Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Nicholas Long' _publ_contact_author_address ; Department of Chemistry Imperial College of Science, Techno South Kensington LONDON SW7 2AY UNITED KINGDOM ; _publ_contact_author_email N.LONG@IMPERIAL.AC.UK _publ_section_title ; A novel tetrakis(pyrazolyl)borate ligand bearing triphenylphosphine oxide substituents ; loop_ _publ_author_name 'Nicholas Long' 'Antony Gee' 'Steven Kealey' 'Andrew J. P. White' data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 653717' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H64 B N8 O4 P4 Tl, 3.5(C H Cl3), 0.5(C5 H12)' _chemical_formula_sum 'C90 H73.50 B Cl10.50 N8 O4 P4 Tl' _chemical_formula_weight 2042.35 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' B B 0.0013 0.0007 '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' P P 0.1023 0.0942 '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' Tl Tl -2.8358 9.6688 '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 14.6110(3) _cell_length_b 19.0394(3) _cell_length_c 19.8132(4) _cell_angle_alpha 62.012(2) _cell_angle_beta 73.056(2) _cell_angle_gamma 85.878(2) _cell_volume 4642.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20433 _cell_measurement_theta_min 3.7193 _cell_measurement_theta_max 28.9162 _exptl_crystal_description blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2052 _exptl_absorpt_coefficient_mu 2.164 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.742 _exptl_absorpt_correction_T_max 0.892 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52575 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0936 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 29.01 _reflns_number_total 21105 _reflns_number_gt 14291 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21105 _refine_ls_number_parameters 1165 _refine_ls_number_restraints 195 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.0940 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tl Tl 0.629982(10) 0.432816(10) 0.138303(9) 0.03380(6) Uani 1 1 d . . . B B 0.5866(3) 0.3373(2) 0.3517(2) 0.0245(9) Uani 1 1 d . . . P1 P 0.39167(6) 0.37353(6) 0.14251(6) 0.0272(2) Uani 1 1 d . . . O1 O 0.49737(17) 0.36641(17) 0.12378(16) 0.0365(7) Uani 1 1 d . . . P2 P 0.91125(7) 0.21436(6) 0.13747(6) 0.0324(2) Uani 1 1 d . . . O2 O 0.9225(2) 0.14528(18) 0.21101(17) 0.0504(8) Uani 1 1 d . . . P3 P 0.58876(7) 0.09232(6) 0.71185(6) 0.0316(2) Uani 1 1 d D . . O3 O 0.5853(2) 0.15412(17) 0.73777(18) 0.0505(8) Uani 1 1 d . A . P4 P 0.80998(6) 0.61111(6) 0.34900(6) 0.0259(2) Uani 1 1 d . . . O4 O 0.89395(16) 0.58593(15) 0.30427(15) 0.0321(6) Uani 1 1 d . . . N1 N 0.48659(19) 0.40968(17) 0.25743(16) 0.0244(6) Uani 1 1 d . . . N2 N 0.48988(18) 0.36109(17) 0.33319(16) 0.0222(6) Uani 1 1 d . . . N3 N 0.64177(19) 0.28948(17) 0.24545(16) 0.0237(6) Uani 1 1 d . . . N4 N 0.63857(19) 0.28036(17) 0.31872(16) 0.0240(6) Uani 1 1 d . . . N5 N 0.5179(2) 0.22244(17) 0.48724(17) 0.0281(7) Uani 1 1 d . . . N6 N 0.56878(19) 0.29477(17) 0.44138(16) 0.0230(6) Uani 1 1 d . . . N7 N 0.61442(18) 0.48020(16) 0.31527(16) 0.0225(6) Uani 1 1 d . . . N8 N 0.65108(19) 0.41384(16) 0.31249(16) 0.0214(6) Uani 1 1 d . . . C9 C 0.4053(2) 0.3571(2) 0.3851(2) 0.0315(9) Uani 1 1 d . . . H9A H 0.3897 0.3269 0.4416 0.038 Uiso 1 1 calc R . . C10 C 0.3446(3) 0.4037(2) 0.3431(2) 0.0346(9) Uani 1 1 d . . . H10A H 0.2800 0.4125 0.3641 0.042 Uiso 1 1 calc R . . C11 C 0.3983(2) 0.4351(2) 0.2637(2) 0.0266(8) Uani 1 1 d . . . C12 C 0.3689(2) 0.4911(2) 0.1916(2) 0.0251(8) Uani 1 1 d . . . C13 C 0.3582(2) 0.4689(2) 0.1358(2) 0.0247(8) Uani 1 1 d . . . C14 C 0.3250(3) 0.5239(2) 0.0729(2) 0.0311(9) Uani 1 1 d . . . H14A H 0.3164 0.5092 0.0354 0.037 Uiso 1 1 calc R . . C15 C 0.3043(3) 0.5990(2) 0.0638(2) 0.0350(9) Uani 1 1 d . . . H15A H 0.2827 0.6359 0.0200 0.042 Uiso 1 1 calc R . . C16 C 0.3153(3) 0.6199(2) 0.1182(2) 0.0390(10) Uani 1 1 d . . . H16A H 0.3011 0.6717 0.1121 0.047 Uiso 1 1 calc R . . C17 C 0.3467(3) 0.5669(2) 0.1822(2) 0.0335(9) Uani 1 1 d . . . H17A H 0.3532 0.5822 0.2199 0.040 Uiso 1 1 calc R . . C18 C 0.6939(3) 0.2228(2) 0.3516(2) 0.0378(10) Uani 1 1 d . . . H18A H 0.7033 0.2056 0.4024 0.045 Uiso 1 1 calc R . . C19 C 0.7346(3) 0.1927(2) 0.3001(2) 0.0379(10) Uani 1 1 d . . . H19A H 0.7773 0.1514 0.3074 0.045 Uiso 1 1 calc R . . C20 C 0.6995(2) 0.2361(2) 0.2338(2) 0.0249(8) Uani 1 1 d . . . C21 C 0.7107(2) 0.22326(19) 0.1643(2) 0.0240(8) Uani 1 1 d . . . C22 C 0.7982(2) 0.2104(2) 0.1196(2) 0.0262(8) Uani 1 1 d . . . C23 C 0.7975(3) 0.1883(2) 0.0613(2) 0.0316(9) Uani 1 1 d . . . H23A H 0.8560 0.1776 0.0323 0.038 Uiso 1 1 calc R . . C24 C 0.7135(3) 0.1820(2) 0.0453(2) 0.0334(9) Uani 1 1 d . . . H24A H 0.7143 0.1662 0.0062 0.040 Uiso 1 1 calc R . . C25 C 0.6286(3) 0.1985(2) 0.0861(2) 0.0341(9) Uani 1 1 d . . . H25A H 0.5711 0.1961 0.0739 0.041 Uiso 1 1 calc R . . C26 C 0.6272(3) 0.2186(2) 0.1448(2) 0.0329(9) Uani 1 1 d . . . H26A H 0.5680 0.2297 0.1728 0.039 Uiso 1 1 calc R . . C27 C 0.5885(2) 0.3221(2) 0.4879(2) 0.0255(8) Uani 1 1 d . . . H27A H 0.6225 0.3714 0.4697 0.031 Uiso 1 1 calc R . . C28 C 0.5507(3) 0.2659(2) 0.5662(2) 0.0314(9) Uani 1 1 d . . . H28A H 0.5531 0.2681 0.6126 0.038 Uiso 1 1 calc R . . C29 C 0.5079(2) 0.2052(2) 0.5628(2) 0.0227(8) Uani 1 1 d . A . C30 C 0.4505(2) 0.1312(2) 0.6278(2) 0.0278(8) Uani 1 1 d . . . C31 C 0.4790(3) 0.0772(2) 0.6948(2) 0.0302(8) Uani 1 1 d . A . C32 C 0.4165(3) 0.0113(2) 0.7543(3) 0.0452(11) Uani 1 1 d . . . H32A H 0.4352 -0.0255 0.7998 0.054 Uiso 1 1 calc R A . C33 C 0.3277(3) -0.0015(3) 0.7481(3) 0.0595(13) Uani 1 1 d . A . H33A H 0.2856 -0.0463 0.7896 0.071 Uiso 1 1 calc R . . C34 C 0.3007(3) 0.0509(3) 0.6815(3) 0.0566(13) Uani 1 1 d . . . H34A H 0.2402 0.0422 0.6767 0.068 Uiso 1 1 calc R A . C35 C 0.3620(3) 0.1161(3) 0.6219(3) 0.0437(10) Uani 1 1 d . A . H35A H 0.3434 0.1515 0.5758 0.052 Uiso 1 1 calc R . . C36 C 0.7479(2) 0.4258(2) 0.2813(2) 0.0279(8) Uani 1 1 d . . . H36A H 0.7897 0.3880 0.2735 0.034 Uiso 1 1 calc R . . C37 C 0.7748(3) 0.5004(2) 0.2631(2) 0.0342(9) Uani 1 1 d . . . H37A H 0.8381 0.5255 0.2398 0.041 Uiso 1 1 calc R . . C38 C 0.6895(2) 0.5330(2) 0.2861(2) 0.0228(7) Uani 1 1 d . . . C39 C 0.6707(2) 0.6146(2) 0.2751(2) 0.0234(8) Uani 1 1 d . . . C40 C 0.7234(2) 0.6578(2) 0.2957(2) 0.0241(8) Uani 1 1 d . . . C41 C 0.7010(3) 0.7353(2) 0.2799(2) 0.0309(9) Uani 1 1 d . . . H41A H 0.7359 0.7644 0.2936 0.037 Uiso 1 1 calc R . . C42 C 0.6300(3) 0.7708(2) 0.2453(2) 0.0352(9) Uani 1 1 d . . . H42A H 0.6175 0.8244 0.2337 0.042 Uiso 1 1 calc R . . C43 C 0.5772(3) 0.7286(2) 0.2277(2) 0.0374(10) Uani 1 1 d . . . H43A H 0.5264 0.7523 0.2055 0.045 Uiso 1 1 calc R . . C44 C 0.5973(2) 0.6518(2) 0.2419(2) 0.0294(8) Uani 1 1 d . . . H44A H 0.5603 0.6235 0.2289 0.035 Uiso 1 1 calc R . . C45 C 0.3276(3) 0.3000(2) 0.2408(2) 0.0312(9) Uani 1 1 d . . . C46 C 0.3788(4) 0.2414(3) 0.2868(3) 0.0546(13) Uani 1 1 d . . . H46A H 0.4462 0.2414 0.2660 0.066 Uiso 1 1 calc R . . C47 C 0.3304(5) 0.1834(3) 0.3629(3) 0.0753(18) Uani 1 1 d . . . H47A H 0.3653 0.1436 0.3940 0.090 Uiso 1 1 calc R . . C48 C 0.2353(5) 0.1822(3) 0.3936(3) 0.0691(16) Uani 1 1 d . . . H48A H 0.2029 0.1410 0.4451 0.083 Uiso 1 1 calc R . . C49 C 0.1848(4) 0.2415(3) 0.3496(3) 0.0570(13) Uani 1 1 d . . . H49A H 0.1179 0.2419 0.3720 0.068 Uiso 1 1 calc R . . C50 C 0.2303(3) 0.2998(3) 0.2736(3) 0.0394(10) Uani 1 1 d . . . H50A H 0.1947 0.3400 0.2438 0.047 Uiso 1 1 calc R . . C51 C 0.3495(2) 0.3625(2) 0.0701(2) 0.0269(8) Uani 1 1 d . . . C52 C 0.2542(3) 0.3547(2) 0.0750(2) 0.0394(10) Uani 1 1 d . . . H52A H 0.2052 0.3533 0.1195 0.047 Uiso 1 1 calc R . . C53 C 0.2301(3) 0.3489(2) 0.0151(3) 0.0432(11) Uani 1 1 d . . . H53A H 0.1644 0.3436 0.0188 0.052 Uiso 1 1 calc R . . C54 C 0.2997(3) 0.3509(2) -0.0492(3) 0.0415(10) Uani 1 1 d . . . H54A H 0.2826 0.3480 -0.0906 0.050 Uiso 1 1 calc R . . C55 C 0.3946(3) 0.3571(2) -0.0537(2) 0.0406(10) Uani 1 1 d . . . H55A H 0.4433 0.3570 -0.0976 0.049 Uiso 1 1 calc R . . C56 C 0.4192(3) 0.3634(2) 0.0054(2) 0.0318(9) Uani 1 1 d . . . H56A H 0.4850 0.3683 0.0016 0.038 Uiso 1 1 calc R . . C57 C 1.0043(3) 0.2226(2) 0.0500(2) 0.0351(9) Uani 1 1 d . . . C58 C 1.0115(3) 0.2810(3) -0.0268(3) 0.0433(10) Uani 1 1 d . . . H58A H 0.9656 0.3198 -0.0356 0.052 Uiso 1 1 calc R . . C59 C 1.0840(3) 0.2843(3) -0.0914(3) 0.0529(12) Uani 1 1 d . . . H59A H 1.0877 0.3245 -0.1440 0.064 Uiso 1 1 calc R . . C60 