# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Qin Wang' _publ_contact_author_email wangqin000@126.com loop_ _publ_author_name 'Qin Wang' 'Kuan-Zhen Tang' 'Xiao-Jie Jin' 'Xiaoguang Huang' 'Weisheng Liu' 'Xiaojun Yao' 'Yu Tang' data_060514t _database_code_depnum_ccdc_archive 'CCDC 826838' #TrackingRef '1-.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H75 Cl3 Eu N11 O20' _chemical_formula_weight 1504.60 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.415(5) _cell_length_b 14.760(5) _cell_length_c 19.746(7) _cell_angle_alpha 98.206(6) _cell_angle_beta 100.862(6) _cell_angle_gamma 93.150(6) _cell_volume 4069(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1548 _exptl_absorpt_coefficient_mu 0.934 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6785 _exptl_absorpt_correction_T_max 0.9042 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19136 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.1614 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12967 _reflns_number_gt 6194 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _vrf_PLAT029_060514t ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.904 RESPONSE:The crystals diffracted very weakly and higher angle reflections are not included in the refinement. These theoretical reflections were simply the reslut of noise. ; _vrf_PLAT234_060514t ; PROBLEM: Large Hirshfeld Difference C55 -- C56 .. 0.27 Ang. RESPONSE: Contributions of disordered acetone solvent molecules. ; _vrf_PLAT331_060514t ; PROBLEM: Small Average Phenyl C-C Dist. C15 -C20 1.36 Ang. RESPONSE: Contributions of disordered benzyl. ; _vrf_PLAT332_060514t ; PROBLEM: Large Phenyl C-C Range C8 -C13 0.35 Ang. RESPONSE: Contributions of disordered benzyl. ; _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^)+(0.1051P)^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 12967 _refine_ls_number_parameters 883 _refine_ls_number_restraints 2123 _refine_ls_R_factor_all 0.1727 _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_ref 0.2236 _refine_ls_wR_factor_gt 0.1643 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.955 _refine_ls_shift/su_max 0.000 _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 0.27932(3) 0.73678(3) 0.21088(3) 0.0583(2) Uani 1 1 d . . . Cl1 Cl 0.4591(5) 0.8737(4) 0.5728(3) 0.108(2) Uani 0.50 1 d PDU . . Cl2 Cl 0.4318(8) 0.6831(6) 0.5675(7) 0.196(5) Uani 0.50 1 d PDU . . Cl3 Cl 0.6169(6) 0.7738(8) 0.6014(5) 0.157(3) Uani 0.50 1 d PDU . . Cl4 Cl 0.4232(7) 0.8031(6) 0.9250(6) 0.165(3) Uani 0.50 1 d PDU . . Cl5 Cl 