#------------------------------------------------------------------------------ #$Date: 2019-05-21 04:37:11 +0300 (Tue, 21 May 2019) $ #$Revision: 215338 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/00/7700030.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_7700030 loop_ _publ_author_name 'Fecker, Ann Christin' 'Freytag, Matthias' 'Jones, Peter G.' 'Walter, Marc D.' _publ_section_title ; Synthesis and molecular structure of enantiomerically pure pentadienyl complexes of the rare-earth metals ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C9DT01721F _journal_year 2019 _chemical_absolute_configuration ad _chemical_formula_sum 'C39 H57 La' _chemical_formula_weight 664.75 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2017/1 _audit_update_record ; 2019-04-24 deposited with the CCDC. 2019-05-10 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.105(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.5001(6) _cell_length_b 18.0623(18) _cell_length_c 19.7718(15) _cell_measurement_reflns_used 5970 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.7120 _cell_measurement_theta_min 2.4220 _cell_volume 3366.7(5) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 16.1419 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1899 _diffrn_reflns_av_unetI/netI 0.1022 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 144004 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 2.076 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 1.293 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.95582 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1392 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _refine_diff_density_max 1.115 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.115 _refine_ls_abs_structure_details ; Flack x determined using 4520 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.014(11) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 811 _refine_ls_number_reflns 13782 _refine_ls_number_restraints 565 _refine_ls_restrained_S_all 1.010 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_gt 0.0519 _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^)+(0.0193P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.0845 _reflns_Friedel_coverage 0.936 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 11494 _reflns_number_total 13782 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt01721f2.cif _cod_data_source_block ann48 _cod_database_code 7700030 _shelx_shelxl_version_number 2017/1 _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_min 0.830 _shelx_estimated_absorpt_t_max 0.962 _shelx_res_file ; TITL ann48 in P2(1) shelx.res created by SHELXL-2017/1 at 10:34:43 on 17-Apr-2019 CELL 0.71073 9.500090 18.062280 19.771831 90.0000 97.1053 90.0000 ZERR 4.00 0.000600 0.001800 0.001500 0.0000 0.0060 0.0000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H LA UNIT 156 228 4 TEMP -173 SIZE 0.15 0.12 0.03 FMAP 2 PLAN 10 L.S. 10 SHEL 999 0.8 ACTA CONF C101 > C313 C401 > C413 RTAB CONT LA1 C105 RTAB CONT LA1 C205 RTAB CONT LA1 C305 RTAB CONT LA2 C405 RTAB CONT LA2 C505 RTAB CONT LA2 C605 SADI C101 H10X C101 H10Y C201 H20X C201 H20Y C301 H30X C301 H30Y = C401 H40X C401 H40Y C501 H50X C501 H50Y C601 H60X C601 H60Y SADI C103 H103 C203 H203 C303 H303 C403 H403 C503 H503 C603 H603 SADI C105 H105 C205 H205 C305 H305 C405 H405 C505 H505 C605 H605 ISOR $C 0.0025 WGHT 0.019300 FVAR 0.62041 LA1 3 0.764181 0.205522 0.677649 11.00000 0.01215 0.01541 = 0.01476 -0.00035 0.00080 -0.00053 C101 1 0.487003 0.170981 0.707622 11.00000 0.02095 0.02237 = 0.02430 0.00196 0.00479 -0.00284 H10X 2 0.489087 0.220097 0.723394 11.00000 -1.20000 H10Y 2 0.470758 0.134313 0.740007 11.00000 -1.20000 C102 1 0.484700 0.148208 0.641486 11.00000 0.01384 0.01645 = 0.01980 -0.00016 -0.00441 0.00119 C103 1 0.523008 0.188995 0.586395 11.00000 0.01436 0.01981 = 0.01884 -0.00364 0.00169 0.00131 H103 2 0.529203 0.157246 0.550412 11.00000 -1.20000 C104 1 0.538286 0.266918 0.578344 11.00000 0.01420 0.02115 = 0.01890 -0.00053 -0.00261 0.00022 C105 1 0.535832 0.322487 0.625023 11.00000 0.01946 0.02281 = 0.01881 0.00101 0.00154 -0.00014 H105 2 0.503922 0.314164 0.667015 11.00000 -1.20000 C106 1 0.542794 0.403068 0.604187 11.00000 0.01910 0.02229 = 0.02474 -0.00131 0.00112 0.00177 AFIX 23 H10A 2 0.453986 0.428477 0.612151 11.00000 -1.20000 H10B 2 0.622677 0.427726 0.632366 11.00000 -1.20000 AFIX 0 C107 1 0.563037 0.409053 0.529564 11.00000 0.01886 0.02207 = 0.02002 0.00185 0.00362 0.00020 AFIX 13 H107 2 0.572629 0.460555 0.512147 11.00000 -1.20000 AFIX 0 C108 1 0.681122 0.355293 0.516042 11.00000 0.02277 0.02403 = 0.02170 -0.00233 0.00258 0.00035 AFIX 23 H10C 2 0.755146 0.348061 0.555339 11.00000 -1.20000 H10D 2 0.723422 0.365589 0.473702 11.00000 -1.20000 AFIX 0 C109 1 0.564981 0.294821 0.508551 11.00000 0.01467 0.01788 = 0.01734 -0.00201 0.00189 0.00139 AFIX 13 H109 2 0.575964 0.255647 0.473849 11.00000 -1.20000 AFIX 0 C110 1 0.457872 0.358641 0.484675 11.00000 0.02221 0.02044 = 0.01965 0.00033 0.00334 0.00213 C111 1 0.305810 0.353801 0.500536 11.00000 0.01241 0.02343 = 0.03299 -0.00050 -0.00205 0.00053 AFIX 137 H11A 2 0.260254 0.402329 0.493404 11.00000 -1.50000 H11B 2 0.305158 0.338612 0.548080 11.00000 -1.50000 H11C 2 0.253864 0.317337 0.470362 11.00000 -1.50000 AFIX 0 C112 1 0.456391 0.373953 0.409030 11.00000 0.02636 0.02378 = 0.02582 0.00042 -0.00056 -0.00118 AFIX 137 H11D 2 0.405375 0.420247 0.397251 11.00000 -1.50000 H11E 2 0.408784 0.333147 0.382709 11.00000 -1.50000 H11F 2 0.554059 0.378340 0.398338 11.00000 -1.50000 AFIX 0 C113 1 0.452582 0.067209 0.627754 11.00000 0.02548 0.02560 = 0.03771 0.00239 -0.00232 0.00001 AFIX 137 H11G 2 0.483326 0.038318 0.668891 11.00000 -1.50000 