C 1.1502(3) 0.2286(4) -0.0782(3) 0.0616(14) Uani 1 1 d . . . H60A H 1.2005 0.2308 -0.1224 0.074 Uiso 1 1 calc R . . C61 C 1.1454(3) 0.1695(3) -0.0025(3) 0.0613(14) Uani 1 1 d . . . H61A H 1.1918 0.1311 0.0058 0.074 Uiso 1 1 calc R . . C62 C 1.0717(3) 0.1667(3) 0.0621(3) 0.0473(11) Uani 1 1 d . . . H62A H 1.0677 0.1260 0.1147 0.057 Uiso 1 1 calc R . . C63 C 0.9242(2) 0.3085(3) 0.1362(3) 0.0364(10) Uani 1 1 d . . . C64 C 0.9747(3) 0.3109(4) 0.1846(3) 0.0605(14) Uani 1 1 d . . . H64A H 0.9969 0.2632 0.2191 0.073 Uiso 1 1 calc R . . C65 C 0.9927(4) 0.3804(4) 0.1833(4) 0.0773(18) Uani 1 1 d . . . H65A H 1.0273 0.3813 0.2167 0.093 Uiso 1 1 calc R . . C66 C 0.9613(3) 0.4484(4) 0.1343(4) 0.0714(18) Uani 1 1 d . . . H66A H 0.9760 0.4968 0.1332 0.086 Uiso 1 1 calc R . . C67 C 0.9075(3) 0.4502(3) 0.0847(3) 0.0624(14) Uani 1 1 d . . . H67A H 0.8844 0.4983 0.0517 0.075 Uiso 1 1 calc R . . C68 C 0.8897(3) 0.3778(3) 0.0865(3) 0.0435(11) Uani 1 1 d . . . H68A H 0.8544 0.3761 0.0539 0.052 Uiso 1 1 calc R . . C69 C 0.6089(3) -0.0025(2) 0.7880(2) 0.0397(10) Uani 1 1 d . A . C70 C 0.6440(3) -0.0660(3) 0.7742(3) 0.0600(13) Uani 1 1 d . . . H70A H 0.6563 -0.0608 0.7222 0.072 Uiso 1 1 calc R A . C71 C 0.6610(4) -0.1357(3) 0.8337(4) 0.0827(19) Uani 1 1 d . A . H71A H 0.6839 -0.1785 0.8230 0.099 Uiso 1 1 calc R . . C72 C 0.6455(4) -0.1435(3) 0.9062(5) 0.085(2) Uani 1 1 d . . . H72A H 0.6599 -0.1915 0.9466 0.102 Uiso 1 1 calc R A . C73 C 0.6091(5) -0.0839(4) 0.9244(4) 0.092(2) Uani 1 1 d . A . H73A H 0.5972 -0.0908 0.9770 0.110 Uiso 1 1 calc R . . C74 C 0.5897(4) -0.0121(3) 0.8636(3) 0.0632(14) Uani 1 1 d . . . H74A H 0.5634 0.0294 0.8753 0.076 Uiso 1 1 calc R A . C75 C 0.6850(4) 0.1094(4) 0.6212(4) 0.044(3) Uani 0.669(17) 1 d PGD A 1 C76 C 0.7622(4) 0.1628(5) 0.5973(5) 0.063(3) Uani 0.669(17) 1 d PG A 1 H76 H 0.7616 0.1919 0.6253 0.075 Uiso 0.669(17) 1 calc PR A 1 C77 C 0.8403(3) 0.1736(6) 0.5322(4) 0.088(5) Uani 0.669(17) 1 d PG A 1 H77 H 0.8931 0.2101 0.5159 0.105 Uiso 0.669(17) 1 calc PR A 1 C78 C 0.8412(4) 0.1310(7) 0.4912(3) 0.088(6) Uani 0.669(17) 1 d PG A 1 H78 H 0.8946 0.1383 0.4468 0.105 Uiso 0.669(17) 1 calc PR A 1 C79 C 0.7640(6) 0.0776(5) 0.5151(3) 0.076(4) Uani 0.669(17) 1 d PG A 1 H79 H 0.7646 0.0484 0.4871 0.091 Uiso 0.669(17) 1 calc PR A 1 C80 C 0.6859(5) 0.0668(4) 0.5801(4) 0.055(2) Uani 0.669(17) 1 d PG A 1 H80 H 0.6331 0.0303 0.5965 0.066 Uiso 0.669(17) 1 calc PR A 1 C75' C 0.6910(7) 0.1211(9) 0.6280(7) 0.024(4) Uiso 0.331(17) 1 d PGD A 2 C76' C 0.7516(8) 0.1830(8) 0.6130(7) 0.036(4) Uiso 0.331(17) 1 d PG A 2 H76' H 0.7354 0.2084 0.6458 0.043 Uiso 0.331(17) 1 calc PR A 2 C77' C 0.8359(6) 0.2078(7) 0.5500(6) 0.042(4) Uiso 0.331(17) 1 d PG A 2 H77' H 0.8773 0.2501 0.5398 0.050 Uiso 0.331(17) 1 calc PR A 2 C78' C 0.8595(6) 0.1706(8) 0.5019(6) 0.038(4) Uiso 0.331(17) 1 d PG A 2 H78' H 0.9171 0.1876 0.4589 0.046 Uiso 0.331(17) 1 calc PR A 2 C79' C 0.7989(8) 0.1087(8) 0.5169(6) 0.031(4) Uiso 0.331(17) 1 d PG A 2 H79' H 0.8151 0.0833 0.4841 0.037 Uiso 0.331(17) 1 calc PR A 2 C80' C 0.7146(8) 0.0839(8) 0.5799(7) 0.033(4) Uiso 0.331(17) 1 d PG A 2 H80' H 0.6732 0.0416 0.5901 0.040 Uiso 0.331(17) 1 calc PR A 2 C81 C 0.8510(2) 0.6814(2) 0.3731(2) 0.0309(9) Uani 1 1 d . . . C82 C 0.8006(3) 0.6932(3) 0.4368(3) 0.0443(11) Uani 1 1 d . . . H82 H 0.7398 0.6647 0.4690 0.053 Uiso 1 1 calc R . . C83 C 0.8356(3) 0.7452(3) 0.4553(3) 0.0538(12) Uani 1 1 d . . . H83 H 0.7988 0.7531 0.4990 0.065 Uiso 1 1 calc R . . C84 C 0.9223(4) 0.7847(3) 0.4110(4) 0.0658(15) Uani 1 1 d . . . H84 H 0.9470 0.8204 0.4235 0.079 Uiso 1 1 calc R . . C85 C 0.9756(4) 0.7732(4) 0.3471(4) 0.096(2) Uani 1 1 d U . . H85 H 1.0370 0.8008 0.3159 0.115 Uiso 1 1 calc R . . C86 C 0.9390(3) 0.7212(3) 0.3287(4) 0.0732(17) Uani 1 1 d . . . H86 H 0.9755 0.7132 0.2849 0.088 Uiso 1 1 calc R . . C87 C 0.7419(2) 0.5320(2) 0.4438(2) 0.0274(8) Uani 1 1 d . . . C88 C 0.7874(3) 0.4660(2) 0.4845(3) 0.0427(10) Uani 1 1 d . . . H88A H 0.8523 0.4610 0.4603 0.051 Uiso 1 1 calc R . . C89 C 0.7400(3) 0.4079(3) 0.5592(3) 0.0536(12) Uani 1 1 d . . . H89A H 0.7719 0.3624 0.5860 0.064 Uiso 1 1 calc R . . C90 C 0.6463(3) 0.4146(3) 0.5963(3) 0.0462(11) Uani 1 1 d . . . H90A H 0.6141 0.3742 0.6484 0.055 Uiso 1 1 calc R . . C91 C 0.5999(3) 0.4797(3) 0.5573(3) 0.0421(10) Uani 1 1 d . . . H91A H 0.5357 0.4853 0.5826 0.051 Uiso 1 1 calc R . . C92 C 0.6474(3) 0.5374(2) 0.4806(2) 0.0358(9) Uani 1 1 d . . . H92A H 0.6144 0.5815 0.4529 0.043 Uiso 1 1 calc R . . C100 C 1.0256(3) 0.0371(3) 0.3224(3) 0.0540(12) Uani 1 1 d . . . H100 H 0.9875 0.0704 0.2854 0.065 Uiso 1 1 calc R . . Cl1 Cl 1.09551(10) -0.02133(9) 0.28361(10) 0.0774(4) Uani 1 1 d . . . Cl2 Cl 1.09866(12) 0.10047(12) 0.32943(14) 0.1126(7) Uani 1 1 d . . . Cl3 Cl 0.94638(14) -0.02149(10) 0.41642(12) 0.1145(6) Uani 1 1 d U . . C110 C 0.2937(4) 0.8215(3) 0.1762(3) 0.0679(15) Uani 1 1 d . . . H110 H 0.3181 0.8366 0.2102 0.082 Uiso 1 1 calc R . . Cl4 Cl 0.39167(10) 0.82037(11) 0.10043(9) 0.0859(5) Uani 1 1 d . . . Cl5 Cl 0.23244(13) 0.72715(10) 0.23620(10) 0.0919(5) Uani 1 1 d . . . Cl6 Cl 0.21627(13) 0.89138(11) 0.13520(12) 0.1089(6) Uani 1 1 d . . . C120 C 0.0526(9) 0.4863(5) 0.3356(5) 0.050(4) Uiso 0.399(4) 1 d PDU B 1 H120 H -0.0088 0.5130 0.3355 0.060 Uiso 0.399(4) 1 calc PR B 1 Cl7 Cl 0.1122(8) 0.4986(9) 0.2401(6) 0.064(2) Uani 0.399(4) 1 d PDU B 1 Cl8 Cl 0.1260(4) 0.5265(4) 0.3661(4) 0.0839(16) Uani 0.399(4) 1 d PDU B 1 Cl9 Cl 0.0290(5) 0.3836(3) 0.4030(5) 0.120(3) Uani 0.399(4) 1 d PDU B 1 C130 C 0.0258(9) 0.4547(8) 0.3495(6) 0.044(4) Uiso 0.341(10) 1 d PDU C 2 H130 H -0.0237 0.4946 0.3439 0.053 Uiso 0.341(10) 1 calc PR C 2 Cl10 Cl 0.1147(13) 0.4929(12) 0.2585(8) 0.090(4) Uani 0.341(10) 1 d PDU C 2 Cl11 Cl 0.0699(7) 0.4471(10) 0.4252(7) 0.113(3) Uani 0.341(10) 1 d PDU C 2 Cl12 Cl -0.0314(6) 0.3671(4) 0.3727(6) 0.095(3) Uani 0.341(10) 1 d PDU C 2 C140 C 0.0394(17) 0.4781(11) 0.3354(10) 0.074(9) Uiso 0.260(10) 1 d PDU D 3 H140 H -0.0178 0.5103 0.3329 0.088 Uiso 0.260(10) 1 calc PR D 3 Cl13 Cl 0.111(2) 0.5070(16) 0.2390(11) 0.098(6) Uani 0.260(10) 1 d PDU D 3 Cl14 Cl 0.0971(9) 0.4921(9) 0.3941(9) 0.083(3) Uani 0.260(10) 1 d PDU D 3 Cl15 Cl -0.0005(11) 0.3776(8) 0.3857(7) 0.075(3) Uani 0.260(10) 1 d PDU D 3 C150 C 0.4615(14) -0.0315(11) 0.5472(13) 0.082(9) Uani 0.50 1 d P E -1 H150 H 0.4640 -0.0784 0.5370 0.099 Uiso 0.50 1 calc PR E -1 Cl16 Cl 0.46912(18) -0.07690(16) 0.63121(16) 0.0627(7) Uani 0.50 1 d P E -1 Cl17 Cl 0.3406(2) -0.00460(16) 0.53570(17) 0.0728(8) Uani 0.50 1 d P E -1 Cl18 Cl 0.5464(5) 0.0259(4) 0.4648(5) 0.120(3) Uani 0.50 1 d P E -1 C160 C -0.1839(10) -0.0349(11) 1.0869(11) 0.058(5) Uiso 0.275(6) 1 d PDU F -1 H16H H -0.2276 -0.0365 1.1357 0.086 Uiso 0.275(6) 1 calc PR F -1 H16I H -0.1969 -0.0833 1.0843 0.086 Uiso 0.275(6) 1 calc PR F -1 H16J H -0.1937 0.0121 1.0401 0.086 Uiso 0.275(6) 1 calc PR F -1 C161 C -0.0720(11) -0.0302(18) 1.0877(14) 0.088(6) Uiso 0.275(6) 1 d PDU F -1 H16B H -0.0651 -0.0768 1.1369 0.106 Uiso 0.275(6) 1 calc PR F -1 H16C H -0.0615 0.0181 1.0922 0.106 Uiso 0.275(6) 1 calc PR F -1 C162 C 0.0153(13) -0.0279(15) 1.0114(10) 0.091(6) Uiso 0.275(6) 1 d PDU F -1 H16D H 0.0766 -0.0189 1.0191 0.109 Uiso 0.275(6) 1 calc PR F -1 H16E H 0.0146 -0.0819 1.0158 0.109 Uiso 0.275(6) 1 calc PR F -1 C163 C 0.0190(19) 0.0364(15) 0.9185(10) 0.098(6) Uiso 0.275(6) 1 d PDU F -1 H16F H 0.0504 0.0876 0.9050 0.118 Uiso 0.275(6) 1 calc PR F -1 H16G H -0.0477 0.0460 0.9161 0.118 Uiso 0.275(6) 1 calc PR F -1 C164 C 0.0759(16) 0.0101(15) 0.8486(12) 0.091(6) Uiso 0.275(6) 1 d PDU F -1 H16K H 0.0723 0.0517 0.7963 0.136 Uiso 0.275(6) 1 calc PR F -1 H16L H 0.0455 -0.0404 0.8607 0.136 Uiso 0.275(6) 1 calc PR F -1 H16M H 0.1432 0.0034 0.8478 0.136 Uiso 0.275(6) 1 calc PR F -1 C170 C -0.0942(16) -0.0626(15) 1.1421(13) 0.060(6) Uiso 0.225(6) 1 d PDU F -2 H17H H -0.1582 -0.0639 1.1768 0.090 Uiso 0.225(6) 1 calc PR F -2 H17I H -0.0460 -0.0431 1.1561 0.090 Uiso 0.225(6) 1 calc PR F -2 H17J H -0.0812 -0.1165 1.1492 0.090 Uiso 0.225(6) 1 calc PR F -2 C171 C -0.0897(16) -0.0043(17) 1.0507(12) 0.105(7) Uiso 0.225(6) 1 d PDU F -2 H17B H -0.1096 0.0479 1.0469 0.126 Uiso 0.225(6) 1 calc PR F -2 H17C H -0.1391 -0.0259 1.0387 0.126 Uiso 0.225(6) 1 calc PR F -2 C172 C 0.010(2) 0.013(2) 0.9796(12) 0.100(7) Uiso 0.225(6) 1 d PDU F -2 H17D H 0.0144 -0.0300 0.9640 0.120 Uiso 0.225(6) 1 calc PR F -2 H17E H 0.0644 0.0102 1.0005 0.120 Uiso 0.225(6) 1 calc