0.6088(5) 0.7430(6) 0.9435(4) 0.122(2) Uani 0.50 1 d PDU . . Cl6 Cl 0.4501(5) 0.6152(4) 0.9172(3) 0.1037(19) Uani 0.50 1 d PDU . . N1 N 0.3652(5) 0.8919(5) 0.2925(4) 0.0676(18) Uani 1 1 d U . . N2 N 0.2490(7) 1.0281(6) 0.1714(5) 0.093(2) Uani 1 1 d U . . H2 H 0.2978 1.0521 0.1553 0.112 Uiso 1 1 d R . . N3 N 0.5310(6) 0.7590(6) 0.3899(5) 0.078(2) Uani 1 1 d U . . H3 H 0.5862 0.7882 0.3870 0.094 Uiso 1 1 d R . . N4 N 0.2485(7) 0.8409(6) 0.4307(5) 0.083(2) Uani 1 1 d U . . H4 H 0.3068 0.8551 0.4573 0.099 Uiso 1 1 d R . . N5 N 0.3696(5) 0.5979(5) 0.1525(4) 0.0574(16) Uani 1 1 d U . . N6 N 0.5387(6) 0.7652(6) 0.1139(5) 0.078(2) Uani 1 1 d U . . H6 H 0.5918 0.7431 0.1347 0.093 Uiso 1 1 d R . . N7 N 0.2292(7) 0.6179(6) -0.0184(5) 0.086(2) Uani 1 1 d DU . . H7 H 0.2827 0.6139 -0.0356 0.104 Uiso 1 1 d R . . N8 N 0.2660(7) 0.4419(6) 0.2452(5) 0.084(2) Uani 1 1 d U . . H8 H 0.2605 0.3981 0.2076 0.101 Uiso 1 1 d R . . N9 N 0.2885(9) 0.3939(9) 0.9119(7) 0.109(3) Uani 1 1 d U . . N10 N 0.3757(9) 0.2403(6) 0.2239(5) 0.087(3) Uani 1 1 d U . . N11 N 0.2920(9) 0.0747(8) 0.5169(7) 0.109(3) Uani 1 1 d U . . O1 O 0.2289(5) 0.8798(4) 0.1772(4) 0.0785(16) Uani 1 1 d U . . O2 O 0.4149(4) 0.7142(4) 0.2974(3) 0.0692(15) Uani 1 1 d U . . O3 O 0.2322(5) 0.7667(4) 0.3218(4) 0.0779(16) Uani 1 1 d U . . O4 O 0.4146(5) 0.7859(4) 0.1640(3) 0.0688(14) Uani 1 1 d U . . O5 O 0.2334(5) 0.6989(4) 0.0863(4) 0.0740(16) Uani 1 1 d U . . O6 O 0.2368(5) 0.5832(4) 0.2294(4) 0.0716(15) Uani 1 1 d U . . O7 O 0.1077(6) 0.7231(5) 0.1889(5) 0.102(2) Uani 1 1 d DU . . O8 O 0.2248(8) 0.4406(8) 0.9034(6) 0.147(4) Uani 1 1 d U . . O9 O 0.3687(8) 0.4270(8) 0.9451(6) 0.132(3) Uani 1 1 d U . . O10 O 0.2781(8) 0.3119(8) 0.8896(7) 0.147(4) Uani 1 1 d U . . O11 O 0.4156(6) 0.3159(5) 0.2349(4) 0.096(2) Uani 1 1 d U . . O12 O 0.2864(8) 0.2301(6) 0.2112(5) 0.122(3) Uani 1 1 d U . . O13 O 0.4177(7) 0.1715(5) 0.2200(5) 0.111(3) Uani 1 1 d U . . O14 O 0.2904(8) 0.1515(7) 0.5415(7) 0.153(4) Uani 1 1 d U . . O15 O 0.2296(9) 0.0243(9) 0.4938(8) 0.185(5) Uani 1 1 d U . . O16 O 0.3681(9) 0.0414(8) 0.5199(6) 0.145(4) Uani 1 1 d U . . O17 O 0.0751(9) 0.5984(11) 0.7215(7) 0.183(5) Uani 1 1 d U . . H61 H 0.0999 0.5591 0.6945 0.220 Uiso 1 1 d R . . H62 H 0.0868 0.6511 0.7086 0.220 Uiso 1 1 d R . . O18 O 0.1510(12) 0.1231(10) 0.3053(9) 0.175(5) Uani 0.85 1 d PU . . H63 H 0.1742 0.1207 0.3489 0.210 Uiso 0.85 1 d PR . . H64 H 0.0931 0.0985 0.2986 0.210 Uiso 0.85 1 d PR . . O19 O 0.0595(8) 0.9551(8) 0.2880(6) 0.152(3) Uani 1 1 d U . . H65 H 0.1177 0.9787 0.2944 0.182 Uiso 1 1 