# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Shaowu Du' _publ_contact_author_email swdu@fjirsm.ac.cn loop_ _publ_author_name 'Huabin Zhang' 'Shaowu Du' data_1 _database_code_depnum_ccdc_archive 'CCDC 888382' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H34 Eu4 N O29, C3 H7 N O, 2(H O)' _chemical_formula_sum 'C54 H43 Eu4 N2 O32' _chemical_formula_weight 1839.74 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' Eu Eu -0.1578 3.6682 '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 10.849(3) _cell_length_b 14.172(5) _cell_length_c 20.208(7) _cell_angle_alpha 86.734(7) _cell_angle_beta 83.852(9) _cell_angle_gamma 79.093(7) _cell_volume 3031.2(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8881 _cell_measurement_theta_min 3.0437 _cell_measurement_theta_max 27.4758 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.016 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1778 _exptl_absorpt_coefficient_mu 4.178 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3707 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17415 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0756 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 24.00 _reflns_number_total 9130 _reflns_number_gt 7438 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0270P)^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 9130 _refine_ls_number_parameters 829 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.91444(3) 0.23152(2) 0.198240(16) 0.02092(10) Uani 1 1 d . . . Eu2 Eu 0.95526(3) -0.01258(2) 0.352541(17) 0.02360(11) Uani 1 1 d . . . Eu3 Eu 1.27052(3) -0.30708(2) 0.308763(16) 0.01930(10) Uani 1 1 d . . . Eu4 Eu 1.28967(3) -0.55458(2) 0.174336(16) 0.01899(10) Uani 1 1 d . . . O20 O 1.0726(4) -0.5344(3) 0.2028(2) 0.0321(12) Uani 1 1 d . . . O19 O 1.2759(5) -0.7202(3) 0.2097(2) 0.0337(12) Uani 1 1 d . . . O18 O 1.0539(5) -0.2303(3) 0.3234(2) 0.0308(12) Uani 1 1 d . . . O17 O 1.2109(4) -0.3396(3) 0.2046(2) 0.0285(12) Uani 1 1 d . . . O16 O 1.1298(4) 0.1762(3) 0.1620(2) 0.0399(14) Uani 1 1 d . . . H16A H 1.1351 0.1444 0.1288 0.060 Uiso 1 1 calc R . . O15 O 0.7669(4) 0.0980(3) 0.3462(2) 0.0306(12) Uani 1 1 d . . . O14 O 1.4615(4) -0.3632(3) 0.2487(2) 0.0326(12) Uani 1 1 d . . . O13 O 1.0682(4) -0.0894(3) 0.4435(2) 0.0339(12) Uani 1 1 d . . . H13A H 1.1232 -0.1337 0.4295 0.051 Uiso 1 1 calc R . . O11 O 1.4599(4) -0.4800(3) 0.1788(2) 0.0294(12) Uani 1 1 d . . . O10 O 0.7401(4) 0.2179(3) 0.2696(2) 0.0297(12) Uani 1 1 d . . . O6 O 1.4706(4) -0.6978(3) 0.1933(2) 0.0346(13) Uani 1 1 d . . . O3 O 0.9738(5) 0.3184(4) 0.0937(2) 0.0408(14) Uani 1 1 d . . . H3A H 0.9566 0.3764 0.0991 0.061 Uiso 1 1 calc R . . O2 O 0.9104(5) 0.0853(3) 0.1487(2) 0.0383(13) Uani 1 1 d . . . O29 O 1.2056(5) -0.4078(3) 0.1104(2) 0.0362(13) Uani 1 1 d . . . O28 O 0.7281(4) 0.2934(3) 0.1434(2) 0.0388(13) Uani 1 1 d . . . H28A H 0.6654 0.2875 0.1687 0.058 Uiso 1 1 calc R . . O27 O 0.9243(5) -0.6213(3) 0.2335(2) 0.0408(14) Uani 1 1 d . . . O26 O 1.2690(5) -0.5382(4) 0.2893(3) 0.0470(15) Uani 1 1 d . . . O25 O 0.8601(5) -0.1488(3) 0.3460(3) 0.0547(17) Uani 1 1 d . . . O24 O 1.1993(5) -0.4349(3) 0.3684(3) 0.0471(15) Uani 1 1 d . . . O23 O 0.8134(5) -0.0184(4) 0.4579(3) 0.0455(14) Uani 1 1 d . . . O22 O 0.9566(5) -0.0061(4) 0.2388(2) 0.0482(15) Uani 1 1 d . . . C4 C 1.3923(7) -0.7532(5) 0.2096(3) 0.0224(16) Uani 1 1 d . . . C3 C 1.4975(6) -0.4071(5) 0.1940(3) 0.0255(17) Uani 1 1 d . . . C2 C 0.9708(7) -0.5458(4) 0.2339(3) 0.0259(17) Uani 1 1 d . . . C23 C 0.9930(6) -0.0806(4) 0.1345(3) 0.0216(16) Uani 1 1 d . . . C22 C 0.7251(6) 0.1834(5) 0.3285(3) 0.0229(16) Uani 1 1 d . . . C21 C 1.1052(6) -0.2447(4) 0.1194(3) 0.0212(16) Uani 1 1 d . . . C20 C 1.4331(6) -0.8583(4) 0.2251(3) 0.0222(16) Uani 1 1 d . . . C19 C 1.0617(6) -0.1648(4) 0.1601(3) 0.0219(16) Uani 1 1 d . . . H19A H 1.0794 -0.1687 0.2043 0.026 Uiso 1 1 calc R . . C18 C 0.5653(7) 0.3288(5) 0.3615(3) 0.0301(18) Uani 1 1 d . . . H18A H 0.5499 0.3394 0.3171 0.036 Uiso 1 1 calc R . . C17 C 0.6530(6) 0.2506(4) 0.3795(3) 0.0211(16) Uani 1 1 d . . . C16 C 0.9512(6) 0.0045(5) 0.1774(4) 0.0262(17) Uani 1 1 d . . . C15 C 1.6029(6) -0.3929(4) 0.0790(3) 0.0240(17) Uani 1 1 d . . . H15A H 1.5546 -0.4352 0.0662 0.029 Uiso 1 1 calc R . . C14 C 0.8954(6) -0.4674(4) 0.2759(3) 0.0223(16) Uani 1 1 d . . . C13 C 1.5923(6) -0.3696(4) 0.1451(3) 0.0237(16) Uani 1 1 d . . . C12 C 1.0762(6) -0.2366(4) 0.0533(3) 0.0260(17) Uani 1 1 d . . . H12A H 1.1029 -0.2890 0.0262 0.031 Uiso 1 1 calc R . . C11 C 1.1785(6) -0.3365(5) 0.1459(3) 0.0243(16) Uani 1 1 d . . . C10 C 1.6657(7) -0.3066(5) 0.1644(4) 0.036(2) Uani 1 1 d . . . H10A H 1.6604 -0.2906 0.2088 0.044 Uiso 1 1 calc R . . C43 C 1.3433(6) -0.9110(4) 0.2522(3) 0.0231(16) Uani 1 1 d . . . H43A H 1.2614 -0.8797 0.2645 0.028 Uiso 1 1 calc R . . C41 C 1.1136(6) -0.6646(4) 0.3574(3) 0.0261(17) Uani 1 1 d . . . H41A H 1.1349 -0.6744 0.3121 0.031 Uiso 1 1 calc R . . C40 C 1.6822(7) -0.3558(5) 0.0320(3) 0.0263(17) Uani 1 1 d . . . C39 C 0.8783(6) -0.3111(4) 0.3223(3) 0.0238(16) Uani 1 1 d . . . C38 C 0.6798(6) 0.2373(5) 0.4455(3) 0.0240(16) Uani 1 1 d . . . H38A H 0.7399 0.1853 0.4580 0.029 Uiso 1 1 calc R . . C34 C 1.1472(6) -0.5873(4) 0.3864(3) 0.0242(17) Uani 1 1 d . . . C33 C 0.9462(6) -0.3854(4) 0.2839(3) 0.0262(17) Uani 1 1 d . . . H33A H 1.0259 -0.3807 0.2633 0.031 Uiso 1 1 calc R . . C32 C 0.9356(8) -0.2250(5) 0.3310(4) 0.0315(19) Uani 1 1 d . . . C31 C 1.1227(7) -0.5772(5) 0.4537(3) 0.037(2) Uani 1 1 d . . . H31A H 1.1497 -0.5281 0.4737 0.044 Uiso 1 1 calc R . . C65 C 1.0487(6) -0.7266(4) 0.3957(3) 0.0249(17) Uani 1 1 d . . . C63 C 1.0095(7) -0.1536(5) 0.0276(3) 0.0292(18) Uani 1 1 d . . . H63A H 0.9925 -0.1495 -0.0167 0.035 Uiso 1 1 calc R . . C61 C 1.2105(7) -0.5161(5) 0.3444(4) 0.0287(18) Uani 1 1 d . . . C60 C 0.7780(7) -0.4741(5) 0.3078(4) 0.039(2) Uani 1 1 d . . . H60A H 0.7451 -0.5294 0.3041 0.047 Uiso 1 1 calc R . . C59 C 0.9667(6) -0.0747(5) 0.0679(3) 0.0267(17) Uani 1 1 d . . . H59A H 0.9209 -0.0184 0.0504 0.032 Uiso 1 1 calc R . . C58 C 0.4995(7) 0.3920(5) 0.4085(4) 0.041(2) Uani 1 1 d . . . H58A H 0.4388 0.4436 0.3959 0.049 Uiso 1 1 calc R . . C57 C 1.0204(7) -0.7126(5) 0.4638(3) 0.035(2) Uani 1 1 d . . . H57A H 0.9757 -0.7534 0.4899 0.042 Uiso 1 1 calc R . . C56 C 1.5570(7) -0.9046(5) 0.2118(4) 0.039(2) Uani 1 1 d . . . H56A H 1.6184 -0.8692 0.1954 0.047 Uiso 1 1 calc R . . C55 C 0.7594(7) -0.3187(5) 0.3522(4) 0.042(2) Uani 1 1 d . . . H55A H 0.7130 -0.2684 0.3771 0.051 Uiso 1 1 calc R . . C80 C 1.7549(7) -0.2921(6) 0.0510(4) 0.042(2) Uani 1 1 d . . . H80A H 1.8090 -0.2660 0.0194 0.050 Uiso 1 1 calc R . . O49 O 1.2434(7) 0.0703(6) 0.0605(4) 0.091(2) Uani 1 1 d . . . C77 C 1.0581(8) -0.6393(5) 0.4923(4) 0.046(2) Uani 1 1 d . . . H77A H 1.0402 -0.6309 0.5379 0.055 Uiso 1 1 calc R . . C76 C 1.7460(7) -0.2681(5) 0.1172(4) 0.045(2) Uani 1 1 d . . . H76A H 1.7944 -0.2259 0.1299 0.054 Uiso 1 1 calc R . . C75 C 1.5901(7) -1.0025(5) 0.2226(4) 0.051(2) Uani 1 1 d . . . H75A H 1.6736 -1.0330 0.2141 0.061 Uiso 1 1 calc R . . N1 N 0.6740(7) -0.0789(6) 0.5295(5) 0.070(2) Uani 1 1 d . . . C73 C 0.7082(7) -0.3994(5) 0.3457(4) 0.047(2) Uani 1 1 d . . . H73A H 0.6285 -0.4038 0.3662 0.056 Uiso 1 1 calc R . . N2 N 1.3545(8) -0.0771(6) 0.0397(5) 0.079(3) Uani 1 1 d . . . C71 C 0.7674(10) -0.0817(8) 0.4887(5) 0.075(3) Uani 1 1 d . . . C70 C 1.2882(10) -0.0066(8) 0.0811(7) 0.092(4) Uani 1 1 d . . . H70A H 1.2788 -0.0203 0.1267 0.110 Uiso 1 1 calc R . . O51 O 0.6554(5) 0.3659(4) 0.0239(3) 0.0521(15) Uani 1 1 d . . . H51B H 0.6315 0.4301 0.0192 0.063 Uiso 1 1 d R . . O50 O 0.9515(10) 0.5092(7) 0.0643(5) 0.178(5) Uani 1 1 d . . . H50B H 0.9353 0.5670 0.0830 0.214 Uiso 1 1 d R . . C88 C 0.6276(11) -0.1534(9) 0.5683(6) 0.113(5) Uani 1 1 d . . . H88A H 0.6619 -0.2140 0.5486 0.170 Uiso 1 1 calc R . . H88B H 0.5373 -0.1421 0.5700 0.170 Uiso 1 1 calc R . . H88C H 0.6523 -0.1545 0.6126 0.170 Uiso 1 1 calc R . . C87 C 0.6186(12) 0.0182(9) 0.5602(6) 0.118(5) Uani 1 1 d . . . H87A H 0.6507 0.0684 0.5339 0.177 Uiso 1 1 calc R . . H87B H 0.6420 0.0175 0.6047 0.177 Uiso 1 1 calc R . . H87C H 0.5283 0.0295 0.5613 0.177 Uiso 1 1 calc R . . C86 C 1.4093(11) -0.1695(9) 0.0723(7) 0.127(5) Uani 1 1 d . . . H86A H 1.3917 -0.1655 0.1197 0.191 Uiso 1 1 calc R . . H86B H 1.4989 -0.1827 0.0608 0.191 Uiso 1 1 calc R . . H86C H 1.3729 -0.2202 0.0573 0.191 Uiso 1 1 calc R . . C85 C 1.3688(12) -0.0667(12) -0.0299(7) 0.150(7) Uani 1 1 d . . . H85A H 1.3294 -0.0031 -0.0433 0.225 Uiso 1 1 calc R . . H85B H 1.3300 -0.1131 -0.0487 0.225 Uiso 1 1 calc R . . H85C H 1.4570 -0.0769 -0.0453 0.225 Uiso 1 1 calc R . . C64A C 1.0133(6) -0.8112(5) 0.3660(4) 0.0247(17) Uani 1 1 d . . . O12A O 0.9937(5) -0.8798(3) 0.4076(2) 0.0335(13) Uani 1 1 d . . . O9A O 1.0043(4) -0.8141(3) 0.3044(2) 0.0323(12) Uani 1 1 d . . . C36A C 1.6916(7) -0.3833(5) -0.0397(3) 0.0257(17) Uani 1 1 d . . . O7A O 1.6058(4) -0.4215(3) -0.0591(2) 0.0298(12) Uani 1 1 d . . . O5A O 1.7845(5) -0.3704(4) -0.0793(2) 0.0411(14) Uani 1 1 d . . . C35A C 1.3749(7) -1.0103(5) 0.2612(3) 0.0264(17) Uani 1 1 d . . . C1A C 1.2734(7) -1.0669(5) 0.2855(3) 0.0245(17) Uani 1 1 d . . . C78A C 1.4981(7) -1.0555(5) 0.2464(4) 0.043(2) Uani 1 1 d . . . H78A H 1.5199 -1.1219 0.2523 0.052 Uiso 1 1 calc R . . O4A O 1.1721(5) -1.0250(3) 0.3128(3) 0.0364(13) Uani 1 1 d . . . O21A O 1.3002(5) -1.1558(3) 0.2759(3) 0.0421(14) Uani 1 1 d . . . C62A C 0.5249(7) 0.3777(5) 0.4734(4) 0.0370(19) Uani 1 1 d . . . H62A H 0.4798 0.4196 0.5050 0.044 Uiso 1 1 calc R . . C42A C 0.6160(6) 0.3026(5) 0.4935(3) 0.0248(17) Uani 1 1 d . . . C37A C 0.6490(7) 0.2949(5) 0.5640(3) 0.0259(17) Uani 1 1 d . . . O8A O 0.5842(5) 0.3483(4) 0.6067(2) 0.0423(14) Uani 1 1 d . . . O1A O 0.7454(5) 0.2366(3) 0.5806(2) 0.0359(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0269(2) 0.01467(18) 0.0231(2) -0.00710(14) -0.00238(16) -0.00693(15) Eu2 0.0329(2) 0.01448(18) 0.0247(2) -0.00554(15) -0.00617(17) -0.00433(16) Eu3 0.0278(2) 0.01205(17) 0.0190(2) -0.00410(14) 0.00019(16) -0.00654(15) Eu4 0.0244(2) 0.01402(18) 0.0197(2) -0.00222(14) -0.00122(16) -0.00646(15) O20 0.019(3) 0.031(3) 0.046(3) -0.017(2) 0.007(3) -0.004(2) O19 0.032(3) 