H11H 2 0.503292 0.050094 0.590423 11.00000 -1.50000 H11I 2 0.350313 0.060721 0.615047 11.00000 -1.50000 AFIX 0 C201 1 0.787000 0.212049 0.821622 11.00000 0.02581 0.02599 = 0.02157 0.00132 0.00688 -0.00389 H20X 2 0.748689 0.177436 0.850278 11.00000 -1.20000 H20Y 2 0.876853 0.194534 0.814528 11.00000 -1.20000 C202 1 0.738191 0.280575 0.802843 11.00000 0.01904 0.02132 = 0.01950 -0.00581 0.00050 -0.00421 C203 1 0.790899 0.329166 0.756882 11.00000 0.01390 0.01563 = 0.01546 -0.00163 -0.00042 -0.00088 H203 2 0.744990 0.373911 0.751795 11.00000 -1.20000 C204 1 0.928288 0.330851 0.732964 11.00000 0.01423 0.01347 = 0.01277 -0.00243 0.00108 -0.00215 C205 1 1.036670 0.283109 0.745184 11.00000 0.02042 0.01955 = 0.01668 0.00037 0.00202 -0.00278 H205 2 1.045243 0.242347 0.774426 11.00000 -1.20000 C206 1 1.181030 0.301039 0.723903 11.00000 0.01529 0.02230 = 0.02382 -0.00021 0.00502 0.00147 AFIX 23 H20A 2 1.251797 0.305310 0.764898 11.00000 -1.20000 H20B 2 1.211122 0.260424 0.695283 11.00000 -1.20000 AFIX 0 C207 1 1.175061 0.372906 0.684307 11.00000 0.01555 0.01935 = 0.01646 0.00135 0.00167 -0.00156 AFIX 13 H207 2 1.265566 0.387719 0.667042 11.00000 -1.20000 AFIX 0 C208 1 1.043055 0.370104 0.629806 11.00000 0.02208 0.02446 = 0.02363 0.00100 0.00447 0.00051 AFIX 23 H20C 2 1.017953 0.319886 0.612211 11.00000 -1.20000 H20D 2 1.044637 0.406294 0.592303 11.00000 -1.20000 AFIX 0 C209 1 0.958719 0.396106 0.688229 11.00000 0.01411 0.01566 = 0.01548 -0.00112 -0.00124 0.00188 AFIX 13 H209 2 0.876522 0.429634 0.674182 11.00000 -1.20000 AFIX 0 C210 1 1.099168 0.435445 0.720136 11.00000 0.01569 0.01752 = 0.02067 0.00090 0.00087 -0.00115 C211 1 1.124985 0.442147 0.797082 11.00000 0.02195 0.01965 = 0.02907 -0.00321 -0.00263 -0.00461 AFIX 137 H21A 2 1.220475 0.461767 0.810665 11.00000 -1.50000 H21B 2 1.116466 0.393245 0.817660 11.00000 -1.50000 H21C 2 1.054705 0.475762 0.812676 11.00000 -1.50000 AFIX 0 C212 1 1.114508 0.511727 0.689547 11.00000 0.02622 0.03418 = 0.03484 0.00392 0.00271 -0.00259 AFIX 137 H21D 2 1.042030 0.544851 0.703864 11.00000 -1.50000 H21E 2 1.102473 0.508021 0.639716 11.00000 -1.50000 H21F 2 1.208917 0.531524 0.705325 11.00000 -1.50000 AFIX 0 C213 1 0.598212 0.304487 0.827279 11.00000 0.02802 0.04360 = 0.03067 -0.01464 0.01311 -0.00992 AFIX 137 H21G 2 0.548626 0.260824 0.841845 11.00000 -1.50000 H21H 2 0.538644 0.329141 0.789933 11.00000 -1.50000 H21I 2 0.617830 0.338792 0.865689 11.00000 -1.50000 AFIX 0 C301 1 0.812416 0.056462 0.713769 11.00000 0.02004 0.01916 = 0.01834 0.00082 0.00039 -0.00086 H30X 2 0.756173 0.046101 0.672394 11.00000 -1.20000 H30Y 2 0.778431 0.032139 0.750616 11.00000 -1.20000 C302 1 0.949298 0.083648 0.714571 11.00000 0.01791 0.01721 = 0.02018 -0.00028 -0.00089 0.00467 C303 1 1.002743 0.121923 0.661486 11.00000 0.01385 0.01695 = 0.01719 -0.00272 -0.00009 0.00234 H303 2 1.094760 0.138364 0.670656 11.00000 -1.20000 C304 1 0.951455 0.127600 0.590662 11.00000 0.01427 0.01231 = 0.01478 -0.00242 0.00363 0.00161 C305 1 0.827620 0.103094 0.556718 11.00000 0.01948 0.01878 = 0.01803 0.00040 0.00231 -0.00129 H305 2 0.773247 0.065586 0.574228 11.00000 -1.20000 C306 1 0.798884 0.108241 0.479967 11.00000 0.01857 0.01954 = 0.01646 -0.00124 0.00022 0.00127 AFIX 23 H30A 2 0.710431 0.136545 0.466971 11.00000 -1.20000 H30B 2 0.785716 0.057905 0.460391 11.00000 -1.20000 AFIX 0 C307 1 0.921171 0.146176 0.451351 11.00000 0.01609 0.01626 = 0.01385 -0.00086 0.00158 0.00292 AFIX 13 H307 2 0.909654 0.153079 0.400786 11.00000 -1.20000 AFIX 0 C308 1 0.958975 0.216925 0.494430 11.00000 0.01883 0.02105 = 0.02047 -0.00020 0.00544 0.00132 AFIX 23 H30C 2 1.015059 0.253813 0.472141 11.00000 -1.20000 H30D 2 0.877111 0.240274 0.512555 11.00000 -1.20000 AFIX 0 C309 1 1.048942 0.165674 0.545902 11.00000 0.01973 0.01931 = 0.02022 -0.00023 0.00144 -0.00052 AFIX 13 H309 2 1.137906 0.187648 0.570053 11.00000 -1.20000 AFIX 0 C310 1 1.067076 0.114649 0.483513 11.00000 0.01864 0.01665 = 0.01401 -0.00166 0.00301 0.00133 C311 1 1.082944 0.031681 0.496263 11.00000 0.01792 0.02403 = 0.02682 -0.00674 0.00003 0.00548 AFIX 137 H31A 2 1.093153 0.006388 0.453291 11.00000 -1.50000 H31B 2 0.998677 0.012889 0.514660 11.00000 -1.50000 H31C 2 1.167204 0.022413 0.529039 11.00000 -1.50000 AFIX 0 C312 1 1.189857 0.139110 0.445977 11.00000 0.02336 0.03238 = 0.02371 -0.00545 0.00445 0.00420 AFIX 137 H31D 2 1.279788 0.124253 0.472153 11.00000 -1.50000 H31E 2 1.187755 0.193064 0.440717 11.00000 -1.50000 H31F 2 1.181012 0.115750 0.400914 11.00000 -1.50000 AFIX 0 C313 1 1.046934 0.077854 0.781189 11.00000 0.02052 0.02647 = 0.02671 0.00367 -0.00319 0.00285 AFIX 137 H31G 2 0.990012 0.074074 0.819136 11.00000 -1.50000 H31H 2 1.107119 0.122015 0.787167 11.00000 -1.50000 H31I 2 1.106707 0.033734 0.780274 11.00000 -1.50000 AFIX 0 LA2 3 0.109696 0.258627 0.075001 11.00000 0.01375 0.01938 = 0.01465 -0.00003 0.00293 -0.00203 C401 1 0.110458 0.301257 -0.060683 11.00000 0.02789 0.02516 = 0.02422 0.00027 0.00376 -0.00077 H40X 2 0.062276 0.272283 -0.095987 11.00000 -1.20000 H40Y 2 0.088041 0.348579 -0.044980 11.00000 -1.20000 C402 1 0.249366 0.280568 -0.041889 11.00000 0.02406 0.02526 = 0.02136 0.00173 0.00683 -0.00555 C403 1 0.341336 0.308768 0.014591 11.00000 0.01722 0.01863 = 0.02033 -0.00057 0.00463 -0.00017 H403 2 0.429540 0.287453 0.023905 11.00000 -1.20000 C404 1 0.326054 0.372731 0.055661 11.00000 0.01540 0.01238 = 0.01780 0.00296 0.00322 -0.00409 C405 1 0.212701 0.418007 0.058024 11.00000 0.01916 0.02156 = 0.01722 0.00151 0.00231 0.00006 H405 2 0.134233 0.412630 0.023788 11.00000 -1.20000 C406 1 0.222686 0.486373 0.100728 11.00000 0.01975 0.02267 = 0.02351 0.00125 0.00344 0.00240 AFIX 23 H40A 2 0.149097 0.484898 0.132051 11.00000 -1.20000 H40B 2 0.204432 