Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global #====================================================== _journal_coden_Cambridge 186 # 1. SUBMISSION DETAILS loop_ _publ_author_name 'Leverd, Pascal Claude' 'Nierlich, Martine' 'Rinaldo, David' _publ_contact_author 'Dr Pascal Claude Leverd' _publ_contact_author_address ; Dr pascal claude leverd SCM CEA-Saclay Bāt. 125 Gif sur Yvette 91191 FRANCE ; _publ_contact_author_phone '16(1)69 08 54 21' _publ_contact_author_fax '16(1)69 08 66 40' _publ_contact_author_email leverd@drecam.cea.fr _publ_requested_journal ; Dalton Transactions ; _publ_section_title ; Crystal Structure Determination of 4f-5f Heterometallic Complexes ; data_struc _database_code_CSD 151550 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C267 H295 Cl4 La2 N27 O12 U' _chemical_formula_weight 4731.95 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' 'U' 'U' -9.6767 9.6646 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.646(3) _cell_length_b 16.759(3) _cell_length_c 23.203(5) _cell_angle_alpha 89.79(3) _cell_angle_beta 79.67(3) _cell_angle_gamma 87.41(3) _cell_volume 5979(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 'all' _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 25.63 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2456 _exptl_absorpt_coefficient_mu 1.137 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Crystal-to-detector distance dx == 27 mm, 90 images recorded by applying a 180\% scan on Phi in 2\% increments. Data were 76 % complete to a 2theta value of 51.26\%. ; _diffrn_ambient_temperature 100(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 CCD' _diffrn_measurement_method 'Phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26187 _diffrn_reflns_av_R_equivalents 0.133 _diffrn_reflns_av_sigmaI/netI 0.2669 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.63 _reflns_number_total 17157 _reflns_number_gt 7013 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1993)' _computing_molecular_graphics 'Bruker SHELXTL, V.5, Madison/WI, 1997' _computing_publication_material 'Bruker SHELXTL, V.5, Madison/WI, 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. All atoms were considered as anisotropic. All hydrogen atoms were introduced in the calculation as riding on calculated positions (U == 1.2 times that of the corresponding atom). ; _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^)+(0.1114P)^2^+28.8427P] 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 17157 _refine_ls_number_parameters 820 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2730 _refine_ls_R_factor_gt 0.1168 _refine_ls_wR_factor_ref 0.3055 _refine_ls_wR_factor_gt 0.2270 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.004 _diffrn_measured_fraction_theta_max 0.760 _diffrn_reflns_theta_full 25.63 _diffrn_measured_fraction_theta_full 0.760 _refine_diff_density_max 1.025 _refine_diff_density_min -0.997 _refine_diff_density_rms 0.124 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 U1 U 0.0000 0.0000 0.0000 0.05782(14) Uani 1 2 d S . . La1 La -0.14855(2) -0.09371(2) -0.371551(14) 0.03291(10) Uani 1 1 d . . . Cl1 Cl -0.27949(13) -0.17869(15) -0.33050(9) 0.0800(8) Uani 1 1 d . . . Cl2 Cl -0.03490(13) 0.00351(15) -0.41895(9) 0.0814(8) Uani 1 1 d . . . N1B N -0.21692(9) -0.08222(9) -0.46199(6) 0.064(2) Uani 1 1 d G . . C1B C -0.29936(9) -0.10841(9) -0.46140(6) 0.085(3) Uani 1 1 d G . . H1B H -0.3302 -0.1303 -0.4275 0.102 Uiso 1 1 calc R . . C2B C -0.33605(9) -0.10214(10) -0.51106(6) 0.102(4) Uani 1 1 d G . . H2B H -0.3916 -0.1198 -0.5106 0.122 Uiso 1 1 calc R . . C3B C -0.29035(9) -0.06962(10) -0.56136(6) 0.101(3) Uani 1 1 d G . . H3B H -0.3151 -0.0654 -0.5949 0.121 Uiso 1 1 calc R . . C4B C -0.20794(9) -0.04343(10) -0.56197(6) 0.083(3) Uani 1 1 d G . . H4B H -0.1771 -0.0215 -0.5959 0.100 Uiso 1 1 calc R . . C5B C -0.17118(9) -0.04975(9) -0.51230(6) 0.079(3) Uani 1 1 d G . . H5B H -0.1156 -0.0321 -0.5127 0.095 Uiso 1 1 calc R . . N1A N -0.08461(9) -0.19510(9) -0.44539(6) 0.074(2) Uani 1 1 d G . . C1A C -0.01238(9) -0.18087(9) -0.48754(6) 0.088(3) Uani 1 1 d G . . H1A H 0.0086 -0.1297 -0.4921 0.106 Uiso 1 1 calc R . . C2A C 0.02870(9) -0.24277(10) -0.52288(6) 0.110(4) Uani 1 1 d G . . H2A H 0.0772 -0.2332 -0.5512 0.133 Uiso 1 1 calc R . . C3A C -0.00249(10) -0.31888(9) -0.51604(7) 0.201(5) Uani 1 1 d G . . H3A H 0.0251 -0.3604 -0.5398 0.241 Uiso 1 1 calc R . . C4A C -0.07473(10) -0.33314(9) -0.47384(7) 0.102(4) Uani 1 1 d G . . H4A H -0.0956 -0.3843 -0.4692 0.122 Uiso 1 1 calc R . . C5A C -0.11578(9) -0.27122(9) -0.43855(6) 0.082(3) Uani 1 1 d G . . H5A H -0.1643 -0.2808 -0.4102 0.099 Uiso 1 1 calc R . . N1C N -0.24637(9) 0.03732(9) -0.35821(6) 0.110(3) Uani 1 1 d G . . C1C C -0.21482(10) 0.10945(9) -0.36587(6) 0.155(6) Uani 1 1 d G . . H1C H -0.1572 0.1145 -0.3837 0.186 Uiso 1 1 calc R . . C2C C -0.26660(10) 0.17790(9) -0.34764(7) 0.281(12) Uani 1 1 d G . . H2C H -0.2426 0.2278 -0.3516 0.338 Uiso 1 1 calc R . . C3C C -0.35438(10) 0.17137(10) -0.32351(7) 0.175(6) Uani 1 1 d G . . H3C H -0.3889 0.2170 -0.3114 0.210 Uiso 1 1 calc R . . C4C C -0.39033(10) 0.09640(10) -0.31755(6) 0.157(6) Uani 1 1 d G . . H4C H -0.4488 0.0921 -0.3015 0.188 Uiso 1 1 calc R . . C5C C -0.33851(9) 0.02793(9) -0.33575(6) 0.127(5) Uani 1 1 d G . . H5C H -0.3621 -0.0222 -0.3336 0.152 Uiso 1 1 calc R . . N1D N -0.15759(10) -0.02586(10) -0.27752(6) 0.066(2) Uani 1 1 d G . . C1D C -0.21471(10) -0.05222(10) -0.22870(6) 0.069(3) Uani 1 1 d G . . H1D H -0.2543 -0.0905 -0.2331 0.083 Uiso 1 1 calc R . . C2D C -0.21244(11) -0.02111(11) -0.17333(6) 0.070(3) Uani 1 1 d G . . H2D H -0.2506 -0.0386 -0.1408 0.084 Uiso 1 1 calc R . . C3D C -0.15294(11) 0.03629(11) -0.16679(6) 0.069(3) Uani 1 1 d G . . H3D H -0.1514 0.0570 -0.1299 0.082 Uiso 1 1 calc R . . C4D C -0.09580(11) 0.06269(11) -0.21564(6) 0.096(3) Uani 1 1 d G . . H4D H -0.0562 0.1010 -0.2113 0.116 Uiso 1 1 calc R . . C5D C -0.09810(10) 0.03159(10) -0.27101(6) 0.092(3) Uani 1 1 d G . . H5D H -0.0600 0.0491 -0.3036 0.110 Uiso 1 1 calc R . . N1E N 0.41606(12) 0.10002(15) -0.23169(10) 0.128(2) Uani 1 1 d G . . C1E C 0.33388(12) 0.13613(14) -0.22643(9) 0.128(2) Uani 1 1 d G . . H1E H 0.3128 0.1527 -0.2597 0.153 Uiso 1 1 calc R . . C2E C 0.28302(13) 0.14759(14) -0.17168(9) 0.128(2) Uani 1 1 d G . . H2E H 0.2277 0.1718 -0.1681 0.153 Uiso 1 1 calc R . . C3E C 0.31440(13) 0.12300(15) -0.12219(9) 0.128(2) Uani 1 1 d G . . H3E H 0.2802 0.1307 -0.0853 0.153 Uiso 1 1 calc R . . C4E C 0.39659(13) 0.08692(16) -0.12748(10) 0.128(2) Uani 1 1 d G . . H4E H 0.4177 0.0704 -0.0942 0.153 Uiso 1 1 calc R . . C5E C 0.44743(12) 0.07544(16) -0.18225(10) 0.128(2) Uani 1 1 d G . . H5E H 0.5028 0.0512 -0.1858 0.153 Uiso 1 1 calc R . . N1F N 0.29145(12) -0.34914(13) -0.24002(9) 0.1143(18) Uani 1 1 d G . . C1F C 0.23024(11) -0.29423(12) -0.25557(8) 0.1143(18) Uani 1 1 d G . . H1F H 0.2482 -0.2519 -0.2802 0.137 Uiso 1 1 calc R . . C2F C 0.14212(11) -0.30260(12) -0.23435(8) 0.1143(18) Uani 1 1 d G . . H2F H 0.1012 -0.2659 -0.2448 0.137 Uiso 1 1 calc R . . C3F C 0.11521(12) -0.36593(12) -0.19755(8) 0.1143(18) Uani 1 1 d G . . H3F H 0.0563 -0.3715 -0.1834 0.137 Uiso 1 1 calc R . . C4F C 0.17642(13) -0.42085(13) -0.18199(9) 0.1143(18) Uani 1 1 d G . . H4F H 0.1584 -0.4632 -0.1574 0.137 Uiso 1 1 calc R . . C5F C 0.26455(13) -0.41247(13) -0.20320(9) 0.1143(18) Uani 1 1 d G . . H5F H 0.3055 -0.4492 -0.1928 0.137 Uiso 1 1 calc R . . N1G N 0.25791(16) 0.31470(16) -0.03549(10) 0.158(3) Uani 1 1 d G . . C1G C 0.19062(15) 0.29816(15) -0.06474(10) 0.158(3) Uani 1 1 d G . . H1G H 0.1663 0.2484 -0.0608 0.189 Uiso 1 1 calc R . . C2G C 0.15972(15) 0.35592(14) -0.09984(10) 0.158(3) Uani 1 1 d G . . H2G H 0.1146 0.3449 -0.1194 0.189 Uiso 1 1 calc R . . C3G C 0.19617(16) 0.43020(15) -0.10581(11) 0.158(3) Uani 1 1 d G . . H3G H 0.1755 0.4689 -0.1294 0.189 Uiso 1 1 calc R . . C4G C 0.26345(17) 0.44674(16) -0.07660(11) 0.158(3) Uani 1 1 d G . . H4G H 0.2878 0.4965 -0.0806 0.189 Uiso 1 1 calc R . . C5G C 0.29435(17) 0.38898(17) -0.04144(11) 0.158(3) Uani 1 1 d G . . H5G H 0.3394 0.4000 -0.0219 0.189 Uiso 1 1 calc R . . N1H N 0.17505(14) -0.28755(15) -0.06390(8) 0.175(3) Uani 1 1 d G . . C1H C 0.19317(13) -0.22529(14) -0.10326(8) 0.175(3) Uani 1 1 d G . . H1H H 0.1481 -0.1927 -0.1127 0.209 Uiso 1 1 calc R . . C2H C 0.27868(13) -0.21176(15) -0.12849(8) 0.175(3) Uani 1 1 d G . . H2H H 0.2908 -0.1701 -0.1548 0.209 Uiso 1 1 calc R . . C3H C 0.34604(13) -0.26052(16) -0.11442(9) 0.175(3) Uani 1 1 d G . . H3H H 0.4033 -0.2515 -0.1314 0.209 Uiso 1 1 calc R . . C4H C 0.32792(14) -0.32280(16) -0.07505(9) 0.175(3) Uani 1 1 d G . . H4H H 0.3730 -0.3554 -0.0656 0.209 Uiso 1 1 calc R . . C5H C 0.24244(15) -0.33628(16) -0.04981(9) 0.175(3) Uani 1 1 d G . . H5H H 0.2303 -0.3780 -0.0235 0.209 Uiso 1 1 calc R . . N1I N 0.54360(11) -0.42760(15) -0.46210(11) 0.168(2) Uani 1 1 d G . . C1I C 0.58700(11) -0.41697(16) -0.51914(11) 0.168(2) Uani 1 1 d G . . H1I H 0.5715 -0.4454 -0.5497 0.201 Uiso 1 1 calc R . . C2I C 0.65353(10) -0.36376(17) -0.53045(11) 0.168(2) Uani 1 1 d G . . H2I H 0.6826 -0.3566 -0.5686 0.201 Uiso 1 1 calc R . . C3I C 0.67664(10) -0.32123(17) -0.48476(11) 0.168(2) Uani 1 1 d G . . H3I H 0.7212 -0.2856 -0.4924 0.201 Uiso 1 1 calc R . . C4I C 0.63325(10) -0.33187(16) -0.42768(11) 0.168(2) Uani 1 1 d G . . H4I H 0.6487 -0.3034 -0.3971 0.201 Uiso 1 1 calc R . . C5I C 0.56673(11) -0.38507(15) -0.41639(11) 0.168(2) Uani 1 1 d G . . H5I H 0.5377 -0.3922 -0.3782 0.201 Uiso 1 1 calc R . . N1J N -0.3341(2) 0.6030(2) 0.25822(11) 0.193(3) Uani 1 1 d G . . C1J C -0.3635(2) 0.65325(19) 0.21828(12) 0.193(3) Uani 1 1 d G . . H1J H -0.3272 0.6645 0.1832 0.232 Uiso 1 1 calc R . . C2J C -0.4467(2) 0.6868(2) 0.23024(12) 0.193(3) Uani 1 1 d G . . H2J H -0.4665 0.7208 0.2032 0.232 Uiso 1 1 calc R . . C3J C -0.5005(2) 0.6701(2) 0.28214(12) 0.193(3) Uani 1 1 d G . . H3J H -0.5567 0.6928 0.2902 0.232 Uiso 1 1 calc R . . C4J C -0.4711(2) 0.6199(2) 0.32209(12) 0.193(3) Uani 1 1 d G . . H4J H -0.5075 0.6086 0.3572 0.232 Uiso 1 1 calc R . . C5J C -0.3880(2) 0.5863(2) 0.31013(11) 0.193(3) Uani 1 1 d G . . H5J H -0.3681 0.5523 0.3371 0.232 Uiso 1 1 calc R . . N1K N -0.35699(11) -0.35007(11) -0.23213(7) 0.217(4) Uani 1 1 d G . . C1K C -0.43386(11) -0.33752(11) -0.25315(7) 0.217(4) Uani 