PR F -2 C173 C 0.0197(18) 0.1025(14) 0.8970(12) 0.091(6) Uiso 0.225(6) 1 d PDU F -2 H17F H -0.0446 0.1178 0.8904 0.110 Uiso 0.225(6) 1 calc PR F -2 H17G H 0.0489 0.1441 0.9026 0.110 Uiso 0.225(6) 1 calc PR F -2 C174 C 0.088(2) 0.0945(19) 0.8179(14) 0.110(9) Uiso 0.225(6) 1 d PDU F -2 H17K H 0.0951 0.1458 0.7697 0.164 Uiso 0.225(6) 1 calc PR F -2 H17L H 0.0588 0.0535 0.8126 0.164 Uiso 0.225(6) 1 calc PR F -2 H17M H 0.1519 0.0796 0.8249 0.164 Uiso 0.225(6) 1 calc PR F -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 Tl 0.02910(8) 0.04139(10) 0.02239(8) -0.00850(7) -0.00709(6) 0.00275(6) B 0.029(2) 0.026(2) 0.017(2) -0.0087(19) -0.0088(17) 0.0045(17) P1 0.0287(5) 0.0335(6) 0.0272(5) -0.0185(5) -0.0131(4) 0.0083(4) O1 0.0306(13) 0.0567(18) 0.0421(17) -0.0365(15) -0.0170(12) 0.0125(13) P2 0.0339(5) 0.0385(6) 0.0290(6) -0.0188(5) -0.0113(4) 0.0080(4) O2 0.0560(18) 0.060(2) 0.0355(18) -0.0214(16) -0.0195(15) 0.0236(16) P3 0.0409(6) 0.0246(5) 0.0296(6) -0.0104(5) -0.0162(5) 0.0075(4) O3 0.081(2) 0.0400(18) 0.056(2) -0.0305(16) -0.0466(18) 0.0238(16) P4 0.0246(5) 0.0276(5) 0.0268(5) -0.0146(5) -0.0060(4) 0.0018(4) O4 0.0255(13) 0.0389(16) 0.0329(16) -0.0201(13) -0.0048(11) 0.0044(11) N1 0.0258(15) 0.0326(17) 0.0152(16) -0.0104(14) -0.0074(12) -0.0006(13) N2 0.0243(15) 0.0244(16) 0.0166(16) -0.0092(13) -0.0046(12) -0.0001(12) N3 0.0271(15) 0.0261(17) 0.0180(16) -0.0113(14) -0.0040(12) -0.0027(12) N4 0.0325(16) 0.0219(16) 0.0154(15) -0.0069(13) -0.0066(13) 0.0000(13) N5 0.0365(17) 0.0236(17) 0.0212(17) -0.0076(14) -0.0069(14) -0.0081(13) N6 0.0261(15) 0.0236(16) 0.0179(16) -0.0087(14) -0.0057(12) -0.0006(12) N7 0.0252(15) 0.0213(16) 0.0217(16) -0.0112(14) -0.0065(12) 0.0039(12) N8 0.0267(15) 0.0209(16) 0.0195(16) -0.0109(13) -0.0086(12) 0.0032(12) C9 0.032(2) 0.040(2) 0.020(2) -0.0143(18) -0.0033(16) -0.0021(17) C10 0.0262(19) 0.047(3) 0.033(2) -0.023(2) -0.0060(17) 0.0036(18) C11 0.0258(18) 0.031(2) 0.027(2) -0.0170(18) -0.0069(16) -0.0006(15) C12 0.0220(17) 0.030(2) 0.023(2) -0.0125(17) -0.0064(15) 0.0004(15) C13 0.0214(17) 0.030(2) 0.021(2) -0.0114(17) -0.0042(15) -0.0002(15) C14 0.038(2) 0.032(2) 0.022(2) -0.0100(18) -0.0099(17) 0.0001(17) C15 0.048(2) 0.027(2) 0.028(2) -0.0093(19) -0.0172(19) 0.0062(18) C16 0.050(2) 0.021(2) 0.045(3) -0.015(2) -0.012(2) 0.0022(18) C17 0.040(2) 0.031(2) 0.030(2) -0.0146(19) -0.0110(18) 0.0016(17) C18 0.061(3) 0.034(2) 0.021(2) -0.0133(19) -0.0181(19) 0.019(2) C19 0.060(3) 0.027(2) 0.024(2) -0.0108(18) -0.0135(19) 0.0168(19) C20 0.0328(19) 0.0198(19) 0.021(2) -0.0105(16) -0.0048(15) -0.0013(15) C21 0.038(2) 0.0119(17) 0.0206(19) -0.0075(16) -0.0056(16) -0.0031(14) C22 0.0331(19) 0.0194(19) 0.023(2) -0.0081(16) -0.0068(16) 0.0010(15) C23 0.037(2) 0.032(2) 0.024(2) -0.0146(18) -0.0029(17) 0.0030(17) C24 0.048(2) 0.028(2) 0.030(2) -0.0171(19) -0.0134(19) 0.0018(18) C25 0.041(2) 0.030(2) 0.040(2) -0.019(2) -0.0175(19) 0.0026(17) C26 0.033(2) 0.027(2) 0.041(2) -0.019(2) -0.0085(18) 0.0042(16) C27 0.0340(19) 0.0221(19) 0.027(2) -0.0149(18) -0.0130(16) 0.0035(15) C28 0.050(2) 0.027(2) 0.024(2) -0.0134(18) -0.0186(18) 0.0056(18) C29 0.0252(17) 0.028(2) 0.0152(18) -0.0108(16) -0.0066(14) 0.0050(15) C30 0.035(2) 0.028(2) 0.0165(19) -0.0081(17) -0.0062(16) 0.0041(16) C31 0.039(2) 0.022(2) 0.029(2) -0.0117(18) -0.0097(17) 0.0042(16) C32 0.043(2) 0.037(2) 0.038(3) -0.001(2) -0.016(2) -0.0012(19) C33 0.049(3) 0.039(3) 0.052(3) 0.007(2) -0.007(2) -0.020(2) C34 0.043(3) 0.052(3) 0.054(3) -0.003(3) -0.018(2) -0.014(2) C35 0.039(2) 0.041(3) 0.037(3) -0.004(2) -0.013(2) -0.0046(19) C36 0.0263(19) 0.029(2) 0.030(2) -0.0164(18) -0.0065(16) 0.0041(16) C37 0.0254(19) 0.036(2) 0.043(3) -0.023(2) -0.0038(17) 0.0008(16) C38 0.0244(17) 0.026(2) 0.0176(18) -0.0089(16) -0.0072(14) 0.0028(15) C39 0.0249(17) 0.0236(19) 0.0186(19) -0.0103(16) -0.0007(14) -0.0002(14) C40 0.0239(17) 0.0236(19) 0.0214(19) -0.0106(16) -0.0017(15) 0.0014(15) C41 0.041(2) 0.026(2) 0.028(2) -0.0169(18) -0.0079(17) 0.0026(17) C42 0.048(2) 0.024(2) 0.033(2) -0.0149(19) -0.0109(19) 0.0129(18) C43 0.035(2) 0.042(3) 0.031(2) -0.015(2) -0.0124(18) 0.0163(19) C44 0.0312(19) 0.032(2) 0.027(2) -0.0143(18) -0.0102(17) 0.0060(16) C45 0.043(2) 0.028(2) 0.033(2) -0.0215(19) -0.0139(18) 0.0079(17) C46 0.077(3) 0.057(3) 0.035(3) -0.025(3) -0.025(2) 0.035(3) C47 0.129(5) 0.046(3) 0.038(3) -0.015(3) -0.022(3) 0.038(3) C48 0.121(5) 0.035(3) 0.036(3) -0.014(3) -0.003(3) -0.010(3) C49 0.063(3) 0.057(3) 0.051(3) -0.033(3) 0.002(3) -0.019(3) C50 0.045(2) 0.040(3) 0.036(3) -0.019(2) -0.011(2) -0.0014(19) C51 0.033(2) 0.024(2) 0.028(2) -0.0135(17) -0.0134(17) 0.0036(16) C52 0.035(2) 0.050(3) 0.040(3) -0.024(2) -0.0149(19) 0.0081(19) C53 0.041(2) 0.043(3) 0.050(3) -0.017(2) -0.027(2) -0.0003(19) C54 0.059(3) 0.039(3) 0.035(3) -0.018(2) -0.023(2) -0.001(2) C55 0.054(3) 0.041(3) 0.034(2) -0.023(2) -0.014(2) -0.001(2) C56 0.036(2) 0.032(2) 0.032(2) -0.0151(19) -0.0139(18) 0.0013(17) C57 0.032(2) 0.042(2) 0.033(2) -0.022(2) -0.0063(18) 0.0003(18) C58 0.047(2) 0.044(3) 0.043(3) -0.026(2) -0.010(2) -0.001(2) C59 0.056(3) 0.058(3) 0.037(3) -0.024(3) 0.006(2) -0.019(2) C60 0.050(3) 0.085(4) 0.055(4) -0.048(3) 0.009(2) -0.012(3) C61 0.046(3) 0.078(4) 0.074(4) -0.052(4) -0.009(3) 0.013(3) C62 0.044(2) 0.058(3) 0.040(3) -0.026(2) -0.006(2) 0.005(2) C63 0.0250(19) 0.049(3) 0.045(3) -0.033(2) -0.0053(18) -0.0012(18) C64 0.047(3) 0.086(4) 0.082(4) -0.064(4) -0.023(3) 0.012(3) C65 0.053(3) 0.109(5) 0.110(5) -0.084(5) -0.021(3) 0.007(3) C66 0.041(3) 0.085(4) 0.113(5) -0.083(4) 0.017(3) -0.029(3) C67 0.050(3) 0.049(3) 0.075(4) -0.033(3) 0.011(3) -0.008(2) C68 0.037(2) 0.039(3) 0.052(3) -0.025(2) 0.000(2) -0.0088(19) C69 0.044(2) 0.031(2) 0.038(3) -0.006(2) -0.021(2) 0.0047(19) C70 0.070(3) 0.034(3) 0.065(4) -0.010(3) -0.029(3) 0.013(2) C71 0.094(4) 0.035(3) 0.093(5) -0.001(3) -0.044(4) 0.013(3) C72 0.091(4) 0.038(3) 0.107(6) 0.005(4) -0.069(4) -0.007(3) C73 0.116(5) 0.087(5) 0.053(4) 0.002(4) -0.050(4) -0.026(4) C74 0.092(4) 0.047(3) 0.044(3) -0.008(3) -0.030(3) -0.002(3) C75 0.038(4) 0.028(4) 0.048(5) -0.002(4) -0.019(3) 0.009(3) C76 0.051(5) 0.053(6) 0.065(6) -0.012(5) -0.020(4) 0.003(4) C77 0.043(5) 0.096(9) 0.064(7) 0.010(7) -0.006(5) -0.022(5) C78 0.038(5) 0.104(11) 0.066(7) -0.006(6) -0.003(5) 0.025(6) C79 0.071(6) 0.075(7) 0.065(6) -0.030(5) -0.009(5) 0.034(6) C80 0.058(5) 0.048(5) 0.047(5) -0.022(4) -0.001(4) 0.015(4) C81 0.0294(19) 0.031(2) 0.035(2) -0.0181(19) -0.0086(17) -0.0019(16) C82 0.039(2) 0.055(3) 0.043(3) -0.030(2) -0.003(2) -0.010(2) C83 0.059(3) 0.061(3) 0.062(3) -0.045(3) -0.018(3) -0.004(2) C84 0.068(3) 0.064(4) 0.099(5) -0.062(4) -0.028(3) -0.004(3) C85 0.073(3) 0.103(5) 0.123(5) -0.080(4) 0.017(3) -0.051(3) C86 0.059(3) 0.084(4) 0.087(4) -0.064(4) 0.016(3) -0.034(3) C87 0.0304(19) 0.027(2) 0.030(2) -0.0160(18) -0.0100(16) -0.0009(16) C88 0.043(2) 0.040(3) 0.038(3) -0.014(2) -0.010(2) 0.007(2) C89 0.072(3) 0.044(3) 0.032(3) -0.007(2) -0.017(2) 0.006(2) C90 0.057(3) 0.048(3) 0.025(2) -0.012(2) -0.004(2) -0.018(2) C91 0.038(2) 0.052(3) 0.039(3) -0.025(2) -0.005(2) -0.011(2) C92 0.030(2) 0.042(2) 0.034(2) -0.018(2) -0.0066(18) -0.0010(17) C100 0.058(3) 0.043(3) 0.068(4) -0.024(3) -0.034(3) 0.009(2) Cl1 0.0791(9) 0.0623(9) 0.0906(11) -0.0395(8) -0.0211(8) 0.0166(7) Cl2 0.0975(12) 0.1148(15) 0.180(2) -0.0984(15) -0.0653(13) 0.0088(11) Cl3 0.1324(15) 0.0697(11) 0.0981(14) -0.0347(10) 0.0177(11) 0.0075(10) C110 0.077(4) 0.092(4) 0.067(4) -0.054(4) -0.042(3) 0.026(3) Cl4 0.0696(9) 0.1457(15) 0.0836(11) -0.0796(12) -0.0352(8) 0.0121(9) Cl5 0.1239(13) 0.0874(12) 0.0738(11) -0.0461(10) -0.0281(10) 0.0104(10) Cl6 0.1007(12) 0.1058(14) 0.1309(17) -0.0516(13) -0.0641(12) 0.0439(11) Cl7 0.032(4) 0.102(6) 0.091(5) -0.077(5) -0.005(4) -0.006(4) Cl8 0.075(3) 0.110(5) 0.105(4) -0.072(4) -0.047(3) 0.025(3) Cl9 0.085(4) 0.064(3) 0.147(6) -0.012(3) -0.018(4) 0.025(3) Cl10 0.062(6) 0.092(7) 0.107(7) -0.064(6) 0.018(5) 0.006(5) Cl11 0.088(4) 0.169(9) 0.103(5) -0.069(6) -0.059(4) 0.056(5) Cl12 0.063(4) 0.066(3) 0.113(5) -0.023(3) 0.002(3) -0.001(3) Cl13 0.065(8) 0.108(10) 0.097(10) -0.042(7) 0.001(8) -0.009(8) Cl14 0.082(4) 0.083(4) 0.083(4) -0.0391(18) -0.0251(14) 0.0069(11) Cl15 0.075(3) 0.075(3) 0.075(3) -0.0366(17) -0.0199(12) 0.0067(11) C150 0.077(12) 0.065(11) 0.051(11) -0.004(8) 0.002(8) 0.062(10) Cl16 0.0642(15) 0.0600(16) 0.0634(17) -0.0239(14) -0.0242(13) -0.0054(12) Cl17 