0.018(3) 0.053(4) 0.003(2) -0.006(3) -0.010(2) O18 0.034(3) 0.032(3) 0.032(3) -0.008(2) -0.005(2) -0.017(2) O17 0.029(3) 0.031(3) 0.023(3) 0.002(2) -0.007(2) 0.001(2) O16 0.033(3) 0.040(3) 0.051(4) -0.019(3) -0.002(3) -0.013(3) O15 0.034(3) 0.027(3) 0.028(3) -0.003(2) -0.001(2) 0.000(2) O14 0.027(3) 0.043(3) 0.029(3) -0.018(2) 0.008(2) -0.011(2) O13 0.045(3) 0.021(3) 0.033(3) -0.006(2) -0.009(2) 0.007(2) O11 0.030(3) 0.027(3) 0.034(3) -0.009(2) 0.002(2) -0.014(2) O10 0.032(3) 0.040(3) 0.019(3) 0.002(2) -0.002(2) -0.011(2) O6 0.032(3) 0.019(3) 0.055(4) 0.005(2) -0.005(3) -0.013(2) O3 0.048(4) 0.045(3) 0.035(3) -0.004(2) -0.006(3) -0.020(3) O2 0.053(4) 0.011(3) 0.052(4) -0.014(2) -0.004(3) -0.005(2) O29 0.057(4) 0.016(3) 0.035(3) -0.006(2) -0.014(3) 0.001(2) O28 0.026(3) 0.049(3) 0.039(3) 0.012(3) 0.000(2) -0.006(3) O27 0.060(4) 0.019(3) 0.049(4) -0.014(2) 0.001(3) -0.021(3) O26 0.056(4) 0.068(4) 0.026(3) 0.005(3) -0.004(3) -0.036(3) O25 0.036(4) 0.025(3) 0.107(5) -0.032(3) 0.000(3) -0.010(3) O24 0.077(4) 0.025(3) 0.046(4) 0.010(3) -0.004(3) -0.030(3) O23 0.050(4) 0.042(3) 0.043(4) 0.009(3) 0.005(3) -0.012(3) O22 0.065(4) 0.053(4) 0.022(3) -0.022(3) -0.010(3) 0.011(3) C4 0.027(5) 0.022(4) 0.019(4) -0.001(3) -0.007(3) -0.005(3) C3 0.026(4) 0.026(4) 0.027(4) -0.006(3) -0.008(3) -0.006(3) C2 0.029(5) 0.017(4) 0.034(5) -0.008(3) -0.012(4) -0.004(3) C23 0.028(4) 0.016(3) 0.020(4) -0.009(3) 0.002(3) -0.003(3) C22 0.018(4) 0.030(4) 0.023(5) -0.005(3) -0.002(3) -0.010(3) C21 0.026(4) 0.016(3) 0.022(4) -0.001(3) -0.002(3) -0.005(3) C20 0.024(4) 0.017(3) 0.028(4) -0.006(3) -0.004(3) -0.008(3) C19 0.027(4) 0.022(4) 0.018(4) -0.005(3) -0.005(3) -0.006(3) C18 0.034(5) 0.035(4) 0.021(4) -0.001(3) -0.008(4) -0.004(4) C17 0.025(4) 0.019(4) 0.020(4) 0.003(3) -0.003(3) -0.008(3) C16 0.020(4) 0.023(4) 0.036(5) -0.016(3) -0.005(3) -0.001(3) C15 0.030(4) 0.024(4) 0.021(4) -0.014(3) 0.002(3) -0.009(3) C14 0.027(4) 0.017(4) 0.024(4) -0.011(3) 0.001(3) -0.006(3) C13 0.020(4) 0.021(4) 0.031(5) -0.005(3) 0.000(3) -0.006(3) C12 0.042(5) 0.015(4) 0.023(4) -0.011(3) -0.006(3) -0.005(3) C11 0.026(4) 0.022(4) 0.027(4) -0.001(3) -0.005(3) -0.009(3) C10 0.047(5) 0.046(5) 0.023(4) -0.011(4) 0.003(4) -0.024(4) C43 0.025(4) 0.022(4) 0.022(4) -0.003(3) 0.002(3) -0.003(3) C41 0.028(4) 0.024(4) 0.027(4) -0.007(3) -0.005(3) -0.007(3) C40 0.032(5) 0.027(4) 0.022(4) -0.009(3) 0.002(3) -0.011(3) C39 0.021(4) 0.017(4) 0.033(4) -0.013(3) 0.000(3) -0.001(3) C38 0.025(4) 0.020(4) 0.025(4) 0.001(3) -0.001(3) -0.002(3) C34 0.039(5) 0.021(4) 0.017(4) 0.003(3) -0.002(3) -0.019(3) C33 0.024(4) 0.025(4) 0.033(5) -0.005(3) -0.006(3) -0.010(3) C32 0.046(6) 0.017(4) 0.036(5) -0.012(3) -0.010(4) -0.008(4) C31 0.072(6) 0.025(4) 0.022(5) -0.006(3) -0.001(4) -0.032(4) C65 0.034(5) 0.011(3) 0.031(5) 0.003(3) -0.003(4) -0.011(3) C63 0.040(5) 0.020(4) 0.027(4) -0.006(3) -0.007(4) 0.000(3) C61 0.037(5) 0.029(4) 0.026(5) 0.004(3) -0.013(4) -0.017(4) C60 0.034(5) 0.035(5) 0.053(6) -0.016(4) 0.005(4) -0.018(4) C59 0.041(5) 0.017(4) 0.021(4) -0.002(3) -0.008(3) 0.000(3) C58 0.045(5) 0.032(4) 0.041(5) -0.003(4) -0.020(4) 0.011(4) C57 0.063(6) 0.024(4) 0.020(4) -0.003(3) 0.012(4) -0.024(4) C56 0.039(5) 0.026(4) 0.058(6) 0.001(4) -0.003(4) -0.020(4) C55 0.032(5) 0.032(4) 0.063(6) -0.025(4) 0.008(4) -0.005(4) C80 0.040(5) 0.057(5) 0.036(5) -0.011(4) 0.011(4) -0.034(4) O49 0.087(6) 0.083(6) 0.095(6) -0.025(5) -0.010(5) 0.010(5) C77 0.086(7) 0.042(5) 0.015(4) -0.002(4) 0.008(4) -0.034(5) C76 0.054(6) 0.052(5) 0.039(5) -0.021(4) 0.007(4) -0.040(5) C75 0.027(5) 0.026(4) 0.095(7) 0.003(4) 0.002(5) 0.000(4) N1 0.045(5) 0.058(5) 0.098(7) 0.029(5) 0.016(5) -0.010(4) C73 0.037(5) 0.046(5) 0.063(6) -0.031(4) 0.012(4) -0.021(4) N2 0.060(6) 0.061(6) 0.119(9) -0.038(6) -0.022(6) 0.004(5) C71 0.053(7) 0.089(8) 0.080(9) 0.033(7) 0.007(6) -0.019(6) C70 0.068(9) 0.062(8) 0.152(13) 0.004(8) -0.049(8) -0.009(7) O51 0.056(4) 0.050(4) 0.043(4) 0.013(3) -0.013(3) 0.009(3) O50 0.201(11) 0.104(8) 0.218(12) 0.033(8) -0.050(9) 0.006(8) C88 0.116(11) 0.133(11) 0.107(10) 0.055(9) -0.019(8) -0.078(9) C87 0.116(12) 0.141(13) 0.105(11) -0.028(9) -0.002(9) -0.043(10) C86 0.090(10) 0.084(10) 0.209(16) -0.015(10) -0.044(10) 0.000(8) C85 0.102(12) 0.26(2) 0.091(12) -0.056(12) 0.016(9) -0.031(12) C64A 0.014(4) 0.021(4) 0.040(5) -0.008(3) -0.001(3) -0.003(3) O12A 0.053(4) 0.016(3) 0.037(3) 0.001(2) -0.010(3) -0.017(2) O9A 0.032(3) 0.032(3) 0.036(3) -0.014(2) -0.010(2) -0.005(2) C36A 0.033(5) 0.018(4) 0.027(4) -0.005(3) 0.000(4) -0.005(3) O7A 0.030(3) 0.041(3) 0.021(3) -0.012(2) 0.009(2) -0.014(2) O5A 0.048(4) 0.054(4) 0.028(3) -0.012(3) 0.007(3) -0.030(3) C35A 0.033(5) 0.019(4) 0.029(4) 0.004(3) -0.006(4) -0.010(3) C1A 0.033(5) 0.021(4) 0.019(4) 0.000(3) 0.002(4) -0.007(3) C78A 0.039(5) 0.019(4) 0.070(6) 0.001(4) -0.004(5) -0.002(4) O4A 0.027(3) 0.027(3) 0.053(4) -0.002(2) 0.011(3) -0.008(2) O21A 0.054(4) 0.015(3) 0.058(4) -0.004(2) 0.011(3) -0.014(3) C62A 0.036(5) 0.033(4) 0.040(5) -0.014(4) -0.002(4) 0.001(4) C42A 0.026(4) 0.024(4) 0.025(4) -0.003(3) -0.004(3) -0.005(3) C37A 0.028(5) 0.028(4) 0.023(4) -0.006(3) 0.000(4) -0.009(4) O8A 0.035(3) 0.059(4) 0.027(3) -0.017(3) -0.005(3) 0.011(3) O1A 0.040(3) 0.035(3) 0.029(3) -0.016(2) -0.012(3) 0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O27 2.267(4) 1_565 ? Eu1 O10 2.284(5) . ? Eu1 O2 2.362(4) . ? Eu1 O16 2.370(5) . ? Eu1 O28 2.405(5) . ? Eu1 O9A 2.455(5) 1_565 ? Eu1 O3 2.471(5) . ? Eu1 C16 3.213(6) . ? Eu2 O22 2.294(5) . ? Eu2 O15 2.339(5) . ? Eu2 O12A 2.365(4) 1_565 ? Eu2 O25 2.371(5) . ? Eu2 O4A 2.380(5) 1_565 ? Eu2 O13 2.410(4) . ? Eu2 O23 2.497(5) . ? Eu2 O9A 3.047(5) 1_565 ? Eu2 C64A 3.069(6) 1_565 ? Eu2 C32 3.115(6) . ? Eu2 O18 3.136(5) . ? Eu3 O21A 2.279(4) 1_565 ? Eu3 O14 2.313(5) . ? Eu3 O24 2.326(4) . ? Eu3 O17 2.362(4) . ? Eu3 O18 2.391(5) . ? Eu3 O8A 2.421(5) 2_756 ? Eu3 O1A 2.476(4) 2_756 ? Eu3 C37A 2.826(7) 2_756 ? Eu3 C61 3.178(7) . ? Eu4 O11 2.307(4) . ? Eu4 O26 2.330(5) . ? Eu4 O20 2.331(5) . ? Eu4 O19 2.441(4) . ? Eu4 O29 2.462(4) . ? Eu4 O7A 2.490(4) 2_845 ? Eu4 O5A 2.520(4) 2_845 ? Eu4 O6 2.586(5) . ? Eu4 C36A 2.882(7) 2_845 ? Eu4 C4 2.903(7) . ? Eu4 O17 3.083(4) . ? Eu4 C11 3.142(7) . ? O20 C2 1.245(8) . ? O19 C4 1.261(7) . ? O18 C32 1.265(8) . ? O17 C11 1.268(7) . ? O15 C22 1.256(8) . ? O14 C3 1.286(7) . ? O11 C3 1.245(7) . ? O10 C22 1.266(7) . ? O6 C4 1.268(7) . ? O2 C16 1.277(8) . ? O29 C11 1.243(7) . ? O27 C2 1.266(7) . ? O27 Eu1 2.267(4) 1_545 ? O26 C61 1.246(8) . ? O25 C32 1.256(8) . ? O24 C61 1.255(8) . ? O23 C71 1.216(10) . ? O22 C16 1.247(8) . ? C4 C20 1.497(9) . ? C3 C13 1.498(9) . ? C2 C14 1.496(9) . ? C23 C19 1.387(8) . ? C23 C59 1.400(9) . ? C23 C16 1.497(8) . ? C22 C17 1.497(9) . ? C21 C12 1.398(8) . ? C21 C19 1.415(8) . ? C21 C11 1.494(9) . ? C20 C56 1.384(9) . ? C20 C43 1.386(9) . ? C18 C17 1.377(9) . ? C18 C58 1.386(9) . ? C17 C38 1.389(9) . ? C15 C40 1.363(9) . ? C15 C13 1.382(9) . ? C14 C60 1.382(9) . ? C14 C33 1.402(8) . ? C13 C10 1.400(9) . ? C12 C63 1.367(9) . ? C10 C76 1.382(10) . ? C43 C35A 1.390(8) . ? C41 C65 1.381(9) . ? C41 C34 1.396(8) . ? C40 C80 1.400(9) . ? C40 C36A 1.509(9) . ? C39 C55 1.385(9) . ? C39 C33 1.391(9) . ? C39 C32 1.497(9) . ? C38 C42A 1.412(9) . ? C34 C31 1.368(9) . ? C34 C61 1.501(9) . ? C31 C77 1.383(9) . ? C65 C57 1.395(9) . ? C65 C64A 1.501(8) . ? C63 C59 1.397(8) . ? C60 C73 1.394(10) . ? C58 C62A 1.366(10) . ? C57 C77 1.363(9) . ? C56 C75 1.376(9) . ? C55 C73 1.380(9) . ? C80 C76 1.387(10) . ? O49 C70 1.178(11) . ? C75 C78A 1.389(10) . ? N1 C71 1.232(11) . ? N1 C88 1.416(11) . ? N1 C87 1.531(13) . ? N2 C70 1.381(14) . ? N2 C85 1.401(13) . ? N2 C86 1.481(13) . ? C64A O9A 1.263(8) . ? C64A O12A 1.282(8) . ? C64A Eu2 3.069(6) 1_545 ? O12A Eu2 2.365(4) 1_545 ? O9A Eu1 2.455(5) 1_545 ? O9A Eu2 3.047(5) 1_545 ? C36A O5A 1.254(8) . ? C36A O7A 1.268(7) . ? C36A Eu4 2.882(7) 2_845 ? O7A Eu4 2.490(4) 2_845 ? O5A Eu4 2.520(4) 2_845 ? C35A C78A 1.378(9) . ? C35A C1A 1.507(9) . ? C1A O4A 1.235(8) . ? C1A O21A 1.260(8) . ? O4A Eu2 2.380(5) 1_545 ? O21A Eu3 2.279(4) 1_545 ? C62A C42A 1.384(9) . ? C42A C37A 1.499(9) . ? C37A O8A 1.246(8) . ? C37A O1A 1.267(8) . ? C37A Eu3 2.826(7) 2_756 ? O8A Eu3 2.421(5) 2_756 ? O1A Eu3 2.476(4) 2_756 ? 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 O27 Eu1 O10 93.24(17) 1_565 . ? O27 Eu1 O2 173.25(17) 1_565 . ? O10 Eu1 O2 91.91(17) . . ? O27 Eu1 O16 100.19(17) 1_565 . ? O10 Eu1 O16 149.75(17) . . ? O2 Eu1 O16 77.31(16) . . ? O27 Eu1 O28 92.31(18) 1_565 . ? O10 Eu1 O28 70.71(16) . . ? O2 Eu1 O28 85.27(17) . . ? O16 Eu1 O28 134.86(17) . . ? O27 Eu1 O9A 79.81(17) 1_565 1_565 ? O10 Eu1 O9A 77.54(16) . 1_565 ? O2 Eu1 O9A 105.60(16) . 1_565 ? O16 Eu1 O9A 78.34(16) . 1_565 ? O28 Eu1 O9A 146.79(16) . 1_565 ? O27 Eu1 O3 77.30(17) 1_565 . ? O10 Eu1 O3 139.86(17) . . ? O2 Eu1 O3 95.95(17) . . ? O16 Eu1 O3 70.04(17) . . ? O28 Eu1 O3 70.83(16) . . ? O9A Eu1 O3 136.48(15) 1_565 . ? O27 Eu1 C16 164.87(18) 1_565 . ? O10 Eu1 C16 87.77(17) . . ? O2 Eu1 C16 19.92(17) . . ? O16 Eu1 C16 72.44(16) . . ? O28 Eu1 C16 102.25(17) . . ? O9A Eu1 C16 85.68(17) 1_565 . ? O3 Eu1 C16 111.23(18) . . ? O22 Eu2 O15 82.77(17) . . ? O22 Eu2 O12A 119.99(18) . 1_565 ? O15 Eu2 O12A 77.60(16) . 1_565 ? O22 Eu2 O25 83.7(2) . . ? O15 Eu2 O25 94.28(17) . . ? O12A Eu2 O25 153.00(18) 1_565 . ? O22 Eu2 O4A 75.78(19) . 1_565 ? O15 Eu2 O4A 138.06(16) . 1_565 ? O12A Eu2 O4A 82.57(16) 1_565 1_565 ? O25 Eu2 O4A 118.17(17) . 1_565 ? O22 Eu2 O13 143.30(17) . . ? O15 Eu2 O13 133.89(15) . . ? O12A Eu2 O13 77.69(15) 1_565 . ? O25 Eu2 O13 90.56(18) . . ? O4A Eu2 O13 75.23(17) 1_565 . ? O22 Eu2 O23 142.52(19) . . ? O15 Eu2 O23 69.30(17) . . ? O12A Eu2 O23 78.75(17) 1_565 . ? O25 Eu2 O23 74.30(18) . . ? O4A Eu2 O23 141.50(18) 1_565 . ? O13 Eu2 O23 68.07(17) . . ? O22 Eu2 O9A 73.28(16) . 1_565 ? O15 Eu2 O9A 68.47(14) . 1_565 ? O12A Eu2 O9A 46.73(14) 1_565 1_565 ? O25 Eu2 O9A 152.51(17) . 1_565 ? O4A Eu2 O9A 70.98(14) 1_565 1_565 ? O13 Eu2 O9A 116.88(14) . 1_565 ? O23 Eu2 O9A 115.90(15) . 1_565 ? O22 Eu2 C64A 97.1(2) . 1_565 ? O15 Eu2 C64A 72.40(16) . 1_565 ? O12A Eu2 C64A 22.92(17) 1_565 1_565 ? O25 Eu2 C64A 166.37(17) . 