1 1 d G . . H1K H -0.4419 -0.2927 -0.2756 0.260 Uiso 1 1 calc R . . C2K C -0.49878(12) -0.39171(11) -0.24074(8) 0.217(4) Uani 1 1 d G . . H2K H -0.5504 -0.3833 -0.2549 0.260 Uiso 1 1 calc R . . C3K C -0.48685(13) -0.45845(12) -0.20724(8) 0.217(4) Uani 1 1 d G . . H3K H -0.5305 -0.4948 -0.1989 0.260 Uiso 1 1 calc R . . C4K C -0.40999(13) -0.47103(12) -0.18622(8) 0.217(4) Uani 1 1 d G . . H4K H -0.4020 -0.5159 -0.1637 0.260 Uiso 1 1 calc R . . C5K C -0.34508(12) -0.41683(11) -0.19867(7) 0.217(4) Uani 1 1 d G . . H5K H -0.2934 -0.4253 -0.1845 0.260 Uiso 1 1 calc R . . N1L N 0.42558(9) -0.10886(14) -0.53868(9) 0.254(5) Uani 1 1 d G . . C1L C 0.36747(9) -0.12542(13) -0.52301(8) 0.254(5) Uani 1 1 d G . . H1L H 0.3298 -0.0842 -0.5058 0.305 Uiso 1 1 calc R . . C2L C 0.32259(9) -0.21292(12) -0.52105(8) 0.254(5) Uani 1 1 d G . . H2L H 0.2637 -0.2229 -0.5160 0.305 Uiso 1 1 calc R . . C3L C 0.39477(9) -0.26990(13) -0.52884(9) 0.254(5) Uani 1 1 d G . . H3L H 0.3829 -0.3230 -0.5207 0.305 Uiso 1 1 calc R . . C4L C 0.48136(9) -0.25196(14) -0.54769(9) 0.254(5) Uani 1 1 d G . . H4L H 0.5239 -0.2929 -0.5556 0.305 Uiso 1 1 calc R . . C5L C 0.50416(9) -0.17261(15) -0.55471(9) 0.254(5) Uani 1 1 d G . . H5L H 0.5611 -0.1582 -0.5678 0.305 Uiso 1 1 calc R . . N1M N -0.1815(5) 0.3932(4) -0.3159(3) 0.213(4) Uani 1 1 d G . . C1M C -0.1221(6) 0.4354(6) -0.3453(4) 0.213(4) Uani 1 1 d G . . H1M H -0.0666 0.4338 -0.3362 0.255 Uiso 1 1 calc R . . C2M C -0.1397(9) 0.4799(6) -0.3875(4) 0.213(4) Uani 1 1 d G . . H2M H -0.0969 0.5104 -0.4088 0.255 Uiso 1 1 calc R . . C3M C -0.2167(10) 0.4822(7) -0.4001(4) 0.213(4) Uani 1 1 d G . . H3M H -0.2293 0.5143 -0.4305 0.255 Uiso 1 1 calc R . . C4M C -0.2761(8) 0.4400(8) -0.3706(5) 0.213(4) Uani 1 1 d G . . H4M H -0.3316 0.4416 -0.3798 0.255 Uiso 1 1 calc R . . C5M C -0.2585(5) 0.3954(6) -0.3285(4) 0.213(4) Uani 1 1 d G . . H5M H -0.3013 0.3649 -0.3072 0.255 Uiso 1 1 calc R . . C2N C -0.4448 -0.5065 -0.0430 0.200 Uani 1 1 d . . . C3N C -0.5047 -0.4674 -0.0486 0.200 Uani 1 1 d . . . C1N C -0.4248 -0.5307 -0.0153 0.200 Uani 1 1 d . . . O11 O -0.0900(3) 0.1015(3) 0.01304(18) 0.0652(18) Uani 1 1 d . . . O12 O 0.0461(3) 0.0420(3) -0.0843(2) 0.0704(18) Uani 1 1 d . . . O13 O 0.0487(3) -0.0820(3) -0.2688(2) 0.076(2) Uani 1 1 d . . . O14 O -0.0536(3) -0.1677(3) -0.3286(2) 0.0710(18) Uani 1 1 d . . . O15 O -0.1015(3) -0.1895(3) -0.2109(2) 0.0712(19) Uani 1 1 d . . . O16 O -0.1015(3) -0.0605(3) -0.02780(19) 0.0614(17) Uani 1 1 d . . . C11 C -0.14069(19) 0.1297(2) -0.02510(13) 0.059(2) Uani 1 1 d G . . C12 C -0.2262(2) 0.1059(2) -0.01967(16) 0.064(3) Uani 1 1 d G . . C13 C -0.2810(2) 0.1401(3) -0.0552(2) 0.057(2) Uani 1 1 d G . . H13 H -0.3379 0.1243 -0.0516 0.068 Uiso 1 1 calc R . . C14 C -0.2504(3) 0.1982(3) -0.0962(2) 0.056(2) Uani 1 1 d G . . C15 C -0.1649(3) 0.2220(3) -0.10161(18) 0.067(3) Uani 1 1 d G . . H15 H -0.1445 0.2606 -0.1289 0.081 Uiso 1 1 calc R . . C16 C -0.1101(2) 0.1878(2) -0.06606(15) 0.063(3) Uani 1 1 d G . . C17 C -0.0123(4) 0.2047(4) -0.0762(3) 0.054(2) Uani 1 1 d . . . H17A H -0.0055 0.2620 -0.0764 0.065 Uiso 1 1 calc R . . H17B H 0.0133 0.1823 -0.0443 0.065 Uiso 1 1 calc R . . C18 C -0.3135(4) 0.2323(4) -0.1326(3) 0.055(2) Uani 1 1 d . . . C19A C -0.2692(6) 0.2822(6) -0.1822(4) 0.126(4) Uani 1 1 d . . . H19A H -0.2267 0.2495 -0.2077 0.189 Uiso 1 1 calc R . . H19B H -0.2411 0.3249 -0.1667 0.189 Uiso 1 1 calc R . . H19C H -0.3116 0.3041 -0.2038 0.189 Uiso 1 1 calc R . . C19B C -0.3739(7) 0.2893(8) -0.0982(5) 0.170(6) Uani 1 1 d . . . H19D H -0.4141 0.3108 -0.1216 0.254 Uiso 1 1 calc R . . H19E H -0.3425 0.3318 -0.0855 0.254 Uiso 1 1 calc R . . H19F H -0.4053 0.2630 -0.0646 0.254 Uiso 1 1 calc R . . C19C C -0.3596(6) 0.1650(5) -0.1590(4) 0.108(3) Uani 1 1 d . . . H19G H -0.3167 0.1290 -0.1812 0.162 Uiso 1 1 calc R . . H19H H -0.3965 0.1880 -0.1841 0.162 Uiso 1 1 calc R . . H19I H -0.3940 0.1364 -0.1279 0.162 Uiso 1 1 calc R . . C21 C 0.06502(18) 0.0898(2) -0.13384(13) 0.050(2) Uani 1 1 d G . . C22 C 0.0346(3) 0.1697(2) -0.13307(17) 0.060(3) Uani 1 1 d G . . C23 C 0.0480(4) 0.2145(2) -0.1846(2) 0.064(3) Uani 1 1 d G . . H23 H 0.0278 0.2675 -0.1841 0.077 Uiso 1 1 calc R . . C24 C 0.0917(4) 0.1795(3) -0.23685(17) 0.068(3) Uani 1 1 d G . . C25 C 0.1220(3) 0.0997(3) -0.23763(14) 0.067(3) Uani 1 1 d G . . H25 H 0.1510 0.0764 -0.2724 0.080 Uiso 1 1 calc R . . C26 C 0.1087(2) 0.0549(2) -0.18614(15) 0.053(2) Uani 1 1 d G . . C27 C 0.1412(5) -0.0303(5) -0.1874(3) 0.068(3) Uani 1 1 d . . . H27A H 0.1810 -0.0357 -0.1599 0.082 Uiso 1 1 calc R . . H27B H 0.0920 -0.0625 -0.1727 0.082 Uiso 1 1 calc R . . C28 C 0.1031(5) 0.2299(5) -0.2945(3) 0.070(3) Uani 1 1 d . . . C29A C 0.1966(7) 0.2348(5) -0.3212(4) 0.119(4) Uani 1 1 d . . . H29A H 0.2221 0.1819 -0.3289 0.179 Uiso 1 1 calc R . . H29B H 0.2263 0.2617 -0.2947 0.179 Uiso 1 1 calc R . . H29C H 0.2015 0.2640 -0.3573 0.179 Uiso 1 1 calc R . . C29B C 0.0702(8) 0.3165(7) -0.2835(5) 0.147(6) Uani 1 1 d . . . H29D H 0.0100 0.3181 -0.2652 0.221 Uiso 1 1 calc R . . H29E H 0.0764 0.3445 -0.3201 0.221 Uiso 1 1 calc R . . H29F H 0.1035 0.3416 -0.2582 0.221 Uiso 1 1 calc R . . C29C C 0.0619(9) 0.1814(8) -0.3396(4) 0.169(6) Uani 1 1 d . . . H29G H 0.0867 0.1278 -0.3425 0.254 Uiso 1 1 calc R . . H29H H 0.0737 0.2065 -0.3773 0.254 Uiso 1 1 calc R . . H29I H 0.0002 0.1803 -0.3265 0.254 Uiso 1 1 calc R . . C31 C 0.13531(18) -0.08835(19) -0.28455(14) 0.071(3) Uani 1 1 d G . . C32 C 0.1852(2) -0.0651(3) -0.24309(15) 0.051(2) Uani 1 1 d G . . C33 C 0.2766(2) -0.0739(3) -0.25604(19) 0.058(3) Uani 1 1 d G . . H33 H 0.3095 -0.0586 -0.2287 0.070 Uiso 1 1 calc R . . C34 C 0.31818(18) -0.1059(3) -0.3105(2) 0.059(3) Uani 1 1 d G . . C35 C 0.2683(2) -0.1291(3) -0.35204(18) 0.054(2) Uani 1 1 d G . . H35 H 0.2958 -0.1502 -0.3880 0.065 Uiso 1 1 calc R . . C36 C 0.1769(2) -0.1203(3) -0.33904(15) 0.059(3) Uani 1 1 d G . . C37 C 0.1241(4) -0.1460(4) -0.3851(3) 0.056(2) Uani 1 1 d . . . H37A H 0.0783 -0.1057 -0.3870 0.067 Uiso 1 1 calc R . . H37B H 0.1619 -0.1484 -0.4231 0.067 Uiso 1 1 calc R . . C38 C 0.4197(5) -0.1184(5) -0.3259(3) 0.071(3) Uani 1 1 d . . . C39A C 0.4580(5) -0.1165(5) -0.2718(3) 0.081(3) Uani 1 1 d . . . H39A H 0.4362 -0.1591 -0.2464 0.122 Uiso 1 1 calc R . . H39B H 0.4424 -0.0662 -0.2521 0.122 Uiso 1 1 calc R . . H39C H 0.5202 -0.1228 -0.2819 0.122 Uiso 1 1 calc R . . C39B C 0.4443(6) -0.2017(5) -0.3588(4) 0.106(4) Uani 1 1 d . . . H39D H 0.4193 -0.2023 -0.3937 0.159 Uiso 1 1 calc R . . H39E H 0.4219 -0.2442 -0.3335 0.159 Uiso 1 1 calc R . . H39F H 0.5064 -0.2087 -0.3691 0.159 Uiso 1 1 calc R . . C39C C 0.4550(6) -0.0511(6) -0.3682(4) 0.116(4) Uani 1 1 d . . . H39G H 0.4283 -0.0524 -0.4024 0.174 Uiso 1 1 calc R . . H39H H 0.5169 -0.0589 -0.3796 0.174 Uiso 1 1 calc R . . H39I H 0.4416 -0.0003 -0.3490 0.174 Uiso 1 1 calc R . . C41 C -0.0005(2) -0.2341(2) -0.34171(13) 0.058(3) Uani 1 1 d G . . C42 C 0.0840(2) -0.2252(3) -0.37294(17) 0.063(3) Uani 1 1 d G . . C43 C 0.1397(2) -0.2928(3) -0.3882(2) 0.074(3) Uani 1 1 d G . . H43 H 0.1958 -0.2870 -0.4089 0.089 Uiso 1 1 calc R . . C44 C 0.1108(3) -0.3692(3) -0.3723(3) 0.073(3) Uani 1 1 d G . . C45 C 0.0263(3) -0.3781(2) -0.3410(2) 0.063(3) Uani 1 1 d G . . H45 H 0.0071 -0.4287 -0.3305 0.075 Uiso 1 1 calc R . . C46 C -0.0294(2) -0.3105(2) -0.32579(17) 0.057(2) Uani 1 1 d G . . C47 C -0.1151(4) -0.3220(5) -0.2870(3) 0.064(3) Uani 1 1 d . . . H47A H -0.1399 -0.3694 -0.3000 0.077 Uiso 1 1 calc R . . H47B H -0.1541 -0.2768 -0.2918 0.077 Uiso 1 1 calc R . . C48 C 0.1647(5) -0.4457(5) -0.3930(3) 0.073(3) Uani 1 1 d . . . C49A C 0.2600(7) -0.4232(7) -0.4256(6) 0.180(7) Uani 1 1 d . . . H49A H 0.2933 -0.4711 -0.4390 0.269 Uiso 1 1 calc R . . H49B H 0.2885 -0.3956 -0.3988 0.269 Uiso 1 1 calc R . . H49C H 0.2550 -0.3894 -0.4584 0.269 Uiso 1 1 calc R . . C49B C 0.1775(7) -0.4922(6) -0.3361(5) 0.118(5) Uani 1 1 d . . . H49D H 0.2123 -0.5404 -0.3467 0.177 Uiso 1 1 calc R . . H49E H 0.1219 -0.5054 -0.3143 0.177 Uiso 1 1 calc R . . H49F H 0.2063 -0.4593 -0.3124 0.177 Uiso 1 1 calc R . . C49C C 0.1237(7) -0.4994(7) -0.4300(5) 0.155(5) Uani 1 1 d . . . H49G H 0.1625 -0.5445 -0.4423 0.232 Uiso 1 1 calc R . . H49H H 0.1117 -0.4708 -0.4638 0.232 Uiso 1 1 calc R . . H49I H 0.0704 -0.5174 -0.4077 0.232 Uiso 1 1 calc R . . C51 C -0.1044(2) -0.2644(2) -0.18809(15) 0.048(2) Uani 1 1 d G . . C52 C -0.1113(3) -0.3309(2) -0.22220(17) 0.062(3) Uani 1 1 d G . . C53 C -0.1113(3) -0.4066(2) -0.1978(2) 0.072(3) Uani 1 1 d G . . H53 H -0.1158 -0.4512 -0.2206 0.087 Uiso 1 1 calc R . . C54 C -0.1045(4) -0.4159(3) -0.1393(2) 0.067(3) Uani 1 1 d G . . C55 C -0.0976(4) -0.3494(3) -0.10515(18) 0.082(3) Uani 1 1 d G . . H55 H -0.0931 -0.3556 -0.0660 0.099 Uiso 1 1 calc R . . C56 C -0.0976(3) -0.2736(3) -0.12954(15) 0.057(3) Uani 1 1 d G . . C57 C -0.0907(4) -0.1986(5) -0.0943(3) 0.063(3) Uani 1 1 d . . . H57A H -0.0618 -0.2127 -0.0618 0.076 Uiso 1 1 calc R . . H57B H -0.0548 -0.1616 -0.1190 0.076 Uiso 1 1 calc R . . C58 C -0.1050(5) -0.5028(5) -0.1130(3) 0.075(3) Uani 1 1 d . . . C59A C -0.0590(7) -0.5614(5) -0.1563(4) 0.113(4) Uani 1 1 d . . . H59A H 0.0008 -0.5483 -0.1670 0.170 Uiso 1 1 calc R . . H59B H -0.0857 -0.5601 -0.1905 0.170 Uiso 1 1 calc R . . H59C H -0.0624 -0.6139 -0.1396 0.170 Uiso 1 1 calc R . . C59B C -0.1964(6) -0.5265(6) -0.0977(5) 0.128(5) Uani 1 1 d . . . H59D H -0.2233 -0.5223 -0.1318 0.191 Uiso 1 1 calc R . . H59E H -0.2276 -0.4918 -0.0675 0.191 Uiso 1 1 calc R . . H59F H -0.1976 -0.5806 -0.0841 0.191 Uiso 1 1 calc R . . C59C C -0.0663(6) -0.5129(7) -0.0564(4) 0.119(5) Uani 1 1 d . . . H59G H -0.0065 -0.4989 -0.0641 0.179 Uiso 1 1 calc R . . H59H H -0.0700 -0.5674 -0.0438 0.179 Uiso 1 1 calc R . . H59I H -0.0984 -0.4786 -0.0263 0.179 Uiso 1 1 calc R . . C61 C -0.17580(19) -0.0866(2) -0.03773(13) 0.047(2) Uani 1 1 d G . . C62 C -0.1781(2) -0.1571(2) -0.07057(18) 0.063(3) Uani 1 1 d G . . C63 C -0.2582(3) -0.1830(3) -0.0818(2) 0.062(3) Uani 1 1 d G . . H63 H -0.2597 -0.2293 -0.1034 0.074 Uiso 1 1 calc R . . C64 C -0.3362(2) -0.1384(4) -0.0602(2) 0.074(3) Uani 1 1 d G . . C65 C -0.3339(2) -0.0679(3) -0.0274(2) 0.082(3) Uani 1 1 d G . . H65 H -0.3852 -0.0385 -0.0132 0.098 Uiso 1 1 calc R . . C66 C -0.2537(2) -0.0419(2) -0.01613(17) 0.055(2) Uani 1 1 d G . . C67 C -0.2539(5) 0.0338(5) 0.0199(3) 0.066(3) Uani 1 1 d . . . H67A H -0.2143 0.0258 0.0474 0.079 Uiso 1 1 calc R . . H67B H -0.3118 0.0450 0.0423 0.079 Uiso 1 1 calc R . . C68 C -0.4206(4) -0.1660(5) -0.0768(3) 0.068(3) Uani 1 1 d . . . C69A C -0.4193(6) -0.1574(7) -0.1414(4) 0.119(5) Uani 1 1 d . . . H69A H -0.3673 -0.1834 -0.1627 0.178 Uiso 1 1 calc R . . H69B H -0.4206 -0.1017 -0.1514 0.178 Uiso 1 1 calc R . . H69C H -0.4693 -0.1815 -0.1515 0.178 Uiso 1 1 calc R . . C69B C -0.4988(5) -0.1239(7) -0.0479(5) 0.140(5) Uani 1 1 d . . . H69D H -0.5024 -0.1274 -0.0063 0.211 Uiso 1 1 calc R . . H69E H -0.5485 -0.1475 -0.0588 0.211 Uiso 1 1 calc R . . H69F H -0.4977 -0.0689 -0.0595 0.211 Uiso 1 1 calc R . . C69C C -0.4313(5) -0.2513(6) -0.0585(5) 0.111(4) Uani 1 1 d . . . H69G H -0.3823 -0.2835 -0.0779 0.167 Uiso 1 1 calc R . . H69H H -0.4836 -0.2699 -0.0690 0.167 Uiso 1 1 calc R . . H69I H -0.4348 -0.2552 -0.0168 0.167 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 U1 0.0579(2) 0.0736(3) 0.0413(2) -0.0077(2) -0.00672(17) -0.0036(2) La1 0.03905(16) 0.0398(2) 0.02086(16) -0.00186(14) -0.00685(12) -0.00615(15) Cl1 0.0728(11) 0.1024(19) 0.0687(12) 0.0002(12) -0.0206(9) -0.0141(12) Cl2 0.0818(12) 0.1045(19) 0.0573(12) 0.0002(12) -0.0065(10) -0.0217(12) N1B 0.064(3) 0.077(5) 0.050(3) -0.007(3) -0.006(3) -0.016(3) C1B 0.079(5) 0.129(8) 0.049(5) 0.014(5) -0.017(4) -0.007(5) C2B 0.138(6) 0.121(8) 0.061(5) -0.011(5) -0.056(4) -0.022(6) C3B 0.181(7) 0.058(6) 0.085(5) -0.006(4) -0.089(4) 0.015(6) C4B 0.115(6) 0.114(8) 0.029(4) 0.002(4) -0.029(4) -0.017(5) C5B 0.118(6) 0.081(6) 0.042(4) 0.022(4) -0.014(4) -0.039(5) N1A 0.089(4) 0.090(5) 0.046(3) -0.013(3) -0.013(3) -0.009(4) C1A 0.061(5) 0.138(8) 0.058(5) -0.035(5) 0.007(4) 0.002(5) C2A 0.079(5) 0.168(10) 0.088(6) -0.032(6) -0.023(5) -0.008(6) C3A 0.104(7) 0.349(14) 0.148(7) -0.164(7) -0.010(6) -0.031(8) C4A 0.131(7) 0.092(8) 0.080(6) -0.003(5) -0.006(5) -0.031(6) C5A 0.067(5) 0.095(6) 0.073(5) -0.041(4) 0.025(4) -0.025(4) N1C 0.091(5) 0.118(7) 0.108(6) 0.000(5) 0.014(4) 0.003(5) C1C 0.141(8) 0.053(7) 0.266(15) 0.034(9) -0.015(9) -0.045(6) C2C 0.270(15) 0.064(9) 0.49(3) 0.055(13) -0.041(18) 0.101(9) C3C 0.135(9) 0.270(15) 0.117(8) -0.069(9) -0.005(7) -0.030(10) C4C 0.051(5) 0.218(13) 0.201(11) -0.013(10) -0.033(6) 0.042(6) C5C 0.122(7) 0.099(9) 0.169(10) 0.051(7) -0.047(7) -0.034(6) N1D 0.082(4) 0.090(5) 0.029(3) -0.006(3) -0.013(3) -0.004(4) C1D 0.095(5) 0.050(5) 0.067(5) 0.020(4) -0.024(4) -0.016(4) C2D 0.087(5) 0.064(6) 0.055(5) -0.007(4) -0.001(4) 0.002(4) C3D 0.070(4) 0.089(7) 0.050(4) 0.001(4) -0.016(3) -0.008(4) C4D 0.125(5) 0.099(7) 0.071(5) -0.036(4) -0.050(4) 0.069(5) C5D 0.097(5) 0.089(7) 0.093(6) -0.018(5) -0.016(5) -0.037(5) N1E 0.123(3) 0.136(4) 0.117(4) 0.003(3) -0.007(3) 0.006(3) C1E 0.123(3) 0.136(4) 0.117(4) 0.003(3) -0.007(3) 0.006(3) C2E 0.123(3) 0.136(4) 0.117(4) 0.003(3) -0.007(3) 0.006(3) C3E 0.123(3) 0.136(4) 0.117(4) 0.003(3) -0.007(3) 0.006(3) C4E 0.123(3) 0.136(4) 0.117(4) 0.003(3) -0.007(3) 0.006(3) C5E 0.123(3) 0.136(4) 0.117(4) 0.003(3) -0.007(3) 0.006(3) N1F 0.109(3) 0.102(4) 0.136(3) -0.011(2) -0.033(3) -0.011(3) C1F 0.109(3) 0.102(4) 0.136(3) -0.011(2) -0.033(3) -0.011(3) C2F 0.109(3) 0.102(4) 0.136(3) -0.011(2) -0.033(3) -0.011(3) C3F 0.109(3) 0.102(4) 0.136(3) -0.011(2) -0.033(3) -0.011(3) C4F 0.109(3) 0.102(4) 0.136(3) -0.011(2) -0.033(3) -0.011(3) C5F 0.109(3) 0.102(4) 0.136(3) -0.011(2) -0.033(3) -0.011(3) N1G 0.188(5) 0.131(5) 0.166(5) 0.020(4) -0.057(3) -0.046(4) C1G 0.188(5) 0.131(5) 0.166(5) 0.020(4) -0.057(3) -0.046(4) C2G 0.188(5) 0.131(5) 0.166(5) 0.020(4) -0.057(3) -0.046(4) C3G 0.188(5) 0.131(5) 0.166(5) 0.020(4) -0.057(3) -0.046(4) C4G 0.188(5) 0.131(5) 0.166(5) 0.020(4) -0.057(3) -0.046(4) C5G 0.188(5) 0.131(5) 0.166(5) 0.020(4) -0.057(3) -0.046(4) N1H 0.194(5) 0.172(6) 0.160(5) -0.016(4) -0.047(4) 0.031(5) C1H 0.194(5) 0.172(6) 0.160(5) -0.016(4) -0.047(4) 0.031(5) C2H 0.194(5) 0.172(6) 0.160(5) -0.016(4) -0.047(4) 0.031(5) C3H 0.194(5) 0.172(6) 0.160(5) -0.016(4) -0.047(4) 0.031(5) C4H 0.194(5) 0.172(6) 0.160(5) -0.016(4) -0.047(4) 0.031(5) C5H 0.194(5) 0.172(6) 0.160(5) -0.016(4) -0.047(4) 0.031(5) N1I 0.140(3) 0.132(4) 0.242(6) -0.080(4) -0.065(3) 0.010(3) C1I 0.140(3) 0.132(4) 0.242(6) -0.080(4) -0.065(3) 0.010(3) C2I 0.140(3) 0.132(4) 0.242(6) -0.080(4) -0.065(3) 0.010(3) C3I 0.140(3) 0.132(4) 0.242(6) -0.080(4) -0.065(3) 0.010(3) C4I 0.140(3) 0.132(4) 0.242(6) -0.080(4) -0.065(3) 0.010(3) C5I 0.140(3) 0.132(4) 0.242(6) -0.080(4) -0.065(3) 0.010(3) N1J 0.183(5) 0.202(6) 0.186(6) -0.008(5) -0.021(5) 0.034(5) C1J 0.183(5) 0.202(6) 0.186(6) -0.008(5) -0.021(5) 0.034(5) C2J 0.183(5) 0.202(6) 0.186(6) -0.008(5) -0.021(5) 0.034(5) C3J 0.183(5) 0.202(6) 0.186(6) -0.008(5) -0.021(5) 0.034(5) C4J 0.183(5) 0.202(6) 0.186(6) -0.008(5) -0.021(5) 0.034(5) C5J 0.183(5) 0.202(6) 0.186(6) -0.008(5) -0.021(5) 0.034(5) N1K 0.173(5) 0.206(7) 0.283(7) 0.081(6) -0.068(5) -0.038(5) C1K 0.173(5) 0.206(7) 0.283(7) 0.081(6) -0.068(5) -0.038(5) C2K 0.173(5) 0.206(7) 0.283(7) 0.081(6) -0.068(5) -0.038(5) C3K 0.173(5) 0.206(7) 0.283(7) 0.081(6) -0.068(5) -0.038(5) C4K 0.173(5) 0.206(7) 0.283(7) 0.081(6) -0.068(5) -0.038(5) C5K 0.173(5) 0.206(7) 0.283(7) 0.081(6) -0.068(5) -0.038(5) N1L 0.184(8) 0.350(10) 0.227(6) -0.028(7) -0.021(6) -0.068(7) C1L 0.184(8) 0.350(10) 0.227(6) -0.028(7) -0.021(6) -0.068(7) C2L 0.184(8) 0.350(10) 0.227(6) -0.028(7) -0.021(6) -0.068(7) C3L 0.184(8) 0.350(10) 0.227(6) -0.028(7) -0.021(6) -0.068(7) C4L 0.184(8) 0.350(10) 0.227(6) -0.028(7) -0.021(6) -0.068(7) C5L 0.184(8) 0.350(10) 0.227(6) -0.028(7) -0.021(6) -0.068(7) N1M 0.196(6) 0.257(8) 0.192(6) 0.066(5) -0.057(5) 0.004(6) C1M 0.196(6) 0.257(8) 0.192(6) 0.066(5) -0.057(5) 0.004(6) C2M 0.196(6) 0.257(8) 0.192(6) 0.066(5) -0.057(5) 0.004(6) C3M 0.196(6) 0.257(8) 0.192(6) 0.066(5) -0.057(5) 0.004(6) C4M 0.196(6) 0.257(8) 0.192(6) 0.066(5) -0.057(5) 0.004(6) C5M 0.196(6) 0.257(8) 0.192(6) 0.066(5) -0.057(5) 0.004(6) C2N 0.200 0.200 0.200 0.001 -0.036 -0.009 C3N 0.200 0.200 0.200 0.001 -0.036 -0.009 C1N 0.200 0.200 0.200 0.001 -0.036 -0.009 O11 0.037(2) 0.122(4) 0.034(2) -0.018(3) -0.0039(18) 0.007(3) O12 0.083(3) 0.062(4) 0.064(3) -0.029(2) -0.012(2) 0.014(3) O13 0.069(3) 0.090(4) 0.066(3) -0.014(3) -0.001(2) -0.003(3) O14 0.069(3) 0.096(4) 0.056(3) 0.018(3) -0.032(2) 0.004(3) O15 0.069(3) 0.061(4) 0.076(3) -0.013(3) 0.005(3) 0.004(3) O16 0.062(3) 0.067(4) 0.054(3) 0.000(2) -0.012(2) 0.020(2) C11 0.057(4) 0.063(5) 0.061(4) 0.000(4) -0.025(3) 0.028(3) C12 0.052(4) 0.098(7) 0.047(4) -0.009(4) -0.020(3) 0.004(4) C13 0.063(4) 0.061(5) 0.047(4) -0.001(4) -0.010(3) -0.008(4) C14 0.086(4) 0.042(5) 0.042(4) 0.002(3) -0.019(3) 0.024(4) C15 0.042(3) 0.083(6) 0.082(5) -0.004(4) -0.027(3) 0.016(4) C16 0.075(5) 0.048(5) 0.053(4) 0.005(4) 0.011(4) 0.019(4) C17 0.066(4) 0.054(5) 0.047(4) -0.011(3) -0.020(3) -0.011(4) C18 0.069(4) 0.052(5) 0.043(4) 0.010(3) -0.013(3) 0.010(4) C19A 0.163(7) 0.098(8) 0.143(7) 0.044(6) -0.102(5) 0.002(6) C19B 0.145(7) 0.222(15) 0.161(9) -0.012(10) -0.092(6) 0.043(9) C19C 0.154(6) 0.045(6) 0.152(7) 0.041(5) -0.098(5) -0.029(5) C21 0.059(4) 0.057(5) 0.034(3) 0.014(3) -0.008(3) -0.013(3) C22 0.078(4) 0.067(6) 0.040(4) 0.005(4) -0.024(3) -0.004(4) C23 0.079(5) 0.040(5) 0.076(5) 0.005(4) -0.019(4) -0.004(4) C24 0.068(4) 0.089(7) 0.040(4) 0.005(4) 0.008(3) -0.002(4) C25 0.066(4) 0.063(6) 0.073(5) -0.007(4) -0.017(4) -0.006(4) C26 0.049(4) 0.053(5) 0.052(4) 0.015(3) 0.011(3) -0.013(3) C27 0.092(5) 0.062(6) 0.047(4) -0.006(4) -0.002(4) -0.002(4) C28 0.068(5) 0.081(6) 0.056(4) 0.028(4) -0.002(4) 0.003(4) C29A 0.163(9) 0.056(6) 0.124(7) 0.060(5) 0.010(7) 0.010(6) C29B 0.206(11) 0.136(11) 0.079(7) 0.025(7) 0.030(8) -0.003(9) C29C 0.290(13) 0.189(13) 0.043(5) 0.038(6) -0.067(7) -0.015(11) C31 0.072(5) 0.063(6) 0.073(5) -0.002(4) -0.007(4) 0.011(4) C32 0.055(4) 0.052(5) 0.050(4) 0.011(3) -0.017(3) -0.001(3) C33 0.075(4) 0.061(5) 0.030(4) 0.002(3) 0.013(3) -0.009(4) C34 0.034(3) 0.080(6) 0.068(4) -0.003(4) -0.017(3) -0.012(3) C35 0.055(4) 0.053(5) 0.051(4) 0.005(4) -0.002(3) 0.001(4) C36 0.063(4) 0.045(5) 0.070(5) -0.008(4) -0.012(3) -0.010(4) C37 0.043(3) 0.087(6) 0.036(4) -0.008(4) 0.001(3) -0.016(4) C38 0.062(4) 0.082(7) 0.069(5) -0.006(4) -0.013(4) -0.001(4) C39A 0.081(5) 0.099(7) 0.065(5) -0.017(5) -0.020(4) 0.006(5) C39B 0.126(7) 0.063(7) 0.123(8) -0.011(6) -0.015(6) 0.033(6) C39C 0.075(6) 0.141(10) 0.123(8) 0.038(7) 0.008(5) -0.028(6) C41 0.068(4) 0.075(6) 0.032(4) 0.008(4) -0.013(3) -0.008(4) C42 0.063(4) 0.075(6) 0.050(4) 0.009(4) 0.000(3) -0.023(4) C43 0.057(4) 0.072(6) 0.093(6) 0.011(5) -0.006(4) -0.021(4) C44 0.098(5) 0.072(6) 0.043(4) -0.026(4) -0.003(4) 0.006(5) C45 0.067(4) 0.048(5) 0.074(5) 0.012(4) -0.010(4) -0.022(4) C46 0.076(4) 0.050(5) 0.041(4) -0.008(3) 0.000(3) -0.005(4) C47 0.074(4) 0.062(6) 0.064(4) 0.009(4) -0.029(3) -0.016(4) C48 0.088(5) 0.069(6) 0.055(4) -0.021(4) 0.009(4) -0.005(5) C49A 0.112(8) 0.124(11) 0.264(15) 0.037(10) 0.057(9) 0.044(7) C49B 0.130(7) 0.080(8) 0.150(9) 0.026(7) -0.036(7) -0.020(6) C49C 0.159(9) 0.152(9) 0.151(8) -0.100(6) -0.024(7) 0.006(8) C51 0.041(3) 0.033(4) 0.068(4) 0.004(3) -0.009(3) 0.010(3) C52 0.055(4) 0.069(5) 0.062(4) -0.025(4) -0.004(3) -0.014(4) C53 0.079(5) 0.075(6) 0.062(5) 0.000(4) -0.004(4) -0.018(4) C54 0.076(4) 0.070(6) 0.058(4) -0.018(4) -0.016(3) -0.019(4) C55 0.081(5) 0.081(7) 0.087(6) 0.013(5) -0.023(4) -0.008(5) C56 0.039(3) 0.075(6) 0.053(4) -0.006(4) 0.007(3) -0.009(4) C57 0.037(3) 0.090(6) 0.062(4) -0.006(4) -0.012(3) 0.011(4) C58 0.070(5) 0.084(7) 0.071(5) -0.010(5) -0.017(4) 0.003(5) C59A 0.221(10) 0.045(6) 0.072(6) -0.007(5) -0.032(6) 0.030(7) C59B 0.138(8) 0.072(8) 0.177(10) 0.042(7) -0.033(7) -0.047(6) C59C 0.120(7) 0.164(11) 0.075(6) -0.010(7) -0.025(5) 0.009(7) C61 0.042(3) 0.058(5) 0.041(4) 0.002(3) -0.005(3) -0.007(3) C62 0.084(5) 0.077(6) 0.028(4) 0.000(4) -0.006(3) -0.011(4) C63 0.038(3) 0.099(6) 0.049(4) -0.023(4) -0.010(3) 0.007(4) C64 0.072(4) 0.093(6) 0.057(4) -0.021(4) -0.005(4) -0.026(4) C65 0.082(5) 0.099(7) 0.061(5) 0.001(5) -0.003(4) -0.009(5) C66 0.054(4) 0.062(5) 0.047(4) 0.014(4) -0.008(3) 0.005(4) C67 0.074(5) 0.071(6) 0.043(4) -0.003(4) 0.015(3) -0.009(4) C68 0.056(4) 0.077(6) 0.067(5) -0.032(4) 0.002(3) 0.001(4) C69A 0.088(6) 0.143(10) 0.135(8) 0.010(7) -0.041(5) -0.020(6) C69B 0.058(5) 