0.100(2) 0.0560(16) 0.0621(18) -0.0167(14) -0.0424(16) 0.0049(15) Cl18 0.132(5) 0.137(5) 0.060(3) -0.036(4) 0.013(3) -0.061(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tl N1 2.536(3) . ? Tl O1 2.541(2) . ? Tl N3 2.587(3) . ? B N6 1.513(5) . ? B N8 1.524(5) . ? B N2 1.547(4) . ? B N4 1.561(5) . ? P1 O1 1.491(2) . ? P1 C45 1.788(4) . ? P1 C13 1.801(4) . ? P1 C51 1.816(3) . ? P2 O2 1.480(3) . ? P2 C22 1.801(3) . ? P2 C63 1.803(4) . ? P2 C57 1.811(4) . ? P3 O3 1.481(3) . ? P3 C75' 1.763(7) . ? P3 C31 1.801(4) . ? P3 C69 1.802(4) . ? P3 C75 1.831(4) . ? P4 O4 1.484(2) . ? P4 C40 1.801(3) . ? P4 C87 1.804(4) . ? P4 C81 1.806(4) . ? N1 C11 1.337(4) . ? N1 N2 1.358(4) . ? N2 C9 1.338(4) . ? N3 C20 1.335(4) . ? N3 N4 1.366(4) . ? N4 C18 1.337(4) . ? N5 C29 1.337(4) . ? N5 N6 1.362(4) . ? N6 C27 1.354(4) . ? N7 C38 1.338(4) . ? N7 N8 1.355(4) . ? N8 C36 1.356(4) . ? C9 C10 1.374(5) . ? C10 C11 1.384(5) . ? C11 C12 1.491(5) . ? C12 C17 1.391(5) . ? C12 C13 1.405(5) . ? C13 C14 1.392(5) . ? C14 C15 1.377(5) . ? C15 C16 1.365(5) . ? C16 C17 1.381(5) . ? C18 C19 1.368(5) . ? C19 C20 1.408(5) . ? C20 C21 1.472(5) . ? C21 C26 1.402(5) . ? C21 C22 1.406(5) . ? C22 C23 1.405(5) . ? C23 C24 1.381(5) . ? C24 C25 1.374(5) . ? C25 C26 1.380(5) . ? C27 C28 1.372(5) . ? C28 C29 1.389(5) . ? C29 C30 1.479(5) . ? C30 C35 1.393(5) . ? C30 C31 1.404(5) . ? C31 C32 1.395(5) . ? C32 C33 1.388(6) . ? C33 C34 1.379(6) . ? C34 C35 1.381(6) . ? C36 C37 1.349(5) . ? C37 C38 1.403(5) . ? C38 C39 1.482(5) . ? C39 C44 1.396(5) . ? C39 C40 1.423(5) . ? C40 C41 1.393(5) . ? C41 C42 1.373(5) . ? C42 C43 1.369(5) . ? C43 C44 1.379(5) . ? C45 C50 1.380(5) . ? C45 C46 1.399(5) . ? C46 C47 1.387(7) . ? C47 C48 1.342(8) . ? C48 C49 1.382(7) . ? C49 C50 1.376(6) . ? C51 C56 1.379(5) . ? C51 C52 1.381(5) . ? C52 C53 1.384(5) . ? C53 C54 1.367(6) . ? C54 C55 1.373(5) . ? C55 C56 1.378(5) . ? C57 C58 1.378(6) . ? C57 C62 1.381(5) . ? C58 C59 1.380(6) . ? C59 C60 1.366(7) . ? C60 C61 1.375(7) . ? C61 C62 1.392(6) . ? C63 C64 1.387(6) . ? C63 C68 1.392(6) . ? C64 C65 1.354(7) . ? C65 C66 1.349(8) . ? C66 C67 1.415(7) . ? C67 C68 1.404(6) . ? C69 C74 1.365(6) . ? C69 C70 1.393(6) . ? C70 C71 1.366(7) . ? C71 C72 1.325(9) . ? C72 C73 1.373(9) . ? C73 C74 1.414(7) . ? C75 C76 1.3900 . ? C75 C80 1.3900 . ? C76 C77 1.3900 . ? C77 C78 1.3900 . ? C78 C79 1.3900 . ? C79 C80 1.3900 . ? C75' C76' 1.3900 . ? C75' C80' 1.3900 . ? C76' C77' 1.3900 . ? C77' C78' 1.3900 . ? C78' C79' 1.3900 . ? C79' C80' 1.3900 . ? C81 C86 1.362(6) . ? C81 C82 1.373(5) . ? C82 C83 1.378(5) . ? C83 C84 1.346(7) . ? C84 C85 1.385(7) . ? C85 C86 1.388(6) . ? C87 C92 1.383(5) . ? C87 C88 1.383(5) . ? C88 C89 1.368(6) . ? C89 C90 1.381(6) . ? C90 C91 1.371(6) . ? C91 C92 1.388(6) . ? C100 Cl3 1.741(5) . ? C100 Cl2 1.744(5) . ? C100 Cl1 1.748(5) . ? C110 Cl6 1.735(5) . ? C110 Cl5 1.746(6) . ? C110 Cl4 1.754(5) . ? C120 Cl8 1.742(7) . ? C120 Cl7 1.745(7) . ? C120 Cl9 1.760(7) . ? C130 Cl12 1.718(9) . ? C130 Cl10 1.735(9) . ? C130 Cl11 1.741(8) . ? C140 Cl13 1.727(10) . ? C140 Cl14 1.739(10) . ? C140 Cl15 1.740(10) . ? C150 Cl16 1.51(2) . ? C150 Cl18 1.654(16) . ? C150 Cl17 1.852(18) . ? C160 C161 1.649(16) . ? C161 C162 1.655(15) . ? C162 C163 1.650(16) . ? C163 C164 1.667(17) . ? C170 C171 1.603(16) . ? C171 C172 1.626(19) . ? C172 C173 1.701(19) . ? C173 C174 1.664(17) . ? 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 N1 Tl O1 74.78(8) . . ? N1 Tl N3 75.72(9) . . ? O1 Tl N3 83.30(9) . . ? N6 B N8 111.1(3) . . ? N6 B N2 109.1(3) . . ? N8 B N2 107.3(3) . . ? N6 B N4 107.7(3) . . ? N8 B N4 108.5(3) . . ? N2 B N4 113.2(3) . . ? O1 P1 C45 112.68(17) . . ? O1 P1 C13 113.28(16) . . ? C45 P1 C13 106.45(16) . . ? O1 P1 C51 108.50(15) . . ? C45 P1 C51 108.93(17) . . ? C13 P1 C51 106.77(15) . . ? P1 O1 Tl 131.63(13) . . ? O2 P2 C22 113.99(18) . . ? O2 P2 C63 112.93(18) . . ? C22 P2 C63 107.15(17) . . ? O2 P2 C57 111.06(17) . . ? C22 P2 C57 106.78(17) . . ? C63 P2 C57 104.28(18) . . ? O3 P3 C75' 105.5(4) . . ? O3 P3 C31 113.39(16) . . ? C75' P3 C31 114.5(5) . . ? O3 P3 C69 110.01(18) . . ? C75' P3 C69 107.0(6) . . ? C31 P3 C69 106.31(18) . . ? O3 P3 C75 115.5(3) . . ? C31 P3 C75 106.1(3) . . ? C69 P3 C75 104.8(3) . . ? O4 P4 C40 114.38(15) . . ? O4 P4 C87 114.95(16) . . ? C40 P4 C87 105.13(16) . . ? O4 P4 C81 109.18(15) . . ? C40 P4 C81 107.56(16) . . ? C87 P4 C81 105.00(17) . . ? C11 N1 N2 106.4(3) . . ? C11 N1 Tl 132.7(2) . . ? N2 N1 Tl 120.92(19) . . ? C9 N2 N1 109.6(3) . . ? C9 N2 B 126.9(3) . . ? N1 N2 B 121.2(3) . . ? C20 N3 N4 106.5(3) . . ? C20 N3 Tl 126.3(2) . . ? N4 N3 Tl 116.33(19) . . ? C18 N4 N3 110.0(3) . . ? C18 N4 B 126.7(3) . . ? N3 N4 B 122.9(3) . . ? C29 N5 N6 105.3(3) . . ? C27 N6 N5 110.6(3) . . ? C27 N6 B 128.6(3) . . ? N5 N6 B 120.5(3) . . ? C38 N7 N8 106.0(2) . . ? N7 N8 C36 109.9(3) . . ? N7 N8 B 120.1(3) . . ? C36 N8 B 129.4(3) . . ? N2 C9 C10 108.8(3) . . ? C9 C10 C11 104.7(3) . . ? N1 C11 C10 110.6(3) . . ? N1 C11 C12 121.4(3) . . ? C10 C11 C12 128.1(3) . . ? C17 C12 C13 119.3(3) . . ? C17 C12 C11 118.0(3) . . ? C13 C12 C11 122.7(3) . . ? C14 C13 C12 118.5(3) . . ? C14 C13 P1 120.5(3) . . ? C12 C13 P1 121.0(3) . . ? C15 C14 C13 121.6(3) . . ? C16 C15 C14 119.3(3) . . ? C15 C16 C17 120.9(4) . . ? C16 C17 C12 120.3(3) . . ? N4 C18 C19 108.7(3) . . ? C18 C19 C20 105.0(3) . . ? N3 C20 C19 109.8(3) . . ? N3 C20 C21 120.9(3) . . ? C19 C20 C21 128.9(3) . . ? C26 C21 C22 118.2(3) . . ? C26 C21 C20 117.3(3) . . ? C22 C21 C20 124.3(3) . . ? C23 C22 C21 118.8(3) . . ? C23 C22 P2 117.7(3) . . ? C21 C22 P2 123.4(3) . . ? C24 C23 C22 121.4(3) . . ? C25 C24 C23 119.8(3) . . ? C24 C25 C26 119.9(3) . . ? C25 C26 C21 121.7(3) . . ? N6 C27 C28 107.8(3) . . ? C27 C28 C29 105.0(3) . . ? N5 C29 C28 111.3(3) . . ? N5 C29 C30 118.3(3) . . ? C28 C29 C30 130.2(3) . . ? C35 C30 C31 119.0(4) . . ? C35 C30 C29 117.0(3) . . ? C31 C30 C29 124.0(3) . . ? C32 C31 C30 118.8(3) . . ? C32 C31 P3 117.7(3) . . ? C30 C31 P3 123.3(3) . . ? C33 C32 C31 121.2(4) . . ? C34 C33 C32 119.8(4) . . ? C33 C34 C35 119.7(4) . . ? C34 C35 C30 121.5(4) . . ? C37 C36 N8 108.6(3) . . ? C36 C37 C38 105.2(3) . . ? N7 C38 C37 110.2(3) . . ? N7 C38 C39 118.3(3) . . ? C37 C38 C39 131.1(3) . . ? C44 C39 C40 117.9(3) . . ? C44 C39 C38 118.0(3) . . ? C40 C39 C38 124.1(3) . . ? C41 C40 C39 118.7(3) . . ? C41 C40 P4 120.0(3) . . ? C39 C40 P4 121.1(2) . . ? C42 C41 C40 121.9(3) . . ? C43 C42 C41 119.5(3) . . ? C42 C43 C44 120.4(3) . . ? C43 C44 C39 121.6(3) . . ? C50 C45 C46 118.8(4) . . ? C50 C45 P1 122.7(3) . . ? C46 C45 P1 118.5(3) . . ? C47 C46 C45 119.5(5) . . ? C48 C47 C46 121.3(5) . . ? C47 C48 C49 119.5(5) . . ? C50 C49 C48 120.8(5) . . ? C49 C50 C45 120.1(4) . . ? C56 C51 C52 118.8(3) . . ? C56 C51 P1 116.3(3) . . ? C52 C51 P1 124.8(3) . . ? C51 C52 C53 120.0(4) . . ? C54 C53 C52 120.7(4) . . ? C53 C54 C55 119.6(4) . . ? C54 C55 C56 120.1(4) . . ? C55 C56 C51 120.8(3) . . ? C58 C57 C62 118.8(4) . . ? C58 C57 P2 123.9(3) . . ? C62 C57 P2 117.2(3) . . ? C57 C58 C59 121.4(4) . . ? C60 C59 C58 118.9(5) . . ? C59 C60 C61 121.3(4) . . ? C60 C61 C62 119.2(5) . . ? C57 C62 C61 120.3(4) . . ? C64 C63 C68 120.0(4) . . ? C64 C63 P2 117.3(4) . . ? C68 C63 P2 122.6(3) . . ? C65 C64 C63 120.9(5) . . ? C66 C65 C64 119.8(5) . . ? C65 C66 C67 122.5(5) . . ? C68 C67 C66 117.0(5) . . ? C63 C68 C67 119.8(4) . . ? C74 C69 C70 118.1(4) . . ? C74 C69 P3 117.7(3) . . ? C70 C69 P3 124.1(3) . . ? C71 C70 C69 121.6(5) . . ? C72 C71 C70 120.0(6) . . ? C71 C72 C73 121.5(5) . . ? C72 C73 C74 119.0(6) . . ? C69 C74 C73 119.8(5) . . ? C76 C75 C80 120.0 . . ? C76 C75 P3 117.7(3) . . ? C80 C75 P3 122.1(3) . . ? C75 C76 C77 120.0 . . ? C78 C77 C76 120.0 . . ? C77 C78 C79 120.0 . . ? C80 C79 C78 120.0 . . ? C79 C80 C75 120.0 . . ? C76' C75' C80' 120.0 . . ? C76' C75' P3 115.9(6) . . ? C80' C75' P3 124.1(6) . . ? C75' C76' C77' 120.0 . . ? C78' C77' C76' 120.0 . . ? C79' C78' C77' 120.0 . . ? C78' C79' C80' 120.0 . . ? C79' C80' C75' 120.0 . . ? C86 C81 C82 118.4(4) . . ? C86 C81 P4 118.2(3) . . ? C82 C81 P4 123.2(3) . . ? C81 C82 C83 121.8(4) . . ? C84 C83 C82 119.6(4) . . ? C83 C84 C85 120.0(4) . . ? C84 C85 C86 119.8(5) . . ? C81 C86 C85 120.4(5) . . ? C92 C87 C88 118.2(4) . . ? C92 C87 P4 122.4(3) . . ? C88 C87 P4 119.2(3) . . ? C89 C88 C87 120.7(4) . . ? C88 C89 C90 120.7(4) . . ? C91 C90 C89 119.6(4) . . ? C90 C91 C92 119.4(4) . . ? C87 C92 C91 121.3(4) . . ? Cl3 C100 Cl2 109.1(3) . . ? Cl3 C100 Cl1 111.6(3) . . ? Cl2 C100 Cl1 110.3(3) . . ? Cl6 C110 Cl5 110.0(3) . . ? Cl6 C110 Cl4 110.4(3) . . ? Cl5 C110 Cl4 110.4(3) . . ? Cl8 C120 Cl7 109.5(6) . . ? Cl8 C120 Cl9 108.0(6) . . ? Cl7 C120 Cl9 109.0(7) . . ? Cl12 C130 Cl10 112.6(8) . . ? Cl12 C130 Cl11 112.8(7) . . ? Cl10 C130 Cl11 111.1(8) . . ? Cl13 C140 Cl14 113.2(12) . . ? Cl13 C140 Cl15 112.1(12) . . ? Cl14 C140 Cl15 106.2(9) . . ? Cl16 C150 Cl18 127.8(13) . . ? Cl16 C150 Cl17 117.2(11) . . ? Cl18 C150 Cl17 111.1(9) . . ? C160 C161 C162 118.4(13) . . ? C163 C162 C161 120.9(13) . . ? C162 C163 C164 116.3(15) . . ? C170 C171 C172 120.4(17) . . ? C171 C172 C173 113.9(17) . . ? C174 C173 C172 108.3(14) . . ? _diffrn_measured_fraction_theta_max 0.855 _diffrn_reflns_theta_full 29.01 _diffrn_measured_fraction_theta_full 0.855 _refine_diff_density_max 1.657 _refine_diff_density_min -0.941 _refine_diff_density_rms 0.093 #===END data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 653718' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C84 H64 N9 O7 P4 B Eu), (N O3), 4(C H4 O)' _chemical_formula_sum 'C88 H80 B Eu N10 O14 P4' _chemical_formula_weight 1788.