0.530244 0.070918 11.00000 -1.20000 AFIX 0 C407 1 0.368012 0.493618 0.141999 11.00000 0.02198 0.02217 = 0.02161 0.00068 0.00138 0.00160 AFIX 13 H407 2 0.381929 0.537474 0.172973 11.00000 -1.20000 AFIX 0 C408 1 0.405922 0.417104 0.175239 11.00000 0.02369 0.02521 = 0.02553 0.00147 0.00181 -0.00336 AFIX 23 H40C 2 0.323294 0.388846 0.187318 11.00000 -1.20000 H40D 2 0.483388 0.418601 0.213622 11.00000 -1.20000 AFIX 0 C409 1 0.454377 0.395041 0.105709 11.00000 0.01637 0.01629 = 0.02055 -0.00109 0.00353 0.00032 AFIX 13 H409 2 0.537960 0.361065 0.108142 11.00000 -1.20000 AFIX 0 C410 1 0.486683 0.479272 0.096036 11.00000 0.01847 0.02063 = 0.02163 0.00020 0.00264 -0.00029 C411 1 0.631123 0.503162 0.132145 11.00000 0.02415 0.03195 = 0.03390 -0.00259 0.00397 -0.00144 AFIX 137 H41A 2 0.634519 0.557279 0.135502 11.00000 -1.50000 H41B 2 0.706080 0.485879 0.106101 11.00000 -1.50000 H41C 2 0.645375 0.481643 0.177982 11.00000 -1.50000 AFIX 0 C412 1 0.469597 0.513223 0.024371 11.00000 0.01739 0.02862 = 0.03077 0.00452 0.00305 0.00188 AFIX 137 H41D 2 0.463585 0.567226 0.027858 11.00000 -1.50000 H41E 2 0.382760 0.494210 -0.001785 11.00000 -1.50000 H41F 2 0.551530 0.499924 0.001258 11.00000 -1.50000 AFIX 0 C413 1 0.308353 0.218694 -0.081659 11.00000 0.03515 0.03677 = 0.03028 -0.00182 0.01593 -0.01131 AFIX 137 H41G 2 0.233404 0.182482 -0.095351 11.00000 -1.50000 H41H 2 0.386506 0.194395 -0.053025 11.00000 -1.50000 H41I 2 0.343347 0.239138 -0.122352 11.00000 -1.50000 AFIX 0 C501 1 -0.184117 0.263517 0.027059 11.00000 0.02266 0.02677 = 0.02366 0.00008 0.00146 -0.00246 H50X 2 -0.222087 0.257641 -0.019038 11.00000 -1.20000 H50Y 2 -0.200721 0.222744 0.054963 11.00000 -1.20000 C502 1 -0.155722 0.334145 0.044620 11.00000 0.01719 0.02339 = 0.02323 -0.00231 0.00311 0.00371 C503 1 -0.090158 0.359767 0.108485 11.00000 0.01696 0.02030 = 0.02088 -0.00147 0.00135 0.00294 H503 2 -0.073133 0.410018 0.115216 11.00000 -1.20000 C504 1 -0.064063 0.321855 0.173132 11.00000 0.01727 0.01998 = 0.01664 0.00130 0.00373 0.00195 C505 1 -0.084578 0.250323 0.188479 11.00000 0.02159 0.02317 = 0.02160 -0.00474 0.00476 0.00277 H505 2 -0.132119 0.213176 0.161234 11.00000 -1.20000 C506 1 -0.053087 0.223203 0.261820 11.00000 0.01715 0.02043 = 0.02009 0.00104 0.00408 0.00046 AFIX 23 H50A 2 -0.141908 0.205476 0.277787 11.00000 -1.20000 H50B 2 0.013984 0.181090 0.263714 11.00000 -1.20000 AFIX 0 C507 1 0.009607 0.283807 0.307902 11.00000 0.02054 0.02082 = 0.01883 0.00246 0.00212 -0.00069 AFIX 13 H507 2 0.038242 0.269098 0.356413 11.00000 -1.20000 AFIX 0 C508 1 0.124771 0.323519 0.272993 11.00000 0.02182 0.02387 = 0.02078 -0.00097 0.00359 -0.00163 AFIX 23 H50C 2 0.191345 0.353638 0.304200 11.00000 -1.20000 H50D 2 0.176023 0.291014 0.243974 11.00000 -1.20000 AFIX 0 C509 1 0.002627 0.368031 0.233687 11.00000 0.01446 0.01407 = 0.01598 0.00288 0.00237 0.00039 AFIX 13 H509 2 0.024797 0.420639 0.223318 11.00000 -1.20000 AFIX 0 C510 1 -0.078915 0.355760 0.297509 11.00000 0.02113 0.01747 = 0.01644 -0.00090 0.00198 0.00211 C511 1 -0.038477 0.411552 0.353779 11.00000 0.03740 0.02222 = 0.02336 -0.00217 0.00978 0.00226 AFIX 137 H51A 2 -0.089696 0.457971 0.342853 11.00000 -1.50000 H51B 2 0.063881 0.420783 0.357916 11.00000 -1.50000 H51C 2 -0.063457 0.391993 0.396966 11.00000 -1.50000 AFIX 0 C512 1 -0.240385 0.348916 0.286619 11.00000 0.02980 0.02859 = 0.02539 0.00166 0.01045 0.00352 AFIX 137 H51D 2 -0.273280 0.327204 0.327294 11.00000 -1.50000 H51E 2 -0.268868 0.317053 0.247177 11.00000 -1.50000 H51F 2 -0.282607 0.398100 0.278399 11.00000 -1.50000 AFIX 0 C513 1 -0.183103 0.392640 -0.010376 11.00000 0.03483 0.04018 = 0.03369 0.00149 0.00428 0.00712 AFIX 137 H51G 2 -0.166189 0.371581 -0.054333 11.00000 -1.50000 H51H 2 -0.119144 0.434668 0.000681 11.00000 -1.50000 H51I 2 -0.281685 0.409499 -0.013043 11.00000 -1.50000 AFIX 0 C601 1 0.070429 0.121527 0.005882 11.00000 0.02107 0.01857 = 0.01947 -0.00236 0.00014 -0.00250 H60X 2 0.002142 0.112320 -0.031732 11.00000 -1.20000 H60Y 2 0.163882 0.134902 -0.000783 11.00000 -1.20000 C602 1 0.033806 0.105332 0.069660 11.00000 0.01796 0.01989 = 0.02263 0.00046 0.00375 -0.00254 C603 1 0.116039 0.119593 0.131459 11.00000 0.01776 0.01319 = 0.01565 0.00439 0.00521 -0.00062 H603 2 0.072556 0.104692 0.168636 11.00000 -1.20000 C604 1 0.265952 0.136139 0.146945 11.00000 0.01638 0.01954 = 0.01624 0.00059 0.00395 0.00083 C605 1 0.363315 0.142471 0.102459 11.00000 0.02307 0.02152 = 0.02328 -0.00102 0.00349 0.00113 H605 2 0.336078 0.122932 0.058566 11.00000 -1.20000 C606 1 0.518788 0.152211 0.130478 11.00000 0.02457 0.02956 = 0.03349 0.00359 0.00537 0.00089 AFIX 23 H60A 2 0.557381 0.196341 0.109464 11.00000 -1.20000 H60B 2 0.573323 0.108455 0.118448 11.00000 -1.20000 AFIX 0 C607 1 0.535960 0.161420 0.207802 11.00000 0.01791 0.02332 = 0.02855 0.00114 -0.00124 -0.00181 AFIX 13 H607 2 0.635126 0.171040 0.229356 11.00000 -1.20000 AFIX 0 C608 1 0.426161 0.218460 0.224173 11.00000 0.02812 0.02878 = 0.03164 -0.00145 0.00432 -0.00225 AFIX 23 H60C 2 0.402050 0.256120 0.188223 11.00000 -1.20000 H60D 2 0.446443 0.241429 0.269801 11.00000 -1.20000 AFIX 0 C609 1 0.321322 0.150941 0.220858 11.00000 0.01710 0.01928 = 0.01915 -0.00019 0.00321 -0.00007 AFIX 13 H609 2 0.248252 0.152664 0.253146 11.00000 -1.20000 AFIX 0 C610 1 0.454633 0.101831 0.243515 11.00000 0.01814 0.02015 = 0.02240 -0.00103 0.00058 0.00259 C611 1 0.492049 0.102403 0.319872 11.00000 0.02605 0.03426 = 0.02918 -0.00126 -0.00330 0.00551 AFIX 137 H61A 2 0.420204 0.074767 0.341017 11.00000 -1.50000 H61B 2 0.495233 0.153615 0.336360 11.00000 -1.50000 H61C 2 0.585031 0.079198 0.331873 11.00000 -1.50000 AFIX 0 C612 1 0.451576 0.023888 0.217576 11.00000 0.02542 0.02609 = 0.03043 0.00369 -0.00189 0.00521 AFIX 137 