7 La1 N1 135.43(13) . . ? O7 La1 N2 79.40(12) . . ? O7 La1 C17 72.15(13) . 3_666 ? O3 La1 La1 115.88(9) . 3_666 ? O3 La1 O5 138.92(12) . 3_666 ? O3 La1 O7 72.91(12) . . ? O3 La1 O8 141.86(13) . 3_666 ? O3 La1 O6 133.72(13) . 3_666 ? O3 La1 O1 72.41(13) . . ? O3 La1 N1 104.20(13) . . ? O3 La1 N2 69.75(13) . . ? O3 La1 C17 142.80(14) . 3_666 ? O8 La1 La1 66.67(8) 3_666 3_666 ? O8 La1 O5 66.78(12) 3_666 3_666 ? O8 La1 O7 132.24(12) 3_666 . ? O8 La1 O6 83.73(13) 3_666 3_666 ? O8 La1 O1 72.96(13) 3_666 . ? O8 La1 N1 77.62(13) 3_666 . ? O8 La1 N2 134.05(13) 3_666 . ? O8 La1 C17 73.87(13) 3_666 3_666 ? O6 La1 La1 84.66(8) 3_666 3_666 ? O6 La1 O5 49.29(11) 3_666 3_666 ? O6 La1 O1 138.15(13) 3_666 . ? O6 La1 N1 72.22(13) 3_666 . ? O6 La1 N2 69.57(13) 3_666 . ? O6 La1 C17 24.22(13) 3_666 3_666 ? O1 La1 La1 115.35(9) . 3_666 ? O1 La1 O5 137.78(12) . 3_666 ? O1 La1 N1 69.16(13) . . ? O1 La1 N2 102.69(13) . . ? O1 La1 C17 144.59(14) . 3_666 ? N1 La1 La1 139.27(10) . 3_666 ? N1 La1 O5 112.43(12) . 3_666 ? N1 La1 N2 59.19(14) . . ? N1 La1 C17 91.93(14) . 3_666 ? N2 La1 La1 141.60(10) . 3_666 ? N2 La1 O5 114.07(12) . 3_666 ? N2 La1 C17 91.56(14) . 3_666 ? C17 La1 La1 60.47(10) 3_666 3_666 ? La1 O5 La1 103.82(13) . 3_666 ? C17 O5 La1 89.2(3) . 3_666 ? C17 O5 La1 166.5(4) . . ? C9 O7 La1 135.2(3) . . ? C25 O3 La1 146.9(4) . . ? C9 O8 La1 137.8(3) . 3_666 ? C17 O6 La1 100.6(3) . 3_666 ? C1 O1 La1 141.9(4) . . ? C1 O2 H2 109.5 . . ? C33 N1 La1 124.1(4) . . ? C36 N1 La1 117.8(3) . . ? C36 N1 C33 118.1(5) . . ? C39 N2 La1 123.0(4) . . ? C43 N2 La1 117.9(3) . . ? C43 N2 C39 119.1(5) . . ? C23 C18 C17 120.5(5) . . ? C23 C18 C19 119.9(5) . . ? C19 C18 C17 119.6(5) . . ? N1 C33 C39 116.5(5) . . ? N1 C33 C34 120.3(5) . . ? C34 C33 C39 123.2(5) . . ? O5 C17 La1 65.7(3) . 3_666 ? O5 C17 C18 119.7(5) . . ? O6 C17 La1 55.2(3) . 3_666 ? O6 C17 O5 120.9(5) . . ? O6 C17 C18 119.4(5) . . ? C18 C17 La1 174.3(4) . 3_666 ? O7 C9 C10 117.9(5) . . ? O8 C9 O7 125.4(5) . . ? O8 C9 C10 116.7(5) . . ? C18 C23 H23 119.5 . . ? C18 C23 C22 121.0(5) . . ? C22 C23 H23 119.5 . . ? O3 C25 O4 123.1(6) . . ? O3 C25 C26 117.9(5) . . ? O4 C25 C26 119.0(5) . . ? N2 C39 C33 117.2(5) . . ? N2 C39 C40 120.5(5) . . ? C40 C39 C33 122.3(5) . . ? C18 C19 H19 120.5 . . ? C20 C19 C18 119.0(5) . . ? C20 C19 H19 120.5 . . ? C39 C40 H40 120.2 . . ? C41 C40 C39 119.5(6) . . ? C41 C40 H40 120.2 . . ? O1 C1 O2 124.4(6) . . ? O1 C1 C2 120.7(5) . . ? O2 C1 C2 114.9(5) . . ? C15 C10 C9 120.7(5) . . ? C11 C10 C9 120.2(5) . . ? C11 C10 C15 119.1(5) . . ? N1 C36 H36 117.6 . . ? N1 C36 C37 124.8(5) . . ? C37 C36 H36 117.6 . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C22 C21 C20 120.8(5) . . ? C33 C34 H34 120.0 . . ? C35 C34 C33 120.0(6) . . ? C35 C34 H34 120.0 . . ? N2 C43 H43 118.0 . . ? N2 C43 C42 123.9(5) . . ? C42 C43 H43 118.0 . . ? C19 C20 H20 119.6 . . ? C21 C20 C19 120.8(5) . . ? C21 C20 H20 119.6 . . ? C23 C22 C24 119.9(5) . . ? C21 C22 C23 118.5(5) . . ? C21 C22 C24 121.5(5) . . ? C10 C15 H15 119.7 . . ? C14 C15 C10 120.6(6) . . ? C14 C15 H15 119.7 . . ? C32 C26 C25 120.2(6) . . ? C27 C26 C25 120.3(7) . . ? C27 C26 C32 119.4(7) . . ? C36 C37 C38 121.0(5) . . ? C35 C37 C36 116.9(5) . . ? C35 C37 C38 122.1(5) . . ? C34 C35 H35 120.1 . . ? C37 C35 C34 119.8(5) . . ? C37 C35 H35 120.1 . . ? C2 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C6 C7 C2 120.9(7) . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C40 C41 H41 119.8 . . ? C40 C41 C42 120.5(5) . . ? C42 C41 H41 119.8 . . ? C10 C11 H11 119.6 . . ? C12 C11 C10 120.9(6) . . ? C12 C11 H11 119.6 . . ? C43 C42 C41 116.4(5) . . ? C43 C42 C44 120.7(5) . . ? C41 C42 C44 122.9(5) . . ? C7 C2 C1 121.1(6) . . ? C3 C2 C1 119.4(5) . . ? C3 C2 C7 119.5(6) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C7 C6 H6 120.4 . . ? C7 C6 C8 116.6(9) . . ? C5 C6 C7 119.2(7) . . ? C5 C6 H6 120.4 . . ? C5 C6 C8 123.9(9) . . ? C15 C14 H14 120.4 . . ? C13 C14 C15 119.3(6) . . ? C13 C14 H14 120.4 . . ? C2 C3 H3 119.9 . . ? C2 C3 C4 120.1(6) . . ? C4 C3 H3 119.9 . . ? C14 C13 H13 119.4 . . ? C14 C13 C12 121.2(6) . . ? C12 C13 H13 119.4 . . ? C11 C12 C13 118.9(6) . . ? C11 C12 C16 120.2(6) . . ? C13 C12 C16 120.8(6) . . ? C26 C32 H32 118.3 . . ? C26 C32 C31 123.5(8) . . ? C31 C32 H32 118.3 . . ? C26 C27 H27 121.2 . . ? C26 C27 C28 117.6(8) . . ? C28 C27 H27 121.2 . . ? C3 C4 H4 120.4 . . ? C3 C4 C8A 122.7(8) . . ? C5 C4 C3 119.1(7) . . ? C5 C4 H4 120.4 . . ? C5 C4 C8A 118.1(8) . . ? C27 C28 C29 121.2(9) . . ? C30 C28 C27 119.1(7) . . ? C30 C28 C29 119.4(9) . . ? C28 C30 H30 117.8 . . ? C31 C30 C28 124.4(9) . . ? C31 C30 H30 117.8 . . ? C6 C5 C4 121.1(7) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C32 C31 H31 122.1 . . ? C30 C31 C32 115.8(10) . . ? C30 C31 H31 122.1 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C4 C8A H8AA 109.5 . . ? C4 C8A H8AB 109.5 . . ? C4 C8A H8AC 109.5 . . ? H8AA C8A H8AB 109.5 . . ? H8AA C8A H8AC 109.5 . . ? H8AB C8A H8AC 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? 