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 25.0529(2) _cell_length_b 13.1352(1) _cell_length_c 26.4601(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.560(1) _cell_angle_gamma 90.00 _cell_volume 8346.19(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 60276 _cell_measurement_theta_min 1.7394 _cell_measurement_theta_max 71.1341 _exptl_crystal_description blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3672 _exptl_absorpt_coefficient_mu 6.686 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67974 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 112068 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 71.37 _reflns_number_total 16144 _reflns_number_gt 14231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+7.2616P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16144 _refine_ls_number_parameters 1093 _refine_ls_number_restraints 155 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0986 _refine_ls_wR_factor_gt 0.0918 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu Eu 0.822182(6) 0.210415(12) 0.513810(6) 0.02795(6) Uani 1 1 d . . . B B 0.70765(13) 0.1502(3) 0.56916(14) 0.0362(7) Uani 1 1 d . . . P1 P 0.75872(3) 0.43006(6) 0.44821(3) 0.03546(16) Uani 1 1 d . . . O1 O 0.77108(8) 0.31766(16) 0.44915(8) 0.0380(4) Uani 1 1 d . . . P2 P 0.81932(3) -0.03790(6) 0.46402(3) 0.03447(15) Uani 1 1 d . . . O2 O 0.84591(8) 0.04462(15) 0.50250(8) 0.0354(4) Uani 1 1 d . . . P3 P 0.92322(3) 0.25552(6) 0.63623(3) 0.03387(15) Uani 1 1 d . . . O3 O 0.87908(8) 0.28575(15) 0.58662(8) 0.0351(4) Uani 1 1 d . . . P4 P 0.48867(3) 0.10907(8) 0.64672(4) 0.0544(2) Uani 1 1 d . . . O4 O 0.47215(11) 0.0012(2) 0.63643(13) 0.0754(8) Uani 1 1 d . . . N1 N 0.75435(9) 0.31107(19) 0.55403(10) 0.0337(5) Uani 1 1 d . . . N2 N 0.71544(10) 0.26708(19) 0.57448(10) 0.0364(5) Uani 1 1 d . . . N3 N 0.73206(9) 0.11152(18) 0.48377(9) 0.0337(5) Uani 1 1 d . . . N4 N 0.69265(9) 0.12309(19) 0.50985(10) 0.0363(5) Uani 1 1 d . . . N5 N 0.81303(9) 0.11183(18) 0.59377(9) 0.0320(5) Uani 1 1 d . . . N6 N 0.76217(9) 0.09587(19) 0.60178(9) 0.0344(5) Uani 1 1 d . . . N7 N 0.65482(10) 0.1515(2) 0.63655(11) 0.0417(6) Uani 1 1 d . . . N8 N 0.66116(10) 0.1116(2) 0.59087(10) 0.0400(6) Uani 1 1 d . . . C9 C 0.69221(14) 0.3383(3) 0.59838(15) 0.0496(8) Uani 1 1 d . . . H9A H 0.6640 0.3265 0.6152 0.060 Uiso 1 1 calc R . . C10 C 0.71620(14) 0.4304(3) 0.59430(15) 0.0497(8) Uani 1 1 d . . . H10A H 0.7083 0.4941 0.6076 0.060 Uiso 1 1 calc R . . C11 C 0.75464(12) 0.4107(2) 0.56651(12) 0.0369(6) Uani 1 1 d . . . C12 C 0.79390(12) 0.4845(2) 0.55456(12) 0.0375(6) Uani 1 1 d . . . C13 C 0.80160(12) 0.4976(2) 0.50428(12) 0.0386(6) Uani 1 1 d . . . C14 C 0.84192(13) 0.5659(3) 0.49773(13) 0.0458(8) Uani 1 1 d . . . H14A H 0.8483 0.5731 0.4642 0.055 Uiso 1 1 calc R . . C15 C 0.87279(15) 0.6234(3) 0.54026(14) 0.0513(8) Uani 1 1 d . . . H15A H 0.9005 0.6690 0.5357 0.062 Uiso 1 1 calc R . . C16 C 0.86342(15) 0.6143(3) 0.58853(14) 0.0508(8) Uani 1 1 d . . . H16A H 0.8836 0.6556 0.6171 0.061 Uiso 1 1 calc R . . C17 C 0.82455(13) 0.5451(2) 0.59587(13) 0.0431(7) Uani 1 1 d . . . H17A H 0.8187 0.5388 0.6297 0.052 Uiso 1 1 calc R . . C18 C 0.64141(12) 0.1138(3) 0.47529(13) 0.0437(7) Uani 1 1 d . . . H18A H 0.6072 0.1207 0.4837 0.052 Uiso 1 1 calc R . . C19 C 0.64670(12) 0.0928(3) 0.42652(13) 0.0440(7) Uani 1 1 d . . . H19A H 0.6176 0.0814 0.3950 0.053 Uiso 1 1 calc R . . C20 C 0.70430(12) 0.0917(2) 0.43287(12) 0.0379(6) Uani 1 1 d . . . C21 C 0.73194(12) 0.0678(2) 0.39202(12) 0.0392(7) Uani 1 1 d . . . C22 C 0.78106(12) 0.0095(2) 0.39976(12) 0.0380(6) Uani 1 1 d . . . C23 C 0.80054(14) -0.0133(3) 0.35665(13) 0.0456(7) Uani 1 1 d . . . H23A H 0.8339 -0.0516 0.3621 0.055 Uiso 1 1 calc R . . C24 C 0.77248(16) 0.0186(3) 0.30601(14) 0.0574(9) Uani 1 1 d . . . H24A H 0.7860 0.0012 0.2771 0.069 Uiso 1 1 calc R . . C25 C 0.72473(17) 0.0757(4) 0.29831(14) 0.0636(11) Uani 1 1 d . . . H25A H 0.7053 0.0984 0.2639 0.076 Uiso 1 1 calc R . . C26 C 0.70489(15) 0.1001(3) 0.34065(13) 0.0528(9) Uani 1 1 d . . . H26A H 0.6720 0.1399 0.3347 0.063 Uiso 1 1 calc R . . C27 C 0.76728(13) 0.0315(3) 0.64239(13) 0.0433(7) Uani 1 1 d . . . H27A H 0.7378 0.0089 0.6556 0.052 Uiso 1 1 calc R . . C28 C 0.82199(13) 0.0038(3) 0.66162(13) 0.0444(7) Uani 1 1 d . . . H28A H 0.8379 -0.0411 0.6901 0.053 Uiso 1 1 calc R . . C29 C 0.84936(12) 0.0559(2) 0.63034(11) 0.0359(6) Uani 1 1 d . . . C30 C 0.90900(12) 0.0444(2) 0.63230(11) 0.0377(6) Uani 1 1 d . . . C31 C 0.94598(12) 0.1260(2) 0.63300(11) 0.0380(6) Uani 1 1 d . . . C32 C 1.00042(13) 0.1051(3) 0.63211(14) 0.0482(8) Uani 1 1 d . . . H32A H 1.0252 0.1597 0.6318 0.058 Uiso 1 1 calc R . . C33 C 1.01869(14) 0.0053(3) 0.63174(15) 0.0569(9) Uani 1 1 d . . . H33A H 1.0555 -0.0081 0.6302 0.068 Uiso 1 1 calc R . . C34 C 0.98368(15) -0.0738(3) 0.63359(16) 0.0582(9) Uani 1 1 d . . . H34A H 0.9966 -0.1419 0.6345 0.070 Uiso 1 1 calc R . . C35 C 0.92933(13) -0.0546(3) 0.63406(14) 0.0474(8) Uani 1 1 d . . . H35A H 0.9055 -0.1101 0.6356 0.057 Uiso 1 1 calc R . . C36 C 0.63191(14) 0.0230(3) 0.57912(15) 0.0492(8) Uani 1 1 d . . . H36A H 0.6308 -0.0206 0.5502 0.059 Uiso 1 1 calc R . . C37 C 0.60446(15) 0.0082(3) 0.61630(15) 0.0540(9) Uani 1 1 d . . . H37A H 0.5802 -0.0464 0.6182 0.065 Uiso 1 1 calc R . . C38 C 0.61965(12) 0.0900(3) 0.65082(13) 0.0434(7) Uani 1 1 d . . . C39 C 0.60512(12) 0.1142(3) 0.69983(14) 0.0446(7) Uani 1 1 d . . . C40 C 0.55006(13) 0.1261(3) 0.70255(14) 0.0491(8) Uani 1 1 d . . . C41 C 0.54139(15) 0.1482(4) 0.75099(16) 0.0657(11) Uani 1 1 d . . . H41A H 0.5043 0.1549 0.7531 0.079 Uiso 1 1 calc R . . C42 C 0.58522(17) 0.1608(4) 0.79619(16) 0.0724(12) Uani 1 1 d . . . H42A H 0.5783 0.1763 0.8288 0.087 Uiso 1 1 calc R . . C43 C 0.63917(16) 0.1506(4) 0.79337(16) 0.0657(11) Uani 1 1 d . . . H43A H 0.6697 0.1594 0.8241 0.079 Uiso 1 1 calc R . . C44 C 0.64856(14) 0.1277(3) 0.74583(15) 0.0542(9) Uani 1 1 d . . . H44A H 0.6858 0.1210 0.7443 0.065 Uiso 1 1 calc R . . C45 C 0.68752(12) 0.4505(2) 0.44740(12) 0.0384(6) Uani 1 1 d . . . C46 C 0.65111(13) 0.3688(3) 0.43503(13) 0.0455(7) Uani 1 1 d . . . H46A H 0.6642 0.3038 0.4282 0.055 Uiso 1 1 calc R . . C47 C 0.59564(15) 0.3820(3) 0.43267(16) 0.0572(9) Uani 1 1 d . . . H47A H 0.5706 0.3262 0.4239 0.069 Uiso 1 1 calc R . . C48 C 0.57681(14) 0.4755(3) 0.44299(15) 0.0561(9) Uani 1 1 d . . . H48A H 0.5387 0.4842 0.4413 0.067 Uiso 1 1 calc R . . C49 C 0.61279(15) 0.5569(3) 0.45582(18) 0.0603(10) Uani 1 1 d . . . H49A H 0.5996 0.6216 0.4630 0.072 Uiso 1 1 calc R . . C50 C 0.66822(14) 0.5442(3) 0.45817(16) 0.0538(9) Uani 1 1 d . . . H50A H 0.6932 0.6002 0.4672 0.065 Uiso 1 1 calc R . . C51 C 0.76903(11) 0.4836(2) 0.38898(12) 0.0389(7) Uani 1 1 d . . . C52 C 0.76066(14) 0.5869(3) 0.37614(13) 0.0473(8) Uani 1 1 d . . . H52A H 0.7496 0.6322 0.3992 0.057 Uiso 1 1 calc R . . C53 C 0.76863(14) 0.6225(3) 0.32955(14) 0.0522(9) Uani 1 1 d . . . H53A H 0.7641 0.6930 0.3213 0.063 Uiso 1 1 calc R . . C54 C 0.78305(13) 0.5567(3) 0.29492(14) 0.0507(8) Uani 1 1 d . . . H54A H 0.7873 0.5816 0.2626 0.061 Uiso 1 1 calc R . . C55 C 0.79118(13) 0.4551(3) 0.30725(14) 0.0504(8) Uani 1 1 d . . . H55A H 0.8012 0.4100 0.2834 0.060 Uiso 1 1 