d R . . H66 H 0.0397 0.9776 0.3254 0.182 Uiso 1 1 d R . . O20 O 0.2187(16) 0.7225(16) 0.7310(14) 0.200(7) Uani 0.65 1 d PU . . H67 H 0.1849 0.7671 0.7425 0.241 Uiso 0.65 1 d PR . . H68 H 0.2240 0.7270 0.6885 0.241 Uiso 0.65 1 d PR . . O21 O 0.138(2) 0.666(2) 0.6136(16) 0.203(7) Uani 0.50 1 d PU . . H69 H 0.1767 0.7135 0.6340 0.244 Uiso 0.50 1 d PR . . H70 H 0.0852 0.6879 0.5955 0.244 Uiso 0.50 1 d PR . . C1 C 0.2760(8) 0.9551(7) 0.1976(6) 0.075(2) Uani 1 1 d U . . C2 C 0.3688(8) 0.9638(6) 0.2484(6) 0.078(2) Uani 1 1 d U . . H2A H 0.4205 0.9562 0.2235 0.093 Uiso 1 1 calc R . . H2B H 0.3789 1.0240 0.2769 0.093 Uiso 1 1 calc R . . C3 C 0.4662(7) 0.7762(6) 0.3370(5) 0.066(2) Uani 1 1 d U . . C4 C 0.4614(7) 0.8737(6) 0.3264(6) 0.072(2) Uani 1 1 d U . . H4A H 0.4796 0.9132 0.3712 0.087 Uiso 1 1 calc R . . H4B H 0.5061 0.8884 0.2977 0.087 Uiso 1 1 calc R . . C5 C 0.2623(8) 0.8361(7) 0.3665(6) 0.080(2) Uani 1 1 d U . . C6 C 0.3074(8) 0.9192(6) 0.3456(6) 0.077(2) Uani 1 1 d U . . H6A H 0.2584 0.9564 0.3267 0.092 Uiso 1 1 calc R . . H6B H 0.3473 0.9559 0.3864 0.092 Uiso 1 1 calc R . . C7 C 0.1647(10) 1.0251(9) 0.1190(8) 0.105(3) Uani 1 1 d U . . H7A H 0.1333 1.0806 0.1287 0.126 Uiso 1 1 calc R . . H7B H 0.1221 0.9733 0.1220 0.126 Uiso 1 1 calc R . . C8 C 0.1824(12) 1.0168(10) 0.0451(9) 0.121(3) Uani 1 1 d U . . C9 C 0.1745(13) 1.0876(12) 0.0007(10) 0.142(4) Uani 1 1 d U . . H9 H 0.1577 1.1437 0.0208 0.170 Uiso 1 1 calc R . . C10 C 0.1883(14) 1.0841(13) -0.0680(11) 0.157(4) Uani 1 1 d U . . H10 H 0.1878 1.1349 -0.0910 0.189 Uiso 1 1 calc R . . C11 C 0.2038(14) 0.9910(14) -0.0998(12) 0.157(5) Uani 1 1 d U . . H11 H 0.1950 0.9743 -0.1479 0.188 Uiso 1 1 calc R . . C12 C 0.2279(15) 0.9386(14) -0.0611(11) 0.161(5) Uani 1 1 d U . . H12 H 0.2636 0.8925 -0.0770 0.193 Uiso 1 1 calc R . . C13 C 0.2070(12) 0.9380(12) 0.0120(10) 0.138(3) Uani 1 1 d U . . H13 H 0.2112 0.8854 0.0328 0.166 Uiso 1 1 calc R . . C14 C 0.5435(8) 0.6668(8) 0.4029(6) 0.087(3) Uani 1 1 d U . . H14A H 0.4822 0.6348 0.4006 0.104 Uiso 1 1 calc R . . H14B H 0.5808 0.6683 0.4494 0.104 Uiso 1 1 calc R . . C15 C 0.5962(8) 0.6126(7) 0.3465(6) 0.080(2) Uani 1 1 d U . . C16 C 0.5794(9) 0.5213(8) 0.3313(7) 0.097(3) Uani 1 1 d U . . H16 H 0.5386 0.4908 0.3534 0.116 Uiso 1 1 calc R . . C17 C 0.6224(11) 0.4723(10) 0.2830(8) 0.111(3) Uani 1 1 d U . . H17 H 0.6108 0.4088 0.2725 0.133 Uiso 1 1 calc R . . C18 C 0.6816(10) 0.5171(10) 0.2507(8) 0.111(3) Uani 1 1 d U . . H18 H 0.7098 0.4852 0.2169 0.133 Uiso 1 1 calc R . . C19 C 0.6996(10) 0.6127(9) 0.2695(8) 