1_565 ? O4A Eu2 C64A 75.00(16) 1_565 1_565 ? O13 Eu2 C64A 96.67(17) . 1_565 ? O23 Eu2 C64A 97.67(18) . 1_565 ? O9A Eu2 C64A 23.83(14) 1_565 1_565 ? O22 Eu2 C32 80.71(19) . . ? O15 Eu2 C32 114.69(19) . . ? O12A Eu2 C32 158.08(17) 1_565 . ? O25 Eu2 C32 21.45(19) . . ? O4A Eu2 C32 97.02(19) 1_565 . ? O13 Eu2 C32 81.01(17) . . ? O23 Eu2 C32 88.57(19) . . ? O9A Eu2 C32 153.28(16) 1_565 . ? C64A Eu2 C32 172.0(2) 1_565 . ? O22 Eu2 O18 80.11(15) . . ? O15 Eu2 O18 136.86(14) . . ? O12A Eu2 O18 144.51(14) 1_565 . ? O25 Eu2 O18 44.77(15) . . ? O4A Eu2 O18 74.22(14) 1_565 . ? O13 Eu2 O18 70.72(13) . . ? O23 Eu2 O18 103.25(15) . . ? O9A Eu2 O18 140.24(12) 1_565 . ? C64A Eu2 O18 148.82(15) 1_565 . ? C32 Eu2 O18 23.34(15) . . ? O21A Eu3 O14 87.25(17) 1_565 . ? O21A Eu3 O24 162.05(18) 1_565 . ? O14 Eu3 O24 109.31(18) . . ? O21A Eu3 O17 93.77(17) 1_565 . ? O14 Eu3 O17 76.84(16) . . ? O24 Eu3 O17 96.69(17) . . ? O21A Eu3 O18 82.99(17) 1_565 . ? O14 Eu3 O18 155.51(16) . . ? O24 Eu3 O18 84.18(18) . . ? O17 Eu3 O18 81.43(15) . . ? O21A Eu3 O8A 101.48(19) 1_565 2_756 ? O14 Eu3 O8A 76.30(17) . 2_756 ? O24 Eu3 O8A 76.74(19) . 2_756 ? O17 Eu3 O8A 148.28(16) . 2_756 ? O18 Eu3 O8A 127.65(16) . 2_756 ? O21A Eu3 O1A 80.67(17) 1_565 2_756 ? O14 Eu3 O1A 122.80(16) . 2_756 ? O24 Eu3 O1A 84.36(17) . 2_756 ? O17 Eu3 O1A 158.90(15) . 2_756 ? O18 Eu3 O1A 77.71(15) . 2_756 ? O8A Eu3 O1A 52.48(15) 2_756 2_756 ? O21A Eu3 C37A 93.19(19) 1_565 2_756 ? O14 Eu3 C37A 100.45(19) . 2_756 ? O24 Eu3 C37A 77.39(18) . 2_756 ? O17 Eu3 C37A 172.40(18) . 2_756 ? O18 Eu3 C37A 102.48(18) . 2_756 ? O8A Eu3 C37A 26.03(17) 2_756 2_756 ? O1A Eu3 C37A 26.60(16) 2_756 2_756 ? O21A Eu3 C61 174.58(18) 1_565 . ? O14 Eu3 C61 93.99(19) . . ? O24 Eu3 C61 19.50(19) . . ? O17 Eu3 C61 81.40(17) . . ? O18 Eu3 C61 93.81(17) . . ? O8A Eu3 C61 83.94(18) 2_756 . ? O1A Eu3 C61 102.97(18) 2_756 . ? C37A Eu3 C61 91.77(18) 2_756 . ? O11 Eu4 O26 82.78(16) . . ? O11 Eu4 O20 142.04(15) . . ? O26 Eu4 O20 76.57(17) . . ? O11 Eu4 O19 126.76(16) . . ? O26 Eu4 O19 81.04(17) . . ? O20 Eu4 O19 81.17(16) . . ? O11 Eu4 O29 83.82(16) . . ? O26 Eu4 O29 114.51(18) . . ? O20 Eu4 O29 76.49(17) . . ? O19 Eu4 O29 148.37(16) . . ? O11 Eu4 O7A 79.52(15) . 2_845 ? O26 Eu4 O7A 158.93(17) . 2_845 ? O20 Eu4 O7A 124.50(16) . 2_845 ? O19 Eu4 O7A 100.54(16) . 2_845 ? O29 Eu4 O7A 74.92(15) . 2_845 ? O11 Eu4 O5A 131.13(16) . 2_845 ? O26 Eu4 O5A 145.44(17) . 2_845 ? O20 Eu4 O5A 77.36(16) . 2_845 ? O19 Eu4 O5A 72.86(16) . 2_845 ? O29 Eu4 O5A 80.55(16) . 2_845 ? O7A Eu4 O5A 51.75(15) 2_845 2_845 ? O11 Eu4 O6 77.37(15) . . ? O26 Eu4 O6 86.51(18) . . ? O20 Eu4 O6 131.69(15) . . ? O19 Eu4 O6 51.36(15) . . ? O29 Eu4 O6 149.80(16) . . ? O7A Eu4 O6 78.55(16) 2_845 . ? O5A Eu4 O6 94.23(16) 2_845 . ? O11 Eu4 C36A 105.45(18) . 2_845 ? O26 Eu4 C36A 167.66(18) . 2_845 ? O20 Eu4 C36A 100.88(18) . 2_845 ? O19 Eu4 C36A 86.65(17) . 2_845 ? O29 Eu4 C36A 76.04(16) . 2_845 ? O7A Eu4 C36A 26.01(16) 2_845 2_845 ? O5A Eu4 C36A 25.74(16) 2_845 2_845 ? O6 Eu4 C36A 86.39(17) . 2_845 ? O11 Eu4 C4 102.37(18) . . ? O26 Eu4 C4 83.06(19) . . ? O20 Eu4 C4 106.27(18) . . ? O19 Eu4 C4 25.46(15) . . ? O29 Eu4 C4 162.15(16) . . ? O7A Eu4 C4 89.61(17) 2_845 . ? O5A Eu4 C4 82.88(17) 2_845 . ? O6 Eu4 C4 25.89(16) . . ? C36A Eu4 C4 86.15(18) 2_845 . ? O11 Eu4 O17 67.21(14) . . ? O26 Eu4 O17 71.02(16) . . ? O20 Eu4 O17 76.02(13) . . ? O19 Eu4 O17 147.20(15) . . ? O29 Eu4 O17 44.90(13) . . ? O7A Eu4 O17 111.74(14) 2_845 . ? O5A Eu4 O17 123.29(15) 2_845 . ? O6 Eu4 O17 139.72(13) . . ? C36A Eu4 O17 120.42(15) 2_845 . ? C4 Eu4 O17 152.85(15) . . ? O11 Eu4 C11 76.58(16) . . ? O26 Eu4 C11 93.24(19) . . ? O20 Eu4 C11 73.21(17) . . ? O19 Eu4 C11 154.38(17) . . ? O29 Eu4 C11 21.58(15) . . ? O7A Eu4 C11 93.69(17) 2_845 . ? O5A Eu4 C11 100.52(17) 2_845 . ? O6 Eu4 C11 153.77(15) . . ? C36A Eu4 C11 97.58(18) 2_845 . ? C4 Eu4 C11 176.27(17) . . ? O17 Eu4 C11 23.48(13) . . ? C2 O20 Eu4 159.0(5) . . ? C4 O19 Eu4 98.2(4) . . ? C32 O18 Eu3 156.8(4) . . ? C32 O18 Eu2 77.4(4) . . ? Eu3 O18 Eu2 125.56(16) . . ? C11 O17 Eu3 166.8(4) . . ? C11 O17 Eu4 80.9(4) . . ? Eu3 O17 Eu4 111.47(15) . . ? C22 O15 Eu2 141.9(4) . . ? C3 O14 Eu3 136.0(4) . . ? C3 O11 Eu4 146.8(5) . . ? C22 O10 Eu1 133.2(4) . . ? C4 O6 Eu4 91.2(4) . . ? C16 O2 Eu1 121.0(4) . . ? C11 O29 Eu4 111.7(4) . . ? C2 O27 Eu1 154.6(5) . 1_545 ? C61 O26 Eu4 155.0(5) . . ? C32 O25 Eu2 114.9(5) . . ? C61 O24 Eu3 122.3(5) . . ? C71 O23 Eu2 134.0(7) . . ? C16 O22 Eu2 174.9(5) . . ? O19 C4 O6 119.3(6) . . ? O19 C4 C20 118.3(6) . . ? O6 C4 C20 122.3(6) . . ? O19 C4 Eu4 56.3(3) . . ? O6 C4 Eu4 62.9(3) . . ? C20 C4 Eu4 173.9(5) . . ? O11 C3 O14 124.4(6) . . ? O11 C3 C13 117.1(6) . . ? O14 C3 C13 118.5(6) . . ? O20 C2 O27 124.6(6) . . ? O20 C2 C14 119.8(6) . . ? O27 C2 C14 115.7(6) . . ? C19 C23 C59 119.7(6) . . ? C19 C23 C16 119.9(6) . . ? C59 C23 C16 120.4(6) . . ? O15 C22 O10 124.4(6) . . ? O15 C22 C17 118.9(6) . . ? O10 C22 C17 116.7(6) . . ? C12 C21 C19 118.3(6) . . ? C12 C21 C11 120.1(6) . . ? C19 C21 C11 121.5(6) . . ? C56 C20 C43 119.3(6) . . ? C56 C20 C4 122.0(6) . . ? C43 C20 C4 118.7(6) . . ? C23 C19 C21 120.4(6) . . ? C17 C18 C58 121.2(7) . . ? C18 C17 C38 119.3(6) . . ? C18 C17 C22 120.9(6) . . ? C38 C17 C22 119.7(6) . . ? O22 C16 O2 123.1(6) . . ? O22 C16 C23 119.4(6) . . ? O2 C16 C23 117.5(6) . . ? O22 C16 Eu1 86.6(4) . . ? O2 C16 Eu1 39.0(3) . . ? C23 C16 Eu1 150.6(5) . . ? C40 C15 C13 121.9(6) . . ? C60 C14 C33 119.0(6) . . ? C60 C14 C2 122.0(6) . . ? C33 C14 C2 119.0(6) . . ? C15 C13 C10 119.0(6) . . ? C15 C13 C3 119.8(6) . . ? C10 C13 C3 121.1(6) . . ? C63 C12 C21 121.5(6) . . ? O29 C11 O17 121.7(6) . . ? O29 C11 C21 119.6(6) . . ? O17 C11 C21 118.7(6) . . ? O29 C11 Eu4 46.7(3) . . ? O17 C11 Eu4 75.6(4) . . ? C21 C11 Eu4 163.8(4) . . ? C76 C10 C13 119.6(6) . . ? C20 C43 C35A 120.4(6) . . ? C65 C41 C34 120.0(6) . . ? C15 C40 C80 119.2(6) . . ? C15 C40 C36A 120.4(6) . . ? C80 C40 C36A 120.5(6) . . ? C55 C39 C33 119.2(6) . . ? C55 C39 C32 121.4(6) . . ? C33 C39 C32 119.3(6) . . ? C17 C38 C42A 120.1(6) . . ? C31 C34 C41 119.5(6) . . ? C31 C34 C61 120.1(6) . . ? C41 C34 C61 120.4(6) . . ? C39 C33 C14 120.3(6) . . ? O25 C32 O18 122.8(6) . . ? O25 C32 C39 116.4(7) . . ? O18 C32 C39 120.8(6) . . ? O25 C32 Eu2 43.7(3) . . ? O18 C32 Eu2 79.2(4) . . ? C39 C32 Eu2 159.8(5) . . ? C34 C31 C77 120.5(6) . . ? C41 C65 C57 119.3(6) . . ? C41 C65 C64A 121.2(6) . . ? C57 C65 C64A 119.4(6) . . ? C12 C63 C59 120.1(6) . . ? O26 C61 O24 123.7(6) . . ? O26 C61 C34 120.8(6) . . ? O24 C61 C34 115.5(7) . . ? O26 C61 Eu3 85.6(4) . . ? O24 C61 Eu3 38.2(3) . . ? C34 C61 Eu3 153.3(5) . . ? C14 C60 C73 121.1(7) . . ? C63 C59 C23 119.9(6) . . ? C62A C58 C18 119.2(7) . . ? C77 C57 C65 120.2(6) . . ? C75 C56 C20 120.6(7) . . ? C73 C55 C39 121.3(7) . . ? C76 C80 C40 119.8(6) . . ? C57 C77 C31 120.3(7) . . ? C10 C76 C80 120.4(7) . . ? C56 C75 C78A 119.7(7) . . ? C71 N1 C88 130.7(10) . . ? C71 N1 C87 116.9(9) . . ? C88 N1 C87 109.7(9) . . ? C55 C73 C60 118.9(7) . . ? C70 N2 C85 124.0(11) . . ? C70 N2 C86 116.7(11) . . ? C85 N2 C86 119.3(10) . . ? O23 C71 N1 131.8(11) . . ? O49 C70 N2 122.2(13) . . ? O9A C64A O12A 122.9(6) . . ? O9A C64A C65 121.9(6) . . ? O12A C64A C65 115.1(6) . . ? O9A C64A Eu2 77.1(4) . 1_545 ? O12A C64A Eu2 45.9(3) . 1_545 ? C65 C64A Eu2 160.7(5) . 1_545 ? C64A O12A Eu2 111.1(4) . 1_545 ? C64A O9A Eu1 156.7(4) . 1_545 ? C64A O9A Eu2 79.1(4) . 1_545 ? Eu1 O9A Eu2 109.79(15) 1_545 1_545 ? O5A C36A O7A 120.2(6) . . ? O5A C36A C40 120.4(6) . . ? O7A C36A C40 119.3(6) . . ? O5A C36A Eu4 60.8(3) . 2_845 ? O7A C36A Eu4 59.5(3) . 2_845 ? C40 C36A Eu4 177.2(4) . 2_845 ? C36A O7A Eu4 94.5(4) . 2_845 ? C36A O5A Eu4 93.5(4) . 2_845 ? C78A C35A C43 119.4(6) . . ? C78A C35A C1A 121.1(6) . . ? C43 C35A C1A 119.4(6) . . ? O4A C1A O21A 124.7(6) . . ? O4A C1A C35A 119.5(6) . . ? O21A C1A C35A 115.8(6) . . ? C35A C78A C75 120.4(7) . . ? C1A O4A Eu2 153.5(4) . 1_545 ? C1A O21A Eu3 148.2(5) . 1_545 ? C58 C62A C42A 121.8(7) . . ? C62A C42A C38 118.3(6) . . ? C62A C42A C37A 119.9(6) . . ? C38 C42A C37A 121.7(6) . . ? O8A C37A O1A 119.1(6) . . ? O8A C37A C42A 120.3(6) . . ? O1A C37A C42A 120.6(6) . . ? O8A C37A Eu3 58.5(4) . 2_756 ? O1A C37A Eu3 61.1(3) . 2_756 ? C42A C37A Eu3 170.6(5) . 2_756 ? C37A O8A Eu3 95.5(4) . 2_756 ? C37A O1A Eu3 92.3(4) . 2_756 ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 2.004 _refine_diff_density_min -1.491 _refine_diff_density_rms 0.164 #==END data_2 _database_code_depnum_ccdc_archive 'CCDC 888383' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H31 Gd4 N O29, C3 H7 N O, 2(H O)' _chemical_formula_sum 'C54 H40 Gd4 N2 O32' _chemical_formula_weight 1857.88 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' Gd Gd -0.1653 3.9035 '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 10.836(3) _cell_length_b 14.156(4) _cell_length_c 20.139(5) _cell_angle_alpha 86.706(7) _cell_angle_beta 83.875(7) _cell_angle_gamma 78.990(4) _cell_volume 3012.9(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7985 _cell_measurement_theta_min 3.0540 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.4000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 4.443 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6235 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19167 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10103 _reflns_number_gt 9040 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0482P)^2^+3.0970P] 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 10103 _refine_ls_number_parameters 829 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0834 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.052 _refine_ls_shift/su_mean 0.002 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 Gd1 Gd 0.41401(2) 0.732321(18) 0.198168(13) 0.02023(8) Uani 1 1 d . . . Gd2 Gd 0.77070(2) 0.193064(18) 0.308852(13) 0.01900(8) Uani 1 1 d . . . Gd3 Gd 0.78944(2) 0.945058(18) 0.174118(13) 0.01881(8) Uani 1 1 d . . . Gd4 Gd 0.45489(3) 0.487688(19) 0.352538(14) 0.02318(8) Uani 1 1 d . . . O1 O 0.6708(4) 0.4742(3) 0.3121(2) 0.0389(11) Uani 1 1 d . . . O2 O 0.8002(4) 0.3438(3) 0.2762(2) 0.0422(11) Uani 1 1 d . . . O3 O 0.9706(4) 0.8022(3) 0.1931(2) 0.0330(10) Uani 1 1 d . . . O4 O 