calc R . . C56 C 0.78476(12) 0.4183(3) 0.35439(12) 0.0420(7) Uani 1 1 d . . . H56A H 0.7911 0.3483 0.3630 0.050 Uiso 1 1 calc R . . C57 C 0.77085(12) -0.1136(2) 0.48692(12) 0.0381(6) Uani 1 1 d . . . C58 C 0.72039(14) -0.1466(3) 0.45312(15) 0.0488(8) Uani 1 1 d . . . H58A H 0.7120 -0.1345 0.4163 0.059 Uiso 1 1 calc R . . C59 C 0.68260(16) -0.1970(3) 0.47338(19) 0.0595(10) Uani 1 1 d . . . H59A H 0.6478 -0.2177 0.4504 0.071 Uiso 1 1 calc R . . C60 C 0.69485(18) -0.2171(3) 0.52589(19) 0.0628(11) Uani 1 1 d . . . H60A H 0.6685 -0.2514 0.5394 0.075 Uiso 1 1 calc R . . C61 C 0.7456(2) -0.1878(3) 0.55982(17) 0.0661(11) Uani 1 1 d . . . H61A H 0.7545 -0.2034 0.5963 0.079 Uiso 1 1 calc R . . C62 C 0.78341(16) -0.1355(3) 0.54017(14) 0.0516(8) Uani 1 1 d . . . H62A H 0.8181 -0.1146 0.5633 0.062 Uiso 1 1 calc R . . C63 C 0.87487(13) -0.1207(2) 0.45901(13) 0.0397(7) Uani 1 1 d . . . C64 C 0.92752(14) -0.0993(3) 0.49118(14) 0.0475(8) Uani 1 1 d . . . H64A H 0.9338 -0.0390 0.5119 0.057 Uiso 1 1 calc R . . C65 C 0.97146(16) -0.1655(3) 0.49345(17) 0.0595(9) Uani 1 1 d . . . H65A H 1.0075 -0.1508 0.5160 0.071 Uiso 1 1 calc R . . C66 C 0.96292(17) -0.2520(3) 0.46325(17) 0.0591(9) Uani 1 1 d . . . H66A H 0.9929 -0.2974 0.4651 0.071 Uiso 1 1 calc R . . C67 C 0.91075(18) -0.2730(3) 0.43015(16) 0.0560(9) Uani 1 1 d . . . H67A H 0.9052 -0.3319 0.4085 0.067 Uiso 1 1 calc R . . C68 C 0.86635(16) -0.2086(2) 0.42829(15) 0.0480(8) Uani 1 1 d . . . H68A H 0.8302 -0.2244 0.4061 0.058 Uiso 1 1 calc R . . C69 C 0.89745(12) 0.2629(2) 0.69296(12) 0.0377(6) Uani 1 1 d . . . C70 C 0.84387(14) 0.2990(3) 0.68623(13) 0.0455(7) Uani 1 1 d . . . H70A H 0.8213 0.3178 0.6522 0.055 Uiso 1 1 calc R . . C71 C 0.82324(17) 0.3076(3) 0.72973(15) 0.0574(9) Uani 1 1 d . . . H71A H 0.7863 0.3311 0.7252 0.069 Uiso 1 1 calc R . . C72 C 0.85636(18) 0.2820(3) 0.77934(15) 0.0564(9) Uani 1 1 d . . . H72A H 0.8426 0.2899 0.8091 0.068 Uiso 1 1 calc R . . C73 C 0.90953(16) 0.2448(3) 0.78586(13) 0.0520(8) Uani 1 1 d . . . H73A H 0.9319 0.2262 0.8200 0.062 Uiso 1 1 calc R . . C74 C 0.93027(15) 0.2347(3) 0.74321(13) 0.0467(7) Uani 1 1 d . . . H74A H 0.9667 0.2086 0.7479 0.056 Uiso 1 1 calc R . . C75 C 0.98059(12) 0.3427(2) 0.64503(12) 0.0386(6) Uani 1 1 d . . . C76 C 1.02900(14) 0.3374(3) 0.68731(14) 0.0517(8) Uani 1 1 d . . . H76A H 1.0339 0.2844 0.7127 0.062 Uiso 1 1 calc R . . C77 C 1.06980(14) 0.4113(3) 0.69148(15) 0.0603(10) Uani 1 1 d . . . H77A H 1.1030 0.4082 0.7199 0.072 Uiso 1 1 calc R . . C78 C 1.06289(14) 0.4886(3) 0.65531(16) 0.0564(9) Uani 1 1 d . . . H78A H 1.0911 0.5387 0.6591 0.068 Uiso 1 1 calc R . . C79 C 1.01504(14) 0.4938(3) 0.61332(16) 0.0508(8) Uani 1 1 d . . . H79A H 1.0103 0.5472 0.5882 0.061 Uiso 1 1 calc R . . C80 C 0.97405(13) 0.4204(2) 0.60827(13) 0.0424(7) Uani 1 1 d . . . H80A H 0.9412 0.4234 0.5794 0.051 Uiso 1 1 calc R . . C81 C 0.49791(14) 0.1732(3) 0.58992(15) 0.0543(9) Uani 1 1 d . . . C82 C 0.52873(14) 0.2608(3) 0.59167(16) 0.0571(9) Uani 1 1 d . . . H82A H 0.5489 0.2886 0.6248 0.069 Uiso 1 1 calc R . . C83 C 0.53046(17) 0.3083(4) 0.54574(17) 0.0664(11) Uani 1 1 d . . . H83A H 0.5520 0.3684 0.5473 0.080 Uiso 1 1 calc R . . C84 C 0.50110(19) 0.2692(4) 0.49756(18) 0.0776(14) Uani 1 1 d . . . H84A H 0.5020 0.3026 0.4660 0.093 Uiso 1 1 calc R . . C85 C 0.4707(2) 0.1823(5) 0.49536(18) 0.0864(16) Uani 1 1 d . . . H85A H 0.4506 0.1552 0.4621 0.104 Uiso 1 1 calc R . . C86 C 0.46879(17) 0.1339(4) 0.54041(16) 0.0722(12) Uani 1 1 d . . . H86A H 0.4476 0.0732 0.5383 0.087 Uiso 1 1 calc R . . C87 C 0.43526(15) 0.1812(4) 0.66522(16) 0.0650(11) Uani 1 1 d . . . C88 C 0.39592(16) 0.1291(5) 0.68249(19) 0.0844(16) Uani 1 1 d . . . H88A H 0.3947 0.0569 0.6806 0.101 Uiso 1 1 calc R . . C89 C 0.3582(2) 0.1810(7) 0.7025(2) 0.106(2) Uani 1 1 d . . . H89A H 0.3310 0.1448 0.7140 0.128 Uiso 1 1 calc R . . C90 C 0.3608(3) 0.2866(7) 0.7055(3) 0.118(3) Uani 1 1 d . . . H90A H 0.3364 0.3226 0.7208 0.142 Uiso 1 1 calc R . . C91 C 0.3981(3) 0.3390(6) 0.6867(3) 0.115(2) Uani 1 1 d . . . H91A H 0.3988 0.4113 0.6878 0.138 Uiso 1 1 calc R . . C92 C 0.4352(2) 0.2862(5) 0.6661(2) 0.0891(17) Uani 1 1 d . . . H92A H 0.4608 0.3227 0.6524 0.107 Uiso 1 1 calc R . . N100 N 0.89182(11) 0.2594(3) 0.44204(11) 0.0472(7) Uani 1 1 d . . . O101 O 0.89879(10) 0.2912(2) 0.48895(10) 0.0641(8) Uani 1 1 d . . . O102 O 0.85385(11) 0.19581(18) 0.42614(10) 0.0523(6) Uani 1 1 d . . . O103 O 0.92022(12) 0.2909(2) 0.41492(11) 0.0707(9) Uani 1 1 d . . . N110 N 0.7944(4) 0.7169(8) 0.7082(4) 0.094(3) Uiso 0.507(4) 1 d PDU A 1 O111 O 0.8329(4) 0.7638(7) 0.7102(4) 0.107(3) Uiso 0.507(4) 1 d PDU A 1 O112 O 0.8046(5) 0.6175(7) 0.7125(5) 0.127(3) Uiso 0.507(4) 1 d PDU A 1 O113 O 0.7438(4) 0.7413(10) 0.7075(6) 0.140(4) Uiso 0.507(4) 1 d PDU A 1 N115 N 0.7901(8) 0.6938(13) 0.7253(8) 0.115(6) Uiso 0.238(7) 1 d PDU B 2 O116 O 0.7513(7) 0.7058(13) 0.7449(8) 0.108(5) Uiso 0.238(7) 1 d PDU B 2 O117 O 0.8265(7) 0.7560(14) 0.7257(8) 0.085(5) Uiso 0.238(7) 1 d PDU B 2 O118 O 0.7818(7) 0.6199(10) 0.6935(6) 0.068(4) Uiso 0.238(7) 1 d PDU B 2 N120 N 0.7754(8) 0.7081(13) 0.7087(8) 0.117(6) Uiso 0.255(7) 1 d PDU C 3 O121 O 0.8204(7) 0.7079(15) 0.7459(7) 0.124(5) Uiso 0.255(7) 1 d PDU C 3 O122 O 0.7546(9) 0.6232(11) 0.6913(7) 0.116(5) Uiso 0.255(7) 1 d PDU C 3 O123 O 0.7465(7) 0.7849(12) 0.6926(8) 0.110(5) Uiso 0.255(7) 1 d PDU C 3 O130 O 0.93014(18) 0.6537(3) 0.72204(18) 0.1164(15) Uani 1 1 d D . . H130 H 0.8988 0.6706 0.7250 0.175 Uiso 1 1 d R . . C130 C 0.9357(3) 0.5460(5) 0.7258(2) 0.107(2) Uani 1 1 d D . . H13A H 0.9751 0.5282 0.7402 0.161 Uiso 1 1 d R . . H13B H 0.9213 0.5159 0.6906 0.161 Uiso 1 1 d R . . H13C H 0.9147 0.5198 0.7490 0.161 Uiso 1 1 d R . . O135 O 0.50410(18) 0.8077(3) 0.62851(18) 0.1049(12) Uani 1 1 d D . . H135 H 0.4860 0.8625 0.6246 0.157 Uiso 1 1 d R . . C135 C 0.5358(4) 0.7994(7) 0.6794(3) 0.152(4) Uani 1 1 d D . . H13D H 0.5679 0.8453 0.6855 0.228 Uiso 1 1 d R . . H13E H 0.5489 0.7291 0.6864 0.228 Uiso 1 1 d R . . H13F H 0.5135 0.8178 0.7030 0.228 Uiso 1 1 d R . . O140 O 0.6591(4) 0.6041(7) 0.6688(3) 0.126(3) Uani 0.595(13) 1 d PDU D 1 H140 H 0.6463 0.5477 0.6748 0.189 Uiso 0.595(13) 1 d PR D 1 C140 C 0.6236(8) 0.6477(17) 0.6218(6) 0.171(7) Uani 0.595(13) 1 d PDU D 1 H14B H 0.6074 0.7106 0.6307 0.257 Uiso 0.595(13) 1 d PR D 1 H14C H 0.5938 0.5993 0.6058 0.257 Uiso 0.595(13) 1 d PR D 1 H14D H 0.6449 0.6629 0.5969 0.257 Uiso 0.595(13) 1 d PR D 1 O145 O 0.6765(10) 0.667(2) 0.6473(10) 0.218(8) Uiso 0.405(13) 1 d PDU D 2 H145 H 0.6862 0.6447 0.6783 0.327 Uiso 0.405(13) 1 d PR D 2 C145 C 0.6283(10) 0.726(2) 0.6383(11) 0.160(8) Uiso 0.405(13) 1 d PDU D 2 H14E H 0.6069 0.7076 0.6628 0.239 Uiso 0.405(13) 1 d PR D 2 H14F H 0.6041 0.7224 0.6020 0.239 Uiso 0.405(13) 1 d PR D 2 H14G H 0.6430 0.7949 0.6459 0.239 Uiso 0.405(13) 1 d PR D 2 O150 O 0.5770(9) 0.4307(15) 0.7169(8) 0.196(9) Uiso 0.417(4) 1 d PDU E 1 H150 H 0.5988 0.3883 0.7096 0.294 Uiso 0.417(4) 1 d PR E 1 C150 C 0.5607(5) 0.5033(9) 0.6758(5) 0.195(11) Uiso 0.417(4) 1 d PDU E 1 H15B H 0.5201 0.5025 0.6614 0.293 Uiso 0.417(4) 1 d PR E 1 H15C H 0.5778 0.4864 0.6478 0.293 Uiso 0.417(4) 1 d PR E 1 H15D H 0.5729 0.5713 0.6896 0.293 Uiso 0.417(4) 1 d PR E 1 O155 O 0.6132(5) 0.4213(9) 0.6786(5) 0.101(4) Uiso 0.390(12) 1 d PRDU F 2 H155 H 0.5916 0.4142 0.6975 0.152 Uiso 0.390(12) 1 d PR F 2 C155 C 0.5901(13) 0.498(2) 0.6378(11) 0.201(11) Uiso 0.390(12) 1 d PDU F 2 H15E H 0.5496 0.4906 0.6244 0.302 Uiso 0.390(12) 1 d PR F 2 H15F H 0.6067 0.4896 0.6087 0.302 Uiso 0.390(12) 1 d PR F 2 H15G H 0.5991 0.5659 0.6533 0.302 Uiso 0.390(12) 1 d PR F 2 O160 O 0.6050(17) 0.452(3) 0.6667(16) 0.151(10) Uiso 0.193(12) 1 d PDU G 3 H160 H 0.6377 0.4655 0.6844 0.227 Uiso 0.193(12) 1 d PR G 3 C160 C 0.568(2) 0.459(4) 0.698(2) 0.128(12) Uiso 0.193(12) 1 d PDU G 3 H16B H 0.5678 0.3940 0.7166 0.192 Uiso 0.193(12) 1 d PR G 3 H16C H 0.5307 0.4752 0.6767 0.192 Uiso 0.193(12) 1 d PR G 3 H16D H 0.5818 0.5129 0.7245 0.192 Uiso 0.193(12) 1 d PR G 3 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 Eu 0.01987(8) 0.02889(9) 0.03133(9) -0.00032(6) 0.00123(6) -0.00084(6) B 0.0232(14) 0.0350(17) 0.0484(18) -0.0016(14) 0.0073(13) -0.0016(12) P1 0.0269(3) 0.0352(4) 0.0383(4) 0.0025(3) -0.0003(3) -0.0007(3) O1 0.0317(10) 0.0366(11) 0.0402(11) 0.0025(9) 0.0015(8) 0.0025(8) P2 0.0310(3) 0.0324(4) 0.0383(4) -0.0019(3) 0.0072(3) -0.0010(3) O2 0.0279(9) 0.0358(11) 0.0394(10) -0.0011(8) 