0.154(10) 0.208(11) -0.060(8) -0.025(6) 0.018(6) C69C 0.049(5) 0.093(8) 0.187(10) -0.023(7) -0.006(5) 0.001(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 U1 O12 2.090(5) . ? U1 O12 2.091(5) 2 ? U1 O16 2.118(5) 2 ? U1 O16 2.118(5) . ? U1 O11 2.145(5) 2 ? U1 O11 2.145(5) . ? La1 O14 2.257(5) . ? La1 N1D 2.4426(15) . ? La1 N1A 2.4651(16) . ? La1 N1B 2.5236(16) . ? La1 Cl2 2.564(2) . ? La1 Cl1 2.586(2) . ? La1 N1C 2.6061(17) . ? N1B C1B 1.3789 . ? N1B C5B 1.3791 . ? C1B C2B 1.3781 . ? C2B C3B 1.3789 . ? C3B C4B 1.3784 . ? C4B C5B 1.3789 . ? N1A C1A 1.3844 . ? N1A C5A 1.3846 . ? C1A C2A 1.3852 . ? C2A C3A 1.3848 . ? C3A C4A 1.3852 . ? C4A C5A 1.3847 . ? N1C C1C 1.3257 . ? N1C C5C 1.4577 . ? C1C C2C 1.3957 . ? C2C C3C 1.3960 . ? C3C C4C 1.3960 . ? C4C C5C 1.3962 . ? N1D C1D 1.3949 . ? N1D C5D 1.3959 . ? C1D C2D 1.3952 . ? C2D C3D 1.3956 . ? C3D C4D 1.3958 . ? C4D C5D 1.3953 . ? N1E C5E 1.3810 . ? N1E C1E 1.3814 . ? C1E C2E 1.3817 . ? C2E C3E 1.3821 . ? C3E C4E 1.3814 . ? C4E C5E 1.3821 . ? N1F C1F 1.3914 . ? N1F C5F 1.3921 . ? C1F C2F 1.3915 . ? C2F C3F 1.3920 . ? C3F C4F 1.3917 . ? C4F C5F 1.3917 . ? N1G C5G 1.3886 . ? N1G C1G 1.3892 . ? C1G C2G 1.3883 . ? C2G C3G 1.3886 . ? C3G C4G 1.3885 . ? C4G C5G 1.3892 . ? N1H C5H 1.3891 . ? N1H C1H 1.3893 . ? C1H C2H 1.3890 . ? C2H C3H 1.3888 . ? C3H C4H 1.3897 . ? C4H C5H 1.3887 . ? N1I C5I 1.3895 . ? N1I C1I 1.3897 . ? C1I C2I 1.3899 . ? C2I C3I 1.3887 . ? C3I C4I 1.3905 . ? C4I C5I 1.3896 . ? N1J C1J 1.3750 . ? N1J C5J 1.3761 . ? C1J C2J 1.3755 . ? C2J C3J 1.3755 . ? C3J C4J 1.3755 . ? C4J C5J 1.3751 . ? N1K C1K 1.3840 . ? N1K C5K 1.3841 . ? C1K C2K 1.3841 . ? C2K C3K 1.3844 . ? C3K C4K 1.3840 . ? C4K C5K 1.3842 . ? N1L C1L 0.9691 . ? N1L C5L 1.5849 . ? C1L C2L 1.6513 . ? C2L C3L 1.4319 . ? C3L C4L 1.3929 . ? C4L C5L 1.3939 . ? N1M C1M 1.2884 . ? N1M C5M 1.2885 . ? C1M C2M 1.2886 . ? C2M C3M 1.2882 . ? C3M C4M 1.2883 . ? C4M C5M 1.2888 . ? C2N C1N 0.8569 . ? C2N C3N 1.1455 . ? C3N C1N 1.6829 2_445 ? C3N C1N 1.8724 . ? C1N C3N 1.6829 2_445 ? O11 C11 1.360(5) . ? O12 C21 1.395(6) . ? O13 C31 1.339(5) . ? O14 C41 1.360(6) . ? O15 C51 1.359(6) . ? O16 C61 1.318(6) . ? C11 C12 1.3967 . ? C11 C16 1.3967 . ? C12 C13 1.3970 . ? C12 C67 1.545(8) . ? C13 C14 1.3970 . ? C14 C15 1.3967 . ? C14 C18 1.504(8) . ? C15 C16 1.3968 . ? C16 C17 1.545(7) . ? C17 C22 1.498(7) . ? C18 C19B 1.448(13) . ? C18 C19A 1.503(11) . ? C18 C19C 1.549(12) . ? C21 C26 1.3981 . ? C21 C22 1.3982 . ? C22 C23 1.3974 . ? C23 C24 1.3979 . ? C24 C25 1.3977 . ? C24 C28 1.567(8) . ? C25 C26 1.3974 . ? C26 C27 1.492(9) . ? C27 C32 1.461(7) . ? C28 C29A 1.488(12) . ? C28 C29B 1.525(14) . ? C28 C29C 1.570(14) . ? C31 C32 1.4089 . ? C31 C36 1.4097 . ? C32 C33 1.4094 . ? C33 C34 1.4100 . ? C34 C35 1.4092 . ? C34 C38 1.569(8) . ? C35 C36 1.4093 . ? C36 C37 1.536(8) . ? C37 C42 1.498(8) . ? C38 C39A 1.486(11) . ? C38 C39C 1.547(13) . ? C38 C39B 1.591(12) . ? C41 C46 1.4030 . ? C41 C42 1.4036 . ? C42 C43 1.4038 . ? C43 C44 1.4033 . ? C44 C45 1.4039 . ? C44 C48 1.531(9) . ? C45 C46 1.4042 . ? C46 C47 1.495(7) . ? C47 C52 1.523(8) . ? C48 C49C 1.487(14) . ? C48 C49B 1.571(13) . ? C48 C49A 1.606(13) . ? C51 C52 1.3882 . ? C51 C56 1.3891 . ? C52 C53 1.3885 . ? C53 C54 1.3883 . ? C54 C55 1.3891 . ? C54 C58 1.576(10) . ? C55 C56 1.3884 . ? C56 C57 1.520(9) . ? C57 C62 1.517(7) . ? C58 C59A 1.475(11) . ? C58 C59B 1.483(12) . ? C58 C59C 1.546(13) . ? C61 C66 1.4135 . ? C61 C62 1.4138 . ? C62 C63 1.4134 . ? C63 C64 1.4138 . ? C64 C65 1.4136 . ? C64 C68 1.532(8) . ? C65 C66 1.4139 . ? C66 C67 1.523(8) . ? C68 C69B 1.440(11) . ? C68 C69C 1.499(12) . ? C68 C69A 1.502(12) . ? 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 O12 U1 O12 180.0 . 2 ? O12 U1 O16 87.35(19) . 2 ? O12 U1 O16 92.65(19) 2 2 ? O12 U1 O16 92.65(19) . . ? O12 U1 O16 87.35(19) 2 . ? O16 U1 O16 180.0 2 . ? O12 U1 O11 91.56(17) . 2 ? O12 U1 O11 88.44(17) 2 2 ? O16 U1 O11 85.82(18) 2 2 ? O16 U1 O11 94.18(18) . 2 ? O12 U1 O11 88.44(17) . . ? O12 U1 O11 91.56(17) 2 . ? O16 U1 O11 94.18(18) 2 . ? O16 U1 O11 85.82(18) . . ? O11 U1 O11 180.0 2 . ? O14 La1 N1D 77.54(13) . . ? O14 La1 N1A 75.01(13) . . ? N1D La1 N1A 152.39(7) . . ? O14 La1 N1B 143.64(13) . . ? N1D La1 N1B 138.79(6) . . ? N1A La1 N1B 68.8 . . ? O14 La1 Cl2 94.23(14) . . ? N1D La1 Cl2 89.86(7) . . ? N1A La1 Cl2 89.23(6) . . ? N1B La1 Cl2 88.36(6) . . ? O14 La1 Cl1 94.26(14) . . ? N1D La1 Cl1 91.64(7) . . ? N1A La1 Cl1 93.29(7) . . ? N1B La1 Cl1 85.00(6) . . ? Cl2 La1 Cl1 171.50(7) . . ? O14 La1 N1C 142.07(13) . . ? N1D La1 N1C 64.8 . . ? N1A La1 N1C 142.05(6) . . ? N1B La1 N1C 74.2 . . ? Cl2 La1 N1C 81.62(6) . . ? Cl1 La1 N1C 91.45(6) . . ? C1B N1B C5B 120.0 . . ? C1B N1B La1 120.4 . . ? C5B N1B La1 119.6 . . ? C2B C1B N1B 120.0 . . ? C1B C2B C3B 120.0 . . ? C4B C3B C2B 120.0 . . ? C3B C4B C5B 120.0 . . ? C4B C5B N1B 120.0 . . ? C1A N1A C5A 120.0 . . ? C1A N1A La1 122.0 . . ? C5A N1A La1 117.4 . . ? N1A C1A C2A 120.0 . . ? C3A C2A C1A 120.0 . . ? C2A C3A C4A 120.0 . . ? C5A C4A C3A 120.0 . . ? N1A C5A C4A 120.0 . . ? C1C N1C C5C 120.5 . . ? C1C N1C La1 123.1 . . ? C5C N1C La1 116.1 . . ? N1C C1C C2C 121.2 . . ? C1C C2C C3C 120.0 . . ? C4C C3C C2C 120.0 . . ? C3C C4C C5C 120.0 . . ? C4C C5C N1C 118.0 . . ? C1D N1D C5D 120.0 . . ? C1D N1D La1 119.4 . . ? C5D N1D La1 120.0 . . ? N1D C1D C2D 120.0 . . ? C1D C2D C3D 120.0 . . ? C2D C3D C4D 120.0 . . ? C5D C4D C3D 120.0 . . ? C4D C5D N1D 120.0 . . ? C5E N1E C1E 120.0 . . ? N1E C1E C2E 120.0 . . ? C1E C2E C3E 120.0 . . ? C4E C3E C2E 120.0 . . ? C3E C4E C5E 120.0 . . ? N1E C5E C4E 120.0 . . ? C1F N1F C5F 120.0 . . ? N1F C1F C2F 120.0 . . ? C1F C2F C3F 120.0 . . ? C4F C3F C2F 120.0 . . ? C5F C4F C3F 120.0 . . ? C4F C5F N1F 120.0 . . ? C5G N1G C1G 120.0 . . ? C2G C1G N1G 120.0 . . ? C1G C2G C3G 120.0 . . ? C4G C3G C2G 120.0 . . ? C3G C4G C5G 120.0 . . ? N1G C5G C4G 120.0 . . ? C5H N1H C1H 120.0 . . ? C2H C1H N1H 120.0 . . ? C3H C2H C1H 120.0 . . ? C2H C3H C4H 120.0 . . ? C5H C4H C3H 120.0 . . ? C4H C5H N1H 120.0 . . ? C5I N1I C1I 120.0 . . ? N1I C1I C2I 120.0 . . ? C3I C2I C1I 120.0 . . ? C2I C3I C4I 120.0 . . ? C5I C4I C3I 120.0 . . ? N1I C5I C4I 120.0 . . ? C1J N1J C5J 120.0 . . ? N1J C1J C2J 120.0 . . ? C3J C2J C1J 120.0 . . ? C2J C3J C4J 120.0 . . ? C5J C4J C3J 120.0 . . ? C4J C5J N1J 120.0 . . ? C1K N1K C5K 120.0 . . ? N1K C1K C2K 120.0 . . ? C1K C2K C3K 120.0 . . ? C4K C3K C2K 120.0 . . ? C3K C4K C5K 120.0 . . ? N1K C5K C4K 120.0 . . ? C1L N1L C5L 120.9 . . ? N1L C1L C2L 132.2 . . ? C3L C2L C1L 104.4 . . ? C4L C3L C2L 125.1 . . ? C3L C4L C5L 120.0 . . ? C4L C5L N1L 114.8 . . ? C1M N1M C5M 120.0 . . ? N1M C1M C2M 120.0 . . ? C3M C2M C1M 120.0 . . ? C2M C3M C4M 120.0 . . ? C3M C4M C5M 120.0 . . ? N1M C5M C4M 120.0 . . ? C1N C2N C3N 138.0 . . ? C2N C3N C1N 107.2 . 2_445 ? C2N C3N C1N 17.8 . . ? C1N C3N C1N 89.5 2_445 . ? C2N C1N C3N 114.3 . 2_445 ? C2N C1N C3N 24.2 . . ? C3N C1N C3N 90.5 2_445 . ? C11 O11 U1 126.6(3) . . ? C21 O12 U1 163.9(3) . . ? C41 O14 La1 137.3(3) . . ? C61 O16 U1 167.4(3) . . ? O11 C11 C12 119.7(3) . . ? O11 C11 C16 120.0(3) . . ? C12 C11 C16 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 C67 118.4(4) . . ? C13 C12 C67 121.1(4) . . ? C14 C13 C12 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 C18 123.2(4) . . ? C13 C14 C18 116.8(4) . . ? C14 C15 C16 120.0 . . ? C11 C16 C15 120.0 . . ? C11 C16 C17 118.3(3) . . ? C15 C16 C17 121.2(3) . . ? C22 C17 C16 111.3(5) . . ? C19B C18 C19A 103.0(8) . . ? C19B C18 C14 109.8(7) . . ? C19A C18 C14 111.8(6) . . ? C19B C18 C19C 112.8(7) . . ? C19A C18 C19C 108.2(7) . . ? C14 C18 C19C 111.0(6) . . ? O12 C21 C26 118.8(3) . . ? O12 C21 C22 121.0(3) . . ? C26 C21 C22 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 C17 121.7(3) . . ? C21 C22 C17 118.3(3) . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 C28 120.8(4) . . ? C23 C24 C28 119.1(4) . . ? C26 C25 C24 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 C27 119.7(3) . . ? C21 C26 C27 120.3(3) . . ? C32 C27 C26 118.7(5) . . ? C29A C28 C29B 104.7(8) . . ? C29A C28 C24 111.3(7) . . ? C29B C28 C24 112.4(6) . . ? C29A C28 C29C 105.3(7) . . ? C29B C28 C29C 116.7(8) . . ? C24 C28 C29C 106.2(7) . . ? O13 C31 C32 117.3(3) . . ? O13 C31 C36 122.6(3) . . ? C32 C31 C36 120.0 . . ? C31 C32 C33 120.0 . . ? C31 C32 C27 119.3(4) . . ? C33 C32 C27 120.6(4) . . ? C32 C33 C34 119.9 . . ? C35 C34 C33 120.0 . . ? C35 C34 C38 118.6(4) . . ? C33 C34 C38 121.4(4) . . ? C34 C35 C36 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 C37 118.9(3) . . ? C31 C36 C37 121.1(3) . . ? C42 C37 C36 113.9(5) . . ? C39A C38 C39C 110.7(7) . . ? C39A C38 C34 110.4(6) . . ? C39C C38 C34 108.0(6) . . ? C39A C38 C39B 110.1(7) . . ? C39C C38 C39B 108.2(7) . . ? C34 C38 C39B 109.5(6) . . ? O14 C41 C46 121.3(3) . . ? O14 C41 C42 118.7(3) . . ? C46 C41 C42 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 C37 123.5(3) . . ? C43 C42 C37 116.0(3) . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? C43 C44 C48 122.5(4) . . ? C45 C44 C48 117.2(4) . . ? C44 C45 C46 120.0 . . ? C41 C46 C45 120.0 . . ? C41 C46 C47 121.7(4) . . ? C45 C46 C47 117.9(4) . . ? C46 C47 C52 114.8(5) . . ? C49C C48 C44 114.9(7) . . ? C49C C48 C49B 108.2(8) . . ? C44 C48 C49B 106.1(6) . . ? C49C C48 C49A 111.1(8) . . ? C44 C48 C49A 109.6(7) . . ? C49B C48 C49A 106.4(8) . . ? O15 C51 C52 121.7(3) . . ? O15 C51 C56 118.2(3) . . ? C52 C51 C56 120.0 . . ? C51 C52 C53 120.0 . . ? C51 C52 C47 120.7(4) . . ? C53 C52 C47 119.3(4) . . ? C54 C53 C52 120.0 . . ? C53 C54 C55 120.0 . . ? C53 C54 C58 118.7(4) . . ? C55 C54 C58 121.4(4) . . ? C56 C55 C54 120.0 . . ? C55 C56 C51 120.0 . . ? C55 C56 C57 122.4(4) . . ? C51 C56 C57 117.6(4) . . ? C62 C57 C56 113.5(5) . . ? C59A C58 C59B 107.0(8) . . ? C59A C58 C59C 107.7(8) . . ? C59B C58 C59C 106.1(8) . . ? C59A C58 C54 111.4(6) . . ? C59B C58 C54 108.4(7) . . ? C59C C58 C54 115.8(7) . . ? O16 C61 C66 119.1(3) . . ? O16 C61 C62 120.9(3) . . ? C66 C61 C62 120.0 . . ? C63 C62 C61 120.0 . . ? C63 C62 C57 123.9(4) . . ? C61 C62 C57 116.1(4) . . ? C62 C63 C64 120.0 . . ? C65 C64 C63 120.0 . . ? C65 C64 C68 121.9(4) . . ? C63 C64 C68 118.0(4) . . ? C64 C65 C66 120.0 . . ? C61 C66 C65 120.0 . . ? C61 C66 C67 121.5(3) . . ? C65 C66 C67 118.6(3) . . ? C66 C67 C12 111.2(5) . . ? C69B C68 C69C 105.1(7) . . ? C69B C68 C69A 106.3(8) . . ? C69C C68 C69A 110.7(8) . . ? C69B C68 C64 115.2(7) . . ? C69C C68 C64 108.2(6) . . ? C69A C68 C64 111.2(6) . . ? #=========================================================================== data_struc2 _database_code_CSD 151551 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H94 Cl15 F18 La9 N18 O26 S6 U' _chemical_formula_weight 4470.