0.7756(4) 0.7801(3) 0.2090(2) 0.0340(10) Uani 1 1 d . . . O5 O 0.9609(4) 0.1359(3) 0.24815(19) 0.0307(9) Uani 1 1 d . . . O6 O 0.9587(3) 0.0197(3) 0.17864(19) 0.0279(9) Uani 1 1 d . . . O7 O 1.1058(4) 0.0789(3) -0.05936(19) 0.0324(10) Uani 1 1 d . . . O8 O 1.2848(4) 0.1293(3) -0.0802(2) 0.0401(11) Uani 1 1 d . . . O9 O 0.4557(5) 0.4928(4) 0.2387(2) 0.0511(13) Uani 1 1 d . . . O10 O 0.4110(4) 0.5856(3) 0.1494(2) 0.0341(10) Uani 1 1 d . . . O11 O 0.7068(4) 0.0916(3) 0.1112(2) 0.0352(10) Uani 1 1 d . . . O12 O 0.7111(4) 0.1611(3) 0.20569(19) 0.0309(9) Uani 1 1 d . . . O13 O 0.0831(4) 0.8481(4) 0.6067(2) 0.0433(12) Uani 1 1 d . . . O14 O 0.2469(4) 0.7376(3) 0.5806(2) 0.0401(11) Uani 1 1 d . . . O15 O 0.2403(4) 0.7185(3) 0.26981(19) 0.0309(9) Uani 1 1 d . . . O16 O 0.2670(3) 0.5980(3) 0.34621(19) 0.0281(9) Uani 1 1 d . . . O17 O 0.3623(4) 1.3512(3) 0.3476(3) 0.0502(13) Uani 1 1 d . . . O18 O 0.5543(4) 1.2691(3) 0.3235(2) 0.0326(10) Uani 1 1 d . . . O19 O 0.5727(3) 0.9655(3) 0.2032(2) 0.0324(10) Uani 1 1 d . . . O20 O 0.4237(4) 0.8787(3) 0.2331(2) 0.0379(11) Uani 1 1 d . . . O21 O 0.4940(4) 0.6196(3) 0.4060(2) 0.0342(10) Uani 1 1 d . . . O24 O 0.7010(5) 1.0650(3) 0.3672(2) 0.0457(12) Uani 1 1 d . . . O22 O 0.5035(4) 0.6862(3) 0.3043(2) 0.0334(10) Uani 1 1 d . . . O23 O 0.7709(4) 0.9608(4) 0.2887(2) 0.0457(12) Uani 1 1 d . . . O25 O 0.3137(4) 0.4830(3) 0.4579(2) 0.0425(11) Uani 1 1 d . . . O26 O 0.7407(6) 0.5697(5) 0.0615(3) 0.086(2) Uani 1 1 d . . . O27 O 0.4484(10) 1.0100(7) 0.0663(6) 0.173(4) Uani 1 1 d . . . H27B H 0.5214 1.0173 0.0678 0.260 Uiso 1 1 calc R . . O28 O 0.1578(4) 0.8667(4) 0.0237(2) 0.0540(14) Uani 1 1 d . . . H28B H 0.0866 0.8754 0.0433 0.081 Uiso 1 1 calc R . . O29 O 0.2276(4) 0.7932(3) 0.1445(2) 0.0361(10) Uani 1 1 d . . . O30 O 0.4707(4) 0.8206(3) 0.0934(2) 0.0403(11) Uani 1 1 d . . . O31 O 0.5696(4) 0.4097(3) 0.4428(2) 0.0350(10) Uani 1 1 d . . . O32 O 0.6281(4) 0.6764(3) 0.1615(2) 0.0398(11) Uani 1 1 d . . . N1 N 0.1729(6) 0.4229(5) 0.5312(4) 0.064(2) Uani 1 1 d . . . N2 N 0.8547(7) 0.4234(6) 0.0393(5) 0.078(2) Uani 1 1 d . . . C1 C 0.8740(5) 0.4902(4) 0.2618(3) 0.0269(13) Uani 1 1 d . . . C2 C 0.9985(6) 0.4437(5) 0.2473(4) 0.0435(17) Uani 1 1 d . . . H2A H 1.0203 0.3772 0.2532 0.052 Uiso 1 1 calc R . . C3 C 1.0898(6) 0.4975(5) 0.2239(4) 0.052(2) Uani 1 1 d . . . H3A H 1.1738 0.4671 0.2161 0.063 Uiso 1 1 calc R . . C4 C 1.0567(6) 0.5956(4) 0.2121(3) 0.0379(16) Uani 1 1 d . . . H4A H 1.1182 0.6307 0.1951 0.045 Uiso 1 1 calc R . . C5 C 0.9334(5) 0.6421(4) 0.2254(3) 0.0243(12) Uani 1 1 d . . . C6 C 0.8435(5) 0.5884(4) 0.2517(3) 0.0254(12) Uani 1 1 d . . . H6A H 0.7608 0.6196 0.2626 0.030 Uiso 1 1 calc R . . C7 C 0.7737(5) 0.4324(4) 0.2857(3) 0.0269(13) Uani 1 1 d . . . C8 C 0.8929(5) 0.7472(4) 0.2087(3) 0.0242(12) Uani 1 1 d . . . C9 C 1.0923(5) 0.1307(4) 0.1462(3) 0.0233(12) Uani 1 1 d . . . C10 C 1.1662(6) 0.1933(5) 0.1642(3) 0.0352(15) Uani 1 1 d . . . H10A H 1.1612 0.2101 0.2085 0.042 Uiso 1 1 calc R . . C11 C 1.2471(7) 0.2308(5) 0.1166(3) 0.048(2) Uani 1 1 d . . . H11A H 1.2961 0.2728 0.1290 0.058 Uiso 1 1 calc R . . C12 C 1.2556(6) 0.2065(5) 0.0513(3) 0.0424(17) Uani 1 1 d . . . H12A H 1.3104 0.2321 0.0197 0.051 Uiso 1 1 calc R . . C13 C 1.1824(5) 0.1435(4) 0.0318(3) 0.0282(13) Uani 1 1 d . . . C14 C 1.1013(5) 0.1062(4) 0.0798(3) 0.0239(12) Uani 1 1 d . . . H14A H 1.0522 0.0642 0.0674 0.029 Uiso 1 1 calc R . . C15 C 0.9973(5) 0.0921(4) 0.1949(3) 0.0235(12) Uani 1 1 d . . . C16 C 1.1915(5) 0.1157(4) -0.0393(3) 0.0272(13) Uani 1 1 d . . . C17 C 0.4933(5) 0.4190(4) 0.1342(3) 0.0224(12) Uani 1 1 d . . . C18 C 0.4673(5) 0.4252(4) 0.0680(3) 0.0284(13) Uani 1 1 d . . . H18A H 0.4223 0.4821 0.0505 0.034 Uiso 1 1 calc R . . C19 C 0.5082(6) 0.3472(4) 0.0282(3) 0.0301(14) Uani 1 1 d . . . H19A H 0.4901 0.3511 -0.0161 0.036 Uiso 1 1 calc R . . C20 C 0.5762(5) 0.2629(4) 0.0541(3) 0.0250(12) Uani 1 1 d . . . H20A H 0.6033 0.2104 0.0271 0.030 Uiso 1 1 calc R . . C21 C 0.6044(5) 0.2560(4) 0.1197(3) 0.0211(12) Uani 1 1 d . . . C22 C 0.5620(5) 0.3347(4) 0.1599(3) 0.0229(12) Uani 1 1 d . . . H22A H 0.5798 0.3307 0.2042 0.027 Uiso 1 1 calc R . . C23 C 0.6789(5) 0.1641(4) 0.1471(3) 0.0228(12) Uani 1 1 d . . . C24 C 0.4501(5) 0.5047(4) 0.1774(3) 0.0288(13) Uani 1 1 d . . . C25 C 0.1165(5) 0.8024(4) 0.4932(3) 0.0250(13) Uani 1 1 d . . . C26 C 0.0233(6) 0.8774(5) 0.4745(3) 0.0341(14) Uani 1 1 d . . . H26A H -0.0230 0.9184 0.5064 0.041 Uiso 1 1 calc R . . C27 C -0.0010(6) 0.8913(5) 0.4086(3) 0.0395(16) Uani 1 1 d . . . H27A H -0.0616 0.9433 0.3961 0.047 Uiso 1 1 calc R . . C28 C 0.0632(6) 0.8294(4) 0.3610(3) 0.0309(14) Uani 1 1 d . . . H28A H 0.0471 0.8398 0.3164 0.037 Uiso 1 1 calc R . . C29 C 0.1529(5) 0.7505(4) 0.3802(3) 0.0242(12) Uani 1 1 d . . . C30 C 0.1784(5) 0.7374(4) 0.4463(3) 0.0250(13) Uani 1 1 d . . . H30A H 0.2373 0.6846 0.4593 0.030 Uiso 1 1 calc R . . C31 C 0.1488(5) 0.7941(4) 0.5638(3) 0.0276(13) Uani 1 1 d . . . C32 C 0.2253(5) 0.6831(4) 0.3287(3) 0.0239(12) Uani 1 1 d . . . C33 C 0.3803(5) 1.1878(4) 0.3223(3) 0.0279(13) Uani 1 1 d . . . C34 C 0.2585(6) 1.1818(5) 0.3526(3) 0.0394(16) Uani 1 1 d . . . H34A H 0.2113 1.2328 0.3768 0.047 Uiso 1 1 calc R . . C35 C 0.2092(6) 1.0995(5) 0.3462(4) 0.0474(19) Uani 1 1 d . . . H35A H 0.1300 1.0943 0.3673 0.057 Uiso 1 1 calc R . . C36 C 0.2780(6) 1.0254(4) 0.3086(3) 0.0374(16) Uani 1 1 d . . . H36A H 0.2452 0.9700 0.3049 0.045 Uiso 1 1 calc R . . C37 C 0.3966(5) 1.0328(4) 0.2759(3) 0.0244(12) Uani 1 1 d . . . C38 C 0.4466(5) 1.1144(4) 0.2842(3) 0.0253(13) Uani 1 1 d . . . H38A H 0.5262 1.1193 0.2635 0.030 Uiso 1 1 calc R . . C39 C 0.4363(5) 1.2746(4) 0.3317(3) 0.0258(13) Uani 1 1 d . . . C40 C 0.4697(5) 0.9532(4) 0.2342(3) 0.0249(13) Uani 1 1 d . . . C41 C 0.5481(5) 0.7732(4) 0.3951(3) 0.0247(12) Uani 1 1 d . . . C42 C 0.5192(6) 0.7880(4) 0.4631(3) 0.0399(16) Uani 1 1 d . . . H42A H 0.4744 0.7471 0.4892 0.048 Uiso 1 1 calc R . . C43 C 0.5561(7) 0.8625(5) 0.4925(3) 0.0437(18) Uani 1 1 d . . . H43A H 0.5374 0.8710 0.5381 0.052 Uiso 1 1 calc R . . C44 C 0.6207(6) 0.9245(4) 0.4540(3) 0.0351(15) Uani 1 1 d . . . H44A H 0.6456 0.9748 0.4737 0.042 Uiso 1 1 calc R . . C45 C 0.6484(5) 0.9116(4) 0.3860(3) 0.0270(13) Uani 1 1 d . . . C46 C 0.6144(5) 0.8357(4) 0.3565(3) 0.0243(12) Uani 1 1 d . . . H46A H 0.6356 0.8264 0.3111 0.029 Uiso 1 1 calc R . . C47 C 0.5126(5) 0.6889(4) 0.3655(3) 0.0263(13) Uani 1 1 d . . . C48 C 0.7120(6) 0.9827(4) 0.3442(3) 0.0292(14) Uani 1 1 d . . . C49 C 0.1173(9) 0.5202(8) 0.5606(5) 0.089(3) Uani 1 1 d . . . H49A H 0.1502 0.5699 0.5339 0.134 Uiso 1 1 calc R . . H49B H 0.1395 0.5205 0.6055 0.134 Uiso 1 1 calc R . . H49C H 0.0270 0.5318 0.5610 0.134 Uiso 1 1 calc R . . C50 C 0.1274(9) 0.3463(8) 0.5685(5) 0.096(4) Uani 1 1 d . . . H50A H 0.1648 0.2864 0.5484 0.143 Uiso 1 1 calc R . . H50B H 0.0372 0.3561 0.5688 0.143 Uiso 1 1 calc R . . H50C H 0.1494 0.3448 0.6135 0.143 Uiso 1 1 calc R . . C51 C 0.2656(7) 0.4216(6) 0.4885(4) 0.062(2) Uani 1 1 d . . . H51A H 0.3065 0.3596 0.4780 0.074 Uiso 1 1 calc R . . C52 C 0.8667(12) 0.4347(12) -0.0291(7) 0.149(6) Uani 1 1 d . . . H52A H 0.8271 0.4987 -0.0419 0.224 Uiso 1 1 calc R . . H52B H 0.8267 0.3889 -0.0479 0.224 Uiso 1 1 calc R . . H52C H 0.9546 0.4243 -0.0453 0.224 Uiso 1 1 calc R . . C53 C 0.9082(11) 0.3304(9) 0.0736(7) 0.127(5) Uani 1 1 d . . . H53A H 0.8910 0.3362 0.1211 0.191 Uiso 1 1 calc R . . H53B H 0.9978 0.3155 0.0621 0.191 Uiso 1 1 calc R . . H53C H 0.8701 0.2799 0.0598 0.191 Uiso 1 1 calc R . . C54 C 0.7871(8) 0.4935(8) 0.0810(6) 0.080(3) Uani 1 1 d . . . H54A H 0.7783 0.4792 0.1267 0.096 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 Gd1 0.02347(15) 0.01802(15) 0.02008(16) -0.00281(11) 0.00050(11) -0.00693(11) Gd2 0.02428(15) 0.01583(14) 0.01700(16) -0.00031(11) 0.00309(11) -0.00691(11) Gd3 0.02134(14) 0.01737(15) 0.01792(16) 0.00113(11) 0.00180(11) -0.00667(11) Gd4 0.02908(16) 0.01842(15) 0.02245(17) -0.00155(12) -0.00315(12) -0.00488(12) O1 0.032(2) 0.030(2) 0.053(3) 0.005(2) 0.006(2) -0.010(2) O2 0.051(3) 0.022(2) 0.050(3) 0.004(2) 0.017(2) -0.014(2) O3 0.028(2) 0.020(2) 0.051(3) 0.0084(19) 0.0005(19) -0.0096(17) O4 0.026(2) 0.023(2) 0.053(3) 0.004(2) -0.0020(19) -0.0084(18) O5 0.028(2) 0.043(3) 0.022(2) -0.0106(19) 0.0101(17) -0.0158(19) O6 0.027(2) 0.028(2) 0.031(2) -0.0080(18) 0.0071(17) -0.0157(18) O7 0.030(2) 0.046(3) 0.024(2) -0.0093(19) 0.0054(17) -0.015(2) O8 0.041(2) 0.063(3) 0.023(2) -0.011(2) 0.0142(19) -0.032(2) O9 0.057(3) 0.063(3) 0.026(3) -0.018(2) -0.009(2) 0.013(3) O10 0.045(3) 0.015(2) 0.042(3) -0.0101(19) 0.003(2) -0.0052(18) O11 0.048(3) 0.019(2) 0.035(3) 0.0021(19) -0.006(2) 0.0036(19) O12 0.033(2) 0.039(2) 0.018(2) 0.0034(18) -0.0035(17) -0.0009(19) O13 0.034(2) 0.061(3) 0.027(3) -0.014(2) -0.0029(19) 0.013(2) O14 0.046(3) 0.038(3) 0.030(3) -0.013(2) -0.009(2) 0.014(2) O15 0.031(2) 0.043(3) 0.019(2) 0.0027(19) 0.0014(17) -0.0086(19) O16 0.028(2) 0.028(2) 0.026(2) 0.0003(18) -0.0027(17) 0.0000(18) O17 0.043(3) 0.024(2) 0.084(4) -0.020(2) 0.004(3) -0.008(2) O18 0.028(2) 0.038(2) 0.035(3) -0.0032(19) -0.0010(18) -0.0145(19) O19 0.021(2) 0.032(2) 0.043(3) -0.011(2) 0.0081(18) -0.0048(18) O20 0.050(3) 0.026(2) 0.042(3) -0.013(2) 0.006(2) -0.021(2) O21 0.043(2) 0.023(2) 0.039(3) -0.0008(19) -0.0044(19) -0.0135(19) O24 0.071(3) 0.029(3) 0.042(3) 0.004(2) -0.002(2) -0.029(2) O22 0.030(2) 0.038(3) 0.034(3) -0.010(2) -0.0069(18) -0.0064(19) O23 0.051(3) 0.070(3) 0.024(3) 0.008(2) 0.002(2) -0.038(3) O25 0.045(3) 0.042(3) 0.038(3) 0.008(2) 0.007(2) -0.011(2) O26 0.079(4) 0.084(5) 0.086(5) -0.012(4) -0.008(4) 0.013(4) O27 0.154(9) 0.130(8) 0.225(12) 0.053(8) -0.056(8) 0.006(7) O28 0.039(3) 0.072(4) 0.040(3) 0.010(3) 0.001(2) 0.011(2) O29 0.023(2) 0.049(3) 0.034(3) 0.011(2) -0.0025(17) -0.0039(19) O30 0.049(3) 0.054(3) 0.023(2) -0.003(2) 0.0006(19) -0.026(2) O31 0.046(3) 0.028(2) 0.027(2) 0.0014(18) -0.0082(19) 0.004(2) O32 0.027(2) 0.044(3) 0.046(3) -0.007(2) 0.0044(19) -0.004(2) N1 0.038(3) 0.059(4) 0.087(5) 0.020(4) 0.017(3) -0.011(3) N2 0.052(4) 0.069(5) 0.110(7) -0.034(5) -0.015(4) 0.007(4) C1 0.026(3) 0.024(3) 0.031(3) 0.003(3) -0.004(2) -0.005(2) C2 0.037(4) 0.027(4) 0.063(5) 0.013(3) -0.004(3) -0.005(3) C3 