0.0044(8) 0.0008(8) P3 0.0251(3) 0.0400(4) 0.0329(3) -0.0007(3) 0.0025(3) -0.0045(3) O3 0.0280(10) 0.0393(11) 0.0337(10) -0.0015(8) 0.0018(8) -0.0055(8) P4 0.0288(4) 0.0758(6) 0.0565(5) -0.0006(5) 0.0089(4) -0.0096(4) O4 0.0490(15) 0.078(2) 0.096(2) -0.0019(17) 0.0148(15) -0.0223(14) N1 0.0233(11) 0.0360(12) 0.0388(13) 0.0010(10) 0.0041(9) -0.0018(9) N2 0.0257(11) 0.0371(13) 0.0458(14) -0.0010(11) 0.0093(10) 0.0000(10) N3 0.0246(11) 0.0348(12) 0.0387(12) -0.0015(10) 0.0041(9) -0.0007(9) N4 0.0227(11) 0.0379(13) 0.0455(14) -0.0008(11) 0.0049(10) -0.0029(9) N5 0.0233(11) 0.0330(12) 0.0370(12) -0.0009(10) 0.0041(9) -0.0008(9) N6 0.0267(11) 0.0366(13) 0.0396(12) 0.0002(10) 0.0088(10) -0.0028(10) N7 0.0252(11) 0.0478(15) 0.0510(15) -0.0012(12) 0.0091(11) -0.0037(11) N8 0.0284(12) 0.0428(14) 0.0491(14) -0.0056(11) 0.0116(11) -0.0053(10) C9 0.0399(17) 0.0454(19) 0.070(2) -0.0032(16) 0.0258(16) 0.0018(14) C10 0.0484(18) 0.0380(17) 0.069(2) -0.0060(16) 0.0265(17) 0.0027(14) C11 0.0315(14) 0.0345(15) 0.0412(15) -0.0010(12) 0.0049(12) 0.0026(12) C12 0.0308(14) 0.0304(14) 0.0469(16) -0.0005(12) 0.0039(12) 0.0021(11) C13 0.0315(14) 0.0364(16) 0.0419(15) 0.0046(12) 0.0006(12) -0.0012(12) C14 0.0396(16) 0.0467(18) 0.0438(17) 0.0076(14) -0.0001(13) -0.0073(14) C15 0.0458(18) 0.0448(19) 0.054(2) 0.0069(15) -0.0008(15) -0.0155(15) C16 0.0503(19) 0.0436(18) 0.0492(18) -0.0056(15) -0.0008(15) -0.0104(15) C17 0.0462(17) 0.0373(16) 0.0419(16) -0.0025(13) 0.0061(13) -0.0030(13) C18 0.0224(13) 0.0472(18) 0.0561(19) -0.0024(15) 0.0025(13) -0.0032(12) C19 0.0263(14) 0.0504(19) 0.0470(17) -0.0012(14) -0.0027(12) -0.0050(13) C20 0.0294(14) 0.0336(15) 0.0439(16) 0.0021(12) -0.0004(12) -0.0025(11) C21 0.0336(15) 0.0409(16) 0.0379(15) -0.0014(13) 0.0015(12) -0.0084(12) C22 0.0341(14) 0.0359(15) 0.0401(15) -0.0012(12) 0.0041(12) -0.0076(12) C23 0.0455(17) 0.0487(19) 0.0432(16) -0.0007(14) 0.0134(14) -0.0086(14) C24 0.059(2) 0.071(3) 0.0440(18) -0.0005(17) 0.0164(16) -0.0121(19) C25 0.057(2) 0.087(3) 0.0402(18) 0.0132(19) 0.0046(16) -0.008(2) C26 0.0409(18) 0.065(2) 0.0455(18) 0.0094(16) 0.0015(14) -0.0030(16) C27 0.0371(16) 0.0469(18) 0.0477(17) 0.0032(14) 0.0150(13) -0.0044(13) C28 0.0407(16) 0.0482(18) 0.0425(16) 0.0096(14) 0.0093(13) 0.0004(14) C29 0.0311(14) 0.0356(15) 0.0376(15) -0.0007(12) 0.0043(11) -0.0003(12) C30 0.0304(14) 0.0427(16) 0.0349(14) 0.0040(12) 0.0013(11) 0.0043(12) C31 0.0304(14) 0.0459(17) 0.0339(14) 0.0015(12) 0.0029(11) -0.0018(12) C32 0.0319(15) 0.058(2) 0.0522(19) 0.0042(16) 0.0083(14) 0.0018(14) C33 0.0325(16) 0.069(2) 0.066(2) -0.0004(19) 0.0082(15) 0.0120(16) C34 0.0447(19) 0.054(2) 0.069(2) 0.0048(18) 0.0047(17) 0.0162(17) C35 0.0371(16) 0.0431(18) 0.0545(19) 0.0051(15) 0.0011(14) 0.0049(14) C36 0.0409(17) 0.0484(19) 0.062(2) -0.0107(16) 0.0204(15) -0.0130(14) C37 0.0435(18) 0.055(2) 0.068(2) -0.0104(18) 0.0227(17) -0.0172(16) C38 0.0280(14) 0.0489(18) 0.0527(18) -0.0019(15) 0.0107(13) -0.0034(13) C39 0.0288(14) 0.0503(19) 0.0537(18) 0.0010(15) 0.0101(13) -0.0026(13) C40 0.0308(15) 0.066(2) 0.0498(18) 0.0030(16) 0.0099(14) -0.0022(15) C41 0.0361(18) 0.103(3) 0.058(2) 0.005(2) 0.0130(16) 0.008(2) C42 0.048(2) 0.115(4) 0.053(2) 0.003(2) 0.0127(18) 0.016(2) C43 0.0418(19) 0.094(3) 0.053(2) 0.003(2) -0.0002(16) 0.008(2) C44 0.0317(16) 0.071(2) 0.057(2) 0.0012(18) 0.0074(15) 0.0016(15) C45 0.0272(13) 0.0412(16) 0.0405(15) 0.0043(13) -0.0003(11) 0.0020(12) C46 0.0376(16) 0.0466(18) 0.0512(18) -0.0046(15) 0.0108(14) -0.0053(14) C47 0.0392(18) 0.063(2) 0.069(2) -0.0116(19) 0.0148(17) -0.0128(16) C48 0.0317(16) 0.070(2) 0.064(2) 0.0029(19) 0.0103(15) 0.0020(16) C49 0.0442(19) 0.048(2) 0.088(3) 0.0074(19) 0.0185(19) 0.0090(16) C50 0.0368(17) 0.0402(18) 0.081(3) 0.0010(17) 0.0111(17) 0.0002(14) C51 0.0248(13) 0.0423(16) 0.0415(15) 0.0049(13) -0.0036(11) -0.0027(12) C52 0.0459(18) 0.0453(18) 0.0454(17) 0.0056(14) 0.0045(14) 0.0025(14) C53 0.0431(18) 0.050(2) 0.056(2) 0.0145(16) 0.0015(15) -0.0028(15) C54 0.0328(16) 0.070(2) 0.0447(17) 0.0111(17) 0.0032(13) -0.0032(15) C55 0.0315(15) 0.068(2) 0.0492(18) 0.0014(17) 0.0067(13) 0.0015(15) C56 0.0270(14) 0.0482(18) 0.0464(17) 0.0035(14) 0.0032(12) 0.0019(13) C57 0.0358(15) 0.0330(15) 0.0457(16) -0.0019(12) 0.0117(13) 0.0001(12) C58 0.0402(17) 0.0402(17) 0.060(2) 0.0035(15) 0.0052(15) -0.0076(14) C59 0.044(2) 0.045(2) 0.087(3) 0.0020(19) 0.0130(19) -0.0074(15) C60 0.062(2) 0.050(2) 0.088(3) -0.004(2) 0.040(2) -0.0142(17) C61 0.089(3) 0.061(2) 0.055(2) -0.0034(19) 0.031(2) -0.018(2) C62 0.056(2) 0.050(2) 0.0473(18) -0.0003(15) 0.0123(16) -0.0109(16) C63 0.0412(16) 0.0341(15) 0.0469(17) -0.0001(13) 0.0175(13) 0.0021(12) C64 0.0411(17) 0.0470(19) 0.0540(19) -0.0039(15) 0.0130(15) 0.0052(14) C65 0.0434(19) 0.063(2) 0.073(2) -0.002(2) 0.0188(18) 0.0114(17) C66 0.055(2) 0.057(2) 0.074(3) 0.004(2) 0.033(2) 0.0164(18) C67 0.076(3) 0.0397(18) 0.066(2) -0.0035(16) 0.042(2) 0.0027(17) C68 0.051(2) 0.0407(18) 0.057(2) -0.0044(14) 0.0233(16) -0.0034(14) C69 0.0351(15) 0.0395(16) 0.0365(15) -0.0029(12) 0.0068(12) -0.0071(12) C70 0.0417(17) 0.053(2) 0.0413(17) -0.0021(14) 0.0107(14) 0.0000(14) C71 0.053(2) 0.069(2) 0.055(2) -0.0066(18) 0.0228(17) 0.0043(18) C72 0.074(3) 0.056(2) 0.0464(19) -0.0087(16) 0.0278(18) -0.0064(18) C73 0.063(2) 0.052(2) 0.0381(17) -0.0008(15) 0.0089(15) -0.0131(18) C74 0.0439(18) 0.0502(19) 0.0421(17) 0.0010(14) 0.0060(14) -0.0049(15) C75 0.0275(14) 0.0457(17) 0.0399(15) -0.0046(13) 0.0053(12) -0.0079(12) C76 0.0353(16) 0.068(2) 0.0449(17) 0.0005(17) 0.0012(14) -0.0115(16) C77 0.0328(17) 0.083(3) 0.057(2) -0.012(2) -0.0008(15) -0.0177(17) C78 0.0366(17) 0.052(2) 0.079(3) -0.0161(19) 0.0150(17) -0.0153(15) C79 0.0403(17) 0.0400(18) 0.073(2) -0.0027(16) 0.0177(16) -0.0060(14) C80 0.0305(14) 0.0420(17) 0.0527(18) -0.0041(14) 0.0086(13) -0.0033(13) C81 0.0304(16) 0.074(2) 0.055(2) -0.0060(18) 0.0058(14) -0.0058(16) C82 0.0363(18) 0.074(3) 0.057(2) -0.0035(19) 0.0061(15) -0.0038(17) C83 0.045(2) 0.085(3) 0.066(2) 0.010(2) 0.0115(18) -0.0039(19) C84 0.053(2) 0.123(4) 0.054(2) 0.013(2) 0.0092(19) -0.013(3) C85 0.067(3) 0.138(5) 0.050(2) -0.012(3) 0.010(2) -0.031(3) C86 0.052(2) 0.105(4) 0.057(2) -0.013(2) 0.0106(18) -0.027(2) C87 0.0297(17) 0.104(4) 0.058(2) 0.008(2) 0.0066(15) 0.0050(19) C88 0.036(2) 0.141(5) 0.077(3) 0.001(3) 0.0176(19) -0.008(2) C89 0.043(2) 0.193(8) 0.088(4) -0.003(5) 0.026(2) 0.003(4) C90 0.061(3) 0.186(8) 0.111(5) 0.013(5) 0.030(3) 0.052(4) C91 0.086(4) 0.144(6) 0.122(5) 0.031(4) 0.039(4) 0.057(4) C92 0.067(3) 0.112(5) 0.092(4) 0.025(3) 0.030(3) 0.034(3) N100 0.0323(13) 0.0688(19) 0.0391(14) 0.0045(13) 0.0081(11) -0.0017(13) O101 0.0393(13) 0.112(2) 0.0404(13) -0.0118(13) 0.0098(10) -0.0267(13) O102 0.0582(15) 0.0426(13) 0.0594(15) -0.0060(11) 0.0219(12) -0.0092(11) O103 0.0572(16) 0.108(3) 0.0528(15) -0.0024(14) 0.0249(13) -0.0255(15) O130 0.100(3) 0.114(3) 0.126(3) -0.058(3) 0.018(2) -0.015(2) C130 0.119(5) 0.105(5) 0.078(3) -0.028(3) -0.004(3) 0.008(4) O135 0.089(3) 0.111(3) 0.110(3) -0.012(2) 0.020(2) -0.009(2) C135 0.130(7) 0.177(9) 0.150(7) 0.074(6) 0.043(6) -0.012(6) O140 0.163(8) 0.108(6) 0.128(6) 0.007(5) 0.074(6) 0.006(5) C140 0.195(14) 0.185(14) 0.129(10) 0.056(11) 0.039(10) 0.059(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu O3 2.2710(19) . ? Eu O2 2.299(2) . ? Eu O1 2.303(2) . ? Eu O101 2.442(2) . ? Eu N3 2.529(2) . ? Eu N5 2.546(2) . ? Eu N1 2.608(2) . ? Eu O102 2.664(3) . ? B N8 1.525(4) . ? B N4 1.548(4) . ? B N2 1.549(4) . ? B N6 1.565(4) . ? P1 O1 1.507(2) . ? P1 C45 1.798(3) . ? P1 C13 1.798(3) . ? P1 C51 1.802(3) . ? P2 O2 1.506(2) . ? P2 C63 1.801(3) . ? P2 C57 1.802(3) . ? P2 C22 1.808(3) . ? P3 O3 1.509(2) . ? P3 C69 1.798(3) . ? P3 C75 1.800(3) . ? P3 C31 1.804(3) . ? P4 O4 1.479(3) . ? P4 C81 1.795(4) . ? P4 C87 1.817(4) . ? P4 C40 1.817(3) . ? N1 C11 1.349(4) . ? N1 N2 1.370(3) . ? N2 C9 1.351(4) . ? N3 C20 1.353(4) . ? N3 N4 1.365(3) . ? N4 C18 1.353(4) . ? N5 C29 1.343(4) . ? N5 N6 1.366(3) . ? N6 C27 1.345(4) . ? N7 C38 1.327(4) . ? N7 N8 1.368(4) . ? N8 C36 1.362(4) . ? C9 C10 1.368(5) . ? C10 C11 1.392(4) . ? C11 C12 1.478(4) . ? C12 C17 1.392(4) . ? C12 C13 1.408(4) . ? C13 C14 1.399(4) . ? C14 C15 1.392(5) . ? C15 C16 1.368(5) . ? C16 C17 1.386(5) . ? C18 C19 1.362(5) . ? C19 C20 1.405(4) . ? C20 C21 1.474(5) . ? C21 C26 1.401(4) . ? C21 C22 1.414(4) . ? C22 C23 1.395(5) . ? C23 C24 1.388(5) . ? C24 C25 