0.104(3) Uani 1 1 d U . . H19 H 0.7425 0.6441 0.2496 0.125 Uiso 1 1 calc R . . C20 C 0.6566(8) 0.6580(8) 0.3146(7) 0.088(3) Uani 1 1 d U . . H20 H 0.6672 0.7216 0.3251 0.105 Uiso 1 1 calc R . . C21 C 0.2056(9) 0.7688(8) 0.4575(7) 0.098(3) Uani 1 1 d U . . H21A H 0.2279 0.7767 0.5077 0.118 Uiso 1 1 calc R . . H21B H 0.2249 0.7107 0.4375 0.118 Uiso 1 1 calc R . . C22 C 0.0955(10) 0.7659(10) 0.4413(7) 0.103(3) Uani 1 1 d U . . C23 C 0.0411(11) 0.6896(11) 0.4110(8) 0.124(3) Uani 1 1 d U . . H23 H 0.0693 0.6356 0.4004 0.149 Uiso 1 1 calc R . . C24 C -0.0563(12) 0.6891(13) 0.3950(9) 0.137(4) Uani 1 1 d U . . H24 H -0.0936 0.6361 0.3723 0.165 Uiso 1 1 calc R . . C25 C -0.0963(12) 0.7669(13) 0.4130(9) 0.131(4) Uani 1 1 d U . . H25 H -0.1620 0.7670 0.4037 0.157 Uiso 1 1 calc R . . C26 C -0.0461(12) 0.8399(12) 0.4423(9) 0.131(4) Uani 1 1 d U . . H26 H -0.0767 0.8924 0.4529 0.157 Uiso 1 1 calc R . . C27 C 0.0507(11) 0.8457(11) 0.4594(8) 0.120(3) Uani 1 1 d U . . H27 H 0.0855 0.9001 0.4820 0.144 Uiso 1 1 calc R . . C28 C 0.4705(7) 0.7352(6) 0.1416(5) 0.064(2) Uani 1 1 d U . . C29 C 0.4615(7) 0.6326(6) 0.1439(6) 0.066(2) Uani 1 1 d U . . H29A H 0.4748 0.6001 0.1010 0.079 Uiso 1 1 calc R . . H29B H 0.5091 0.6194 0.1822 0.079 Uiso 1 1 calc R . . C30 C 0.2577(7) 0.6307(7) 0.0512(6) 0.067(2) Uani 1 1 d U . . C31 C 0.3077(7) 0.5596(6) 0.0829(5) 0.068(2) Uani 1 1 d U . . H31A H 0.2621 0.5122 0.0891 0.081 Uiso 1 1 calc R . . H31B H 0.3466 0.5315 0.0520 0.081 Uiso 1 1 calc R . . C32 C 0.2856(7) 0.5198(6) 0.2268(5) 0.063(2) Uani 1 1 d U . . C33 C 0.3769(7) 0.5286(6) 0.1967(5) 0.068(2) Uani 1 1 d U . . H33A H 0.4314 0.5448 0.2346 0.081 Uiso 1 1 calc R . . H33B H 0.3856 0.4702 0.1702 0.081 Uiso 1 1 calc R . . C34 C 0.5594(9) 0.8623(8) 0.1119(6) 0.089(3) Uani 1 1 d U . . H34A H 0.5005 0.8892 0.0971 0.107 Uiso 1 1 calc R . . H34B H 0.5986 0.8685 0.0777 0.107 Uiso 1 1 calc R . . C35 C 0.6095(8) 0.9142(8) 0.1817(7) 0.086(2) Uani 1 1 d U . . C36 C 0.6740(10) 0.8777(9) 0.2291(7) 0.097(3) Uani 1 1 d U . . H36 H 0.6857 0.8164 0.2189 0.117 Uiso 1 1 calc R . . C37 C 0.7194(10) 0.9264(9) 0.2883(8) 0.106(3) Uani 1 1 d U . . H37 H 0.7643 0.9005 0.3184 0.127 Uiso 1 1 calc R . . C38 C 0.6999(11) 1.0147(10) 0.3048(9) 0.118(4) Uani 1 1 d U . . H38 H 0.7295 1.0483 0.3477 0.141 Uiso 1 1 calc R . . C39 C 0.6410(11) 1.0533(9) 0.2623(8) 0.108(3) Uani 1 1 d U . . H39 H 0.6323 1.1152 0.2734 0.130 Uiso 1 1 calc R . . C40 C 0.5919(9) 1.0042(8) 0.2015(7) 0.097(3) Uani 1 1 d U . . H40 H 0.5461 1.0313 0.1730 0.116 Uiso 1 1 calc R . . C41 C 0.1686(9) 