0.029(4) 0.034(4) 0.092(6) 0.006(4) 0.000(4) -0.007(3) C4 0.025(3) 0.027(3) 0.061(5) 0.002(3) 0.004(3) -0.010(3) C5 0.024(3) 0.020(3) 0.029(3) -0.003(2) -0.003(2) -0.004(2) C6 0.024(3) 0.023(3) 0.028(3) 0.005(2) -0.002(2) -0.006(2) C7 0.029(3) 0.024(3) 0.027(3) 0.010(3) 0.001(2) -0.010(3) C8 0.024(3) 0.027(3) 0.024(3) 0.002(2) -0.002(2) -0.013(2) C9 0.022(3) 0.025(3) 0.024(3) -0.006(2) 0.004(2) -0.010(2) C10 0.045(4) 0.047(4) 0.019(3) -0.012(3) 0.008(3) -0.023(3) C11 0.061(5) 0.066(5) 0.030(4) -0.026(3) 0.019(3) -0.049(4) C12 0.047(4) 0.052(4) 0.032(4) -0.013(3) 0.017(3) -0.026(3) C13 0.026(3) 0.030(3) 0.027(3) -0.009(3) 0.010(2) -0.009(3) C14 0.028(3) 0.023(3) 0.020(3) -0.003(2) 0.004(2) -0.007(2) C15 0.020(3) 0.032(3) 0.017(3) -0.002(3) 0.004(2) -0.005(2) C16 0.029(3) 0.028(3) 0.023(3) 0.000(3) 0.003(2) -0.005(3) C17 0.025(3) 0.021(3) 0.023(3) -0.006(2) 0.000(2) -0.010(2) C18 0.030(3) 0.026(3) 0.027(3) 0.001(3) -0.002(2) -0.002(3) C19 0.043(4) 0.027(3) 0.021(3) 0.000(3) -0.010(3) -0.005(3) C20 0.032(3) 0.019(3) 0.024(3) -0.008(2) -0.001(2) -0.003(2) C21 0.030(3) 0.017(3) 0.016(3) 0.003(2) -0.001(2) -0.006(2) C22 0.032(3) 0.020(3) 0.017(3) 0.000(2) -0.005(2) -0.004(2) C23 0.023(3) 0.022(3) 0.023(3) 0.002(2) -0.001(2) -0.005(2) C24 0.028(3) 0.030(3) 0.031(4) -0.010(3) -0.005(3) -0.010(3) C25 0.020(3) 0.030(3) 0.024(3) -0.010(3) 0.001(2) -0.001(2) C26 0.030(3) 0.038(4) 0.034(4) -0.008(3) -0.003(3) -0.001(3) C27 0.036(4) 0.042(4) 0.035(4) -0.001(3) -0.011(3) 0.011(3) C28 0.037(3) 0.035(4) 0.021(3) 0.004(3) -0.006(3) -0.007(3) C29 0.019(3) 0.026(3) 0.027(3) 0.002(2) 0.000(2) -0.004(2) C30 0.020(3) 0.028(3) 0.026(3) 0.003(3) -0.003(2) -0.002(2) C31 0.021(3) 0.029(3) 0.033(4) -0.005(3) -0.002(3) -0.003(3) C32 0.020(3) 0.030(3) 0.023(3) 0.003(3) -0.004(2) -0.009(2) C33 0.025(3) 0.022(3) 0.039(4) -0.003(3) -0.007(3) -0.009(2) C34 0.030(3) 0.036(4) 0.051(4) -0.019(3) 0.010(3) -0.005(3) C35 0.024(3) 0.048(4) 0.070(5) -0.024(4) 0.019(3) -0.013(3) C36 0.037(4) 0.026(3) 0.050(4) -0.013(3) 0.012(3) -0.013(3) C37 0.028(3) 0.019(3) 0.025(3) -0.005(2) 0.003(2) -0.005(2) C38 0.023(3) 0.025(3) 0.029(3) -0.006(3) 0.003(2) -0.008(2) C39 0.031(3) 0.021(3) 0.027(3) -0.005(2) -0.002(2) -0.007(3) C40 0.031(3) 0.026(3) 0.019(3) -0.002(2) -0.009(2) -0.005(3) C41 0.032(3) 0.017(3) 0.024(3) -0.002(2) 0.001(2) -0.006(2) C42 0.061(4) 0.033(4) 0.032(4) 0.004(3) 0.005(3) -0.031(3) C43 0.080(5) 0.040(4) 0.017(3) -0.009(3) 0.012(3) -0.033(4) C44 0.059(4) 0.026(3) 0.026(4) -0.001(3) 0.001(3) -0.023(3) C45 0.034(3) 0.025(3) 0.025(3) 0.004(2) -0.001(3) -0.017(3) C46 0.032(3) 0.026(3) 0.018(3) 0.000(2) -0.005(2) -0.013(2) C47 0.026(3) 0.023(3) 0.031(4) -0.005(3) -0.006(2) -0.006(2) C48 0.037(3) 0.035(4) 0.021(3) 0.012(3) -0.012(3) -0.021(3) C49 0.082(7) 0.111(9) 0.073(7) -0.019(6) 0.013(5) -0.021(6) C50 0.083(7) 0.102(8) 0.104(8) 0.042(7) 0.009(6) -0.047(6) C51 0.053(5) 0.059(5) 0.068(6) 0.019(4) 0.004(4) -0.009(4) C52 0.101(10) 0.25(2) 0.098(11) -0.064(12) 0.010(8) -0.030(11) C53 0.090(9) 0.104(10) 0.178(14) -0.001(9) -0.018(9) 0.009(8) C54 0.053(5) 0.084(8) 0.103(8) 0.000(7) -0.021(5) -0.008(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 Gd1 O20 2.251(4) . ? Gd1 O15 2.278(4) . ? Gd1 O10 2.355(4) . ? Gd1 O32 2.357(4) . ? Gd1 O29 2.384(4) . ? Gd1 O22 2.445(4) . ? Gd1 O30 2.470(4) . ? Gd2 O2 2.267(4) . ? Gd2 O24 2.308(4) 1_545 ? Gd2 O5 2.310(4) . ? Gd2 O12 2.333(4) . ? Gd2 O18 2.381(4) 1_545 ? Gd2 O13 2.418(4) 2_666 ? Gd2 O14 2.458(4) 2_666 ? Gd2 C31 2.822(6) 2_666 ? Gd3 O6 2.297(4) 1_565 ? Gd3 O23 2.314(4) . ? Gd3 O19 2.325(4) . ? Gd3 O4 2.428(4) . ? Gd3 O11 2.437(4) 1_565 ? Gd3 O7 2.475(4) 2_765 ? Gd3 O8 2.493(4) 2_765 ? Gd3 O3 2.578(4) . ? Gd3 C16 2.869(6) 2_765 ? Gd3 C8 2.886(6) . ? Gd4 O9 2.288(4) . ? Gd4 O16 2.328(4) . ? Gd4 O21 2.336(4) . ? Gd4 O17 2.353(4) 1_545 ? Gd4 O1 2.369(4) . ? Gd4 O31 2.407(4) . ? Gd4 O25 2.485(4) . ? O1 C7 1.238(7) . ? O2 C7 1.254(7) . ? O3 C8 1.256(6) . ? O4 C8 1.267(7) . ? O5 C15 1.259(7) . ? O6 C15 1.249(7) . ? O6 Gd3 2.297(4) 1_545 ? O7 C16 1.260(7) . ? O7 Gd3 2.475(4) 2_765 ? O8 C16 1.270(7) . ? O8 Gd3 2.493(4) 2_765 ? O9 C24 1.244(7) . ? O10 C24 1.265(7) . ? O11 C23 1.259(7) . ? O11 Gd3 2.437(4) 1_545 ? O12 C23 1.262(6) . ? O13 C31 1.255(7) . ? O13 Gd2 2.418(4) 2_666 ? O14 C31 1.267(7) . ? O14 Gd2 2.458(4) 2_666 ? O15 C32 1.267(6) . ? O16 C32 1.248(6) . ? O17 C39 1.254(7) . ? O17 Gd4 2.353(4) 1_565 ? O18 C39 1.260(7) . ? O18 Gd2 2.381(4) 1_565 ? O19 C40 1.257(7) . ? O20 C40 1.251(7) . ? O21 C47 1.271(7) . ? O24 C48 1.258(7) . ? O24 Gd2 2.308(4) 1_565 ? O22 C47 1.249(7) . ? O23 C48 1.250(7) . ? O25 C51 1.204(8) . ? O26 C54 1.164(11) . ? N1 C51 1.249(9) . ? N1 C50 1.418(10) . ? N1 C49 1.521(12) . ? N2 C52 1.372(14) . ? N2 C54 1.384(12) . ? N2 C53 1.495(13) . ? C1 C6 1.375(8) . ? C1 C2 1.392(8) . ? C1 C7 1.504(7) . ? C2 C3 1.388(9) . ? C3 C4 1.381(9) . ? C4 C5 1.378(8) . ? C5 C6 1.390(7) . ? C5 C8 1.497(7) . ? C9 C14 1.389(8) . ? C9 C10 1.388(8) . ? C9 C15 1.503(7) . ? C10 C11 1.382(8) . ? C11 C12 1.367(9) . ? C12 C13 1.399(8) . ? C13 C14 1.387(7) . ? C13 C16 1.495(8) . ? C16 Gd3 2.869(6) 2_765 ? C17 C18 1.385(8) . ? C17 C22 1.385(7) . ? C17 C24 1.505(8) . ? C18 C19 1.379(8) . ? C19 C20 1.383(8) . ? C20 C21 1.380(7) . ? C21 C22 1.392(8) . ? C21 C23 1.503(7) . ? C25 C26 1.384(8) . ? C25 C30 1.385(8) . ? C25 C31 1.493(8) . ? C26 C27 1.376(9) . ? C27 C28 1.376(9) . ? C28 C29 1.399(8) . ? C29 C30 1.382(8) . ? C29 C32 1.502(8) . ? C31 Gd2 2.822(6) 2_666 ? C33 C38 1.369(8) . ? C33 C34 1.409(8) . ? C33 C39 1.501(7) . ? C34 C35 1.389(9) . ? C35 C36 1.379(9) . ? C36 C37 1.400(8) . ? C37 C38 1.392(7) . ? C37 C40 1.493(8) . ? C41 C42 1.390(8) . ? C41 C46 1.395(7) . ? C41 C47 1.495(8) . ? C42 C43 1.381(8) . ? C43 C44 1.377(8) . ? C44 C45 1.385(8) . ? C45 C46 1.384(8) . ? C45 C48 1.498(7) . ? 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 O20 Gd1 O15 93.34(15) . . ? O20 Gd1 O10 173.49(15) . . ? O15 Gd1 O10 91.83(15) . . ? O20 Gd1 O32 100.51(15) . . ? O15 Gd1 O32 149.60(15) . . ? O10 Gd1 O32 76.76(15) . . ? O20 Gd1 O29 92.41(16) . . ? O15 Gd1 O29 70.32(14) . . ? O10 Gd1 O29 85.60(15) . . ? O32 Gd1 O29 135.08(15) . . ? O20 Gd1 O22 80.06(15) . . ? O15 Gd1 O22 77.28(14) . . ? O10 Gd1 O22 104.97(14) . . ? O32 Gd1 O22 78.64(15) . . ? O29 Gd1 O22 146.25(14) . . ? O20 Gd1 O30 76.91(15) . . ? O15 Gd1 O30 139.35(15) . . ? O10 Gd1 O30 96.59(15) . . ? O32 Gd1 O30 70.68(15) . . ? O29 Gd1 O30 70.79(14) . . ? O22 Gd1 O30 137.05(14) . . ? O2 Gd2 O24 162.67(16) . 1_545 ? O2 Gd2 O5 87.56(15) . . ? O24 Gd2 O5 108.53(16) 1_545 . ? O2 Gd2 O12 93.89(16) . . ? O24 Gd2 O12 96.08(15) 1_545 . ? O5 Gd2 O12 76.57(14) . . ? O2 Gd2 O18 83.28(15) . 1_545 ? O24 Gd2 O18 84.28(16) 1_545 1_545 ? O5 Gd2 O18 155.30(14) . 1_545 ? O12 Gd2 O18 81.21(14) . 1_545 ? O2 Gd2 O13 101.24(18) . 2_666 ? O24 Gd2 O13 77.18(17) 1_545 2_666 ? O5 Gd2 O13 76.41(14) . 2_666 ? O12 Gd2 O13 148.28(14) . 2_666 ? O18 Gd2 O13 127.87(14) 1_545 2_666 ? O2 Gd2 O14 80.97(16) . 2_666 ? O24 Gd2 O14 84.59(16) 1_545 2_666 ? O5 Gd2 O14 123.69(14) . 2_666 ? O12 Gd2 O14 158.48(14) . 2_666 ? O18 Gd2 O14 77.45(14) 1_545 2_666 ? O13 Gd2 O14 52.83(14) 2_666 2_666 ? O2 Gd2 C31 92.89(17) . 2_666 ? O24 Gd2 C31 78.08(16) 1_545 2_666 ? O5 Gd2 C31 100.87(15) . 2_666 ? O12 Gd2 C31 172.64(16) . 2_666 ? O18 Gd2 C31 102.46(15) 1_545 2_666 ? O13 Gd2 C31 26.29(14) 2_666 2_666 ? O14 Gd2 C31 26.65(14) 2_666 2_666 ? O6 Gd3 O23 82.39(14) 1_565 . ? O6 Gd3 O19 141.66(14) 1_565 . ? O23 Gd3 O19 76.74(15) . . ? O6 Gd3 O4 127.06(14) 1_565 . ? O23 Gd3 O4 81.15(16) . . ? O19 Gd3 O4 81.11(14) . . ? O6 Gd3 O11 83.24(14) 1_565 1_565 ? O23 Gd3 O11 114.43(16) . 1_565 ? O19 Gd3 O11 76.82(15) . 1_565 ? O4 Gd3 O11 148.68(14) . 1_565 ? O6 Gd3 O7 79.46(13) 1_565 2_765 ? O23 Gd3 O7 158.24(15) . 2_765 ? O19 Gd3 O7 125.02(14) . 2_765 ? O4 Gd3 O7 100.38(14) . 2_765 ? O11 Gd3 O7 75.28(14) 1_565 2_765 ? O6 Gd3 O8 131.45(13) 1_565 2_765 ? O23 Gd3 O8 145.47(14) . 2_765 ? O19 Gd3 O8 77.45(14) . 2_765 ? O4 Gd3 O8 72.52(15) . 2_765 ? O11 Gd3 O8 81.14(15) 1_565 2_765 ? O7 Gd3 O8 52.15(12) 2_765 2_765 ? O6 Gd3 O3 77.42(13) 1_565 . ? O23 Gd3 O3 86.06(16) . . ? O19 Gd3 O3 131.73(13) . . ? O4 Gd3 O3 51.57(12) . . ? O11 Gd3 O3 149.69(13) 1_565 . ? O7 Gd3 O3 78.37(14) 2_765 . ? O8 Gd3 O3 94.37(15) 2_765 . ? O6 Gd3 C16 105.28(15) 1_565 2_765 ? O23 Gd3 C16 167.93(17) . 2_765 ? O19 Gd3 C16 101.31(15) . 2_765 ? O4 Gd3 C16 86.79(15) . 2_765 ? O11 Gd3 C16 76.20(15) 1_565 2_765 ? O7 Gd3 C16 25.94(14) 2_765 2_765 ? O8 Gd3 C16 26.22(14) 2_765 2_765 ? O3 Gd3 C16 86.58(15) . 2_765 ? O6 Gd3 C8 102.38(14) 1_565 . ? O23 Gd3 C8 83.02(17) . . ? O19 Gd3 C8 106.50(14) . . ? O4 Gd3 C8 25.78(13) . . ? O11 Gd3 C8 162.38(15) 1_565 . ? O7 Gd3 C8 89.21(15) 2_765 . ? O8 Gd3 C8 82.74(16) 2_765 . ? O3 Gd3 C8 25.79(13) . . ? C16 Gd3 C8 86.20(16) 2_765 . ? O9 Gd4 O16 82.94(15) . . ? O9 Gd4 O21 119.88(17) . . ? O16 Gd4 O21 77.69(14) . . ? O9 Gd4 O17 84.00(19) . 1_545 ? O16 Gd4 O17 94.90(15) . 1_545 ? O21 Gd4 O17 153.21(16) . 1_545 ? O9 Gd4 O1 75.52(17) . . ? O16 Gd4 O1 138.23(14) . . ? O21 Gd4 O1 82.66(15) . . ? O17 Gd4 O1 117.44(15) 1_545 . ? O9 Gd4 O31 142.49(15) . . ? O16 Gd4 O31 134.50(14) . . ? O21 Gd4 O31 78.42(14) . . ? O17 Gd4 O31 89.48(17) 1_545 . ? O1 Gd4 O31 74.99(15) . . ? O9 Gd4 O25 142.45(17) . . ? O16 Gd4 O25 69.13(14) . . ? O21 Gd4 O25 79.03(15) . . ? O17 Gd4 O25 74.30(17) 1_545 . ? O1 Gd4 O25 141.79(15) . . ? O31 Gd4 O25 68.66(15) . . ? C7 O1 Gd4 154.8(4) . . ? C7 O2 Gd2 148.4(4) . . ? C8 O3 Gd3 91.0(3) . . ? C8 O4 Gd3 97.8(3) . . ? C15 O5 Gd2 137.0(3) . . ? C15 O6 Gd3 147.3(4) . 1_545 ? C16 O7 Gd3 94.8(3) . 2_765 ? C16 O8 Gd3 93.7(3) . 2_765 ? C24 O9 Gd4 173.9(4) . . ? C24 O10 Gd1 122.5(4) . . ? C23 O11 Gd3 112.4(3) . 1_545 ? C23 O12 Gd2 166.8(4) . . ? C31 O13 Gd2 95.1(3) . 2_666 ? C31 O14 Gd2 92.9(3) . 2_666 ? C32 O15 Gd1 133.4(3) . . ? C32 O16 Gd4 141.9(3) . . ? C39 O17 Gd4 116.1(4) . 1_565 ? C39 O18 Gd2 157.2(4) . 1_565 ? C40 O19 Gd3 159.2(4) . . ? C40 O20 Gd1 155.1(4) . . ? C47 O21 Gd4 112.7(4) . . ? C48 O24 Gd2 124.0(4) . 