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' 'U' 'U' -9.6767 9.6646 '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 19.865(4) _cell_length_b 29.031(6) _cell_length_c 25.276(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.33(3) _cell_angle_gamma 90.00 _cell_volume 14384(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 'all' _cell_measurement_theta_min 3.25 _cell_measurement_theta_max 25.72 _exptl_crystal_description block _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.064 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8488 _exptl_absorpt_coefficient_mu 4.187 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Crystal-to-detector distance dx == 27 mm, 90 images recorded by applying a 180\% scan on Phi in 2\% increments. Data were 91 % complete to a 2theta value of 51.44\% ; _diffrn_ambient_temperature 100(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 CCD' _diffrn_measurement_method 'Phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22931 _diffrn_reflns_av_R_equivalents 0.1133 _diffrn_reflns_av_sigmaI/netI 0.1756 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 25.72 _reflns_number_total 12517 _reflns_number_gt 5874 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1993)' _computing_molecular_graphics 'Bruker SHELXTL, V.5, Madison/WI, 1997' _computing_publication_material 'Bruker SHELXTL, V.5, Madison/WI, 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. All atoms were considered as anisotropic.All hydrogen atoms were introduced in the calculation as riding on calculated positions (U == 1.2 times that of the corresponding atom). The pyridine molecules in the lattice are disordered. They are discribed in two parts with 0.5 occupancy. The first part consists of a pyridinium dimer (N1D-N1E), a pyridinium cation bound to the cluster through an H-bond (NIC-O13), two pyridine molecules (N1G and N1I). The second part consists of a pyridinium dimer (N1A-N1B), a pyridinium cation H-bound to the cluster (N1H-F21), a pyridine molecule N1F. ; _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^)+(0.0192P)^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 12517 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1636 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1163 _refine_ls_wR_factor_gt 0.0890 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.909 _refine_ls_shift/su_max 0.044 _refine_ls_shift/su_mean 0.091 _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 25.72 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 1.036 _refine_diff_density_min -1.297 _refine_diff_density_rms 0.157 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 U1 U 0.0000 0.180590(8) 0.2500 0.03733(7) Uani 1 2 d S . . La1 La 0.0000 0.304349(13) 0.2500 0.04229(13) Uani 1 2 d S . . La2 La -0.131885(14) 0.099433(9) 0.278282(10) 0.03285(7) Uani 1 1 d . . . La3 La 0.062595(15) 0.117714(9) 0.369849(10) 0.03666(8) Uani 1 1 d . . . La4 La -0.088451(16) 0.221769(10) 0.356618(11) 0.04522(9) Uani 1 1 d . . . La5 La 0.173437(16) 0.220443(10) 0.301606(11) 0.04421(9) Uani 1 1 d . . . Cl1 Cl 0.0000 0.06692(5) 0.2500 0.0365(5) Uani 1 2 d S . . Cl2 Cl 0.05971(8) 0.23641(4) 0.36063(5) 0.0579(4) Uani 1 1 d . . . Cl3 Cl -0.04680(6) 0.05164(4) 0.37017(4) 0.0381(3) Uani 1 1 d . . . Cl4 Cl 0.15274(6) 0.05276(4) 0.32906(4) 0.0422(4) Uani 1 1 d . . . Cl5 Cl 0.13838(7) 0.32222(4) 0.30077(5) 0.0531(4) Uani 1 1 d . . . Cl6 Cl -0.00831(6) 0.16586(4) 0.44475(4) 0.0425(4) Uani 1 1 d . . . Cl7 Cl -0.05231(9) 0.32350(4) 0.34632(5) 0.0723(5) Uani 1 1 d . . . Cl8 Cl 0.18943(8) 0.16370(4) 0.40325(5) 0.0576(4) Uani 1 1 d . . . O1 O -0.03910(15) 0.15217(10) 0.31905(11) 0.0367(9) Uani 1 1 d . . . O2 O 0.09512(16) 0.15213(9) 0.28997(10) 0.0370(9) Uani 1 1 d . . . O3 O 0.06906(16) 0.23649(10) 0.23520(11) 0.0442(10) Uani 1 1 d . . . O4 O -0.17641(16) 0.17995(10) 0.28676(11) 0.0450(10) Uani 1 1 d . . . O11 O -0.18992(17) 0.10396(10) 0.36242(12) 0.0522(10) Uani 1 1 d . . . O12 O -0.17451(17) 0.17940(10) 0.40432(13) 0.0546(11) Uani 1 1 d . . . O13 O -0.28632(17) 0.14167(10) 0.39366(13) 0.0537(11) Uani 1 1 d . . . S1 S -0.21277(7) 0.13639(5) 0.39948(5) 0.0546(4) Uani 1 1 d . . . C1 C -0.1906(2) 0.10642(18) 0.46448(19) 0.0574(16) Uani 1 1 d . . . F11 F -0.19700(18) 0.13846(11) 0.50288(11) 0.0862(12) Uani 1 1 d . . . F12 F -0.23002(16) 0.07110(10) 0.46970(12) 0.0774(11) Uani 1 1 d . . . F13 F -0.12449(16) 0.09308(10) 0.47359(11) 0.0696(11) Uani 1 1 d . . . O21 O -0.19551(19) 0.27351(11) 0.33973(13) 0.0641(12) Uani 1 1 d . . . O22 O 0.25741(17) 0.26233(10) 0.24989(12) 0.0553(10) Uani 1 1 d . . . O23 O 0.2587(2) 0.33624(11) 0.20741(15) 0.0788(14) Uani 1 1 d . . . S2 S 0.25073(9) 0.28823(5) 0.19991(5) 0.0656(5) Uani 1 1 d . . . C2 C 0.3223(3) 0.2692(2) 0.17058(18) 0.077(2) Uani 1 1 d . . . F21 F 0.38193(19) 0.28036(14) 0.20225(13) 0.0999(14) Uani 1 1 d . . . F22 F 0.32649(19) 0.22561(11) 0.15999(13) 0.0873(12) Uani 1 1 d . . . F23 F 0.32681(19) 0.29328(11) 0.12548(11) 0.0892(13) Uani 1 1 d . . . O31 O 0.28395(18) 0.17210(12) 0.30954(14) 0.0662(13) Uani 1 1 d . . . O32 O -0.26175(17) 0.10121(11) 0.24109(13) 0.0548(11) Uani 1 1 d . . . O33 O -0.3320(2) 0.09968(12) 0.15535(13) 0.0708(14) Uani 1 1 d . . . S3 S -0.30696(7) 0.12510(5) 0.20056(5) 0.0536(4) Uani 1 1 d . . . C3 C -0.3796(3) 0.13350(18) 0.2288(2) 0.0671(19) Uani 1 1 d . . . F31 F -0.36705(19) 0.15782(14) 0.27797(15) 0.1031(15) Uani 1 1 d . . . F32 F -0.42850(16) 0.15874(12) 0.19851(15) 0.0909(13) Uani 1 1 d . . . F33 F -0.40966(16) 0.09517(11) 0.24156(13) 0.0763(11) Uani 1 1 d . . . N4 N -0.0954(2) 0.26474(13) 0.45222(16) 0.0576(14) Uani 1 1 d . . . C14 C -0.1519(3) 0.2706(2) 0.4685(2) 0.108(2) Uani 1 1 d . . . H1AA H -0.1920 0.2596 0.4482 0.130 Uiso 1 1 calc R . . C24 C -0.1543(3) 0.2942(2) 0.5184(2) 0.084(2) Uani 1 1 d . . . H2AA H -0.1959 0.2981 0.5301 0.101 Uiso 1 1 calc R . . C34 C -0.0973(3) 0.3104(2) 0.5480(3) 0.080(2) Uani 1 1 d . . . H34A H -0.0987 0.3264 0.5797 0.096 Uiso 1 1 calc R . . C44 C -0.0361(3) 0.3026(2) 0.5298(2) 0.077(2) Uani 1 1 d . . . H4AA H 0.0054 0.3121 0.5491 0.092 Uiso 1 1 calc R . . C54 C -0.0405(3) 0.27865(19) 0.4789(2) 0.071(2) Uani 1 1 d . . . H5AA H -0.0003 0.2734 0.4653 0.085 Uiso 1 1 calc R . . N2 N -0.1890(2) 0.01340(13) 0.29013(15) 0.0502(14) Uani 1 1 d . . . C12 C -0.2497(3) 0.0095(2) 0.3052(2) 0.072(2) Uani 1 1 d . . . H1BA H -0.2730 0.0363 0.3110 0.086 Uiso 1 1 calc R . . C22 C -0.2791(4) -0.0311(2) 0.3125(3) 0.099(3) Uani 1 1 d . . . H2BA H -0.3211 -0.0313 0.3243 0.119 Uiso 1 1 calc R . . C32 C -0.2547(4) -0.0650(3) 0.3048(3) 0.108(3) Uani 1 1 d . . . H3BA H -0.2767 -0.0922 0.3113 0.130 Uiso 1 1 calc R . . C42 C -0.1873(4) -0.0678(3) 0.2843(3) 0.114(3) Uani 1 1 d . . . H4BA H -0.1676 -0.0951 0.2749 0.137 Uiso 1 1 calc R . . C52 C -0.1576(3) -0.02268(16) 0.2813(2) 0.0545(18) Uani 1 1 d . . . H5BA H -0.1141 -0.0202 0.2725 0.065 Uiso 1 1 calc R . . N1 N 0.0000 0.39814(19) 0.2500 0.0510(19) Uani 1 2 d S . . C11 C -0.0518(3) 0.42294(17) 0.2650(2) 0.0537(18) Uani 1 1 d . . . H1CA H -0.0879 0.4065 0.2750 0.064 Uiso 1 1 calc R . . C21 C -0.0554(3) 0.47051(17) 0.2666(2) 0.0569(18) Uani 1 1 d . . . H2CA H -0.0919 0.4855 0.2779 0.068 Uiso 1 1 calc R . . C31 C 0.0000 0.4958(3) 0.2500 0.073(3) Uani 1 2 d S . . H3CA H 0.0000 0.5279 0.2500 0.088 Uiso 1 2 calc SR . . N3 N 0.1072(2) 0.07222(12) 0.46290(15) 0.0448(13) Uani 1 1 d . . . C13 C 0.1754(3) 0.06060(16) 0.4752(2) 0.0508(17) Uani 1 1 d . . . H1DA H 0.2053 0.0694 0.4524 0.061 Uiso 1 1 calc R . . C23 C 0.2002(3) 0.03550(16) 0.5221(2) 0.0510(17) Uani 1 1 d . . . H2DA H 0.2457 0.0268 0.5306 0.061 Uiso 1 1 calc R . . C33 C 0.1507(3) 0.02395(19) 0.5564(2) 0.066(2) Uani 1 1 d . . . H3DA H 0.1643 0.0083 0.5884 0.080 Uiso 1 1 calc R . . C43 C 0.0859(3) 0.03589(18) 0.5415(2) 0.0531(18) Uani 1 1 d . . . H4DA H 0.0543 0.0278 0.5633 0.064 Uiso 1 1 calc R . . C53 C 0.06391(8) 0.05997(5) 0.49473(6) 0.0452(16) Uani 1 1 d . . . H5DA H 0.0180 0.0676 0.4856 0.054 Uiso 1 1 calc R . . N5 N 0.26563(8) 0.26407(5) 0.37906(6) 0.097(2) Uani 1 1 d R . . C15 C 0.23563(8) 0.27939(5) 0.42186(6) 0.240(4) Uani 1 1 d R . . H15 H 0.1889 0.2761 0.4209 0.288 Uiso 1 1 calc R . . C25 C 0.27546(8) 0.29964(5) 0.46601(6) 0.240(4) Uani 1 1 d R . . H25 H 0.2554 0.3099 0.4946 0.288 Uiso 1 1 calc R . . C35 C 0.34532(8) 0.30460(5) 0.46738(6) 0.240(4) Uani 1 1 d R . . H35 H 0.3720 0.3182 0.4969 0.288 Uiso 1 1 calc R . . C45 C 0.37534(8) 0.28930(5) 0.42459(6) 0.240(4) Uani 1 1 d R . . H45 H 0.4221 0.2926 0.4255 0.288 Uiso 1 1 calc R . . C55 C 0.33549(8) 0.26902(5) 0.38043(6) 0.240(4) Uani 1 1 d R . . H55 H 0.3556 0.2588 0.3518 0.288 Uiso 1 1 calc R . . C5E C 0.63330(8) 0.04100(5) 0.59944(6) 0.108(3) Uani 0.50 1 d PR A 1 H5E H 0.5957 0.0215 0.5940 0.130 Uiso 0.50 1 calc PR B 1 N1E N 0.62416(8) 0.08829(5) 0.59476(6) 0.108(3) Uani 0.50 1 d PR A 1 H1E H 0.5837 0.0995 0.5868 0.130 Uiso 0.50 1 calc PR C 1 C1E C 0.68024(8) 0.11744(5) 0.60290(6) 0.108(3) Uani 0.50 1 d PR A 1 H1E' H 0.6741 0.1491 0.5998 0.130 Uiso 0.50 1 calc PR D 1 C2E C 0.74547(8) 0.09931(5) 0.61571(6) 0.108(3) Uani 0.50 1 d PR A 1 H2E H 0.7831 0.1188 0.6211 0.130 Uiso 0.50 1 calc PR E 1 C3E C 0.75462(8) 0.05201(5) 0.62046(6) 0.108(3) Uani 0.50 1 d PR A 1 H3E H 0.7983 0.0398 0.6291 0.130 Uiso 0.50 1 calc PR F 1 C4E C 0.69853(8) 0.02285(5) 0.61231(6) 0.108(3) Uani 0.50 1 d PR A 1 H4E H 0.7047 -0.0089 0.6155 0.130 Uiso 0.50 1 calc PR G 1 N1F N 0.69406(8) 0.00244(5) 0.60317(6) 0.0433(12) Uani 0.50 1 d PR H 2 C1F C 0.66768(8) 0.01516(5) 0.55099(6) 0.0433(12) Uani 0.50 1 d PR H 2 H1F H 0.6676 -0.0058 0.5231 0.052 Uiso 0.50 1 calc PR I 2 C2F C 0.64137(8) 0.05912(5) 0.54045(6) 0.0433(12) Uani 0.50 1 d PR H 2 H2F H 0.6237 0.0677 0.5055 0.052 Uiso 0.50 1 calc PR J 2 C3F C 0.64147(8) 0.09029(5) 0.58209(6) 0.0433(12) Uani 0.50 1 d PR H 2 H3F H 0.6238 0.1197 0.5750 0.052 Uiso 0.50 1 calc PR K 2 C4F C 0.66787(8) 0.07756(5) 0.63423(6) 0.0433(12) Uani 0.50 1 d PR H 2 H4F H 0.6679 0.0985 