H61D 2 0.546388 0.002067 0.227181 11.00000 -1.50000 H61E 2 0.422264 0.023796 0.168280 11.00000 -1.50000 H61F 2 0.384075 -0.005210 0.240291 11.00000 -1.50000 AFIX 0 C613 1 -0.115152 0.078095 0.071970 11.00000 0.02425 0.02964 = 0.02555 0.00092 0.00100 -0.00833 AFIX 137 H61G 2 -0.115475 0.023854 0.073126 11.00000 -1.50000 H61H 2 -0.176023 0.095326 0.031385 11.00000 -1.50000 H61I 2 -0.151005 0.097362 0.112906 11.00000 -1.50000 AFIX 0 HKLF 4 REM ann48 in P2(1) REM R1 = 0.0519 for 11494 Fo > 4sig(Fo) and 0.0698 for all 13782 data REM 811 parameters refined using 565 restraints END WGHT 0.0220 0.0000 REM Highest difference peak 1.115, deepest hole -0.649, 1-sigma level 0.115 Q1 1 0.0111 0.2044 0.1734 11.00000 0.05 1.08 Q2 1 0.4574 0.2038 0.4705 11.00000 0.05 1.05 Q3 1 0.1051 0.1499 0.0729 11.00000 0.05 0.87 Q4 1 0.7627 0.3132 0.6783 11.00000 0.05 0.84 Q5 1 0.3539 0.2601 0.5742 11.00000 0.05 0.83 Q6 1 0.4183 0.2586 0.2822 11.00000 0.05 0.75 Q7 1 0.7783 0.2504 0.6512 11.00000 0.05 0.69 Q8 1 0.7415 0.1559 0.7020 11.00000 0.05 0.68 Q9 1 0.7722 0.2499 0.7078 11.00000 0.05 0.66 Q10 1 0.1044 0.2079 0.0471 11.00000 0.05 0.64 ; _shelx_res_checksum 69053 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' 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 La1 La 0.76418(5) 0.20552(3) 0.67765(2) 0.01418(12) Uani 1 1 d . . C101 C 0.4870(10) 0.1710(6) 0.7076(5) 0.022(2) Uani 1 1 d D U H10X H 0.489(8) 0.220(2) 0.723(4) 0.027 Uiso 1 1 d D U H10Y H 0.471(8) 0.134(4) 0.740(3) 0.027 Uiso 1 1 d D U C102 C 0.4847(9) 0.1482(5) 0.6415(4) 0.017(2) Uani 1 1 d . U C103 C 0.5230(8) 0.1890(5) 0.5864(4) 0.018(2) Uani 1 1 d D U H103 H 0.529(8) 0.157(4) 0.550(3) 0.021 Uiso 1 1 d D U C104 C 0.5383(8) 0.2669(6) 0.5783(4) 0.0185(19) Uani 1 1 d . U C105 C 0.5358(9) 0.3225(5) 0.6250(5) 0.020(2) Uani 1 1 d D U H105 H 0.504(8) 0.314(5) 0.667(3) 0.025 Uiso 1 1 d D U C106 C 0.5428(9) 0.4031(5) 0.6042(4) 0.022(2) Uani 1 1 d . U H10A H 0.453986 0.428477 0.612151 0.027 Uiso 1 1 calc R U H10B H 0.622677 0.427726 0.632366 0.027 Uiso 1 1 calc R U C107 C 0.5630(8) 0.4091(5) 0.5296(4) 0.020(2) Uani 1 1 d . U H107 H 0.572629 0.460555 0.512147 0.024 Uiso 1 1 calc R U C108 C 0.6811(9) 0.3553(5) 0.5160(5) 0.023(2) Uani 1 1 d . U H10C H 0.755146 0.348061 0.555339 0.027 Uiso 1 1 calc R U H10D H 0.723422 0.365589 0.473702 0.027 Uiso 1 1 calc R U C109 C 0.5650(8) 0.2948(5) 0.5086(4) 0.017(2) Uani 1 1 d . U H109 H 0.575964 0.255647 0.473849 0.020 Uiso 1 1 calc R U C110 C 0.4579(9) 0.3586(5) 0.4847(4) 0.021(2) Uani 1 1 d . U C111 C 0.3058(8) 0.3538(5) 0.5005(5) 0.023(2) Uani 1 1 d . U H11A H 0.260254 0.402329 0.493404 0.035 Uiso 1 1 calc R U H11B H 0.305158 0.338612 0.548080 0.035 Uiso 1 1 calc R U H11C H 0.253864 0.317337 0.470362 0.035 Uiso 1 1 calc R U C112 C 0.4564(10) 0.3740(6) 0.4090(4) 0.026(2) Uani 1 1 d . U H11D H 0.405375 0.420247 0.397251 0.038 Uiso 1 1 calc R U H11E H 0.408784 0.333147 0.382709 0.038 Uiso 1 1 calc R U H11F H 0.554059 0.378340 0.398338 0.038 Uiso 1 1 calc R U C113 C 0.4526(10) 0.0672(5) 0.6278(5) 0.030(3) Uani 1 1 d . U H11G H 0.483326 0.038318 0.668891 0.045 Uiso 1 1 calc R U H11H H 0.503292 0.050094 0.590423 0.045 Uiso 1 1 calc R U H11I H 0.350313 0.060721 0.615047 0.045 Uiso 1 1 calc R U C201 C 0.7870(9) 0.2120(7) 0.8216(4) 0.024(2) Uani 1 1 d D U H20X H 0.749(8) 0.177(4) 0.850(3) 0.029 Uiso 1 1 d D U H20Y H 0.877(5) 0.195(5) 0.815(4) 0.029 Uiso 1 1 d D U C202 C 0.7382(9) 0.2806(5) 0.8028(4) 0.020(2) Uani 1 1 d . U C203 C 0.7909(9) 0.3292(5) 0.7569(4) 0.015(2) Uani 1 1 d D U H203 H 0.745(8) 0.374(3) 0.752(4) 0.018 Uiso 1 1 d D U C204 C 0.9283(9) 0.3309(5) 0.7330(4) 0.014(2) Uani 1 1 d . U C205 C 1.0367(9) 0.2831(5) 0.7452(4) 0.019(2) Uani 1 1 d D U H205 H 1.045(8) 0.242(3) 0.774(3) 0.023 Uiso 1 1 d D U C206 C 1.1810(9) 0.3010(5) 0.7239(5) 0.020(2) Uani 1 1 d . U H20A H 1.251797 0.305310 0.764898 0.024 Uiso 1 1 calc R U H20B H 1.211122 0.260424 0.695283 0.024 Uiso 1 1 calc R U C207 C 1.1751(9) 0.3729(5) 0.6843(4) 0.017(2) Uani 1 1 d . U H207 H 1.265566 0.387719 0.667042 0.021 Uiso 1 1 calc R U C208 C 1.0431(9) 0.3701(5) 0.6298(4) 0.023(2) Uani 1 1 d . U H20C H 1.017953 0.319886 0.612211 0.028 Uiso 1 1 calc R U H20D H 1.044637 0.406294 0.592303 0.028 Uiso 1 1 calc R U C209 C 0.9587(9) 0.3961(5) 0.6882(4) 0.015(2) Uani 1 1 d . U H209 H 0.876522 0.429634 0.674182 0.018 Uiso 1 1 calc R U C210 C 1.0992(9) 0.4354(5) 0.7201(4) 0.018(2) Uani 1 1 d . U C211 C 1.1250(9) 0.4421(5) 0.7971(4) 0.024(2) Uani 1 1 d . U H21A H 1.220475 0.461767 0.810665 0.036 Uiso 1 1 calc R U H21B H 1.116466 0.393245 0.817660 0.036 Uiso 1 1 calc R U H21C H 1.054705 0.475762 0.812676 0.036 Uiso 1 1 calc R U C212 C 1.1145(10) 0.5117(6) 0.6895(5) 0.032(3) Uani 1 1 d . U H21D H 1.042030 0.544851 0.703864 0.048 Uiso 1 1 calc R U H21E H 1.102473 0.508021 0.639716 0.048 Uiso 1 1 calc R U H21F H 1.208917 0.531524 0.705325 0.048 Uiso 1 1 calc R U C213 C 0.5982(9) 0.3045(6) 0.8273(5) 0.033(3) Uani 1 1 d . U H21G H 0.548626 0.260824 0.841845 0.050 Uiso 1 1 calc R U H21H H 0.538644 0.329141 0.789933 0.050 Uiso 1 1 calc R U H21I H 0.617830 0.338792 0.865689 0.050 Uiso 1 1 calc R U C301 C 0.8124(9) 0.0565(5) 0.7138(5) 0.019(2) Uani 1 1 d D U H30X H 0.756(7) 0.046(5) 0.672(2) 0.023 Uiso 1 1 d D U H30Y H 0.778(8) 0.032(4) 0.751(3) 0.023 Uiso 1 1 d D U C302 C 0.9493(9) 0.0836(5) 0.7146(4) 0.019(2) Uani 1 1 d . U C303 C 1.0027(9) 0.1219(5) 0.6615(4) 0.016(2) Uani 1 1 d D U H303 H 1.095(5) 0.138(4) 0.671(4) 0.019 Uiso 1 1 d D U C304 C 0.9515(8) 0.1276(5) 0.5907(4) 0.014(2) Uani 1 1 d . U C305 C 0.8276(9) 0.1031(5) 0.5567(4) 0.019(2) Uani 1 1 d D U H305 H 0.773(7) 0.066(4) 0.574(4) 0.023 Uiso 1 1 d D U C306 C 0.7989(8) 0.1082(5) 0.4800(4) 0.018(2) Uani 1 1 d . U H30A H 0.710431 