0.6768(9) -0.0567(7) 0.101(3) Uani 1 1 d DU . . H41A H 0.1911 0.7399 -0.0368 0.122 Uiso 1 1 calc R . . H41B H 0.1785 0.6676 -0.1044 0.122 Uiso 1 1 calc R . . C42 C 0.0686(11) 0.6677(9) -0.0597(7) 0.106(3) Uani 1 1 d U . . C43 C 0.0181(11) 0.6175(11) -0.0177(8) 0.124(3) Uani 1 1 d U . . H43 H 0.0507 0.5828 0.0132 0.149 Uiso 1 1 calc R . . C44 C -0.0858(14) 0.6218(13) -0.0245(11) 0.150(4) Uani 1 1 d U . . H44 H -0.1185 0.6004 0.0071 0.180 Uiso 1 1 calc R . . C45 C -0.1266(13) 0.6560(12) -0.0754(10) 0.135(4) Uani 1 1 d U . . H45 H -0.1925 0.6495 -0.0854 0.163 Uiso 1 1 calc R . . C46 C -0.0844(14) 0.7007(12) -0.1162(10) 0.139(4) Uani 1 1 d U . . H46 H -0.1185 0.7319 -0.1491 0.167 Uiso 1 1 calc R . . C47 C 0.0015(12) 0.6990(11) -0.1087(9) 0.128(4) Uani 1 1 d U . . H47 H 0.0268 0.7237 -0.1427 0.154 Uiso 1 1 calc R . . C48 C 0.1840(10) 0.4270(8) 0.2817(7) 0.103(3) Uani 1 1 d U . . H48A H 0.1387 0.4716 0.2709 0.123 Uiso 1 1 calc R . . H48B H 0.1523 0.3663 0.2635 0.123 Uiso 1 1 calc R . . C49 C 0.2116(11) 0.4348(9) 0.3548(8) 0.107(3) Uani 1 1 d U . . C50 C 0.2670(12) 0.5134(11) 0.3968(8) 0.128(3) Uani 1 1 d U . . H50 H 0.2918 0.5608 0.3774 0.154 Uiso 1 1 calc R . . C51 C 0.2830(15) 0.5144(14) 0.4770(10) 0.155(4) Uani 1 1 d U . . H51 H 0.3178 0.5605 0.5107 0.186 Uiso 1 1 calc R . . C52 C 0.2368(15) 0.4348(15) 0.4906(10) 0.150(4) Uani 1 1 d U . . H52 H 0.2329 0.4389 0.5374 0.180 Uiso 1 1 calc R . . C53 C 0.2005(14) 0.3619(14) 0.4570(10) 0.148(4) Uani 1 1 d U . . H53 H 0.1797 0.3140 0.4777 0.178 Uiso 1 1 calc R . . C54 C 0.1927(13) 0.3559(13) 0.3873(10) 0.143(4) Uani 1 1 d U . . H54 H 0.1744 0.2992 0.3593 0.171 Uiso 1 1 calc R . . C55 C 0.0002(13) 0.6048(11) 0.1947(12) 0.183(7) Uani 1 1 d DU . . H55A H 0.0511 0.5688 0.1850 0.274 Uiso 1 1 calc R . . H55B H -0.0564 0.5830 0.1608 0.274 Uiso 1 1 calc R . . H55C H -0.0104 0.5992 0.2405 0.274 Uiso 1 1 calc R . . C56 C 0.0257(9) 0.7031(9) 0.1912(8) 0.116(4) Uani 1 1 d DU . . C57 C -0.0451(12) 0.7655(12) 0.2085(12) 0.172(6) Uani 1 1 d DU . . H57A H -0.0278 0.8257 0.1995 0.259 Uiso 1 1 calc R . . H57B H -0.0477 0.7685 0.2570 0.259 Uiso 1 1 calc R . . H57C H -0.1061 0.7432 0.1805 0.259 Uiso 1 1 calc R . . C58 C 0.5020(11) 0.7805(11) 0.6095(12) 0.114(7) Uani 0.50 1 d PDU . . H58 H 0.4988 0.7896 0.6591 0.137 Uiso 0.50 1 calc PR . . C59 C 0.4917(11) 0.7189(11) 0.9009(12) 0.111(7) Uani 0.50 1 d PDU . . H59 H 0.4893 0.7144 0.8506 0.134 Uiso 0.50 1 calc PR . . 