0.6621 0.052 Uiso 0.50 1 calc PR L 2 C5F C 0.69417(8) 0.03361(5) 0.64475(6) 0.0433(12) Uani 0.50 1 d PR H 2 H5F H 0.7119 0.0251 0.6797 0.052 Uiso 0.50 1 calc PR M 2 N1G N 0.88779(8) 0.10076(5) 0.68253(6) 0.0396(12) Uani 0.50 1 d PR N 3 C1G C 0.84457(8) 0.09190(5) 0.63473(6) 0.0396(12) Uani 0.50 1 d PR N 3 H1G H 0.8051 0.1093 0.6253 0.048 Uiso 0.50 1 calc PR O 3 C2G C 0.86025(8) 0.05713(5) 0.60106(6) 0.0396(12) Uani 0.50 1 d PR N 3 H2G H 0.8313 0.0512 0.5691 0.048 Uiso 0.50 1 calc PR P 3 C3G C 0.91917(8) 0.03125(5) 0.61516(6) 0.0396(12) Uani 0.50 1 d PR N 3 H3G H 0.9297 0.0080 0.5926 0.048 Uiso 0.50 1 calc PR Q 3 C4G C 0.96240(8) 0.04013(5) 0.66294(6) 0.0396(12) Uani 0.50 1 d PR N 3 H4G H 1.0019 0.0228 0.6724 0.048 Uiso 0.50 1 calc PR R 3 C5G C 0.94671(8) 0.07487(5) 0.69661(6) 0.0396(12) Uani 0.50 1 d PR N 3 H5G H 0.9757 0.0808 0.7286 0.048 Uiso 0.50 1 calc PR S 3 N1I N 0.97245(8) 0.18724(5) 0.59056(6) 0.086(2) Uani 0.50 1 d PR T 4 C1I C 0.99758(8) 0.21835(5) 0.63059(6) 0.086(2) Uani 0.50 1 d PR T 4 H1I H 0.9807 0.2483 0.6294 0.103 Uiso 0.50 1 calc PR U 4 C2I C 1.04792(8) 0.20482(5) 0.67233(6) 0.086(2) Uani 0.50 1 d PR T 4 H2I H 1.0647 0.2257 0.6992 0.103 Uiso 0.50 1 calc PR V 4 C3I C 1.07318(8) 0.16018(5) 0.67402(6) 0.086(2) Uani 0.50 1 d PR T 4 H3I H 1.1069 0.1511 0.7020 0.103 Uiso 0.50 1 calc PR W 4 C4I C 1.04805(8) 0.12909(5) 0.63394(6) 0.086(2) Uani 0.50 1 d PR T 4 H4I H 1.0650 0.0992 0.6350 0.103 Uiso 0.50 1 calc PR X 4 C5I C 0.99769(8) 0.14260(5) 0.59224(6) 0.086(2) Uani 0.50 1 d PR T 4 H5I H 0.9808 0.1217 0.5654 0.103 Uiso 0.50 1 calc PR Y 4 C5H C 0.94466(8) 0.12332(5) 0.60741(6) 0.263(7) Uani 0.50 1 d PR Z 5 H5H H 0.9368 0.1390 0.5749 0.316 Uiso 0.50 1 calc PR A 5 C4H C 0.96489(8) 0.07754(5) 0.60882(6) 0.263(7) Uani 0.50 1 d PR Z 5 H1H H 0.9706 0.0626 0.5773 0.316 Uiso 0.50 1 calc PR B 5 C3H C 0.97662(8) 0.05407(5) 0.65728(6) 0.263(7) Uani 0.50 1 d PR Z 5 H2H H 0.9902 0.0234 0.6582 0.316 Uiso 0.50 1 calc PR C 5 C2H C 0.96814(8) 0.07638(5) 0.70428(6) 0.263(7) Uani 0.50 1 d PR Z 5 H3H H 0.9760 0.0606 0.7368 0.316 Uiso 0.50 1 calc PR D 5 C1H C 0.94791(8) 0.12219(5) 0.70285(6) 0.263(7) Uani 0.50 1 d PR Z 5 H4H H 0.9422 0.1371 0.7344 0.316 Uiso 0.50 1 calc PR E 5 N1H N 0.93616(8) 0.14565(5) 0.65442(6) 0.263(7) Uani 0.50 1 d PR Z 5 H5H' H 0.9236 0.1740 0.6535 0.316 Uiso 0.50 1 calc PR F 5 N1A N 0.43908(8) 0.01227(5) 0.59253(6) 0.0635(16) Uani 0.50 1 d PR G 6 H5A H 0.4279 0.0397 0.5815 0.076 Uiso 0.50 1 calc PR H 6 C1A C 0.50660(8) -0.00185(5) 0.59818(6) 0.0635(16) Uani 0.50 1 d PR G 6 H1A H 0.5398 0.0183 0.5900 0.076 Uiso 0.50 1 calc PR I 6 C2A C 0.52457(8) -0.04605(5) 0.61597(6) 0.0635(16) Uani 0.50 1 d PR G 6 H1A' H 0.5698 -0.0555 0.6198 0.076 Uiso 0.50 1 calc PR J 6 C3A C 0.47503(8) -0.07617(5) 0.62812(6) 0.0635(16) Uani 0.50 1 d PR G 6 H2A H 0.4871 -0.1058 0.6401 0.076 Uiso 0.50 1 calc PR K 6 C4A C 0.40749(8) -0.06208(5) 0.62243(6) 0.0635(16) Uani 0.50 1 d PR G 6 H3A H 0.3743 -0.0823 0.6305 0.076 Uiso 0.50 1 calc PR L 6 C5A C 0.38950(8) -0.01786(5) 0.60468(6) 0.0635(16) Uani 0.50 1 d PR G 6 H4A H 0.3442 -0.0084 0.6009 0.076 Uiso 0.50 1 calc PR M 6 C3C C 0.49396(8) -0.01424(5) 0.57525(6) 0.143(4) Uani 0.50 1 d PR N 7 C4C C 0.50052(8) -0.04698(5) 0.61572(6) 0.143(4) Uani 0.50 1 d PR N 7 H1C H 0.5421 -0.0507 0.6383 0.171 Uiso 0.50 1 calc PR O 7 C5C C 0.44510(8) -0.07413(5) 0.62258(6) 0.143(4) Uani 0.50 1 d PR N 7 H2C H 0.4495 -0.0961 0.6498 0.171 Uiso 0.50 1 calc PR P 7 N1C N 0.38315(8) -0.06858(5) 0.58892(6) 0.143(4) Uani 0.50 1 d PR N 7 H3C H 0.3488 -0.0854 0.5932 0.171 Uiso 0.50 1 calc PR Q 7 C1C C 0.37659(8) -0.03582(5) 0.54842(6) 0.143(4) Uani 0.50 1 d PR N 7 H4C H 0.3351 -0.0321 0.5259 0.171 Uiso 0.50 1 calc PR R 7 C2C C 0.43200(8) -0.00865(5) 0.54157(6) 0.143(4) Uani 0.50 1 d PR N 7 H5C H 0.4276 0.0133 0.5144 0.171 Uiso 0.50 1 calc PR S 7 N1B N 0.39904(8) 0.09056(5) 0.54879(6) 0.0600(15) Uani 0.50 1 d PR T 1 C1B C 0.37111(8) 0.08803(5) 0.49487(6) 0.0600(15) Uani 0.50 1 d PR T 1 H1B H 0.3724 0.0604 0.4764 0.072 Uiso 0.50 1 calc PR U 1 C2B C 0.34132(8) 0.12667(5) 0.46852(6) 0.0600(15) Uani 0.50 1 d PR T 1 H2B H 0.3226 0.1250 0.4324 0.072 Uiso 0.50 1 calc PR V 1 C3B C 0.33949(8) 0.16787(5) 0.49611(6) 0.0600(15) Uani 0.50 1 d PR T 1 H3B H 0.3195 0.1938 0.4785 0.072 Uiso 0.50 1 calc PR W 1 C4B C 0.36741(8) 0.17039(5) 0.54999(6) 0.0600(15) Uani 0.50 1 d PR T 1 H4B H 0.3662 0.1980 0.5685 0.072 Uiso 0.50 1 calc PR X 1 C5B C 0.39720(8) 0.13175(5) 0.57634(6) 0.0600(15) Uani 0.50 1 d PR T 1 H5B H 0.4159 0.1335 0.6125 0.072 Uiso 0.50 1 calc PR Y 1 N1D N 0.49218(8) 0.10399(5) 0.55913(6) 0.116(3) Uani 0.50 1 d PR Z 2 C1D C 0.47454(8) 0.10023(5) 0.50390(6) 0.116(3) Uani 0.50 1 d PR Z 2 H1D H 0.5080 0.0943 0.4830 0.139 Uiso 0.50 1 calc PR A 2 C2D C 0.40704(8) 0.10536(5) 0.47988(6) 0.116(3) Uani 0.50 1 d PR Z 2 H2D H 0.3952 0.1029 0.4429 0.139 Uiso 0.50 1 calc PR B 2 C3D C 0.35717(8) 0.11422(5) 0.51112(6) 0.116(3) Uani 0.50 1 d PR Z 2 H3D H 0.3119 0.1176 0.4950 0.139 Uiso 0.50 1 calc PR C 2 C4D C 0.37477(8) 0.11800(5) 0.56636(6) 0.116(3) Uani 0.50 1 d PR Z 2 H4D H 0.3413 0.1240 0.5873 0.139 Uiso 0.50 1 calc PR D 2 C5D C 0.44228(8) 0.11288(5) 0.59036(6) 0.116(3) Uani 0.50 1 d PR Z 2 H5D H 0.4541 0.1154 0.6274 0.139 Uiso 0.50 1 calc PR E 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 U1 0.05627(16) 0.03452(13) 0.02576(11) 0.000 0.02035(11) 0.000 La1 0.0685(3) 0.0343(2) 0.02572(19) 0.000 0.01256(19) 0.000 La2 0.03854(14) 0.03716(13) 0.02568(12) 0.00831(12) 0.01372(11) 0.00458(13) La3 0.04750(16) 0.03688(14) 0.02906(13) 0.00043(12) 0.01663(12) 0.00473(14) La4 0.07194(19) 0.04057(14) 0.02945(13) 0.00689(12) 0.02716(13) 0.01659(15) La5 0.06823(19) 0.03956(14) 0.02980(13) -0.01254(12) 0.02278(13) -0.01356(15) Cl1 0.0330(9) 0.0486(9) 0.0290(8) 0.000 0.0080(7) 0.000 Cl2 0.0944(9) 0.0456(7) 0.0418(6) -0.0179(5) 0.0352(6) -0.0194(7) Cl3 0.0527(7) 0.0376(6) 0.0246(5) 0.0041(5) 0.0079(5) 0.0051(6) Cl4 0.0435(7) 0.0476(6) 0.0349(6) -0.0148(5) 0.0045(5) 0.0057(6) Cl5 0.0823(9) 0.0454(7) 0.0343(6) -0.0068(6) 0.0180(6) -0.0156(7) Cl6 0.0583(7) 0.0409(6) 0.0332(6) -0.0006(5) 0.0217(5) 0.0051(6) Cl7 0.1427(12) 0.0444(7) 0.0398(6) 0.0044(6) 0.0442(7) 0.0125(8) Cl8 0.0828(9) 0.0591(7) 0.0329(6) -0.0160(6) 0.0155(6) -0.0268(7) O1 0.0469(18) 0.0399(17) 0.0285(15) 0.0068(13) 0.0215(13) 0.0015(15) O2 0.0587(19) 0.0315(15) 0.0251(14) -0.0149(12) 0.0200(14) -0.0055(15) O3 0.065(2) 0.0425(17) 0.0317(15) -0.0071(14) 0.0268(14) -0.0097(16) O4 0.076(2) 0.0371(16) 0.0308(14) 0.0064(14) 0.0348(14) 0.0060(16) O11 0.071(2) 0.0518(18) 0.0413(16) 0.0301(15) 0.0307(15) 0.0295(17) O12 0.066(2) 0.0441(18) 0.0642(19) 0.0110(17) 0.0418(16) 0.0108(17) O13 0.065(2) 0.0463(18) 0.056(2) 0.0118(16) 0.0284(17) 0.0216(17) S1 0.0642(8) 0.0639(8) 0.0451(6) 0.0255(6) 0.0368(6) 0.0317(7) C1 0.046(3) 0.080(3) 0.055(3) 0.010(3) 0.036(2) 0.044(2) F11 0.138(3) 0.077(2) 0.0562(17) 0.0218(16) 0.0541(17) 0.0455(19) F12 0.073(2) 0.0702(18) 0.097(2) 0.0536(15) 0.0405(17) 0.0115(16) F13 0.075(2) 0.0752(19) 0.0635(18) 0.0302(16) 0.0272(16) 0.0219(17) O21 0.105(3) 0.0491(18) 0.0407(18) 0.0220(16) 0.0185(19) 0.0442(19) O22 0.074(2) 0.0535(18) 0.0465(17) -0.0175(15) 0.0351(15) -0.0394(17) O23 0.120(3) 0.052(2) 0.071(2) -0.0183(19) 0.036(2) -0.048(2) S2 0.1035(11) 0.0569(8) 0.0417(7) -0.0209(6) 0.0281(7) -0.0364(8) C2 0.109(5) 0.112(4) 0.007(2) 0.009(3) 0.000(3) -0.045(4) F21 0.102(3) 0.147(3) 0.0522(19) -0.016(2) 0.0173(19) -0.036(2) F22 0.123(3) 0.075(2) 0.076(2) -0.0234(17) 0.0544(18) -0.008(2) F23 0.147(3) 0.088(2) 0.0427(16) -0.0150(16) 0.0443(17) -0.034(2) O31 0.058(2) 0.073(2) 0.071(2) -0.0383(19) 0.0198(19) -0.007(2) O32 0.047(2) 0.064(2) 0.0505(19) 0.0291(17) -0.0003(17) 0.0057(19) O33 0.112(3) 0.068(2) 0.0344(18) 0.0139(18) 0.019(2) -0.003(2) S3 0.0464(8) 0.0754(9) 0.0423(7) 0.0267(7) 0.0165(6) 0.0179(7) C3 0.070(4) 0.066(3) 0.074(3) 0.039(3) 0.035(3) 0.032(3) F31 0.090(2) 0.137(3) 0.093(2) -0.008(2) 0.0454(19) -0.003(2) F32 0.0530(19) 0.102(2) 0.119(3) 0.016(2) 0.017(2) 0.0452(18) F33 0.071(2) 0.084(2) 0.077(2) 0.0209(18) 0.0230(17) -0.0060(19) N4 0.083(3) 0.046(2) 0.051(2) 0.0091(19) 0.031(2) 0.044(2) C14 0.155(4) 0.147(4) 0.019(3) -0.004(3) 0.002(3) 0.130(3) C24 0.089(4) 0.097(4) 0.070(4) -0.008(3) 0.021(3) 0.049(4) C34 0.099(5) 0.070(4) 0.076(4) -0.007(3) 0.032(4) 0.016(4) C44 0.089(4) 0.087(4) 0.061(4) -0.004(3) 0.030(3) -0.001(4) C54 0.085(4) 0.061(3) 0.069(4) -0.008(3) 0.021(3) 0.001(3) N2 0.058(3) 0.054(2) 0.038(2) -0.005(2) 0.005(2) -0.017(2) C12 0.069(4) 0.084(4) 0.060(3) 0.040(3) 0.005(3) -0.005(3) C22 0.080(5) 0.112(5) 0.095(5) 0.028(4) -0.014(4) -0.024(4) C32 0.119(6) 0.093(5) 0.107(6) 0.010(5) 0.003(5) -0.037(5) C42 0.117(6) 0.092(5) 0.128(6) 0.007(5) 0.005(5) -0.015(5) C52 0.046(3) 0.039(3) 0.076(4) 0.005(3) 0.006(3) -0.014(3) N1 0.055(4) 0.049(3) 0.039(3) 0.000 -0.023(3) 0.000 C11 0.055(3) 0.054(3) 0.052(3) -0.002(3) 0.009(3) -0.006(3) C21 0.058(4) 0.055(3) 0.057(3) -0.003(3) 0.010(3) -0.004(3) C31 0.065(5) 0.077(5) 0.085(6) 0.000 0.032(5) 0.000 N3 0.048(3) 0.037(2) 0.045(2) -0.0042(19) -0.004(2) 0.008(2) C13 0.053(3) 0.049(3) 0.052(3) 0.001(3) 0.016(3) -0.001(3) C23 0.046(3) 0.049(3) 0.057(3) 0.008(3) 0.008(3) 0.004(3) C33 0.065(4) 0.078(4) 0.050(3) 0.000(3) -0.006(3) -0.006(3) C43 0.050(3) 0.070(3) 0.040(3) 0.007(3) 0.012(3) 0.007(3) C53 0.040(3) 0.057(3) 0.039(3) 0.003(2) 0.007(2) 0.005(3) N5 0.160(5) 0.090(3) 0.036(3) -0.021(3) 0.002(3) -0.031(4) C15 0.290(9) 0.232(5) 0.189(6) -0.063(5) 0.012(6) -0.002(6) C25 0.290(9) 0.232(5) 0.189(6) -0.063(5) 0.012(6) -0.002(6) C35 0.290(9) 0.232(5) 0.189(6) -0.063(5) 0.012(6) -0.002(6) C45 0.290(9) 0.232(5) 0.189(6) -0.063(5) 0.012(6) -0.002(6) C55 0.290(9) 0.232(5) 0.189(6) -0.063(5) 0.012(6) -0.002(6) C5E 0.108(5) 0.090(4) 0.132(4) -0.001(4) 0.033(4) 0.013(4) N1E 0.108(5) 0.090(4) 0.132(4) -0.001(4) 0.033(4) 0.013(4) C1E 0.108(5) 0.090(4) 0.132(4) -0.001(4) 0.033(4) 0.013(4) C2E 0.108(5) 0.090(4) 0.132(4) -0.001(4) 0.033(4) 0.013(4) C3E 0.108(5) 0.090(4) 0.132(4) -0.001(4) 0.033(4) 0.013(4) C4E 0.108(5) 0.090(4) 0.132(4) -0.001(4) 0.033(4) 0.013(4) N1F 0.040(2) 0.045(2) 0.047(2) 0.0005(18) 0.0112(19) 0.0020(19) C1F 0.040(2) 0.045(2) 0.047(2) 0.0005(18) 0.0112(19) 0.0020(19) C2F 0.040(2) 0.045(2) 0.047(2) 0.0005(18) 0.0112(19) 0.0020(19) C3F 0.040(2) 0.045(2) 0.047(2) 