0.136545 0.466971 0.022 Uiso 1 1 calc R U H30B H 0.785716 0.057905 0.460391 0.022 Uiso 1 1 calc R U C307 C 0.9212(8) 0.1462(5) 0.4514(4) 0.0154(19) Uani 1 1 d . U H307 H 0.909654 0.153079 0.400786 0.019 Uiso 1 1 calc R U C308 C 0.9590(8) 0.2169(5) 0.4944(4) 0.020(2) Uani 1 1 d . U H30C H 1.015059 0.253813 0.472141 0.024 Uiso 1 1 calc R U H30D H 0.877111 0.240274 0.512555 0.024 Uiso 1 1 calc R U C309 C 1.0489(9) 0.1657(5) 0.5459(4) 0.020(2) Uani 1 1 d . U H309 H 1.137906 0.187648 0.570053 0.024 Uiso 1 1 calc R U C310 C 1.0671(9) 0.1146(5) 0.4835(4) 0.016(2) Uani 1 1 d . U C311 C 1.0829(9) 0.0317(5) 0.4963(5) 0.023(2) Uani 1 1 d . U H31A H 1.093153 0.006388 0.453291 0.035 Uiso 1 1 calc R U H31B H 0.998677 0.012889 0.514660 0.035 Uiso 1 1 calc R U H31C H 1.167204 0.022413 0.529039 0.035 Uiso 1 1 calc R U C312 C 1.1899(9) 0.1391(6) 0.4460(5) 0.026(2) Uani 1 1 d . U H31D H 1.279788 0.124253 0.472153 0.040 Uiso 1 1 calc R U H31E H 1.187755 0.193064 0.440717 0.040 Uiso 1 1 calc R U H31F H 1.181012 0.115750 0.400914 0.040 Uiso 1 1 calc R U C313 C 1.0469(9) 0.0779(6) 0.7812(4) 0.025(2) Uani 1 1 d . U H31G H 0.990012 0.074074 0.819136 0.038 Uiso 1 1 calc R U H31H H 1.107119 0.122015 0.787167 0.038 Uiso 1 1 calc R U H31I H 1.106707 0.033734 0.780274 0.038 Uiso 1 1 calc R U La2 La 0.10970(5) 0.25863(3) 0.07500(2) 0.01583(13) Uani 1 1 d . . C401 C 0.1105(10) 0.3013(6) -0.0607(5) 0.026(2) Uani 1 1 d D U H40X H 0.062(7) 0.272(4) -0.096(3) 0.031 Uiso 1 1 d D U H40Y H 0.088(9) 0.349(3) -0.045(4) 0.031 Uiso 1 1 d D U C402 C 0.2494(9) 0.2806(5) -0.0419(4) 0.023(2) Uani 1 1 d . U C403 C 0.3413(9) 0.3088(5) 0.0146(4) 0.019(2) Uani 1 1 d D U H403 H 0.430(5) 0.287(4) 0.024(4) 0.022 Uiso 1 1 d D U C404 C 0.3261(9) 0.3727(5) 0.0557(4) 0.015(2) Uani 1 1 d . U C405 C 0.2127(9) 0.4180(5) 0.0580(4) 0.019(2) Uani 1 1 d D U H405 H 0.134(6) 0.413(5) 0.024(3) 0.023 Uiso 1 1 d D U C406 C 0.2227(9) 0.4864(5) 0.1007(4) 0.022(2) Uani 1 1 d . U H40A H 0.149097 0.484898 0.132051 0.026 Uiso 1 1 calc R U H40B H 0.204432 0.530244 0.070918 0.026 Uiso 1 1 calc R U C407 C 0.3680(9) 0.4936(5) 0.1420(4) 0.022(2) Uani 1 1 d . U H407 H 0.381929 0.537474 0.172973 0.026 Uiso 1 1 calc R U C408 C 0.4059(10) 0.4171(5) 0.1752(5) 0.025(2) Uani 1 1 d . U H40C H 0.323294 0.388846 0.187318 0.030 Uiso 1 1 calc R U H40D H 0.483388 0.418601 0.213622 0.030 Uiso 1 1 calc R U C409 C 0.4544(9) 0.3950(5) 0.1057(4) 0.018(2) Uani 1 1 d . U H409 H 0.537960 0.361065 0.108142 0.021 Uiso 1 1 calc R U C410 C 0.4867(9) 0.4793(5) 0.0960(4) 0.020(2) Uani 1 1 d . U C411 C 0.6311(9) 0.5032(6) 0.1321(5) 0.030(2) Uani 1 1 d . U H41A H 0.634519 0.557279 0.135502 0.045 Uiso 1 1 calc R U H41B H 0.706080 0.485879 0.106101 0.045 Uiso 1 1 calc R U H41C H 0.645375 0.481643 0.177982 0.045 Uiso 1 1 calc R U C412 C 0.4696(9) 0.5132(6) 0.0244(4) 0.026(2) Uani 1 1 d . U H41D H 0.463585 0.567226 0.027858 0.038 Uiso 1 1 calc R U H41E H 0.382760 0.494210 -0.001785 0.038 Uiso 1 1 calc R U H41F H 0.551530 0.499924 0.001258 0.038 Uiso 1 1 calc R U C413 C 0.3084(9) 0.2187(6) -0.0817(4) 0.033(3) Uani 1 1 d . U H41G H 0.233404 0.182482 -0.095351 0.050 Uiso 1 1 calc R U H41H H 0.386506 0.194395 -0.053025 0.050 Uiso 1 1 calc R U H41I H 0.343347 0.239138 -0.122352 0.050 Uiso 1 1 calc R U C501 C -0.1841(9) 0.2635(7) 0.0271(4) 0.024(2) Uani 1 1 d D U H50X H -0.222(7) 0.258(5) -0.0190(18) 0.029 Uiso 1 1 d D U H50Y H -0.201(8) 0.223(3) 0.055(3) 0.029 Uiso 1 1 d D U C502 C -0.1557(10) 0.3341(6) 0.0446(5) 0.021(2) Uani 1 1 d . U C503 C -0.0902(9) 0.3598(5) 0.1085(5) 0.019(2) Uani 1 1 d D U H503 H -0.073(8) 0.410(2) 0.115(4) 0.023 Uiso 1 1 d D U C504 C -0.0641(9) 0.3219(5) 0.1731(4) 0.018(2) Uani 1 1 d . U C505 C -0.0846(8) 0.2503(6) 0.1885(4) 0.022(2) Uani 1 1 d D U H505 H -0.132(7) 0.213(4) 0.161(3) 0.026 Uiso 1 1 d D U C506 C -0.0531(8) 0.2232(5) 0.2618(4) 0.019(2) Uani 1 1 d . U H50A H -0.141908 0.205476 0.277787 0.023 Uiso 1 1 calc R U H50B H 0.013984 0.181090 0.263714 0.023 Uiso 1 1 calc R U C507 C 0.0096(8) 0.2838(5) 0.3079(4) 0.020(2) Uani 1 1 d . U H507 H 0.038242 0.269098 0.356413 0.024 Uiso 1 1 calc R U C508 C 0.1248(9) 0.3235(5) 0.2730(4) 0.022(2) Uani 1 1 d . U H50C H 0.191345 0.353638 0.304200 0.026 Uiso 1 1 calc R U H50D H 0.176023 0.291014 0.243974 0.026 Uiso 1 1 calc R U C509 C 0.0026(8) 0.3680(5) 0.2337(4) 0.015(2) Uani 1 1 d . U H509 H 0.024797 0.420639 0.223318 0.018 Uiso 1 1 calc R U C510 C -0.0789(9) 0.3558(5) 0.2975(4) 0.018(2) Uani 1 1 d . U C511 C -0.0385(10) 0.4116(5) 0.3538(5) 0.027(2) Uani 1 1 d . U H51A H -0.089696 0.457971 0.342853 0.041 Uiso 1 1 calc R U H51B H 0.063881 0.420783 0.357916 0.041 Uiso 1 1 calc R U H51C H -0.063457 0.391993 0.396966 0.041 Uiso 1 1 calc R U C512 C -0.2404(9) 0.3489(6) 0.2866(5) 0.027(2) Uani 1 1 d . U H51D H -0.273280 0.327204 0.327294 0.041 Uiso 1 1 calc R U H51E H -0.268868 0.317053 0.247177 0.041 Uiso 1 1 calc R U H51F H -0.282607 0.398100 0.278399 0.041 Uiso 1 1 calc R U C513 C -0.1831(10) 0.3926(6) -0.0104(5) 0.036(3) Uani 1 1 d . U H51G H -0.166189 0.371581 -0.054333 0.054 Uiso 1 1 calc R U H51H H -0.119144 0.434668 0.000681 0.054 Uiso 1 1 calc R U H51I H -0.281685 0.409499 -0.013043 0.054 Uiso 1 1 calc R U C601 C 0.0704(10) 0.1215(6) 0.0059(5) 0.020(2) Uani 1 1 d D U H60X H 0.002(6) 0.112(5) -0.032(3) 0.024 Uiso 1 1 d D U H60Y H 0.164(4) 0.135(5) -0.001(4) 0.024 Uiso 1 1 d D U C602 C 0.0338(9) 0.1053(5) 0.0697(4) 0.020(2) Uani 1 1 d . U C603 C 0.1160(9) 0.1196(5) 0.1315(4) 0.015(2) Uani 1 1 d D U H603 H 0.073(7) 0.105(4) 0.169(3) 0.018 Uiso 1 1 d D U C604 C 0.2660(9) 0.1361(5) 0.1469(4) 0.017(2) Uani 1 1 d . U C605 C 0.3633(10) 0.1425(6) 0.1025(5) 0.023(2) Uani 1 1 d D U H605 H 0.336(8) 0.123(5) 0.059(3) 0.027 Uiso 1 1 d D U C606 C 0.5188(9) 