1_565 ? C47 O22 Gd1 156.8(4) . . ? C48 O23 Gd3 154.5(4) . . ? C51 O25 Gd4 134.5(6) . . ? C51 N1 C50 130.5(8) . . ? C51 N1 C49 115.7(7) . . ? C50 N1 C49 112.1(8) . . ? C52 N2 C54 123.3(10) . . ? C52 N2 C53 121.4(10) . . ? C54 N2 C53 115.2(10) . . ? C6 C1 C2 119.2(5) . . ? C6 C1 C7 120.8(5) . . ? C2 C1 C7 119.9(5) . . ? C3 C2 C1 119.5(6) . . ? C4 C3 C2 120.4(6) . . ? C5 C4 C3 120.5(6) . . ? C4 C5 C6 118.7(5) . . ? C4 C5 C8 121.7(5) . . ? C6 C5 C8 119.5(5) . . ? C1 C6 C5 121.6(5) . . ? O1 C7 O2 124.0(5) . . ? O1 C7 C1 119.2(5) . . ? O2 C7 C1 116.7(5) . . ? O3 C8 O4 119.7(5) . . ? O3 C8 C5 122.5(5) . . ? O4 C8 C5 117.8(5) . . ? O3 C8 Gd3 63.2(3) . . ? O4 C8 Gd3 56.4(3) . . ? C5 C8 Gd3 173.9(4) . . ? C14 C9 C10 119.0(5) . . ? C14 C9 C15 118.1(5) . . ? C10 C9 C15 122.8(5) . . ? C11 C10 C9 120.3(6) . . ? C12 C11 C10 120.5(6) . . ? C11 C12 C13 120.5(6) . . ? C14 C13 C12 118.7(5) . . ? C14 C13 C16 120.2(5) . . ? C12 C13 C16 121.0(5) . . ? C13 C14 C9 121.0(5) . . ? O6 C15 O5 125.0(5) . . ? O6 C15 C9 117.3(5) . . ? O5 C15 C9 117.7(5) . . ? O7 C16 O8 119.4(5) . . ? O7 C16 C13 120.0(5) . . ? O8 C16 C13 120.7(5) . . ? O7 C16 Gd3 59.3(3) . 2_765 ? O8 C16 Gd3 60.1(3) . 2_765 ? C13 C16 Gd3 177.8(4) . 2_765 ? C18 C17 C22 119.8(5) . . ? C18 C17 C24 120.0(5) . . ? C22 C17 C24 120.1(5) . . ? C19 C18 C17 120.0(5) . . ? C18 C19 C20 119.9(5) . . ? C19 C20 C21 120.8(5) . . ? C20 C21 C22 119.1(5) . . ? C20 C21 C23 120.1(5) . . ? C22 C21 C23 120.8(5) . . ? C17 C22 C21 120.3(5) . . ? O11 C23 O12 121.5(5) . . ? O11 C23 C21 119.2(5) . . ? O12 C23 C21 119.2(5) . . ? O9 C24 O10 123.2(6) . . ? O9 C24 C17 118.5(5) . . ? O10 C24 C17 118.3(5) . . ? C26 C25 C30 119.6(5) . . ? C26 C25 C31 118.9(5) . . ? C30 C25 C31 121.5(5) . . ? C27 C26 C25 120.0(6) . . ? C26 C27 C28 120.9(6) . . ? C27 C28 C29 119.3(5) . . ? C30 C29 C28 119.7(5) . . ? C30 C29 C32 120.2(5) . . ? C28 C29 C32 120.0(5) . . ? C29 C30 C25 120.3(5) . . ? O13 C31 O14 118.7(5) . . ? O13 C31 C25 120.1(5) . . ? O14 C31 C25 121.1(5) . . ? O13 C31 Gd2 58.6(3) . 2_666 ? O14 C31 Gd2 60.5(3) . 2_666 ? C25 C31 Gd2 170.0(4) . 2_666 ? O16 C32 O15 124.8(5) . . ? O16 C32 C29 118.9(5) . . ? O15 C32 C29 116.3(5) . . ? C38 C33 C34 119.8(5) . . ? C38 C33 C39 120.3(5) . . ? C34 C33 C39 119.9(5) . . ? C35 C34 C33 119.7(6) . . ? C36 C35 C34 119.9(6) . . ? C35 C36 C37 120.6(6) . . ? C38 C37 C36 119.0(5) . . ? C38 C37 C40 120.6(5) . . ? C36 C37 C40 120.4(5) . . ? C33 C38 C37 121.0(5) . . ? O17 C39 O18 122.2(5) . . ? O17 C39 C33 117.9(5) . . ? O18 C39 C33 119.9(5) . . ? O20 C40 O19 124.9(5) . . ? O20 C40 C37 117.3(5) . . ? O19 C40 C37 117.8(5) . . ? C42 C41 C46 118.9(5) . . ? C42 C41 C47 119.6(5) . . ? C46 C41 C47 121.4(5) . . ? C43 C42 C41 120.9(5) . . ? C44 C43 C42 119.9(6) . . ? C43 C44 C45 119.8(5) . . ? C46 C45 C44 120.6(5) . . ? C46 C45 C48 120.1(5) . . ? C44 C45 C48 119.2(5) . . ? C45 C46 C41 119.8(5) . . ? O22 C47 O21 122.1(5) . . ? O22 C47 C41 121.9(5) . . ? O21 C47 C41 116.1(5) . . ? O23 C48 O24 122.5(5) . . ? O23 C48 C45 120.9(5) . . ? O24 C48 C45 116.6(5) . . ? O25 C51 N1 134.2(9) . . ? O26 C54 N2 123.0(11) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 1.173 _refine_diff_density_min -1.090 _refine_diff_density_rms 0.135 #==END data_3 _database_code_depnum_ccdc_archive 'CCDC 888384' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H31 N O29 Tb4, C3 H7 N O, 2(H O)' _chemical_formula_sum 'C54 H40 N2 O32 Tb4' _chemical_formula_weight 1864.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Tb Tb -0.1723 4.1537 '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 10.850(4) _cell_length_b 14.135(5) _cell_length_c 20.084(7) _cell_angle_alpha 86.494(9) _cell_angle_beta 83.743(7) _cell_angle_gamma 78.839(8) _cell_volume 3001.4(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7843 _cell_measurement_theta_min 3.0636 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.063 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1788 _exptl_absorpt_coefficient_mu 4.753 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4491 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19074 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10078 _reflns_number_gt 8820 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0569P)^2^+0.3798P] 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 10078 _refine_ls_number_parameters 824 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1088 _refine_ls_wR_factor_gt 0.1017 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.41359(3) 0.23285(2) 0.197775(15) 0.02085(10) Uani 1 1 d . . . Tb2 Tb 0.77131(3) -0.30703(2) 0.309353(14) 0.01896(10) Uani 1 1 d . . . Tb3 Tb 0.78951(3) 0.44406(2) 0.173697(14) 0.01892(10) Uani 1 1 d . . . Tb4 Tb 0.45467(3) -0.01202(2) 0.352841(16) 0.02365(10) Uani 1 1 d . . . O1 O 0.6703(5) -0.0255(4) 0.3120(3) 0.0384(13) Uani 1 1 d . . . O2 O 0.8003(5) -0.1571(3) 0.2766(3) 0.0418(14) Uani 1 1 d . . . O3 O 0.9710(5) 0.3014(3) 0.1926(3) 0.0331(12) Uani 1 1 d . . . O4 O 0.7762(4) 0.2793(3) 0.2077(3) 0.0332(12) Uani 1 1 d . . . O5 O 0.9597(4) -0.3660(4) 0.2487(2) 0.0308(12) Uani 1 1 d . . . O6 O 0.9570(4) -0.4808(3) 0.1782(2) 0.0262(11) Uani 1 1 d . . . O7 O 1.2859(5) -0.3717(4) -0.0795(2) 0.0414(14) Uani 1 1 d . . . O8 O 1.1060(5) -0.4215(4) -0.0596(2) 0.0332(12) Uani 1 1 d . . . O9 O 0.4548(5) -0.0073(4) 0.2400(3) 0.0471(15) Uani 1 1 d . . . O10 O 0.4118(5) 0.0861(3) 0.1503(2) 0.0318(12) Uani 1 1 d . . . O11 O 0.7111(5) -0.3375(4) 0.2069(2) 0.0318(12) Uani 1 1 d . . . O12 O 0.7076(5) -0.4091(3) 0.1129(2) 0.0351(12) Uani 1 1 d . . . O13 O 0.2675(4) 0.0978(3) 0.3456(2) 0.0285(11) Uani 1 1 d . . . O14 O 0.6263(4) 0.1778(4) 0.1612(3) 0.0390(13) Uani 1 1 d . . . O15 O 0.2474(5) 0.2373(4) 0.5806(2) 0.0357(13) Uani 1 1 d . . . O16 O 0.0832(5) 0.3472(4) 0.6071(2) 0.0417(14) Uani 1 1 d . . . O17 O 0.5739(4) 0.4629(4) 0.2032(2) 0.0326(12) Uani 1 1 d . . . O18 O 0.4248(5) 0.3773(4) 0.2328(3) 0.0363(12) Uani 1 1 d . . . O19 O 0.5570(5) 0.7676(4) 0.3245(2) 0.0327(12) Uani 1 1 d . . . O20 O 0.3657(5) 0.8512(4) 0.3477(3) 0.0506(16) Uani 1 1 d . . . O21 O 0.7723(5) 0.4567(4) 0.2878(2) 0.0416(14) Uani 1 1 d . . . O22 O 0.7067(5) 0.5622(4) 0.3655(3) 0.0419(14) Uani 1 1 d . . . O23 O 0.5035(4) 0.1864(4) 0.3034(3) 0.0350(12) Uani 1 1 d . . . O24 O 0.4918(5) 0.1199(3) 0.4068(3) 0.0337(12) Uani 1 1 d . . . O25 O 0.3144(5) -0.0169(4) 0.4578(3) 0.0412(13) Uani 1 1 d . . . O26 O 0.7402(8) 0.0706(6) 0.0617(4) 0.090(3) Uani 1 1 d . . . O27 O 0.5688(5) -0.0893(4) 0.4423(2) 0.0346(12) Uani 1 1 d . . . O28 O 0.2281(5) 0.2931(4) 0.1439(3) 0.0400(13) Uani 1 1 d . . . O29 O 0.4704(5) 0.3206(4) 0.0930(2) 0.0397(13) Uani 1 1 d . . . O30 O 0.2417(4) 0.2173(4) 0.2692(2) 0.0300(11) Uani 1 1 d . . . O31 O 0.1566(5) 0.3655(4) 0.0236(3) 0.0514(16) Uani 1 1 d . . . H31A H 0.0847 0.3793 0.0421 0.077 Uiso 1 1 calc R . . O32 O 0.4478(13) 0.5102(10) 0.0656(7) 0.178(5) Uiso 1 1 d . . . H32A H 0.5176 0.5232 0.0678 0.268 Uiso 1 1 calc R . . N1 N 0.1729(7) -0.0772(6) 0.5303(5) 0.069(3) Uani 1 1 d . . . N2 N 0.8549(8) -0.0772(7) 0.0401(6) 0.080(3) Uani 1 1 d . . . C1 C 0.8738(7) -0.0111(5) 0.2616(3) 0.0270(15) Uani 1 1 d . . . C2 C 0.9995(8) -0.0555(6) 0.2480(4) 0.046(2) Uani 1 1 d . . . H2A H 1.0224 -0.1220 0.2548 0.055 Uiso 1 1 calc R . . C3 C 1.0898(8) -0.0031(5) 0.2247(5) 0.052(3) Uani 1 1 d . . . H3A H 1.1735 -0.0342 0.2169 0.063 Uiso 1 1 calc R . . C4 C 1.0588(7) 0.0951(6) 0.2127(4) 0.0384(19) Uani 1 1 d . . . H4A H 1.1204 0.1304 0.1965 0.046 Uiso 1 1 calc R . . C5 C 0.9328(6) 0.1406(5) 0.2253(3) 0.0250(15) Uani 1 1 d . . . C6 C 0.8435(7) 0.0879(5) 0.2508(3) 0.0278(16) Uani 1 1 d . . . H6A H 0.7607 0.1195 0.2611 0.033 Uiso 1 1 calc R . . C7 C 0.7719(7) -0.0685(5) 0.2853(3) 0.0246(15) Uani 1 1 d . . . C8 C 0.8932(6) 0.2463(5) 0.2078(3) 0.0242(15) Uani 1 1 d . . . C9 C 1.0911(6) -0.3707(5) 0.1465(3) 0.0230(14) Uani 1 1 d . . . C10 C 1.1641(7) -0.3078(6) 0.1654(4) 0.0391(19) Uani 1 1 d . . . H10A H 1.1579 -0.2911 0.2099 0.047 Uiso 1 1 calc R . . C11 C 1.2466(8) -0.2698(7) 0.1175(4) 0.049(2) Uani 1 1 d . . . H11A H 1.2951 -0.2277 0.1302 0.058 Uiso 1 1 calc R . . C12 C 1.2567(8) -0.2942(6) 0.0517(4) 0.041(2) Uani 1 1 d . . . H12A H 1.3127 -0.2694 0.0202 0.049 Uiso 1 1 calc R . . C13 C 1.1823(7) -0.3567(5) 0.0320(3) 0.0302(16) Uani 1 1 d . . . C14 C 1.1016(6) -0.3955(5) 0.0797(3) 0.0257(15) Uani 1 1 d . . . H14A H 1.0542 -0.4383 0.0670 0.031 Uiso 1 1 calc R . . C15 C 0.9967(6) -0.4095(5) 0.1950(3) 0.0206(14) Uani 1 1 d . . . C16 C 1.1923(7) -0.3844(5) -0.0399(4) 0.0283(16) Uani 1 1 d . . . C17 C 0.4932(6) -0.0803(5) 0.1348(3) 0.0233(14) Uani 1 1 d . . . C18 C 0.4673(6) -0.0747(5) 0.0682(3) 0.0269(15) Uani 1 1 d . . . H18A H 0.4216 -0.0180 0.0504 0.032 Uiso 1 1 calc R . . C19 C 0.5092(7) -0.1529(5) 0.0284(3) 0.0304(17) Uani 1 1 d . . . H19A H 0.4921 -0.1488 -0.0162 0.036 Uiso 1 1 calc R . . C20 C 0.5764(6) -0.2372(5) 0.0546(3) 0.0258(15) Uani 1 1 d . . . H20A H 0.6029 -0.2901 0.0279 0.031 Uiso 1 1 calc R . . C21 C 0.6051(6) -0.2437(5) 0.1206(3) 0.0197(13) Uani 1 1 d . . . C22 C 0.5622(6) -0.1649(5) 0.1610(3) 0.0251(15) Uani 1 1 d . . . H22A H 0.5799 -0.1689 0.2055 0.030 Uiso 1 1 calc R . . C23 C 0.6793(6) -0.3354(5) 0.1484(3) 0.0232(15) Uani 1 1 d . . . C24 C 0.4497(6) 0.0068(5) 0.1777(3) 0.0258(15) Uani 1 1 d . . . C25 C 0.1164(6) 0.3019(5) 0.4936(3) 0.0264(15) Uani 1 1 d . . . C26 C 0.0230(6) 0.3772(6) 0.4734(4) 0.0364(18) Uani 1 1 d . . . H26A H -0.0241 0.4180 0.5052 0.044 Uiso 1 1 calc R . . C27 C -0.0007(7) 0.3921(6) 0.4082(4) 0.0377(19) Uani 1 1 d . . . H27A H -0.0612 0.4442 0.3956 0.045 Uiso 1 1 calc R . . C28 C 0.0650(7) 0.3299(5) 0.3608(4) 0.0352(18) Uani 1 1 d . . . H28A H 0.0501 0.3410 0.3160 0.042 Uiso 1 1 calc R . . C29 C 0.1534(6) 0.2507(5) 0.3796(3) 0.0236(14) Uani 1 1 d . . . C30 C 0.1806(6) 0.2370(5) 0.4454(3) 0.0252(15) Uani 1 1 d . . . H30A H 0.2414 0.1850 0.4578 0.030 Uiso 1 1 calc R . . C31 C 0.2265(6) 0.1833(5) 0.3282(3) 0.0232(14) Uani 1 1 d . . . C32 C 0.1490(6) 0.2940(5) 0.5633(3) 0.0263(15) Uani 1 1 d . . . C33 C 0.3817(6) 0.6887(5) 0.3223(4) 0.0288(16) Uani 1 1 d . . . C34 C 0.2602(7) 0.6816(6) 0.3523(4) 0.044(2) Uani 1 1 d . . . H34A H 0.2131 0.7322 0.3769 0.053 Uiso 1 1 calc R . . C35 C 0.2099(7) 0.6004(6) 0.3457(5) 0.047(2) Uani 1 1 d . . . H35A H 0.1299 0.5966 0.3663 0.056 Uiso 1 1 calc R . . C36 C 0.2782(7) 0.5245(6) 0.3084(4) 