0.0005(18) 0.0112(19) 0.0020(19) C4F 0.040(2) 0.045(2) 0.047(2) 0.0005(18) 0.0112(19) 0.0020(19) C5F 0.040(2) 0.045(2) 0.047(2) 0.0005(18) 0.0112(19) 0.0020(19) N1G 0.035(2) 0.0320(19) 0.052(2) 0.0126(17) 0.0083(18) 0.0002(17) C1G 0.035(2) 0.0320(19) 0.052(2) 0.0126(17) 0.0083(18) 0.0002(17) C2G 0.035(2) 0.0320(19) 0.052(2) 0.0126(17) 0.0083(18) 0.0002(17) C3G 0.035(2) 0.0320(19) 0.052(2) 0.0126(17) 0.0083(18) 0.0002(17) C4G 0.035(2) 0.0320(19) 0.052(2) 0.0126(17) 0.0083(18) 0.0002(17) C5G 0.035(2) 0.0320(19) 0.052(2) 0.0126(17) 0.0083(18) 0.0002(17) N1I 0.083(4) 0.081(3) 0.092(4) -0.006(3) 0.010(3) 0.015(3) C1I 0.083(4) 0.081(3) 0.092(4) -0.006(3) 0.010(3) 0.015(3) C2I 0.083(4) 0.081(3) 0.092(4) -0.006(3) 0.010(3) 0.015(3) C3I 0.083(4) 0.081(3) 0.092(4) -0.006(3) 0.010(3) 0.015(3) C4I 0.083(4) 0.081(3) 0.092(4) -0.006(3) 0.010(3) 0.015(3) C5I 0.083(4) 0.081(3) 0.092(4) -0.006(3) 0.010(3) 0.015(3) C5H 0.341(14) 0.225(12) 0.203(13) 0.033(10) -0.019(13) 0.045(11) C4H 0.341(14) 0.225(12) 0.203(13) 0.033(10) -0.019(13) 0.045(11) C3H 0.341(14) 0.225(12) 0.203(13) 0.033(10) -0.019(13) 0.045(11) C2H 0.341(14) 0.225(12) 0.203(13) 0.033(10) -0.019(13) 0.045(11) C1H 0.341(14) 0.225(12) 0.203(13) 0.033(10) -0.019(13) 0.045(11) N1H 0.341(14) 0.225(12) 0.203(13) 0.033(10) -0.019(13) 0.045(11) N1A 0.060(3) 0.077(3) 0.051(3) 0.009(2) 0.000(3) 0.006(3) C1A 0.060(3) 0.077(3) 0.051(3) 0.009(2) 0.000(3) 0.006(3) C2A 0.060(3) 0.077(3) 0.051(3) 0.009(2) 0.000(3) 0.006(3) C3A 0.060(3) 0.077(3) 0.051(3) 0.009(2) 0.000(3) 0.006(3) C4A 0.060(3) 0.077(3) 0.051(3) 0.009(2) 0.000(3) 0.006(3) C5A 0.060(3) 0.077(3) 0.051(3) 0.009(2) 0.000(3) 0.006(3) C3C 0.132(7) 0.144(6) 0.151(7) 0.033(5) 0.019(5) 0.004(5) C4C 0.132(7) 0.144(6) 0.151(7) 0.033(5) 0.019(5) 0.004(5) C5C 0.132(7) 0.144(6) 0.151(7) 0.033(5) 0.019(5) 0.004(5) N1C 0.132(7) 0.144(6) 0.151(7) 0.033(5) 0.019(5) 0.004(5) C1C 0.132(7) 0.144(6) 0.151(7) 0.033(5) 0.019(5) 0.004(5) C2C 0.132(7) 0.144(6) 0.151(7) 0.033(5) 0.019(5) 0.004(5) N1B 0.066(3) 0.063(3) 0.052(2) -0.014(2) 0.013(2) -0.013(2) C1B 0.066(3) 0.063(3) 0.052(2) -0.014(2) 0.013(2) -0.013(2) C2B 0.066(3) 0.063(3) 0.052(2) -0.014(2) 0.013(2) -0.013(2) C3B 0.066(3) 0.063(3) 0.052(2) -0.014(2) 0.013(2) -0.013(2) C4B 0.066(3) 0.063(3) 0.052(2) -0.014(2) 0.013(2) -0.013(2) C5B 0.066(3) 0.063(3) 0.052(2) -0.014(2) 0.013(2) -0.013(2) N1D 0.110(5) 0.154(5) 0.087(4) -0.015(4) 0.027(4) -0.007(5) C1D 0.110(5) 0.154(5) 0.087(4) -0.015(4) 0.027(4) -0.007(5) C2D 0.110(5) 0.154(5) 0.087(4) -0.015(4) 0.027(4) -0.007(5) C3D 0.110(5) 0.154(5) 0.087(4) -0.015(4) 0.027(4) -0.007(5) C4D 0.110(5) 0.154(5) 0.087(4) -0.015(4) 0.027(4) -0.007(5) C5D 0.110(5) 0.154(5) 0.087(4) -0.015(4) 0.027(4) -0.007(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 U1 O2 2.158(3) . ? U1 O2 2.158(3) 2 ? U1 O1 2.184(3) . ? U1 O1 2.184(3) 2 ? U1 O3 2.196(3) 2 ? U1 O3 2.196(3) . ? U1 Cl2 3.2828(14) 2 ? U1 Cl2 3.2828(14) . ? U1 La3 3.5824(8) . ? U1 La3 3.5824(8) 2 ? U1 La1 3.5928(8) . ? U1 La4 3.6488(9) . ? La1 O3 2.464(3) 2 ? La1 O3 2.464(3) . ? La1 N1 2.723(6) . ? La1 Cl7 2.8523(16) . ? La1 Cl7 2.8523(16) 2 ? La1 Cl5 2.8859(16) . ? La1 Cl5 2.8860(16) 2 ? La1 La4 4.1990(9) 2 ? La1 La4 4.1991(9) . ? La2 O1 2.488(3) . ? La2 O2 2.502(3) 2 ? La2 O4 2.521(3) . ? La2 O11 2.581(3) . ? La2 O32 2.599(3) . ? La2 N2 2.780(4) . ? La2 Cl1 2.9787(8) . ? La2 Cl3 2.9839(13) . ? La2 Cl4 3.0008(13) 2 ? La2 La5 4.0694(8) 2 ? La2 La4 4.0895(8) . ? La3 O1 2.427(3) . ? La3 O2 2.432(3) . ? La3 N3 2.718(4) . ? La3 Cl8 2.8554(15) . ? La3 Cl6 2.8958(14) . ? La3 Cl3 2.8996(13) . ? La3 Cl4 2.9024(13) . ? La3 La2 4.2268(10) 2 ? La3 La4 4.2326(7) . ? La3 La5 4.2366(8) . ? La4 O3 2.451(3) 2 ? La4 O1 2.499(3) . ? La4 O12 2.561(3) . ? La4 O4 2.578(3) . ? La4 O21 2.582(4) . ? La4 N4 2.743(4) . ? La4 Cl2 2.9591(16) . ? La4 Cl6 2.9970(13) . ? La4 Cl7 3.0605(15) . ? La4 La5 4.0813(12) 2 ? La5 O3 2.491(3) . ? La5 O2 2.508(3) . ? La5 O4 2.533(3) 2 ? La5 O22 2.584(3) . ? La5 O31 2.586(4) . ? La5 N5 2.7619(16) . ? La5 Cl2 2.9389(17) . ? La5 Cl8 3.0250(14) . ? La5 Cl5 3.0348(14) . ? La5 La2 4.0693(8) 2 ? La5 La4 4.0814(12) 2 ? Cl1 La2 2.9787(8) 2 ? Cl4 La2 3.0008(13) 2 ? O2 La2 2.502(3) 2 ? O3 La4 2.451(3) 2 ? O4 La5 2.533(3) 2 ? O11 S1 1.452(3) . ? O12 S1 1.457(3) . ? O13 S1 1.453(4) . ? S1 C1 1.848(5) . ? C1 F12 1.309(6) . ? C1 F13 1.353(5) . ? C1 F11 1.365(6) . ? O21 S2 1.426(4) 2 ? O22 S2 1.458(3) . ? O23 S2 1.412(4) . ? S2 O21 1.426(4) 2 ? S2 C2 1.794(7) . ? C2 F22 1.300(7) . ? C2 F23 1.352(6) . ? C2 F21 1.356(7) . ? O31 S3 1.474(4) 2 ? O32 S3 1.428(3) . ? O33 S3 1.384(4) . ? S3 O31 1.474(4) 2 ? S3 C3 1.728(6) . ? C3 F33 1.327(6) . ? C3 F32 1.351(6) . ? C3 F31 1.416(6) . ? N4 C54 1.253(7) . ? N4 C14 1.268(8) . ? C14 C24 1.442(8) . ? C24 C34 1.337(8) . ? C34 C44 1.387(9) . ? C44 C54 1.453(8) . ? N2 C52 1.258(6) . ? N2 C12 1.325(8) . ? C12 C22 1.340(9) . ? C22 C32 1.128(10) . ? C32 C42 1.514(12) . ? C42 C52 1.444(9) . ? N1 C11 1.359(6) 2 ? N1 C11 1.359(6) . ? C11 C21 1.384(7) . ? C21 C31 1.441(7) . ? C31 C21 1.441(7) 2 ? N3 C53 1.318(5) . ? N3 C13 1.382(6) . ? C13 C23 1.411(7) . ? C23 C33 1.450(8) . ? C33 C43 1.327(8) . ? C43 C53 1.383(5) . ? N5 C55 1.3900 . ? N5 C15 1.3901 . ? C15 C25 1.3895 . ? C25 C35 1.3901 . ? C35 C45 1.3899 . ? C45 C55 1.3902 . ? C5E N1E 1.3874 . ? C5E C4E 1.3878 . ? N1E C1E 1.3875 . ? C1E C2E 1.3874 . ? C2E C3E 1.3878 . ? C3E C4E 1.3878 . ? N1F C5F 1.3866 . ? N1F C1F 1.3880 . ? C1F C2F 1.3884 . ? C2F C3F 1.3878 . ? C3F C4F 1.3872 . ? C4F C5F 1.3880 . ? N1G C5G 1.3880 . ? N1G C1G 1.3881 . ? C1G C2G 1.3878 . ? C2G C3G 1.3879 . ? C3G C4G 1.3879 . ? C4G C5G 1.3873 . ? N1I C1I 1.3874 . ? N1I C5I 1.3877 . ? C1I C2I 1.3876 . ? C2I C3I 1.3879 . ? C3I C4I 1.3879 . ? C4I C5I 1.3871 . ? C5H C4H 1.3873 . ? C5H N1H 1.3877 . ? C4H C3H 1.3879 . ? C3H C2H 1.3871 . ? C2H C1H 1.3881 . ? C1H N1H 1.3871 . ? N1A C1A 1.3876 . ? N1A C5A 1.3883 . ? C1A C2A 1.3871 . ? C2A C3A 1.3876 . ? C3A C4A 1.3876 . ? C4A C5A 1.3875 . ? C3C C4C 1.3869 . ? C3C C2C 1.3879 . ? C4C C5C 1.3875 . ? C5C N1C 1.3874 . ? N1C C1C 1.3878 . ? C1C C2C 1.3876 . ? N1B C5B 1.3872 . ? N1B C1B 1.3876 . ? C1B C2B 1.3872 . ? C2B C3B 1.3880 . ? C3B C4B 1.3867 . ? C4B C5B 1.3872 . ? N1D C1D 1.3874 . ? N1D C5D 1.3878 . ? C1D C2D 1.3874 . ? C2D C3D 1.3873 . ? C3D C4D 1.3876 . ? C4D C5D 1.3874 . ? 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 U1 O2 134.96(14) . 2 ? O2 U1 O1 83.05(11) . . ? O2 U1 O1 80.31(11) 2 . ? O2 U1 O1 80.31(10) . 2 ? O2 U1 O1 83.05(11) 2 2 ? O1 U1 O1 135.61(15) . 2 ? O2 U1 O3 136.65(10) . 2 ? O2 U1 O3 80.73(11) 2 2 ? O1 U1 O3 80.22(11) . 2 ? O1 U1 O3 136.73(10) 2 2 ? O2 U1 O3 80.73(11) . . ? O2 U1 O3 136.65(10) 2 . ? O1 U1 O3 136.74(10) . . ? O1 U1 O3 80.22(11) 2 . ? O3 U1 O3 84.70(16) 2 . ? O2 U1 Cl2 139.12(8) . 2 ? O2 U1 Cl2 67.79(8) 2 2 ? O1 U1 Cl2 137.82(8) . 2 ? O1 U1 Cl2 68.40(8) 2 2 ? O3 U1 Cl2 68.33(8) 2 2 ? O3 U1 Cl2 68.87(8) . 2 ? O2 U1 Cl2 67.80(8) . . ? O2 U1 Cl2 139.12(8) 2 . ? O1 U1 Cl2 68.40(8) . . ? O1 U1 Cl2 137.82(8) 2 . ? O3 U1 Cl2 68.88(8) 2 . ? O3 U1 Cl2 68.33(8) . . ? Cl2 U1 Cl2 120.84(5) 2 . ? O2 U1 La3 41.52(8) . . ? O2 U1 La3 111.00(7) 2 . ? O1 U1 La3 41.53(8) . . ? O1 U1 La3 111.33(7) 2 . ? O3 U1 La3 111.92(7) 2 . ? O3 U1 La3 112.32(8) . . ? Cl2 U1 La3 178.77(2) 2 . ? Cl2 U1 La3 60.22(3) . . ? O2 U1 La3 111.00(7) . 2 ? O2 U1 La3 41.52(8) 2 2 ? O1 U1 La3 111.32(7) . 2 ? O1 U1 La3 41.53(8) 2 2 ? O3 U1 La3 112.32(8) 2 2 ? O3 U1 La3 111.92(7) . 2 ? Cl2 U1 La3 60.22(3) 2 2 ? Cl2 U1 La3 178.76(2) . 2 ? La3 U1 La3 118.73(2) . 2 ? O2 U1 La1 112.52(7) . . ? O2 U1 La1 112.52(7) 2 . ? O1 U1 La1 112.20(7) . . ? O1 U1 La1 112.19(7) 2 . ? O3 U1 La1 42.35(8) 2 . ? O3 U1 La1 42.35(8) . . ? Cl2 U1 La1 60.42(2) 2 . ? Cl2 U1 La1 60.42(2) . . ? La3 U1 La1 120.632(10) . . ? La3 U1 La1 120.633(10) 2 . ? O2 U1 La4 105.64(8) . . ? O2 U1 La4 88.93(8) 2 . ? O1 U1 La4 42.04(8) . . ? O1 U1 La4 171.98(8) 2 . ? O3 U1 La4 40.81(7) 2 . ? O3 U1 La4 105.82(8) . . ? Cl2 U1 La4 108.46(3) 2 . ? Cl2 U1 La4 50.20(3) . . ? La3 U1 La4 71.645(15) . . ? La3 U1 La4 130.450(13) 2 . ? La1 U1 La4 70.875(8) . . ? O3 La1 O3 73.81(15) 2 . ? O3 La1 N1 143.09(7) 2 . ? O3 La1 N1 143.09(7) . . ? O3 La1 Cl7 74.78(8) 2 . ? O3 La1 Cl7 125.05(7) . . ? N1 La1 Cl7 78.76(3) . . ? O3 La1 Cl7 125.05(7) 2 2 ? O3 La1 Cl7 74.78(8) . 2 ? N1 La1 Cl7 78.76(3) . 2 ? Cl7 La1 Cl7 157.52(5) . 2 ? O3 La1 Cl5 126.16(7) 2 . ? O3 La1 Cl5 72.39(7) . . ? N1 La1 Cl5 79.65(3) . . ? Cl7 La1 Cl5 92.17(5) . . ? Cl7 La1 Cl5 83.80(5) 2 . ? O3 La1 Cl5 72.39(7) 2 2 ? O3 La1 Cl5 126.15(7) . 2 ? N1 La1 Cl5 79.65(3) . 2 ? Cl7 La1 Cl5 83.80(5) . 2 ? Cl7 La1 Cl5 92.17(5) 2 2 ? Cl5 La1 Cl5 159.29(5) . 2 ? O3 La1 U1 36.91(7) 2 . ? O3 La1 U1 36.91(7) . . ? N1 La1 U1 180.0 . . ? Cl7 La1 U1 101.24(3) . . ? Cl7 La1 U1 101.24(3) 2 . ? Cl5 La1 U1 100.35(3) . . ? Cl5 La1 U1 100.35(3) 2 . ? O3 La1 La4 86.68(7) 2 2 ? O3 La1 La4 31.22(7) . 2 ? N1 La1 La4 124.814(11) . 2 ? Cl7 La1 La4 155.14(3) . 2 ? Cl7 La1 La4 46.79(3) 2 2 ? Cl5 La1 La4 85.44(3) . 2 ? Cl5 La1 La4 106.54(3) 2 2 ? U1 La1 La4 55.186(11) . 2 ? O3 La1 La4 31.22(7) 2 . ? O3 La1 La4 86.68(7) . . ? N1 La1 La4 124.815(11) . . ? Cl7 La1 La4 46.79(3) . . ? Cl7 La1 La4 155.13(3) 2 . ? Cl5 La1 La4 106.54(3) . . ? Cl5 La1 La4 85.44(3) 2 . ? U1 La1 La4 55.185(11) . . ? La4 La1 La4 110.37(2) 2 . ? O1 La2 O2 68.27(9) . 2 ? O1 La2 O4 68.94(10) . . ? O2 La2 O4 68.73(10) 2 . ? O1 La2 O11 91.56(10) . . ? O2 La2 O11 139.14(9) 2 . ? O4 La2 O11 70.91(10) . . ? O1 La2 O32 139.73(10) . . ? O2 La2 O32 97.01(10) 2 . ? O4 La2 O32 70.79(10) . . ? O11 La2 O32 75.36(10) . . ? O1 La2 N2 142.80(10) . . ? O2 La2 N2 142.53(10) 2 . ? O4 La2 N2 131.98(12) . . ? O11 La2 N2 73.28(11) . . ? O32 La2 N2 70.00(11) . . ? O1 La2 Cl1 70.91(7) . . ? O2 La2 Cl1 70.23(8) 2 . ? O4 La2 Cl1 130.44(8) . . ? O11 La2 Cl1 137.86(7) . . ? O32 La2 Cl1 141.22(8) . . ? N2 La2 Cl1 97.57(10) . . ? O1 La2 Cl3 71.07(7) . . ? O2 La2 Cl3 128.99(7) 2 . ? O4 La2 Cl3 121.83(7) . . ? O11 La2 Cl3 69.80(7) . . ? O32 La2 Cl3 133.99(8) . . ? N2 La2 Cl3 71.83(8) . . ? Cl1 La2 Cl3 68.30(3) . . ? O1 La2 Cl4 129.56(7) . 2 ? O2 La2 Cl4 70.46(7) 2 2 ? O4 La2 Cl4 119.78(7) . 2 ? O11 La2 Cl4 138.87(7) . 2 ? O32 La2 Cl4 72.45(8) . 2 ? N2 La2 Cl4 72.11(9) . 2 ? Cl1 La2 Cl4 68.77(4) . 2 ? Cl3 La2 Cl4 118.14(4) . 