0.1522(6) 0.1305(5) 0.029(3) Uani 1 1 d . U H60A H 0.557381 0.196341 0.109464 0.035 Uiso 1 1 calc R U H60B H 0.573323 0.108455 0.118448 0.035 Uiso 1 1 calc R U C607 C 0.5360(9) 0.1614(5) 0.2078(4) 0.024(2) Uani 1 1 d . U H607 H 0.635126 0.171040 0.229356 0.028 Uiso 1 1 calc R U C608 C 0.4262(8) 0.2185(5) 0.2242(5) 0.029(2) Uani 1 1 d . U H60C H 0.402050 0.256120 0.188223 0.035 Uiso 1 1 calc R U H60D H 0.446443 0.241429 0.269801 0.035 Uiso 1 1 calc R U C609 C 0.3213(9) 0.1509(5) 0.2209(4) 0.018(2) Uani 1 1 d . U H609 H 0.248252 0.152664 0.253146 0.022 Uiso 1 1 calc R U C610 C 0.4546(9) 0.1018(5) 0.2435(4) 0.020(2) Uani 1 1 d . U C611 C 0.4920(10) 0.1024(6) 0.3199(5) 0.030(2) Uani 1 1 d . U H61A H 0.420204 0.074767 0.341017 0.046 Uiso 1 1 calc R U H61B H 0.495233 0.153615 0.336360 0.046 Uiso 1 1 calc R U H61C H 0.585031 0.079198 0.331873 0.046 Uiso 1 1 calc R U C612 C 0.4516(10) 0.0239(5) 0.2176(5) 0.028(2) Uani 1 1 d . U H61D H 0.546388 0.002067 0.227181 0.042 Uiso 1 1 calc R U H61E H 0.422264 0.023796 0.168280 0.042 Uiso 1 1 calc R U H61F H 0.384075 -0.005210 0.240291 0.042 Uiso 1 1 calc R U C613 C -0.1152(9) 0.0781(6) 0.0720(5) 0.027(2) Uani 1 1 d . U H61G H -0.115475 0.023854 0.073126 0.040 Uiso 1 1 calc R U H61H H -0.176023 0.095326 0.031385 0.040 Uiso 1 1 calc R U H61I H -0.151005 0.097362 0.112906 0.040 Uiso 1 1 calc R U 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 0.0121(2) 0.0154(3) 0.0148(3) -0.0003(2) 0.00080(19) -0.0005(3) C101 0.021(3) 0.022(4) 0.024(3) 0.002(3) 0.005(3) -0.003(3) C102 0.014(3) 0.016(3) 0.020(3) 0.000(3) -0.004(3) 0.001(3) C103 0.014(3) 0.020(4) 0.019(3) -0.004(3) 0.002(3) 0.001(3) C104 0.014(3) 0.021(3) 0.019(3) -0.001(3) -0.003(3) 0.000(3) C105 0.019(3) 0.023(4) 0.019(3) 0.001(3) 0.002(3) 0.000(3) C106 0.019(3) 0.022(4) 0.025(3) -0.001(3) 0.001(3) 0.002(3) C107 0.019(3) 0.022(3) 0.020(3) 0.002(3) 0.004(3) 0.000(3) C108 0.023(3) 0.024(4) 0.022(3) -0.002(3) 0.003(3) 0.000(3) C109 0.015(3) 0.018(3) 0.017(3) -0.002(3) 0.002(3) 0.001(3) C110 0.022(3) 0.020(3) 0.020(3) 0.000(3) 0.003(3) 0.002(3) C111 0.012(4) 0.023(5) 0.033(5) 0.000(4) -0.002(4) 0.001(4) C112 0.026(4) 0.024(5) 0.026(5) 0.000(4) -0.001(4) -0.001(4) C113 0.025(5) 0.026(5) 0.038(5) 0.002(4) -0.002(4) 0.000(4) C201 0.026(3) 0.026(4) 0.022(3) 0.001(3) 0.007(3) -0.004(3) C202 0.019(3) 0.021(4) 0.020(3) -0.006(3) 0.000(3) -0.004(3) C203 0.014(3) 0.016(3) 0.015(3) -0.002(3) 0.000(3) -0.001(3) C204 0.014(3) 0.013(3) 0.013(3) -0.002(3) 0.001(3) -0.002(3) C205 0.020(3) 0.020(3) 0.017(3) 0.000(3) 0.002(3) -0.003(3) C206 0.015(3) 0.022(4) 0.024(3) 0.000(3) 0.005(3) 0.001(3) C207 0.016(3) 0.019(3) 0.016(3) 0.001(3) 0.002(3) -0.002(3) C208 0.022(3) 0.024(4) 0.024(3) 0.001(3) 0.004(3) 0.001(3) C209 0.014(3) 0.016(3) 0.015(3) -0.001(3) -0.001(3) 0.002(3) C210 0.016(3) 0.018(3) 0.021(3) 0.001(3) 0.001(3) -0.001(3) C211 0.022(4) 0.020(5) 0.029(5) -0.003(4) -0.003(4) -0.005(4) C212 0.026(5) 0.034(5) 0.035(5) 0.004(4) 0.003(4) -0.003(4) C213 0.028(5) 0.044(5) 0.031(5) -0.015(4) 0.013(4) -0.010(4) C301 0.020(3) 0.019(3) 0.018(3) 0.001(3) 0.000(3) -0.001(3) C302 0.018(3) 0.017(3) 0.020(3) 0.000(3) -0.001(3) 0.005(3) C303 0.014(3) 0.017(3) 0.017(3) -0.003(3) 0.000(3) 0.002(3) C304 0.014(3) 0.012(3) 0.015(3) -0.002(3) 0.004(3) 0.002(3) C305 0.019(3) 0.019(3) 0.018(3) 0.000(3) 0.002(3) -0.001(3) C306 0.019(3) 0.020(3) 0.016(3) -0.001(3) 0.000(3) 0.001(3) C307 0.016(3) 0.016(3) 0.014(3) -0.001(3) 0.002(3) 0.003(3) C308 0.019(3) 0.021(4) 0.020(3) 0.000(3) 0.005(3) 0.001(3) C309 0.020(3) 0.019(3) 0.020(3) 0.000(3) 0.001(3) -0.001(3) C310 0.019(3) 0.017(3) 0.014(3) -0.002(3) 0.003(3) 0.001(3) C311 0.018(4) 0.024(5) 0.027(4) -0.007(4) 0.000(4) 0.005(4) C312 0.023(4) 0.032(5) 0.024(5) -0.005(4) 0.004(4) 0.004(4) C313 0.021(4) 0.026(5) 0.027(5) 0.004(4) -0.003(4) 0.003(4) La2 0.0138(3) 0.0194(3) 0.0147(3) 0.0000(2) 0.0029(2) -0.0020(3) C401 0.028(4) 0.025(4) 0.024(3) 0.000(3) 0.004(3) -0.001(3) C402 0.024(3) 0.025(4) 0.021(3) 0.002(3) 0.007(3) -0.006(3) C403 0.017(3) 0.019(3) 0.020(3) -0.001(3) 0.005(3) 0.000(3) C404 0.015(3) 0.012(3) 0.018(3) 0.003(3) 0.003(3) -0.004(3) C405 0.019(3) 0.022(3) 0.017(3) 0.002(3) 0.002(3) 0.000(3) C406 0.020(3) 0.023(3) 0.024(3) 0.001(3) 0.003(3) 0.002(3) C407 0.022(3) 0.022(4) 0.022(3) 0.001(3) 0.001(3) 0.002(3) C408 0.024(3) 0.025(4) 0.026(3) 0.001(3) 0.002(3) -0.003(3) C409 0.016(3) 0.016(3) 0.021(3) -0.001(3) 0.004(3) 0.000(3) C410 0.018(3) 0.021(3) 0.022(3) 0.000(3) 0.003(3) 0.000(3) C411 0.024(4) 0.032(5) 0.034(5) -0.003(4) 0.004(4) -0.001(4) C412 0.017(4) 0.029(5) 0.031(5) 0.005(4) 0.003(4) 0.002(4) C413 0.035(5) 0.037(6) 0.030(5) -0.002(4) 0.016(4) -0.011(4) C501 0.023(3) 0.027(4) 0.024(3) 0.000(3) 0.001(3) -0.002(3) C502 0.017(3) 0.023(4) 0.023(4) -0.002(3) 0.003(3) 0.004(3) C503 0.017(3) 0.020(3) 0.021(3) -0.001(3) 0.001(3) 0.003(3) C504 0.017(3) 0.020(3) 0.017(3) 0.001(3) 0.004(3) 0.002(3) C505 0.022(3) 0.023(4) 0.022(3) -0.005(3) 0.005(3) 0.003(3) C506 0.017(3) 0.020(4) 0.020(3) 0.001(3) 0.004(3) 0.000(3) C507 0.021(3) 0.021(4) 0.019(3) 0.002(3) 0.002(3) -0.001(3) C508 0.022(3) 0.024(4) 0.021(3) -0.001(3) 0.004(3) -0.002(3) C509 0.014(3) 0.014(3) 0.016(3) 0.003(3) 0.002(3) 0.000(3) C510 0.021(3) 0.017(3) 0.016(3) -0.001(3) 0.002(3) 0.002(3) C511 0.037(5) 0.022(5) 0.023(4) -0.002(4) 0.010(4) 0.002(4) C512 0.030(5) 0.029(5) 0.025(5) 0.002(4) 0.010(4) 0.004(4) C513 0.035(5) 0.040(6) 0.034(5) 0.001(4) 0.004(4) 0.007(4) C601 0.021(3) 0.019(4) 0.019(3) -0.002(3) 0.000(3) -0.003(3) C602 0.018(3) 0.020(3) 0.023(3) 0.000(3) 0.004(3) -0.003(3) C603 0.018(3) 0.013(3) 0.016(3) 0.004(3) 0.005(3) -0.001(3) C604 0.016(3) 0.020(3) 0.016(3) 0.001(3) 0.004(3) 0.001(3) C605 0.023(3) 0.022(4) 0.023(3) -0.001(3) 