1.377(6) . ? C25 C26 1.387(5) . ? C27 C28 1.368(5) . ? C28 C29 1.395(4) . ? C29 C30 1.488(4) . ? C30 C35 1.393(4) . ? C30 C31 1.413(4) . ? C31 C32 1.398(4) . ? C32 C33 1.390(5) . ? C33 C34 1.369(6) . ? C34 C35 1.388(5) . ? C36 C37 1.366(5) . ? C37 C38 1.391(5) . ? C38 C39 1.478(5) . ? C39 C44 1.394(5) . ? C39 C40 1.410(4) . ? C40 C41 1.390(5) . ? C41 C42 1.384(6) . ? C42 C43 1.381(5) . ? C43 C44 1.377(6) . ? C45 C50 1.382(5) . ? C45 C46 1.386(4) . ? C46 C47 1.384(5) . ? C47 C48 1.371(6) . ? C48 C49 1.377(5) . ? C49 C50 1.382(5) . ? C51 C56 1.391(5) . ? C51 C52 1.399(5) . ? C52 C53 1.385(5) . ? C53 C54 1.380(5) . ? C54 C55 1.375(5) . ? C55 C56 1.389(5) . ? C57 C62 1.384(5) . ? C57 C58 1.393(4) . ? C58 C59 1.382(5) . ? C59 C60 1.361(6) . ? C60 C61 1.386(6) . ? C61 C62 1.385(5) . ? C63 C64 1.380(5) . ? C63 C68 1.393(4) . ? C64 C65 1.391(5) . ? C65 C66 1.370(6) . ? C66 C67 1.378(6) . ? C67 C68 1.387(5) . ? C69 C70 1.386(5) . ? C69 C74 1.399(4) . ? C70 C71 1.394(5) . ? C71 C72 1.380(6) . ? C72 C73 1.382(6) . ? C73 C74 1.377(5) . ? C75 C80 1.387(5) . ? C75 C76 1.398(4) . ? C76 C77 1.391(5) . ? C77 C78 1.372(6) . ? C78 C79 1.385(5) . ? C79 C80 1.387(4) . ? C81 C82 1.379(6) . ? C81 C86 1.404(5) . ? C82 C83 1.378(6) . ? C83 C84 1.377(6) . ? C84 C85 1.365(7) . ? C85 C86 1.364(7) . ? C87 C92 1.379(7) . ? C87 C88 1.380(6) . ? C88 C89 1.386(8) . ? C89 C90 1.390(10) . ? C90 C91 1.364(10) . ? C91 C92 1.391(8) . ? N100 O103 1.218(4) . ? N100 O102 1.246(4) . ? N100 O101 1.274(4) . ? N110 O111 1.132(10) . ? N110 O113 1.305(11) . ? N110 O112 1.329(10) . ? N115 O117 1.222(13) . ? N115 O116 1.235(13) . ? N115 O118 1.263(13) . ? N120 O123 1.244(13) . ? N120 O122 1.260(13) . ? N120 O121 1.269(13) . ? O130 C130 1.421(7) . ? O135 C135 1.360(8) . ? O140 C140 1.425(12) . ? O145 C145 1.397(15) . ? O150 C150 1.418(14) . ? O155 C155 1.471(16) . ? O160 C160 1.412(17) . ? 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 O3 Eu O2 113.58(7) . . ? O3 Eu O1 116.45(7) . . ? O2 Eu O1 126.32(7) . . ? O3 Eu O101 71.80(8) . . ? O2 Eu O101 97.15(9) . . ? O1 Eu O101 81.21(9) . . ? O3 Eu N3 141.16(8) . . ? O2 Eu N3 73.34(7) . . ? O1 Eu N3 79.81(7) . . ? O101 Eu N3 146.99(8) . . ? O3 Eu N5 72.55(7) . . ? O2 Eu N5 73.40(7) . . ? O1 Eu N5 139.99(7) . . ? O101 Eu N5 135.14(8) . . ? N3 Eu N5 73.51(7) . . ? O3 Eu N1 75.96(7) . . ? O2 Eu N1 139.12(7) . . ? O1 Eu N1 72.79(8) . . ? O101 Eu N1 122.91(9) . . ? N3 Eu N1 76.19(7) . . ? N5 Eu N1 72.26(7) . . ? O3 Eu O102 119.96(8) . . ? O2 Eu O102 70.50(7) . . ? O1 Eu O102 68.75(8) . . ? O101 Eu O102 49.05(8) . . ? N3 Eu O102 98.64(8) . . ? N5 Eu O102 143.77(7) . . ? N1 Eu O102 141.48(8) . . ? N8 B N4 108.3(2) . . ? N8 B N2 112.7(2) . . ? N4 B N2 108.0(3) . . ? N8 B N6 106.3(3) . . ? N4 B N6 112.1(2) . . ? N2 B N6 109.5(2) . . ? O1 P1 C45 110.17(13) . . ? O1 P1 C13 113.44(13) . . ? C45 P1 C13 107.08(15) . . ? O1 P1 C51 108.47(14) . . ? C45 P1 C51 108.60(14) . . ? C13 P1 C51 108.97(14) . . ? O1 P1 Eu 28.81(8) . . ? C45 P1 Eu 115.92(10) . . ? C13 P1 Eu 85.26(10) . . ? C51 P1 Eu 126.47(10) . . ? P1 O1 Eu 132.81(12) . . ? O2 P2 C63 106.40(13) . . ? O2 P2 C57 112.34(13) . . ? C63 P2 C57 107.49(14) . . ? O2 P2 C22 113.70(13) . . ? C63 P2 C22 110.63(15) . . ? C57 P2 C22 106.18(14) . . ? O2 P2 Eu 28.35(7) . . ? C63 P2 Eu 130.94(11) . . ? C57 P2 Eu 109.26(10) . . ? C22 P2 Eu 88.96(10) . . ? P2 O2 Eu 133.52(11) . . ? O3 P3 C69 111.32(13) . . ? O3 P3 C75 107.77(13) . . ? C69 P3 C75 108.72(14) . . ? O3 P3 C31 111.74(12) . . ? C69 P3 C31 106.51(15) . . ? C75 P3 C31 110.76(14) . . ? O3 P3 Eu 25.03(8) . . ? C69 P3 Eu 116.04(10) . . ? C75 P3 Eu 124.06(10) . . ? C31 P3 Eu 87.27(9) . . ? P3 O3 Eu 138.64(12) . . ? O4 P4 C81 113.06(19) . . ? O4 P4 C87 111.1(2) . . ? C81 P4 C87 105.2(2) . . ? O4 P4 C40 113.27(18) . . ? C81 P4 C40 109.99(16) . . ? C87 P4 C40 103.56(18) . . ? C11 N1 N2 105.5(2) . . ? C11 N1 Eu 129.27(19) . . ? N2 N1 Eu 124.55(18) . . ? C9 N2 N1 110.0(3) . . ? C9 N2 B 132.0(3) . . ? N1 N2 B 117.9(2) . . ? C20 N3 N4 106.5(2) . . ? C20 N3 Eu 124.85(19) . . ? N4 N3 Eu 119.58(17) . . ? C18 N4 N3 109.4(2) . . ? C18 N4 B 128.0(3) . . ? N3 N4 B 122.5(2) . . ? C29 N5 N6 106.0(2) . . ? C29 N5 Eu 132.39(19) . . ? N6 N5 Eu 121.05(16) . . ? C27 N6 N5 109.9(2) . . ? C27 N6 B 126.7(2) . . ? N5 N6 B 123.4(2) . . ? C38 N7 N8 105.7(3) . . ? C36 N8 N7 109.8(3) . . ? C36 N8 B 128.1(3) . . ? N7 N8 B 119.9(2) . . ? N2 C9 C10 108.5(3) . . ? C9 C10 C11 105.3(3) . . ? N1 C11 C10 110.7(3) . . ? N1 C11 C12 122.8(3) . . ? C10 C11 C12 126.4(3) . . ? C17 C12 C13 118.6(3) . . ? C17 C12 C11 117.3(3) . . ? C13 C12 C11 124.1(3) . . ? C14 C13 C12 119.6(3) . . ? C14 C13 P1 119.8(2) . . ? C12 C13 P1 120.6(2) . . ? C15 C14 C13 120.1(3) . . ? C16 C15 C14 120.3(3) . . ? C15 C16 C17 120.1(3) . . ? C16 C17 C12 121.1(3) . . ? N4 C18 C19 109.2(3) . . ? C18 C19 C20 105.2(3) . . ? N3 C20 C19 109.6(3) . . ? N3 C20 C21 123.7(3) . . ? C19 C20 C21 126.6(3) . . ? C26 C21 C22 117.7(3) . . ? C26 C21 C20 116.6(3) . . ? C22 C21 C20 125.5(3) . . ? C23 C22 C21 119.4(3) . . ? C23 C22 P2 118.7(2) . . ? C21 C22 P2 121.9(2) . . ? C24 C23 C22 121.7(3) . . ? C25 C24 C23 119.1(3) . . ? C24 C25 C26 120.2(3) . . ? C25 C26 C21 121.9(4) . . ? N6 C27 C28 108.8(3) . . ? C27 C28 C29 105.0(3) . . ? N5 C29 C28 110.4(3) . . ? N5 C29 C30 123.3(3) . . ? C28 C29 C30 126.0(3) . . ? C35 C30 C31 118.4(3) . . ? C35 C30 C29 116.7(3) . . ? C31 C30 C29 124.9(3) . . ? C32 C31 C30 119.3(3) . . ? C32 C31 P3 120.6(3) . . ? C30 C31 P3 120.0(2) . . ? C33 C32 C31 120.7(3) . . ? C34 C33 C32 120.0(3) . . ? C33 C34 C35 120.2(3) . . ? C34 C35 C30 121.3(3) . . ? N8 C36 C37 107.8(3) . . ? C36 C37 C38 105.2(3) . . ? N7 C38 C37 111.3(3) . . ? N7 C38 C39 117.9(3) . . ? C37 C38 C39 130.7(3) . . ? C44 C39 C40 118.2(3) . . ? C44 C39 C38 117.9(3) . . ? C40 C39 C38 123.9(3) . . ? C41 C40 C39 118.8(3) . . ? C41 C40 P4 117.2(3) . . ? C39 C40 P4 123.9(3) . . ? C42 C41 C40 121.9(3) . . ? C43 C42 C41 119.3(4) . . ? C44 C43 C42 119.7(4) . . ? C43 C44 C39 122.1(3) . . ? C50 C45 C46 119.6(3) . . ? C50 C45 P1 122.3(2) . . ? C46 C45 P1 118.1(2) . . ? C47 C46 C45 119.9(3) . . ? C48 C47 C46 120.1(3) . . ? C47 C48 C49 120.5(3) . . ? C48 C49 C50 119.7(4) . . ? C45 C50 C49 120.3(3) . . ? C56 C51 C52 119.3(3) . . ? C56 C51 P1 118.0(2) . . ? C52 C51 P1 122.7(3) . . ? C53 C52 C51 119.6(3) . . ? C54 C53 C52 120.7(3) . . ? C55 C54 C53 119.9(3) . . ? C54 C55 C56 120.2(4) . . ? C55 C56 C51 120.2(3) . . ? C62 C57 C58 119.4(3) . . ? C62 C57 P2 118.5(2) . . ? C58 C57 P2 122.1(3) . . ? C59 C58 C57 119.8(4) . . ? C60 C59 C58 120.6(4) . . ? C59 C60 C61 120.4(4) . . ? C62 C61 C60 119.6(4) . . ? C57 C62 C61 120.3(3) . . ? C64 C63 C68 119.3(3) . . ? C64 C63 P2 117.0(2) . . ? C68 C63 P2 123.4(3) . . ? C63 C64 C65 120.3(3) . . ? C66 C65 C64 120.2(4) . . ? C65 C66 C67 119.9(3) . . ? C66 C67 C68 120.4(4) . . ? C67 C68 C63 119.8(4) . . ? C70 C69 C74 119.9(3) . . ? C70 C69 P3 118.4(2) . . ? C74 C69 P3 121.7(3) . . ? C69 C70 C71 119.7(3) . . ? C72 C71 C70 120.1(4) . . ? C71 C72 C73 120.1(3) . . ? C74 C73 C72 120.5(3) . . ? C73 C74 C69 119.8(3) . . ? C80 C75 C76 120.0(3) . . ? C80 C75 P3 116.5(2) . . ? C76 C75 P3 123.4(3) . . ? C77 C76 C75 118.6(3) . . ? C78 C77 C76 121.1(3) . . ? C77 C78 C79 120.4(3) . . ? C78 C79 C80 119.4(3) . . ? C75 C80 C79 120.5(3) . . ? C82 C81 C86 118.4(4) . . ? C82 C81 P4 124.6(3) . . ? C86 C81 P4 116.9(3) . . ? C83 C82 C81 120.4(4) . . ? C84 C83 C82 120.3(4) . . ? C85 C84 C83 119.8(4) . . ? C86 C85 C84 120.7(4) . . ? C85 C86 C81 120.4(4) . . ? C92 C87 C88 119.1(5) . . ? C92 C87 P4 122.0(3) . . ? C88 C87 P4 118.7(4) . . ? C87 C88 C89 120.7(6) . . ? C88 C89 C90 119.1(6) . . ? C91 C90 C89 120.6(6) . . ? C90 C91 C92 119.7(7) . . ? C87 C92 C91 120.6(6) . . ? O103 N100 O102 123.2(3) . . ? O103 N100 O101 121.5(3) . . ? O102 N100 O101 115.4(3) . . ? O103 N100 Eu 172.4(3) . . ? O102 N100 Eu 62.78(16) . . ? O101 N100 Eu 52.75(15) . . ? N100 O101 Eu 102.72(19) . . ? N100 O102 Eu 92.64(18) . . ? O111 N110 O113 132.8(11) . . ? O111 N110 O112 113.0(10) . . ? O113 N110 O112 113.8(10) . . ? O117 N115 O116 125.9(14) . . ? O117 N115 O118 120.0(14) . . ? O116 N115 O118 112.2(13) . . ? O123 N120 O122 117.0(13) . . ? O123 N120 O121 124.6(14) . . ? O122 N120 O121 117.8(13) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 71.37 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.992 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.057 #===END