0.0370(19) Uani 1 1 d . . . H36A H 0.2451 0.4693 0.3049 0.044 Uiso 1 1 calc R . . C37 C 0.3976(6) 0.5316(5) 0.2762(3) 0.0238(15) Uani 1 1 d . . . C38 C 0.4487(6) 0.6127(5) 0.2843(3) 0.0249(15) Uani 1 1 d . . . H38A H 0.5289 0.6163 0.2640 0.030 Uiso 1 1 calc R . . C39 C 0.4711(7) 0.4530(5) 0.2344(3) 0.0271(16) Uani 1 1 d . . . C40 C 0.4386(7) 0.7736(5) 0.3315(3) 0.0280(16) Uani 1 1 d . . . C41 C 0.6499(6) 0.4109(5) 0.3855(3) 0.0241(15) Uani 1 1 d . . . C42 C 0.6212(7) 0.4239(5) 0.4537(4) 0.0334(17) Uani 1 1 d . . . H42A H 0.6464 0.4740 0.4733 0.040 Uiso 1 1 calc R . . C43 C 0.5554(9) 0.3628(6) 0.4924(4) 0.045(2) Uani 1 1 d . . . H43A H 0.5361 0.3719 0.5381 0.055 Uiso 1 1 calc R . . C44 C 0.5177(8) 0.2875(5) 0.4634(4) 0.041(2) Uani 1 1 d . . . H44A H 0.4723 0.2470 0.4897 0.049 Uiso 1 1 calc R . . C45 C 0.5480(6) 0.2727(5) 0.3950(3) 0.0244(15) Uani 1 1 d . . . C46 C 0.6143(6) 0.3336(5) 0.3562(3) 0.0263(15) Uani 1 1 d . . . H46A H 0.6355 0.3237 0.3107 0.032 Uiso 1 1 calc R . . C47 C 0.7141(7) 0.4807(5) 0.3429(3) 0.0263(16) Uani 1 1 d . . . C48 C 0.5107(6) 0.1885(5) 0.3656(3) 0.0230(14) Uani 1 1 d . . . C49 C 0.1157(12) 0.0201(10) 0.5599(6) 0.094(4) Uani 1 1 d . . . H49A H 0.1475 0.0703 0.5331 0.141 Uiso 1 1 calc R . . H49B H 0.1381 0.0203 0.6049 0.141 Uiso 1 1 calc R . . H49C H 0.0255 0.0308 0.5605 0.141 Uiso 1 1 calc R . . C50 C 0.1294(12) -0.1563(9) 0.5681(6) 0.093(4) Uani 1 1 d . . . H50A H 0.1680 -0.2158 0.5475 0.140 Uiso 1 1 calc R . . H50B H 0.0394 -0.1477 0.5688 0.140 Uiso 1 1 calc R . . H50C H 0.1520 -0.1581 0.6131 0.140 Uiso 1 1 calc R . . C51 C 0.2668(9) -0.0789(8) 0.4875(5) 0.062(3) Uani 1 1 d . . . H51A H 0.3077 -0.1409 0.4766 0.074 Uiso 1 1 calc R . . C52 C 0.8683(14) -0.0664(13) -0.0290(8) 0.131(6) Uani 1 1 d . . . H52A H 0.8304 -0.0018 -0.0424 0.196 Uiso 1 1 calc R . . H52B H 0.8276 -0.1116 -0.0478 0.196 Uiso 1 1 calc R . . H52C H 0.9564 -0.0781 -0.0449 0.196 Uiso 1 1 calc R . . C53 C 0.9077(13) -0.1678(10) 0.0744(9) 0.127(6) Uani 1 1 d . . . H53A H 0.8888 -0.1620 0.1219 0.191 Uiso 1 1 calc R . . H53B H 0.9976 -0.1818 0.0635 0.191 Uiso 1 1 calc R . . H53C H 0.8715 -0.2190 0.0601 0.191 Uiso 1 1 calc R . . C54 C 0.7874(10) -0.0090(9) 0.0810(8) 0.084(4) Uani 1 1 d . . . H54A H 0.7768 -0.0247 0.1266 0.101 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 Tb1 0.02482(18) 0.01855(18) 0.02012(17) -0.00399(13) -0.00077(13) -0.00628(14) Tb2 0.02526(18) 0.01524(17) 0.01662(17) -0.00209(12) 0.00234(12) -0.00636(13) Tb3 0.02228(18) 0.01705(18) 0.01746(16) -0.00020(12) 0.00113(12) -0.00563(13) Tb4 0.03068(19) 0.01807(18) 0.02252(18) -0.00328(13) -0.00391(14) -0.00393(14) O1 0.027(3) 0.027(3) 0.059(4) 0.001(2) 0.009(2) -0.009(2) O2 0.054(3) 0.014(3) 0.056(4) 0.000(2) 0.014(3) -0.014(2) O3 0.032(3) 0.015(2) 0.053(3) 0.007(2) -0.005(2) -0.009(2) O4 0.022(3) 0.028(3) 0.049(3) 0.006(2) -0.002(2) -0.006(2) O5 0.025(2) 0.045(3) 0.022(2) -0.015(2) 0.007(2) -0.009(2) O6 0.020(2) 0.027(3) 0.033(3) -0.005(2) 0.008(2) -0.013(2) O7 0.043(3) 0.059(4) 0.026(3) -0.012(2) 0.018(2) -0.029(3) O8 0.029(3) 0.046(3) 0.026(3) -0.007(2) 0.007(2) -0.015(2) O9 0.059(4) 0.052(4) 0.025(3) -0.018(3) -0.008(3) 0.010(3) O10 0.040(3) 0.016(3) 0.039(3) -0.012(2) -0.001(2) -0.004(2) O11 0.036(3) 0.034(3) 0.024(3) -0.001(2) -0.007(2) -0.002(2) O12 0.052(3) 0.020(3) 0.029(3) -0.003(2) -0.009(2) 0.006(2) O13 0.029(3) 0.027(3) 0.027(3) -0.004(2) -0.002(2) 0.002(2) O14 0.024(3) 0.049(3) 0.043(3) -0.010(3) 0.005(2) -0.007(2) O15 0.044(3) 0.034(3) 0.025(3) -0.012(2) -0.012(2) 0.010(2) O16 0.033(3) 0.055(4) 0.029(3) -0.017(3) -0.003(2) 0.016(3) O17 0.024(3) 0.035(3) 0.037(3) -0.008(2) 0.010(2) -0.005(2) O18 0.049(3) 0.026(3) 0.039(3) -0.013(2) 0.002(2) -0.017(2) O19 0.035(3) 0.036(3) 0.031(3) -0.010(2) -0.002(2) -0.013(2) O20 0.045(3) 0.021(3) 0.086(5) -0.023(3) -0.003(3) -0.002(3) O21 0.049(3) 0.061(4) 0.022(3) 0.004(2) 0.002(2) -0.032(3) O22 0.062(4) 0.028(3) 0.042(3) 0.006(2) -0.004(3) -0.027(3) O23 0.030(3) 0.039(3) 0.037(3) -0.010(2) -0.006(2) -0.005(2) O24 0.044(3) 0.019(3) 0.040(3) -0.002(2) -0.002(2) -0.012(2) O25 0.044(3) 0.038(3) 0.037(3) 0.013(3) 0.004(2) -0.006(3) O26 0.095(6) 0.081(6) 0.083(6) -0.029(5) -0.002(5) 0.013(5) O27 0.040(3) 0.028(3) 0.033(3) 0.001(2) -0.010(2) 0.004(2) O28 0.031(3) 0.049(3) 0.038(3) 0.011(3) -0.006(2) -0.003(2) O29 0.052(3) 0.048(3) 0.026(3) -0.004(2) 0.001(2) -0.027(3) O30 0.028(3) 0.039(3) 0.023(2) -0.001(2) 0.0018(19) -0.007(2) O31 0.035(3) 0.071(4) 0.040(3) 0.007(3) -0.003(2) 0.004(3) N1 0.038(4) 0.067(6) 0.096(7) 0.030(5) 0.012(4) -0.018(4) N2 0.051(5) 0.076(7) 0.107(8) -0.033(6) -0.014(5) 0.011(5) C1 0.037(4) 0.019(4) 0.026(4) 0.002(3) -0.006(3) -0.009(3) C2 0.039(5) 0.025(4) 0.065(6) 0.006(4) 0.000(4) 0.010(4) C3 0.030(4) 0.018(4) 0.104(8) -0.005(4) 0.011(5) -0.004(3) C4 0.032(4) 0.032(4) 0.051(5) 0.003(4) 0.006(4) -0.014(3) C5 0.024(3) 0.022(4) 0.029(4) 0.004(3) 0.000(3) -0.008(3) C6 0.030(4) 0.028(4) 0.025(4) 0.007(3) -0.002(3) -0.008(3) C7 0.035(4) 0.016(3) 0.024(3) 0.004(3) -0.003(3) -0.010(3) C8 0.033(4) 0.021(4) 0.018(3) 0.000(3) -0.001(3) -0.005(3) C9 0.020(3) 0.024(4) 0.025(3) -0.006(3) 0.001(3) -0.004(3) C10 0.047(5) 0.050(5) 0.026(4) -0.008(4) 0.002(3) -0.021(4) C11 0.054(5) 0.060(6) 0.040(5) -0.021(4) 0.007(4) -0.033(5) C12 0.050(5) 0.046(5) 0.033(4) -0.011(4) 0.012(4) -0.031(4) C13 0.033(4) 0.036(4) 0.022(4) -0.009(3) 0.006(3) -0.012(3) C14 0.026(3) 0.025(4) 0.028(4) -0.004(3) 0.000(3) -0.008(3) C15 0.015(3) 0.022(4) 0.025(3) -0.003(3) 0.003(3) -0.005(3) C16 0.033(4) 0.020(4) 0.030(4) 0.000(3) 0.001(3) -0.003(3) C17 0.023(3) 0.019(3) 0.029(4) -0.002(3) -0.002(3) -0.007(3) C18 0.030(4) 0.022(4) 0.027(4) -0.001(3) -0.006(3) -0.002(3) C19 0.043(4) 0.027(4) 0.019(3) -0.006(3) -0.005(3) 0.002(3) C20 0.035(4) 0.017(3) 0.024(3) -0.002(3) -0.006(3) 0.001(3) C21 0.026(3) 0.020(3) 0.014(3) 0.002(3) 0.001(2) -0.011(3) C22 0.026(4) 0.026(4) 0.023(3) -0.006(3) -0.005(3) -0.001(3) C23 0.028(4) 0.025(4) 0.015(3) 0.003(3) 0.001(3) -0.003(3) C24 0.026(4) 0.025(4) 0.029(4) -0.010(3) -0.003(3) -0.009(3) C25 0.025(4) 0.028(4) 0.028(4) -0.007(3) -0.004(3) -0.007(3) C26 0.021(4) 0.037(4) 0.049(5) -0.014(4) -0.006(3) 0.006(3) C27 0.037(4) 0.037(4) 0.033(4) -0.009(3) -0.014(3) 0.016(4) C28 0.034(4) 0.037(4) 0.032(4) 0.002(3) -0.010(3) 0.004(3) C29 0.020(3) 0.025(4) 0.029(4) 0.004(3) -0.001(3) -0.014(3) C30 0.027(4) 0.021(3) 0.026(4) -0.004(3) -0.006(3) 0.001(3) C31 0.025(3) 0.030(4) 0.015(3) 0.003(3) 0.000(3) -0.008(3) C32 0.029(4) 0.024(4) 0.027(4) -0.002(3) -0.001(3) -0.007(3) C33 0.023(4) 0.029(4) 0.037(4) -0.005(3) -0.004(3) -0.009(3) C34 0.041(5) 0.033(5) 0.058(5) -0.024(4) 0.010(4) -0.008(4) C35 0.024(4) 0.054(6) 0.067(6) -0.030(5) 0.010(4) -0.014(4) C36 0.031(4) 0.029(4) 0.053(5) -0.019(4) 0.005(3) -0.011(3) C37 0.019(3) 0.019(3) 0.033(4) -0.008(3) 0.006(3) -0.005(3) C38 0.027(4) 0.024(4) 0.025(3) -0.005(3) -0.001(3) -0.008(3) C39 0.031(4) 0.024(4) 0.026(4) -0.004(3) -0.003(3) -0.004(3) C40 0.033(4) 0.026(4) 0.027(4) -0.010(3) -0.001(3) -0.010(3) C41 0.030(4) 0.016(3) 0.028(4) 0.001(3) -0.004(3) -0.008(3) C42 0.051(5) 0.027(4) 0.030(4) -0.003(3) -0.001(3) -0.025(4) C43 0.082(6) 0.041(5) 0.018(4) -0.004(3) 0.010(4) -0.031(5) C44 0.058(5) 0.029(4) 0.039(4) 0.002(3) 0.010(4) -0.026(4) C45 0.030(4) 0.018(3) 0.025(3) -0.001(3) 0.000(3) -0.006(3) C46 0.030(4) 0.030(4) 0.019(3) -0.006(3) 0.001(3) -0.006(3) C47 0.038(4) 0.033(4) 0.014(3) 0.007(3) -0.011(3) -0.020(3) C48 0.023(3) 0.019(3) 0.029(4) -0.006(3) -0.007(3) -0.005(3) C49 0.092(9) 0.113(11) 0.070(8) -0.018(7) 0.010(7) -0.004(8) C50 0.082(9) 0.119(11) 0.086(9) 0.040(8) 0.003(7) -0.058(8) C51 0.052(6) 0.066(7) 0.060(6) 0.017(5) 0.001(5) -0.002(5) C52 0.103(11) 0.21(2) 0.096(12) -0.044(12) -0.004(9) -0.053(12) C53 0.088(10) 0.089(11) 0.193(18) -0.011(11) -0.015(11) 0.016(9) C54 0.047(6) 0.078(9) 0.127(12) -0.001(8) -0.025(7) -0.005(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O18 2.229(5) . ? Tb1 O30 2.263(5) . ? Tb1 O10 2.339(4) . ? Tb1 O14 2.340(5) . ? Tb1 O28 2.377(5) . ? Tb1 O23 2.433(5) . ? Tb1 O29 2.457(5) . ? Tb2 O2 2.251(5) . ? Tb2 O22 2.293(5) 1_545 ? Tb2 O5 2.298(4) . ? Tb2 O11 2.315(5) . ? Tb2 O19 2.356(5) 1_545 ? Tb2 O16 2.397(5) 2_656 ? Tb2 O15 2.447(5) 2_656 ? Tb2 C32 2.815(7) 2_656 ? Tb3 O6 2.288(5) 1_565 ? Tb3 O21 2.294(5) . ? Tb3 O17 2.318(5) . ? Tb3 O12 2.409(5) 1_565 ? Tb3 O4 2.413(5) . ? Tb3 O8 2.454(5) 2_755 ? Tb3 O7 2.489(5) 2_755 ? Tb3 O3 2.573(5) . ? Tb3 C16 2.841(7) 2_755 ? Tb3 C8 2.875(7) . ? Tb4 O9 2.264(5) . ? Tb4 O13 2.318(4) . ? Tb4 O24 2.333(5) . ? Tb4 O20 2.334(5) 1_545 ? Tb4 O1 2.368(5) . ? Tb4 O27 2.383(5) . ? Tb4 O25 2.468(5) . ? O1 C7 1.234(8) . ? O2 C7 1.249(8) . ? O3 C8 1.259(8) . ? O4 C8 1.265(8) . ? O5 C15 1.261(8) . ? O6 C15 1.249(8) . ? O6 Tb3 2.288(5) 1_545 ? O7 C16 1.254(8) . ? O7 Tb3 2.489(5) 2_755 ? O8 C16 1.268(9) . ? O8 Tb3 2.454(5) 2_755 ? O9 C24 1.259(8) . ? O10 C24 1.235(8) . ? O11 C23 1.255(8) . ? O12 C23 1.269(8) . ? O12 Tb3 2.409(5) 1_545 ? O13 C31 1.247(8) . ? O15 C32 1.272(8) . ? O15 Tb2 2.447(5) 2_656 ? O16 C32 1.259(8) . ? O16 Tb2 2.397(5) 2_656 ? O17 C39 1.246(8) . ? O18 C39 1.270(9) . ? O19 C40 1.263(8) . ? O19 Tb2 2.356(5) 1_565 ? O20 C40 1.260(8) . ? O20 Tb4 2.334(5) 1_565 ? O21 C47 1.245(8) . ? O22 C47 1.249(8) . ? O22 Tb2 2.293(5) 1_565 ? O23 C48 1.261(8) . ? O24 C48 1.268(8) . ? O25 C51 1.198(11) . ? O26 C54 1.203(13) . ? O30 C31 1.256(8) . ? O31 H31A 0.8200 . ? O32 H32A 0.8200 . ? N1 C51 1.256(12) . ? N1 C50 1.439(12) . ? N1 C49 1.523(14) . ? N2 C54 1.352(14) . ? N2 C52 1.383(17) . ? N2 C53 1.461(16) . ? C1 C6 1.384(9) . ? C1 C2 1.391(10) . ? C1 C7 1.514(10) . ? C2 C3 1.366(11) . ? C2 H2A 0.9300 . ? C3 C4 1.376(10) . ? C3 H3A 0.9300 . ? C4 C5 1.397(10) . ? C4 H4A 0.9300 . ? C5 C6 1.371(9) . ? C5 C8 1.503(9) . ? C6 H6A 0.9300 . ? C9 C10 1.393(10) . ? C9 C14 1.396(9) . ? C9 C15 1.494(9) . ? C10 C11 1.397(11) . ? C10 H10A 0.9300 . ? C11 C12 1.373(11) . ? C11 H11A 0.9300 . ? C12 C13 1.406(10) . ? C12 H12A 0.9300 . ? C13 C14 1.387(10) . ? C13 C16 1.506(9) . ? C14 H14A 0.9300 . ? C16 Tb3 2.841(7) 2_755 ? C17 C22 1.389(9) . ? C17 C18 1.391(9) . ? C17 C24 1.516(9) . ? C18 C19 1.379(9) . ? C18 H18A 0.9300 . ? C19 C20 1.378(9) . ? C19 