0.003(3) 0.001(3) C606 0.025(4) 0.030(4) 0.033(4) 0.004(3) 0.005(3) 0.001(3) C607 0.018(3) 0.023(4) 0.029(3) 0.001(3) -0.001(3) -0.002(3) C608 0.028(3) 0.029(4) 0.032(3) -0.001(3) 0.004(3) -0.002(3) C609 0.017(3) 0.019(3) 0.019(3) 0.000(3) 0.003(3) 0.000(3) C610 0.018(3) 0.020(3) 0.022(3) -0.001(3) 0.001(3) 0.003(3) C611 0.026(4) 0.034(5) 0.029(5) -0.001(4) -0.003(4) 0.006(4) C612 0.025(4) 0.026(5) 0.030(5) 0.004(4) -0.002(4) 0.005(4) C613 0.024(5) 0.030(5) 0.026(5) 0.001(4) 0.001(4) -0.008(4) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C203 La1 C103 118.5(3) C203 La1 C303 119.6(3) C103 La1 C303 119.4(3) C203 La1 C301 129.8(3) C103 La1 C301 99.2(3) C303 La1 C301 53.0(3) C203 La1 C201 52.9(3) C103 La1 C201 128.2(2) C303 La1 C201 100.2(3) C301 La1 C201 78.1(3) C203 La1 C101 94.8(3) C103 La1 C101 52.7(3) C303 La1 C101 134.1(3) C301 La1 C101 82.1(3) C201 La1 C101 75.9(3) C203 La1 C302 118.3(3) C103 La1 C302 121.4(3) C303 La1 C302 28.8(2) C301 La1 C302 28.4(2) C201 La1 C302 78.9(3) C101 La1 C302 109.6(3) C203 La1 C102 117.3(3) C103 La1 C102 28.8(2) C303 La1 C102 121.4(3) C301 La1 C102 80.4(3) C201 La1 C102 102.7(3) C101 La1 C102 27.8(3) C302 La1 C102 108.0(3) C203 La1 C202 28.9(2) C103 La1 C202 117.7(2) C303 La1 C202 121.1(3) C301 La1 C202 105.3(3) C201 La1 C202 27.6(3) C101 La1 C202 75.0(3) C302 La1 C202 105.1(3) C102 La1 C202 102.2(2) C203 La1 C204 29.6(2) C103 La1 C204 134.5(3) C303 La1 C204 93.4(3) C301 La1 C204 126.3(3) C201 La1 C204 67.4(3) C101 La1 C204 124.4(3) C302 La1 C204 102.8(2) C102 La1 C204 145.2(3) C202 La1 C204 53.2(2) C203 La1 C104 94.8(3) C103 La1 C104 28.8(3) C303 La1 C104 131.9(2) C301 La1 C104 127.9(3) C201 La1 C104 127.9(3) C101 La1 C104 66.6(3) C302 La1 C104 146.8(3) C102 La1 C104 52.5(3) C202 La1 C104 105.4(2) C204 La1 C104 105.8(3) C203 La1 C304 134.5(2) C103 La1 C304 94.5(2) C303 La1 C304 28.5(2) C301 La1 C304 66.6(2) C201 La1 C304 128.6(3) C101 La1 C304 130.7(3) C302 La1 C304 52.4(2) C102 La1 C304 106.7(2) C202 La1 C304 147.8(2) C204 La1 C304 104.9(2) C104 La1 C304 103.4(2) C102 C101 La1 76.8(5) C101 C102 C103 127.6(9) C101 C102 C113 116.2(9) C103 C102 C113 115.8(8) C101 C102 La1 75.4(5) C103 C102 La1 71.4(5) C113 C102 La1 123.8(6) C102 C103 C104 130.3(8) C102 C103 La1 79.8(5) C104 C103 La1 83.0(5) C105 C104 C103 129.8(8) C105 C104 C109 112.9(9) C103 C104 C109 117.4(8) C105 C104 La1 84.1(5) C103 C104 La1 68.2(5) C109 C104 La1 122.8(5) C104 C105 C106 121.1(8) C104 C105 La1 70.0(5) C106 C105 La1 133.6(6) C107 C106 C105 110.4(8) C106 C107 C108 108.0(7) C106 C107 C110 111.5(7) C108 C107 C110 87.8(7) C107 C108 C109 86.3(6) C104 C109 C108 110.1(7) C104 C109 C110 110.0(7) C108 C109 C110 86.5(7) C111 C110 C112 108.7(7) C111 C110 C107 118.6(7) C112 C110 C107 112.6(8) C111 C110 C109 119.5(8) C112 C110 C109 110.9(7) C107 C110 C109 84.9(6) C202 C201 La1 77.4(5) C201 C202 C203 127.7(8) C201 C202 C213 116.8(8) C203 C202 C213 115.0(8) C201 C202 La1 75.0(5) C203 C202 La1 70.1(5) C213 C202 La1 125.3(6) C202 C203 C204 129.6(8) C202 C203 La1 81.0(5) C204 C203 La1 81.5(5) C205 C204 C203 129.2(9) C205 C204 C209 113.9(8) C203 C204 C209 116.8(8) C205 C204 La1 86.0(6) C203 C204 La1 68.9(5) C209 C204 La1 121.3(5) C204 C205 C206 120.8(8) C204 C205 La1 68.4(5) C206 C205 La1 135.4(6) C207 C206 C205 110.4(7) C206 C207 C208 107.9(7) C206 C207 C210 112.1(7) C208 C207 C210 87.7(6) C207 C208 C209 85.5(6) C204 C209 C208 110.5(7) C204 C209 C210 109.2(7) C208 C209 C210 86.8(6) C211 C210 C212 108.4(8) C211 C210 C207 119.2(8) C212 C210 C207 113.8(7) C211 C210 C209 117.5(7) C212 C210 C209 111.6(7) C207 C210 C209 84.7(6) C302 C301 La1 77.7(6) C301 C302 C303 126.2(8) C301 C302 C313 117.2(8) C303 C302 C313 116.4(8) C301 C302 La1 73.9(5) C303 C302 La1 72.4(5) C313 C302 La1 124.5(6) C302 C303 C304 131.1(8) C302 C303 La1 78.8(5) C304 C303 La1 83.7(5) C305 C304 C303 129.2(8) C305 C304 C309 114.4(8) C303 C304 C309 116.4(7) C305 C304 La1 84.0(5) C303 C304 La1 67.9(5) C309 C304 La1 124.9(6) C304 C305 C306 121.0(8) C305 C306 C307 110.5(7) C306 C307 C308 107.6(7) C306 C307 C310 111.5(7) C308 C307 C310 86.7(6) C309 C308 C307 86.6(7) C304 C309 C308 109.0(7) C304 C309 C310 109.0(7) C308 C309 C310 86.5(6) C312 C310 C311 107.4(7) C312 C310 C307 113.0(7) C311 C310 C307 119.4(7) C312 C310 C309 112.2(7) C311 C310 C309 117.8(7) C307 C310 C309 85.8(6) C603 La2 C503 119.1(3) C603 La2 C403 119.6(3) C503 La2 C403 119.3(3) C603 La2 C401 129.8(3) C503 La2 C401 97.5(3) C403 La2 C401 53.2(3) C603 La2 C601 52.5(3) C503 La2 C601 129.7(3) C403 La2 C601 98.1(3) C401 La2 C601 78.1(3) C603 La2 C402 118.1(3) C503 La2 C402 120.4(3) C403 La2 C402 29.4(2) C401 La2 C402 28.3(2) C601 La2 C402 77.0(3) C603 La2 C501 97.8(3) C503 La2 C501 52.0(3) C403 La2 C501 130.1(3) C401 La2 C501 77.9(3) C601 La2 C501 78.5(3) C402 La2 C501 105.3(2) C603 La2 C602 28.6(2) C503 La2 C602 118.0(3) C403 La2 C602 120.6(3) C401 La2 C602 105.2(3) C601 La2 C602 28.1(2) C402 La2 C602 104.3(3) C501 La2 C602 77.6(3) C603 La2 C502 119.7(3) C503 La2 C502 29.0(3) C403 La2 C502 118.5(3) C401 La2 C502 76.9(3) C601 La2 C502 104.8(3) C402 La2 C502 104.6(3) C501 La2 C502 27.2(3) C602 La2 C502 104.0(3) C603 La2 C504 94.2(2) C503 La2 C504 29.2(2) C403 La2 C504 134.2(3) C401 La2 C504 126.7(3) C601 La2 C504 127.5(3) C402 La2 C504 147.7(3) C501 La2 C504 66.3(3) C602 La2 C504 104.0(2) C502 La2 C504 53.1(3) C603 La2 C604 29.4(2) C503 La2 C604 134.6(3) C403 La2 C604 94.2(3) C401 La2 C604 127.8(3) C601 La2 C604 66.6(3) C402 La2 C604 104.0(2) C501 La2 C604 127.1(3) C602 La2 C604 53.0(2) C502 La2 C604 147.2(3) C504 La2 C604 105.4(2) C603 La2 C404 135.0(2) C503 La2 C404 94.5(3) C403 La2 C404 28.6(2) C401 La2 C404 66.5(3) C601 La2 C404 126.7(3) C402 La2 C404 52.8(2) C501 La2 C404 127.1(3) C602 La2 