2 ? O1 La2 U1 35.22(7) . . ? O2 La2 U1 34.68(7) 2 . ? O4 La2 U1 72.14(8) . . ? O11 La2 U1 123.69(7) . . ? O32 La2 U1 127.84(7) . . ? N2 La2 U1 155.87(9) . . ? Cl1 La2 U1 58.30(3) . . ? Cl3 La2 U1 96.76(3) . . ? Cl4 La2 U1 96.42(3) 2 . ? O1 La2 La5 75.60(7) . 2 ? O2 La2 La5 35.74(7) 2 2 ? O4 La2 La5 36.47(7) . 2 ? O11 La2 La5 106.44(7) . 2 ? O32 La2 La5 72.17(7) . 2 ? N2 La2 La5 140.86(8) . 2 ? Cl1 La2 La5 105.66(3) . 2 ? Cl3 La2 La5 146.24(2) . 2 ? Cl4 La2 La5 87.36(3) 2 2 ? U1 La2 La5 56.237(15) . 2 ? O1 La2 La4 35.01(7) . . ? O2 La2 La4 74.97(6) 2 . ? O4 La2 La4 37.15(7) . . ? O11 La2 La4 69.16(7) . . ? O32 La2 La4 106.08(7) . . ? N2 La2 La4 141.80(9) . . ? Cl1 La2 La4 105.46(3) . . ? Cl3 La2 La4 88.77(3) . . ? Cl4 La2 La4 144.81(2) 2 . ? U1 La2 La4 55.728(16) . . ? La5 La2 La4 60.029(18) 2 . ? O1 La3 O2 72.65(10) . . ? O1 La3 N3 141.71(11) . . ? O2 La3 N3 145.58(11) . . ? O1 La3 Cl8 125.64(7) . . ? O2 La3 Cl8 73.32(7) . . ? N3 La3 Cl8 79.81(9) . . ? O1 La3 Cl6 72.28(7) . . ? O2 La3 Cl6 124.56(7) . . ? N3 La3 Cl6 78.09(9) . . ? Cl8 La3 Cl6 94.61(4) . . ? O1 La3 Cl3 73.39(7) . . ? O2 La3 Cl3 125.04(7) . . ? N3 La3 Cl3 79.36(9) . . ? Cl8 La3 Cl3 159.11(3) . . ? Cl6 La3 Cl3 82.72(4) . . ? O1 La3 Cl4 126.05(7) . . ? O2 La3 Cl4 73.13(7) . . ? N3 La3 Cl4 81.85(9) . . ? Cl8 La3 Cl4 80.98(4) . . ? Cl6 La3 Cl4 159.93(3) . . ? Cl3 La3 Cl4 94.42(4) . . ? O1 La3 U1 36.63(7) . . ? O2 La3 U1 36.02(7) . . ? N3 La3 U1 177.76(9) . . ? Cl8 La3 U1 100.40(4) . . ? Cl6 La3 U1 99.67(3) . . ? Cl3 La3 U1 100.48(3) . . ? Cl4 La3 U1 100.38(3) . . ? O1 La3 La2 31.64(7) . . ? O2 La3 La2 86.50(7) . . ? N3 La3 La2 123.83(9) . . ? Cl8 La3 La2 155.52(3) . . ? Cl6 La3 La2 85.40(3) . . ? Cl3 La3 La2 45.22(2) . . ? Cl4 La3 La2 106.70(3) . . ? U1 La3 La2 55.71(2) . . ? O1 La3 La2 86.89(7) . 2 ? O2 La3 La2 31.54(6) . 2 ? N3 La3 La2 126.75(9) . 2 ? Cl8 La3 La2 85.54(4) . 2 ? Cl6 La3 La2 154.48(2) . 2 ? Cl3 La3 La2 105.74(3) . 2 ? Cl4 La3 La2 45.21(3) . 2 ? U1 La3 La2 55.469(13) . 2 ? La2 La3 La2 84.18(2) . 2 ? O1 La3 La4 31.28(7) . . ? O2 La3 La4 85.50(7) . . ? N3 La3 La4 122.87(9) . . ? Cl8 La3 La4 105.66(3) . . ? Cl6 La3 La4 45.05(3) . . ? Cl3 La3 La4 87.15(3) . . ? Cl4 La3 La4 154.95(2) . . ? U1 La3 La4 54.906(17) . . ? La2 La3 La4 57.997(13) . . ? La2 La3 La4 110.370(19) 2 . ? O1 La3 La5 86.41(7) . . ? O2 La3 La5 31.49(6) . . ? N3 La3 La5 125.20(8) . . ? Cl8 La3 La5 45.52(3) . . ? Cl6 La3 La5 105.45(3) . . ? Cl3 La3 La5 154.96(2) . . ? Cl4 La3 La5 85.49(3) . . ? U1 La3 La5 55.188(16) . . ? La2 La3 La5 110.897(14) . . ? La2 La3 La5 57.477(15) 2 . ? La4 La3 La5 82.761(18) . . ? O3 La4 O1 69.50(9) 2 . ? O3 La4 O12 138.50(10) 2 . ? O1 La4 O12 97.10(10) . . ? O3 La4 O4 68.07(10) 2 . ? O1 La4 O4 67.86(9) . . ? O12 La4 O4 70.50(10) . . ? O3 La4 O21 89.63(11) 2 . ? O1 La4 O21 140.42(9) . . ? O12 La4 O21 76.26(11) . . ? O4 La4 O21 73.26(10) . . ? O3 La4 N4 142.48(11) 2 . ? O1 La4 N4 141.38(10) . . ? O12 La4 N4 70.77(11) . . ? O4 La4 N4 133.80(12) . . ? O21 La4 N4 73.93(11) . . ? O3 La4 Cl2 72.50(8) 2 . ? O1 La4 Cl2 71.33(7) . . ? O12 La4 Cl2 142.10(7) . . ? O4 La4 Cl2 130.63(8) . . ? O21 La4 Cl2 135.24(8) . . ? N4 La4 Cl2 95.54(10) . . ? O3 La4 Cl6 130.71(8) 2 . ? O1 La4 Cl6 69.56(7) . . ? O12 La4 Cl6 72.82(7) . . ? O4 La4 Cl6 118.26(7) . . ? O21 La4 Cl6 139.64(8) . . ? N4 La4 Cl6 71.83(8) . . ? Cl2 La4 Cl6 69.31(4) . . ? O3 La4 Cl7 71.10(7) 2 . ? O1 La4 Cl7 129.49(8) . . ? O12 La4 Cl7 133.42(8) . . ? O4 La4 Cl7 122.58(7) . . ? O21 La4 Cl7 67.84(8) . . ? N4 La4 Cl7 71.47(9) . . ? Cl2 La4 Cl7 67.58(4) . . ? Cl6 La4 Cl7 118.83(4) . . ? O3 La4 U1 35.84(7) 2 . ? O1 La4 U1 35.81(7) . . ? O12 La4 U1 128.94(7) . . ? O4 La4 U1 72.18(7) . . ? O21 La4 U1 123.42(7) . . ? N4 La4 U1 154.01(9) . . ? Cl2 La4 U1 58.47(3) . . ? Cl6 La4 U1 96.32(3) . . ? Cl7 La4 U1 96.06(3) . . ? O3 La4 La5 34.64(7) 2 2 ? O1 La4 La5 75.26(6) . 2 ? O12 La4 La5 104.78(7) . 2 ? O4 La4 La5 36.63(7) . 2 ? O21 La4 La5 69.19(7) . 2 ? N4 La4 La5 142.71(8) . 2 ? Cl2 La4 La5 106.62(4) . 2 ? Cl6 La4 La5 143.98(3) . 2 ? Cl7 La4 La5 89.50(3) . 2 ? U1 La4 La5 56.318(15) . 2 ? O3 La4 La2 75.30(7) 2 . ? O1 La4 La2 34.81(7) . . ? O12 La4 La2 72.92(7) . . ? O4 La4 La2 36.19(7) . . ? O21 La4 La2 108.77(7) . . ? N4 La4 La2 141.69(8) . . ? Cl2 La4 La2 105.78(3) . . ? Cl6 La4 La2 86.24(3) . . ? Cl7 La4 La2 146.19(3) . . ? U1 La4 La2 56.424(10) . . ? La5 La4 La2 59.741(10) 2 . ? O3 La5 O2 68.67(9) . . ? O3 La5 O4 68.19(10) . 2 ? O2 La5 O4 68.44(10) . 2 ? O3 La5 O22 96.10(10) . . ? O2 La5 O22 138.74(9) . . ? O4 La5 O22 70.31(10) 2 . ? O3 La5 O31 139.22(10) . . ? O2 La5 O31 94.74(10) . . ? O4 La5 O31 71.08(11) 2 . ? O22 La5 O31 71.64(11) . . ? O3 La5 N5 140.87(7) . . ? O2 La5 N5 140.62(7) . . ? O4 La5 N5 136.91(8) 2 . ? O22 La5 N5 74.61(8) . . ? O31 La5 N5 74.74(8) . . ? O3 La5 Cl2 71.83(8) . . ? O2 La5 Cl2 70.79(7) . . ? O4 La5 Cl2 130.58(8) 2 . ? O22 La5 Cl2 142.65(8) . . ? O31 La5 Cl2 139.38(9) . . ? N5 La5 Cl2 92.51(5) . . ? O3 La5 Cl8 129.46(8) . . ? O2 La5 Cl8 69.31(7) . . ? O4 La5 Cl8 118.82(7) 2 . ? O22 La5 Cl8 134.30(8) . . ? O31 La5 Cl8 70.59(9) . . ? N5 La5 Cl8 71.42(4) . . ? Cl2 La5 Cl8 68.79(4) . . ? O3 La5 Cl5 69.40(7) . . ? O2 La5 Cl5 129.17(7) . . ? O4 La5 Cl5 118.93(7) 2 . ? O22 La5 Cl5 72.82(8) . . ? O31 La5 Cl5 136.05(8) . . ? N5 La5 Cl5 71.55(4) . . ? Cl2 La5 Cl5 69.85(4) . . ? Cl8 La5 Cl5 121.90(4) . . ? O3 La5 U1 35.72(7) . . ? O2 La5 U1 34.91(6) . . ? O4 La5 U1 72.23(8) 2 . ? O22 La5 U1 127.93(7) . . ? O31 La5 U1 126.38(8) . . ? N5 La5 U1 150.86(4) . . ? Cl2 La5 U1 58.35(3) . . ? Cl8 La5 U1 95.37(4) . . ? Cl5 La5 U1 95.93(3) . . ? O3 La5 La2 75.37(7) . 2 ? O2 La5 La2 35.63(7) . 2 ? O4 La5 La2 36.27(7) 2 2 ? O22 La5 La2 104.53(7) . 2 ? O31 La5 La2 70.81(8) . 2 ? N5 La5 La2 143.65(3) . 2 ? Cl2 La5 La2 106.10(3) . 2 ? Cl8 La5 La2 86.35(3) . 2 ? Cl5 La5 La2 144.01(3) . 2 ? U1 La5 La2 56.491(13) . 2 ? O3 La5 La4 34.01(7) . 2 ? O2 La5 La4 75.07(6) . 2 ? O4 La5 La4 37.38(7) 2 2 ? O22 La5 La4 72.44(7) . 2 ? O31 La5 La4 106.99(8) . 2 ? N5 La5 La4 144.26(4) . 2 ? Cl2 La5 La4 105.43(3) . 2 ? Cl8 La5 La4 143.83(3) . 2 ? Cl5 La5 La4 85.75(2) . 2 ? U1 La5 La4 55.87(2) . 2 ? La2 La5 La4 60.231(11) 2 2 ? La2 Cl1 La2 143.05(6) 2 . ? La5 Cl2 La4 143.33(5) . . ? La5 Cl2 U1 72.01(3) . . ? La4 Cl2 U1 71.33(4) . . ? La3 Cl3 La2 91.17(4) . . ? La3 Cl4 La2 91.44(4) . 2 ? La1 Cl5 La5 91.67(4) . . ? La3 Cl6 La4 91.81(3) . . ? La1 Cl7 La4 90.43(4) . . ? La3 Cl8 La5 92.14(4) . . ? U1 O1 La3 101.84(12) . . ? U1 O1 La2 103.71(10) . . ? La3 O1 La2 117.57(11) . . ? U1 O1 La4 102.15(11) . . ? La3 O1 La4 118.45(11) . . ? La2 O1 La4 110.18(11) . . ? U1 O2 La3 102.46(13) . . ? U1 O2 La2 104.04(10) . 2 ? La3 O2 La2 117.90(11) . 2 ? U1 O2 La5 103.39(10) . . ? La3 O2 La5 118.08(10) . . ? La2 O2 La5 108.63(12) 2 . ? U1 O3 La4 103.35(11) . 2 ? U1 O3 La1 100.74(13) . . ? La4 O3 La1 117.39(11) 2 . ? U1 O3 La5 102.81(11) . . ? La4 O3 La5 111.35(13) 2 . ? La1 O3 La5 118.06(11) . . ? La2 O4 La5 107.26(11) . 2 ? La2 O4 La4 106.66(11) . . ? La5 O4 La4 105.98(11) 2 . ? S1 O11 La2 142.44(19) . . ? S1 O12 La4 138.7(2) . . ? O11 S1 O13 114.7(2) . . ? O11 S1 O12 113.4(2) . . ? O13 S1 O12 114.9(2) . . ? O11 S1 C1 102.4(2) . . ? O13 S1 C1 103.3(2) . . ? O12 S1 C1 106.5(2) . . ? F12 C1 F13 109.8(4) . . ? F12 C1 F11 109.7(4) . . ? F13 C1 F11 105.9(4) . . ? F12 C1 S1 113.5(3) . . ? F13 C1 S1 111.7(3) . . ? F11 C1 S1 106.0(3) . . ? S2 O21 La4 144.1(2) 2 . ? S2 O22 La5 134.9(2) . . ? O23 S2 O21 116.5(2) . 2 ? O23 S2 O22 113.6(2) . . ? O21 S2 O22 114.0(2) 2 . ? O23 S2 C2 106.3(3) . . ? O21 S2 C2 100.9(2) 2 . ? O22 S2 C2 103.5(2) . . ? F22 C2 F23 108.3(4) . . ? F22 C2 F21 106.0(5) . . ? F23 C2 F21 101.8(5) . . ? F22 C2 S2 117.8(4) . . ? F23 C2 S2 110.8(4) . . ? F21 C2 S2 110.9(4) . . ? S3 O31 La5 140.5(2) 2 . ? S3 O32 La2 137.8(2) . . ? O33 S3 O32 115.7(2) . . ? O33 S3 O31 115.5(2) . 2 ? O32 S3 O31 113.4(2) . 2 ? O33 S3 C3 101.7(3) . . ? O32 S3 C3 104.0(2) . . ? O31 S3 C3 104.1(2) 2 . ? F33 C3 F32 106.4(4) . . ? F33 C3 F31 103.1(4) . . ? F32 C3 F31 103.6(4) . . ? F33 C3 S3 114.9(4) . . ? F32 C3 S3 114.5(4) . . ? F31 C3 S3 113.1(4) . . ? C54 N4 C14 121.5(5) . . ? C54 N4 La4 117.1(4) . . ? C14 N4 La4 121.3(3) . . ? N4 C14 C24 120.2(5) . . ? C34 C24 C14 120.9(6) . . ? C24 C34 C44 117.7(6) . . ? C34 C44 C54 116.3(6) . . ? N4 C54 C44 123.5(6) . . ? C52 N2 C12 118.6(5) . . ? C52 N2 La2 120.4(4) . . ? C12 N2 La2 121.0(3) . . ? N2 C12 C22 123.5(6) . . ? C32 C22 C12 122.2(8) . . ? C22 C32 C42 122.4(8) . . ? C52 C42 C32 111.1(6) . . ? N2 C52 C42 121.9(6) . . ? C11 N1 C11 116.0(6) 2 . ? C11 N1 La1 122.0(3) 2 . ? C11 N1 La1 122.0(3) . . ? N1 C11 C21 125.6(5) . . ? C11 C21 C31 117.1(6) . . ? C21 C31 C21 118.7(7) . 2 ? C53 N3 C13 120.6(4) . . ? C53 N3 La3 120.4(2) . . ? C13 N3 La3 119.0(3) . . ? N3 C13 C23 120.8(5) . . ? C13 C23 C33 116.3(5) . . ? C43 C33 C23 119.4(5) . . ? C33 C43 C53 122.1(5) . . ? N3 C53 C43 120.8(3) . . ? C55 N5 C15 120.0 . . ? C55 N5 La5 127.6 . . ? C15 N5 La5 112.3 . . ? C25 C15 N5 120.0 . . ? C15 C25 C35 120.0 . . ? C45 C35 C25 120.0 . . ? C35 C45 C55 120.0 . . ? N5 C55 C45 120.0 . . ? N1E C5E C4E 120.0 . . ? C5E N1E C1E 120.0 . . ? C2E C1E N1E 120.0 . . ? C1E C2E C3E 120.0 . . ? C2E C3E C4E 120.0 . . ? C5E C4E C3E 120.0 . . ? C5F N1F C1F 120.0 . . ? N1F C1F C2F 120.0 . . ? C3F C2F C1F 120.0 . . ? C4F C3F C2F 120.0 . . ? C3F C4F C5F 120.0 . . ? N1F C5F C4F 120.0 . . ? C5G N1G C1G 120.0 . . ? C2G C1G N1G 120.0 . . ? C1G C2G C3G 120.0 . . ? C2G C3G C4G 120.0 . . ? C5G C4G C3G 120.0 . . ? C4G C5G N1G 120.0 . . ? C1I N1I C5I 120.0 . . ? N1I C1I C2I 120.0 . . ? C1I C2I C3I 120.0 . . ? C4I C3I C2I 120.0 . . ? C5I C4I C3I 120.0 . . ? C4I C5I N1I 120.0 . . ? C4H C5H N1H 120.0 . . ? C5H C4H C3H 120.0 . . ? C2H C3H C4H 120.0 . . ? C3H C2H C1H 120.0 . . ? N1H C1H C2H 120.0 . . ? C1H N1H C5H 120.0 . . ? C1A N1A C5A 120.0 . . ? C2A C1A N1A 120.0 . . ? C1A C2A C3A 120.0 . . ? C2A C3A C4A 120.0 . . ? C5A C4A C3A 120.0 . . ? C4A C5A N1A 120.0 . . ? C4C C3C C2C 120.0 . . ? C3C C4C C5C 120.0 . . ? N1C C5C C4C 120.0 . . ? C5C N1C C1C 120.0 . . ? C2C C1C N1C 120.0 . . ? C1C C2C C3C 120.0 . . ? C5B N1B C1B 120.0 . . ? C2B C1B N1B 120.0 . . ? C1B C2B C3B 120.0 . . ? C4B C3B C2B 120.0 . . ? C3B C4B C5B 120.0 . . ? C4B C5B N1B 120.0 . . ? C1D N1D C5D 120.0 . . ? C2D C1D N1D 120.0 . . ? C3D C2D C1D 120.0 . . ? C2D C3D C4D 120.0 . . ? C5D C4D C3D 120.0 . . ? C4D C5D N1D 120.0 . . ?