H19A 0.9300 . ? C20 C21 1.387(9) . ? C20 H20A 0.9300 . ? C21 C22 1.394(9) . ? C21 C23 1.499(9) . ? C22 H22A 0.9300 . ? C25 C26 1.393(9) . ? C25 C30 1.407(9) . ? C25 C32 1.474(9) . ? C26 C27 1.357(11) . ? C26 H26A 0.9300 . ? C27 C28 1.379(10) . ? C27 H27A 0.9300 . ? C28 C29 1.388(9) . ? C28 H28A 0.9300 . ? C29 C30 1.379(9) . ? C29 C31 1.502(9) . ? C30 H30A 0.9300 . ? C32 Tb2 2.815(7) 2_656 ? C33 C38 1.394(9) . ? C33 C34 1.408(10) . ? C33 C40 1.481(10) . ? C34 C35 1.381(11) . ? C34 H34A 0.9300 . ? C35 C36 1.390(10) . ? C35 H35A 0.9300 . ? C36 C37 1.402(9) . ? C36 H36A 0.9300 . ? C37 C38 1.391(9) . ? C37 C39 1.485(9) . ? C38 H38A 0.9300 . ? C41 C42 1.386(10) . ? C41 C46 1.408(9) . ? C41 C47 1.490(9) . ? C42 C43 1.376(10) . ? C42 H42A 0.9300 . ? C43 C44 1.390(11) . ? C43 H43A 0.9300 . ? C44 C45 1.397(10) . ? C44 H44A 0.9300 . ? C45 C46 1.380(10) . ? C45 C48 1.501(9) . ? C46 H46A 0.9300 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9300 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O18 Tb1 O30 94.13(18) . . ? O18 Tb1 O10 174.09(18) . . ? O30 Tb1 O10 91.10(17) . . ? O18 Tb1 O14 99.81(19) . . ? O30 Tb1 O14 149.27(19) . . ? O10 Tb1 O14 76.87(18) . . ? O18 Tb1 O28 93.4(2) . . ? O30 Tb1 O28 70.59(17) . . ? O10 Tb1 O28 85.77(18) . . ? O14 Tb1 O28 134.93(18) . . ? O18 Tb1 O23 79.57(19) . . ? O30 Tb1 O23 77.42(17) . . ? O10 Tb1 O23 104.30(17) . . ? O14 Tb1 O23 78.37(18) . . ? O28 Tb1 O23 146.66(17) . . ? O18 Tb1 O29 77.23(18) . . ? O30 Tb1 O29 139.88(18) . . ? O10 Tb1 O29 96.99(17) . . ? O14 Tb1 O29 70.41(19) . . ? O28 Tb1 O29 70.92(18) . . ? O23 Tb1 O29 136.79(17) . . ? O2 Tb2 O22 164.4(2) . 1_545 ? O2 Tb2 O5 88.29(19) . . ? O22 Tb2 O5 106.1(2) 1_545 . ? O2 Tb2 O11 93.7(2) . . ? O22 Tb2 O11 95.34(19) 1_545 . ? O5 Tb2 O11 76.62(17) . . ? O2 Tb2 O19 83.62(19) . 1_545 ? O22 Tb2 O19 85.31(19) 1_545 1_545 ? O5 Tb2 O19 155.59(17) . 1_545 ? O11 Tb2 O19 80.96(16) . 1_545 ? O2 Tb2 O16 100.8(2) . 2_656 ? O22 Tb2 O16 77.5(2) 1_545 2_656 ? O5 Tb2 O16 76.39(17) . 2_656 ? O11 Tb2 O16 148.82(16) . 2_656 ? O19 Tb2 O16 127.73(16) 1_545 2_656 ? O2 Tb2 O15 80.76(19) . 2_656 ? O22 Tb2 O15 86.13(19) 1_545 2_656 ? O5 Tb2 O15 124.37(17) . 2_656 ? O11 Tb2 O15 157.73(16) . 2_656 ? O19 Tb2 O15 77.01(16) 1_545 2_656 ? O16 Tb2 O15 53.12(15) 2_656 2_656 ? O2 Tb2 C32 92.7(2) . 2_656 ? O22 Tb2 C32 78.9(2) 1_545 2_656 ? O5 Tb2 C32 101.23(18) . 2_656 ? O11 Tb2 C32 173.15(18) . 2_656 ? O19 Tb2 C32 102.13(18) 1_545 2_656 ? O16 Tb2 C32 26.43(17) 2_656 2_656 ? O15 Tb2 C32 26.82(17) 2_656 2_656 ? O6 Tb3 O21 82.54(18) 1_565 . ? O6 Tb3 O17 141.84(17) 1_565 . ? O21 Tb3 O17 76.96(18) . . ? O6 Tb3 O12 82.64(18) 1_565 1_565 ? O21 Tb3 O12 114.46(18) . 1_565 ? O17 Tb3 O12 77.22(18) . 1_565 ? O6 Tb3 O4 127.47(16) 1_565 . ? O21 Tb3 O4 80.80(19) . . ? O17 Tb3 O4 80.62(17) . . ? O12 Tb3 O4 148.97(17) 1_565 . ? O6 Tb3 O8 79.27(16) 1_565 2_755 ? O21 Tb3 O8 157.72(18) . 2_755 ? O17 Tb3 O8 125.28(17) . 2_755 ? O12 Tb3 O8 75.88(17) 1_565 2_755 ? O4 Tb3 O8 100.24(17) . 2_755 ? O6 Tb3 O7 131.63(16) 1_565 2_755 ? O21 Tb3 O7 145.18(17) . 2_755 ? O17 Tb3 O7 76.94(17) . 2_755 ? O12 Tb3 O7 81.45(18) 1_565 2_755 ? O4 Tb3 O7 72.52(18) . 2_755 ? O8 Tb3 O7 52.59(16) 2_755 2_755 ? O6 Tb3 O3 77.46(16) 1_565 . ? O21 Tb3 O3 85.23(19) . . ? O17 Tb3 O3 131.39(17) . . ? O12 Tb3 O3 149.90(17) 1_565 . ? O4 Tb3 O3 51.80(15) . . ? O8 Tb3 O3 78.37(17) 2_755 . ? O7 Tb3 O3 95.11(18) 2_755 . ? O6 Tb3 C16 105.57(19) 1_565 2_755 ? O21 Tb3 C16 167.1(2) . 2_755 ? O17 Tb3 C16 101.05(19) . 2_755 ? O12 Tb3 C16 77.03(17) 1_565 2_755 ? O4 Tb3 C16 86.30(19) . 2_755 ? O8 Tb3 C16 26.43(18) 2_755 2_755 ? O7 Tb3 C16 26.16(18) 2_755 2_755 ? O3 Tb3 C16 86.77(18) . 2_755 ? O6 Tb3 C8 102.64(18) 1_565 . ? O21 Tb3 C8 82.29(19) . . ? O17 Tb3 C8 106.02(19) . . ? O12 Tb3 C8 163.11(17) 1_565 . ? O4 Tb3 C8 25.84(18) . . ? O8 Tb3 C8 89.22(18) 2_755 . ? O7 Tb3 C8 83.17(19) 2_755 . ? O3 Tb3 C8 25.97(17) . . ? C16 Tb3 C8 86.09(18) 2_755 . ? O9 Tb4 O13 82.46(17) . . ? O9 Tb4 O24 120.5(2) . . ? O13 Tb4 O24 77.73(17) . . ? O9 Tb4 O20 83.5(2) . 1_545 ? O13 Tb4 O20 95.42(18) . 1_545 ? O24 Tb4 O20 153.2(2) . 1_545 ? O9 Tb4 O1 75.7(2) . . ? O13 Tb4 O1 138.04(18) . . ? O24 Tb4 O1 83.11(18) . . ? O20 Tb4 O1 116.74(18) 1_545 . ? O9 Tb4 O27 142.44(17) . . ? O13 Tb4 O27 135.02(16) . . ? O24 Tb4 O27 78.31(17) . . ? O20 Tb4 O27 89.3(2) 1_545 . ? O1 Tb4 O27 74.87(19) . . ? O9 Tb4 O25 142.2(2) . . ? O13 Tb4 O25 69.45(17) . . ? O24 Tb4 O25 78.61(18) . . ? O20 Tb4 O25 74.8(2) 1_545 . ? O1 Tb4 O25 141.88(19) . . ? O27 Tb4 O25 68.84(17) . . ? C7 O1 Tb4 153.7(5) . . ? C7 O2 Tb2 148.3(5) . . ? C8 O3 Tb3 90.6(4) . . ? C8 O4 Tb3 97.9(4) . . ? C15 O5 Tb2 137.7(4) . . ? C15 O6 Tb3 148.1(4) . 1_545 ? C16 O7 Tb3 92.8(4) . 2_755 ? C16 O8 Tb3 94.1(4) . 2_755 ? C24 O9 Tb4 172.6(5) . . ? C24 O10 Tb1 123.3(4) . . ? C23 O11 Tb2 167.7(5) . . ? C23 O12 Tb3 114.0(4) . 1_545 ? C31 O13 Tb4 141.5(4) . . ? C32 O15 Tb2 92.9(4) . 2_656 ? C32 O16 Tb2 95.7(4) . 2_656 ? C39 O17 Tb3 160.5(5) . . ? C39 O18 Tb1 155.6(5) . . ? C40 O19 Tb2 157.5(5) . 1_565 ? C40 O20 Tb4 117.7(5) . 1_565 ? C47 O21 Tb3 153.7(5) . . ? C47 O22 Tb2 126.6(5) . 1_565 ? C48 O23 Tb1 156.1(4) . . ? C48 O24 Tb4 111.9(4) . . ? C51 O25 Tb4 133.5(6) . . ? C31 O30 Tb1 133.8(4) . . ? C51 N1 C50 129.0(10) . . ? C51 N1 C49 116.4(9) . . ? C50 N1 C49 112.6(9) . . ? C54 N2 C52 123.9(13) . . ? C54 N2 C53 114.8(13) . . ? C52 N2 C53 121.2(12) . . ? C6 C1 C2 117.7(7) . . ? C6 C1 C7 120.5(6) . . ? C2 C1 C7 121.8(6) . . ? C3 C2 C1 121.2(7) . . ? C3 C2 H2A 119.4 . . ? C1 C2 H2A 119.4 . . ? C2 C3 C4 120.9(7) . . ? C2 C3 H3A 119.6 . . ? C4 C3 H3A 119.6 . . ? C3 C4 C5 118.7(7) . . ? C3 C4 H4A 120.7 . . ? C5 C4 H4A 120.7 . . ? C6 C5 C4 120.0(6) . . ? C6 C5 C8 119.6(6) . . ? C4 C5 C8 120.3(6) . . ? C5 C6 C1 121.5(6) . . ? C5 C6 H6A 119.2 . . ? C1 C6 H6A 119.2 . . ? O1 C7 O2 125.7(6) . . ? O1 C7 C1 118.6(6) . . ? O2 C7 C1 115.7(6) . . ? O3 C8 O4 119.7(6) . . ? O3 C8 C5 122.8(6) . . ? O4 C8 C5 117.5(6) . . ? O3 C8 Tb3 63.5(3) . . ? O4 C8 Tb3 56.2(3) . . ? C5 C8 Tb3 173.6(5) . . ? C10 C9 C14 119.4(6) . . ? C10 C9 C15 122.2(6) . . ? C14 C9 C15 118.3(6) . . ? C9 C10 C11 120.1(7) . . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C12 C11 C10 120.4(8) . . ? C12 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? C11 C12 C13 120.0(7) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C14 C13 C12 119.6(7) . . ? C14 C13 C16 119.7(6) . . ? C12 C13 C16 120.7(6) . . ? C13 C14 C9 120.5(7) . . ? C13 C14 H14A 119.7 . . ? C9 C14 H14A 119.7 . . ? O6 C15 O5 124.9(6) . . ? O6 C15 C9 117.2(6) . . ? O5 C15 C9 117.9(6) . . ? O7 C16 O8 120.5(6) . . ? O7 C16 C13 120.2(7) . . ? O8 C16 C13 119.3(6) . . ? O7 C16 Tb3 61.0(4) . 2_755 ? O8 C16 Tb3 59.5(3) . 2_755 ? C13 C16 Tb3 177.8(5) . 2_755 ? C22 C17 C18 119.7(6) . . ? C22 C17 C24 120.3(6) . . ? C18 C17 C24 120.0(6) . . ? C19 C18 C17 120.3(6) . . ? C19 C18 H18A 119.9 . . ? C17 C18 H18A 119.9 . . ? C20 C19 C18 120.0(6) . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 C20 C21 120.7(6) . . ? C19 C20 H20A 119.7 . . ? C21 C20 H20A 119.7 . . ? C20 C21 C22 119.3(6) . . ? C20 C21 C23 120.2(6) . . ? C22 C21 C23 120.4(6) . . ? C17 C22 C21 120.0(6) . . ? C17 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? O11 C23 O12 121.6(6) . . ? O11 C23 C21 119.0(6) . . ? O12 C23 C21 119.5(6) . . ? O10 C24 O9 124.2(6) . . ? O10 C24 C17 119.0(6) . . ? O9 C24 C17 116.9(6) . . ? C26 C25 C30 118.3(6) . . ? C26 C25 C32 120.0(6) . . ? C30 C25 C32 121.6(6) . . ? C27 C26 C25 121.5(7) . . ? C27 C26 H26A 119.3 . . ? C25 C26 H26A 119.3 . . ? C26 C27 C28 119.9(7) . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C27 C28 C29 120.2(7) . . ? C27 C28 H28A 119.9 . . ? C29 C28 H28A 119.9 . . ? C30 C29 C28 119.9(6) . . ? C30 C29 C31 119.3(6) . . ? C28 C29 C31 120.6(6) . . ? C29 C30 C25 119.9(6) . . ? C29 C30 H30A 120.0 . . ? C25 C30 H30A 120.0 . . ? O13 C31 O30 123.9(6) . . ? O13 C31 C29 119.1(5) . . ? O30 C31 C29 117.0(6) . . ? O16 C32 O15 117.7(6) . . ? O16 C32 C25 120.6(6) . . ? O15 C32 C25 121.6(6) . . ? O16 C32 Tb2 57.9(4) . 2_656 ? O15 C32 Tb2 60.3(3) . 2_656 ? C25 C32 Tb2 170.3(5) . 2_656 ? C38 C33 C34 118.2(7) . . ? C38 C33 C40 120.4(6) . . ? C34 C33 C40 121.4(6) . . ? C35 C34 C33 121.0(7) . . ? C35 C34 H34A 119.5 . . ? C33 C34 H34A 119.5 . . ? C34 C35 C36 120.4(7) . . ? C34 C35 H35A 119.8 . . ? C36 C35 H35A 119.8 . . ? C35 C36 C37 119.5(7) . . ? C35 C36 H36A 120.2 . . ? C37 C36 H36A 120.2 . . ? C38 C37 C36 119.7(6) . . ? C38 C37 C39 119.6(6) . . ? C36 C37 C39 120.7(6) . . ? C37 C38 C33 121.2(6) . . ? C37 C38 H38A 119.4 . . ? C33 C38 H38A 119.4 . . ? O17 C39 O18 123.2(6) . . ? O17 C39 C37 119.8(6) . . ? O18 C39 C37 117.1(6) . . ? O20 C40 O19 121.1(7) . . ? O20 C40 C33 118.0(7) . . ? O19 C40 C33 120.9(6) . . ? C42 C41 C46 119.8(6) . . ? C42 C41 C47 120.1(6) . . ? C46 C41 C47 120.0(6) . . ? C43 C42 C41 120.1(7) . . ? C43 C42 H42A 119.9 . . ? C41 C42 H42A 119.9 . . ? C42 C43 C44 120.3(7) . . ? C42 C43 H43A 119.9 . . ? C44 C43 H43A 119.9 . . ? C43 C44 C45 120.1(7) . . ? C43 C44 H44A 119.9 . . ? C45 C44 H44A 119.9 . . ? C46 C45 C44 119.7(7) . . ? C46 C45 C48 121.3(6) . . ? C44 C45 C48 119.0(6) . . ? C45 C46 C41 119.9(6) . . ? C45 C46 H46A 120.0 . . ? C41 C46 H46A 120.0 . . ? O21 C47 O22 122.9(7) . . ? O21 C47 C41 120.3(6) . . ? O22 C47 C41 116.8(6) . . ? O23 C48 O24 123.3(6) . . ? O23 C48 C45 121.0(6) . . ? O24 C48 C45 115.6(6) . . ? N1 C49 H49A 109.5 . . ? N1 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N1 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N1 C50 H50A 109.5 . . ? N1 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N1 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O25 C51 N1 133.1(10) . . ? O25 C51 H51A 113.5 . . ? N1 C51 H51A 113.5 . . ? N2 C52 H52A 109.5 . . ? N2 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N2 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N2 C53 H53A 109.5 . . ? N2 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N2 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O26 C54 N2 123.8(14) . . ? O26 C54 H54A 118.1 . . ? N2 C54 H54A 118.1 . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 1.884 _refine_diff_density_min -1.345 _refine_diff_density_rms 0.169 #==END