C404 147.4(2) C502 La2 C404 104.4(3) C504 La2 C404 105.7(2) C604 La2 C404 105.6(2) C402 C401 La2 77.4(5) C401 C402 C403 126.1(9) C401 C402 C413 117.7(8) C403 C402 C413 116.2(8) C401 C402 La2 74.2(5) C403 C402 La2 73.4(5) C413 C402 La2 124.2(6) C402 C403 C404 129.7(8) C402 C403 La2 77.2(5) C404 C403 La2 83.0(5) C405 C404 C403 130.0(8) C405 C404 C409 113.1(8) C403 C404 C409 116.9(7) C405 C404 La2 81.3(5) C403 C404 La2 68.5(5) C409 C404 La2 127.6(5) C404 C405 C406 121.5(8) C404 C405 La2 72.8(5) C406 C405 La2 135.4(6) C405 C406 C407 111.4(7) C406 C407 C408 107.3(8) C406 C407 C410 110.4(7) C408 C407 C410 87.3(7) C407 C408 C409 86.1(7) C404 C409 C408 109.9(7) C404 C409 C410 109.3(7) C408 C409 C410 86.7(7) C411 C410 C412 107.8(7) C411 C410 C407 110.7(7) C412 C410 C407 118.1(7) C411 C410 C409 113.3(7) C412 C410 C409 120.0(8) C407 C410 C409 85.6(6) C502 C501 La2 77.6(6) C501 C502 C503 126.5(10) C501 C502 C513 117.8(9) C503 C502 C513 115.5(9) C501 C502 La2 75.2(6) C503 C502 La2 71.9(5) C513 C502 La2 123.4(6) C502 C503 C504 130.0(9) C502 C503 La2 79.1(5) C504 C503 La2 81.4(5) C505 C504 C503 129.8(9) C505 C504 C509 113.8(8) C503 C504 C509 116.3(8) C505 C504 La2 83.4(5) C503 C504 La2 69.4(5) C509 C504 La2 121.2(5) C504 C505 C506 120.4(8) C504 C505 La2 70.9(5) C506 C505 La2 130.1(5) C507 C506 C505 111.1(8) C506 C507 C508 108.6(7) C506 C507 C510 111.3(7) C508 C507 C510 87.4(6) C509 C508 C507 86.4(6) C504 C509 C508 108.9(7) C504 C509 C510 110.7(7) C508 C509 C510 86.4(6) C511 C510 C512 108.4(7) C511 C510 C507 112.1(7) C512 C510 C507 118.1(8) C511 C510 C509 112.9(7) C512 C510 C509 118.9(7) C507 C510 C509 84.9(6) C602 C601 La2 77.1(6) C601 C602 C603 125.9(8) C601 C602 C613 116.2(8) C603 C602 C613 117.5(8) C601 C602 La2 74.8(6) C603 C602 La2 71.1(5) C613 C602 La2 123.3(6) C602 C603 C604 130.8(8) C602 C603 La2 80.2(5) C604 C603 La2 82.5(5) C605 C604 C603 127.6(8) C605 C604 C609 115.3(8) C603 C604 C609 117.1(7) C605 C604 La2 88.1(6) C603 C604 La2 68.2(5) C609 C604 La2 115.4(6) C604 C605 C606 118.8(8) C605 C606 C607 110.8(7) C606 C607 C608 107.1(7) C606 C607 C610 112.6(8) C608 C607 C610 88.8(6) C607 C608 C609 85.0(7) C604 C609 C610 110.4(7) C604 C609 C608 108.7(7) C610 C609 C608 86.7(6) C612 C610 C611 110.0(8) C612 C610 C607 119.2(8) C611 C610 C607 112.5(8) C612 C610 C609 117.0(7) C611 C610 C609 111.4(7) C607 C610 C609 84.7(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance La1 C203 2.722(9) La1 C103 2.752(8) La1 C303 2.774(9) La1 C301 2.809(10) La1 C201 2.830(8) La1 C101 2.839(10) La1 C302 2.856(9) La1 C102 2.857(9) La1 C202 2.860(8) La1 C204 2.886(9) La1 C104 2.941(8) La1 C304 2.977(8) C101 C102 1.368(12) C102 C103 1.400(12) C102 C113 1.512(13) C103 C104 1.426(14) C104 C105 1.366(12) C104 C109 1.520(11) C105 C106 1.516(12) C106 C107 1.515(11) C107 C108 1.532(12) C107 C110 1.548(12) C108 C109 1.547(12) C109 C110 1.571(12) C110 C111 1.518(11) C110 C112 1.519(12) C201 C202 1.357(14) C202 C203 1.400(12) C202 C213 1.532(11) C203 C204 1.443(12) C204 C205 1.342(12) C204 C209 1.523(12) C205 C206 1.518(11) C206 C207 1.513(12) C207 C208 1.550(11) C207 C210 1.557(12) C208 C209 1.557(11) C209 C210 1.573(11) C210 C211 1.516(12) C210 C212 1.519(12) C301 C302 1.388(12) C302 C303 1.403(12) C302 C313 1.518(11) C303 C304 1.428(11) C304 C305 1.355(11) C304 C309 1.522(11) C305 C306 1.511(11) C306 C307 1.517(11) C307 C308 1.553(12) C307 C310 1.559(11) C308 C309 1.552(11) C309 C310 1.566(11) C310 C312 1.523(11) C310 C311 1.524(12) La2 C603 2.746(9) La2 C503 2.773(9) La2 C403 2.782(8) La2 C401 2.792(10) La2 C601 2.831(10) La2 C402 2.832(8) La2 C501 2.836(8) La2 C602 2.860(9) La2 C502 2.864(9) La2 C504 2.930(8) La2 C604 2.932(9) La2 C404 2.969(8) C401 C402 1.378(12) C402 C403 1.424(12) C402 C413 1.513(12) C403 C404 1.430(12) C404 C405 1.358(12) C404 C409 1.526(11) C405 C406 1.492(12) C406 C407 1.520(11) C407 C408 1.553(12) C407 C410 1.555(11) C408 C409 1.555(12) C409 C410 1.568(12) C410 C411 1.529(12) C410 C412 1.534(12) C501 C502 1.341(14) C502 C503 1.415(13) C502 C513 1.515(13) C503 C504 1.444(12) C504 C505 1.347(13) C504 C509 1.531(12) C505 C506 1.525(11) C506 C507 1.500(11) C507 C508 1.541(11) C507 C510 1.548(12) C508 C509 1.541(11) C509 C510 1.576(11) C510 C511 1.515(12) C510 C512 1.527(11) C601 C602 1.380(12) C602 C603 1.391(12) C602 C613 1.504(11) C603 C604 1.450(11) C604 C605 1.358(11) C604 C609 1.514(11) C605 C606 1.522(12) C606 C607 1.526(12) C607 C608 1.529(12) C607 C610 1.546(12) C608 C609 1.571(12) C609 C610 1.566(11) C610 C612 1.497(12) C610 C611 1.508(12) 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 C101 C102 C103 C104 -18.2(16) C102 C103 C104 C105 8.6(15) C103 C104 C105 C106 -175.1(8) C104 C105 C106 C107 -4.2(12) C105 C106 C107 C108 -46.8(9) C106 C107 C108 C109 83.2(8) C107 C108 C109 C110 28.2(6) C108 C109 C110 C111 -148.1(8) C109 C110 C111 C112 -128.6(12) C113 C201 C202 C203 -90.7(9) C201 C202 C203 C204 -20.0(16) C202 C203 C204 C205 5.2(16) C203 C204 C205 C206 -170.6(9) C204 C205 C206 C207 -4.8(12) C205 C206 C207 C208 -47.5(9) C206 C207 C208 C209 83.3(8) C207 C208 C209 C210 28.9(6) C208 C209 C210 C211 -149.1(8) C209 C210 C211 C212 -127.7(11) C213 C301 C302 C303 -92.2(9) C301 C302 C303 C304 -17.5(16) C302 C303 C304 C305 7.6(17) C303 C304 C305 C306 -174.1(9) C304 C305 C306 C307 -2.6(12) C305 C306 C307 C308 -47.1(9) C306 C307 C308 C309 83.3(7) C307 C308 C309 C310 28.1(6) C308 C309 C310 C311 -149.2(7) C309 C310 C311 C312 -127.9(10) C313 C401 C402 C403 -45.2(7) C401 C402 C403 C404 -14.1(16) C402 C403 C404 C405 9.9(16) C403 C404 C405 C406 -174.6(9) C404 C405 C406 C407 -3.6(12) C405 C406 C407 C408 -46.6(9) C406 C407 C408 C409 82.3(7) C407 C408 C409 C410 28.0(6) C408 C409 C410 C411 82.7(8) C409 C410 C411 C412 135.2(10)