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 La1 4.1162(7) 3_666 ? La1 O5 2.458(4) . ? La1 O5 2.767(4) 3_666 ? La1 O7 2.508(4) . ? La1 O3 2.492(4) . ? La1 O8 2.497(4) 3_666 ? La1 O6 2.534(4) 3_666 ? La1 O1 2.536(4) . ? La1 N1 2.722(4) . ? La1 N2 2.732(5) . ? La1 C17 3.035(5) 3_666 ? O5 C17 1.286(6) . ? O7 C9 1.271(6) . ? O3 C25 1.253(7) . ? O8 C9 1.263(6) . ? O6 C17 1.267(6) . ? O1 C1 1.249(7) . ? O2 H2 0.8400 . ? O2 C1 1.290(7) . ? O4 C25 1.286(7) . ? N1 C33 1.353(7) . ? N1 C36 1.339(7) . ? N2 C39 1.363(7) . ? N2 C43 1.328(7) . ? C18 C17 1.492(8) . ? C18 C23 1.391(8) . ? C18 C19 1.396(7) . ? C33 C39 1.468(8) . ? C33 C34 1.403(8) . ? C9 C10 1.512(7) . ? C23 H23 0.9500 . ? C23 C22 1.395(8) . ? C25 C26 1.509(8) . ? C39 C40 1.384(8) . ? C19 H19 0.9500 . ? C19 C20 1.387(8) . ? C40 H40 0.9500 . ? C40 C41 1.377(9) . ? C1 C2 1.498(8) . ? C10 C15 1.399(8) . ? C10 C11 1.392(8) . ? C36 H36 0.9500 . ? C36 C37 1.387(8) . ? C21 H21 0.9500 . ? C21 C20 1.386(8) . ? C21 C22 1.385(8) . ? C34 H34 0.9500 . ? C34 C35 1.381(9) . ? C43 H43 0.9500 . ? C43 C42 1.389(7) . ? C20 H20 0.9500 . ? C22 C24 1.519(8) . ? C15 H15 0.9500 . ? C15 C14 1.385(9) . ? C26 C32 1.387(10) . ? C26 C27 1.366(9) . ? C37 C35 1.379(8) . ? C37 C38 1.508(8) . ? C35 H35 0.9500 . ? C7 H7 0.9500 . ? C7 C2 1.393(8) . ? C7 C6 1.385(9) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C41 H41 0.9500 . ? C41 C42 1.395(8) . ? C11 H11 0.9500 . ? C11 C12 1.378(8) . ? C42 C44 1.505(8) . ? C2 C3 1.387(8) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C6 H6 0.9500 . ? C6 C5 1.381(11) . ? C6 C8 1.496(16) . ? C14 H14 0.9500 . ? C14 C13 1.376(9) . ? C3 H3 0.9500 . ? C3 C4 1.400(9) . ? C13 H13 0.9500 . ? C13 C12 1.402(10) . ? C12 C16 1.517(9) . ? C32 H32 0.9500 . ? C32 C31 1.401(11) . ? C27 H27 0.9500 . ? C27 C28 1.447(11) . ? C4 H4 0.9500 . ? C4 C5 1.389(10) . ? C4 C8A 1.557(14) . ? C28 C30 1.370(13) . ? C28 C29 1.455(11) . ? C30 H30 0.9500 . ? C30 C31 1.332(13) . ? C5 H5 0.9500 . ? C31 H31 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C8A H8AA 0.9800 . ? C8A H8AB 0.9800 . ? C8A H8AC 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? 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 _geom_hbond_publ_flag O2 H2 O4 0.84 1.66 2.443(6) 154.0 . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag La1 O5 C17 La1 164.5(15) . . . 3_666 ? La1 O5 C17 O6 163.6(12) . . . . ? La1 O5 C17 O6 -0.9(5) 3_666 . . . ? La1 O5 C17 C18 -17.5(18) . . . . ? La1 O5 C17 C18 178.0(5) 3_666 . . . ? La1 O7 C9 O8 18.1(8) . . . . ? La1 O7 C9 C10 -160.9(3) . . . . ? La1 O3 C25 O4 48.7(10) . . . . ? La1 O3 C25 C26 -129.9(6) . . . . ? La1 O8 C9 O7 17.8(9) 3_666 . . . ? La1 O8 C9 C10 -163.2(4) 3_666 . . . ? La1 O6 C17 O5 1.0(6) 3_666 . . . ? La1 O6 C17 C18 -177.9(4) 3_666 . . . ? La1 O1 C1 O2 -46.6(9) . . . . ? La1 O1 C1 C2 134.7(5) . . . . ? La1 N1 C33 C39 -2.8(7) . . . . ? La1 N1 C33 C34 178.2(4) . . . . ? La1 N1 C36 C37 179.2(5) . . . . ? La1 N2 C39 C33 1.7(7) . . . . ? La1 N2 C39 C40 -179.9(5) . . . . ? La1 N2 C43 C42 -178.9(5) . . . . ? O7 C9 C10 C15 159.6(5) . . . . ? O7 C9 C10 C11 -21.5(8) . . . . ? O3 C25 C26 C32 -6.0(8) . . . . ? O3 C25 C26 C27 170.8(6) . . . . ? O8 C9 C10 C15 -19.5(8) . . . . ? O8 C9 C10 C11 159.4(5) . . . . ? O1 C1 C2 C7 -179.9(5) . . . . ? O1 C1 C2 C3 -0.5(8) . . . . ? O2 C1 C2 C7 1.4(8) . . . . ? O2 C1 C2 C3 -179.2(5) . . . . ? O4 C25 C26 C32 175.4(6) . . . . ? O4 C25 C26 C27 -7.8(9) . . . . ? N1 C33 C39 N2 0.7(8) . . . . ? N1 C33 C39 C40 -177.7(6) . . . . ? N1 C33 C34 C35 1.9(9) . . . . ? N1 C36 C37 C35 3.1(9) . . . . ? N1 C36 C37 C38 -176.5(6) . . . . ? N2 C39 C40 C41 -0.8(10) . . . . ? N2 C43 C42 C41 -1.7(9) . . . . ? N2 C43 C42 C44 -180.0(6) . . . . ? C18 C23 C22 C21 -1.6(8) . . . . ? C18 C23 C22 C24 177.8(5) . . . . ? C18 C19 C20 C21 -0.1(8) . . . . ? C33 N1 C36 C37 -1.4(9) . . . . ? C33 C39 C40 C41 177.6(6) . . . . ? C33 C34 C35 C37 -0.2(10) . . . . ? C17 C18 C23 C22 -179.2(5) . . . . ? C17 C18 C19 C20 -179.9(5) . . . . ? C9 C10 C15 C14 179.3(6) . . . . ? C9 C10 C11 C12 -178.6(6) . . . . ? C23 C18 C17 O5 -9.2(8) . . . . ? C23 C18 C17 O6 169.7(5) . . . . ? C23 C18 C19 C20 0.4(8) . . . . ? C25 C26 C32 C31 178.2(6) . . . . ? C25 C26 C27 C28 -174.8(6) . . . . ? C39 N2 C43 C42 0.9(9) . . . . ? C39 C33 C34 C35 -177.0(6) . . . . ? C39 C40 C41 C42 0.0(11) . . . . ? C19 C18 C17 O5 171.2(5) . . . . ? C19 C18 C17 O6 -9.9(8) . . . . ? C19 C18 C23 C22 0.5(8) . . . . ? C40 C41 C42 C43 1.2(10) . . . . ? C40 C41 C42 C44 179.5(7) . . . . ? C1 C2 C3 C4 177.6(6) . . . . ? C10 C15 C14 C13 -0.3(11) . . . . ? C10 C11 C12 C13 -1.0(11) . . . . ? C10 C11 C12 C16 177.5(8) . . . . ? C36 N1 C33 C39 177.8(5) . . . . ? C36 N1 C33 C34 -1.1(8) . . . . ? C36 C37 C35 C34 -2.1(9) . . . . ? C34 C33 C39 N2 179.7(6) . . . . ? C34 C33 C39 C40 1.2(9) . . . . ? C43 N2 C39 C33 -178.0(5) . . . . ? C43 N2 C39 C40 0.4(9) . . . . ? C20 C21 C22 C23 1.9(8) . . . . ? C20 C21 C22 C24 -177.5(5) . . . . ? C22 C21 C20 C19 -1.1(9) . . . . ? C15 C10 C11 C12 0.3(10) . . . . ? C15 C14 C13 C12 -0.4(13) . . . . ? C26 C32 C31 C30 -2.9(11) . . . . ? C26 C27 C28 C30 -3.9(11) . . . . ? C26 C27 C28 C29 169.0(8) . . . . ? C7 C2 C3 C4 -3.0(9) . . . . ? C7 C6 C5 C4 -1.3(12) . . . . ? C11 C10 C15 C14 0.4(10) . . . . ? C2 C7 C6 C5 0.5(11) . . . . ? C2 C7 C6 C8 -173.3(9) . . . . ? C2 C3 C4 C5 2.3(10) . . . . ? C2 C3 C4 C8A -174.5(8) . . . . ? C38 C37 C35 C34 177.5(6) . . . . ? C6 C7 C2 C1 -179.0(6) . . . . ? C6 C7 C2 C3 1.6(9) . . . . ? C14 C13 C12 C11 1.0(13) . . . . ? C14 C13 C12 C16 -177.4(9) . . . . ? C3 C4 C5 C6 -0.1(12) . . . . ? C32 C26 C27 C28 2.0(10) . . . . ? C27 C26 C32 C31 1.4(11) . . . . ? C27 C28 C30 C31 2.5(13) . . . . ? C28 C30 C31 C32 0.8(13) . . . . ? C29 C28 C30 C31 -170.5(9) . . . . ? C8A C4 C5 C6 176.9(9) . . . . ? C8 C6 C5 C4 172.1(10) . . . . ?