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 0.0504(3) 0.0456(3) 0.0729(4) -0.0047(2) 0.0095(2) -0.00079(17) Cl1 0.134(5) 0.089(4) 0.088(4) 0.014(3) -0.006(4) -0.007(4) Cl2 0.200(9) 0.127(6) 0.227(10) 0.052(7) -0.043(8) -0.050(6) Cl3 0.120(6) 0.228(9) 0.124(6) 0.019(6) 0.018(5) 0.054(6) Cl4 0.159(8) 0.158(7) 0.194(9) 0.074(7) 0.034(7) 0.041(6) Cl5 0.095(5) 0.170(7) 0.095(5) 0.014(4) 0.017(4) -0.018(4) Cl6 0.117(5) 0.108(4) 0.089(4) 0.007(3) 0.037(4) 0.000(4) N1 0.061(4) 0.058(3) 0.084(4) 0.005(3) 0.021(3) -0.002(3) N2 0.112(5) 0.062(4) 0.107(5) 0.028(4) 0.019(5) -0.002(4) N3 0.075(4) 0.073(4) 0.080(5) 0.013(4) -0.003(4) -0.003(4) N4 0.088(5) 0.080(4) 0.076(5) 0.001(4) 0.021(4) -0.005(4) N5 0.056(3) 0.053(3) 0.064(4) 0.009(3) 0.013(3) 0.008(3) N6 0.077(4) 0.080(4) 0.084(5) 0.012(4) 0.036(4) 0.003(4) N7 0.095(5) 0.097(5) 0.069(5) 0.006(4) 0.022(4) 0.021(4) N8 0.101(5) 0.071(4) 0.087(5) 0.016(4) 0.032(4) 0.002(4) N9 0.083(8) 0.104(8) 0.132(9) -0.042(7) 0.043(7) 0.017(7) N10 0.108(7) 0.056(5) 0.100(7) 0.025(5) 0.020(6) 0.009(5) N11 0.077(7) 0.093(7) 0.144(9) -0.034(7) 0.033(7) -0.023(6) O1 0.076(4) 0.055(3) 0.102(4) 0.013(3) 0.010(3) 0.001(3) O2 0.067(3) 0.055(3) 0.078(3) 0.002(3) 0.004(3) -0.005(3) O3 0.080(4) 0.068(3) 0.086(4) -0.005(3) 0.034(3) -0.006(3) O4 0.067(3) 0.059(3) 0.082(3) 0.003(3) 0.025(3) 0.006(3) O5 0.077(4) 0.065(3) 0.079(4) 0.011(3) 0.012(3) 0.011(3) O6 0.075(3) 0.051(3) 0.091(4) 0.009(3) 0.026(3) 0.003(3) O7 0.070(4) 0.097(5) 0.134(6) 0.024(4) 0.008(4) 0.000(4) O8 0.101(7) 0.138(8) 0.176(9) -0.042(7) 0.006(6) 0.038(6) O9 0.092(7) 0.155(8) 0.142(8) -0.014(6) 0.035(6) 0.013(6) O10 0.119(8) 0.126(8) 0.188(10) -0.024(7) 0.038(7) 0.020(6) O11 0.112(6) 0.061(4) 0.115(6) 0.014(4) 0.019(5) 0.000(4) O12 0.116(7) 0.105(6) 0.143(7) 0.017(5) 0.022(6) 0.008(5) O13 0.136(7) 0.061(4) 0.145(7) 0.038(5) 0.030(6) 0.023(5) O14 0.129(8) 0.092(6) 0.203(10) -0.066(7) 0.015(7) -0.012(5) O15 0.110(8) 0.147(9) 0.250(13) -0.085(9) 0.012(8) -0.013(7) O16 0.104(8) 0.157(9) 0.162(9) -0.007(7) 0.026(7) 0.008(7) O17 0.145(9) 0.234(12) 0.196(11) 0.071(9) 0.076(8) 0.001(8) O18 0.184(11) 0.155(10) 0.181(11) 0.006(9) 0.038(9) 0.013(9) O19 0.119(6) 0.148(7) 0.163(8) -0.023(6) 0.000(6) 0.006(6) O20 0.176(13) 0.214(14) 0.222(14) 0.049(13) 0.054(12) 0.007(11) O21 0.193(14) 0.234(16) 0.204(15) 0.057(14) 0.079(13) 0.016(13) C1 0.084(5) 0.053(4) 0.095(5) 0.015(4) 0.027(4) 0.011(4) C2 0.079(5) 0.056(4) 0.095(5) 0.009(4) 0.015(4) -0.005(4) C3 0.055(4) 0.061(4) 0.077(5) -0.003(4) 0.012(4) -0.007(4) C4 0.062(4) 0.063(4) 0.083(5) 0.000(4) 0.006(4) -0.007(4) C5 0.073(5) 0.071(4) 0.089(5) -0.012(4) 0.018(4) 0.002(4) C6 0.077(4) 0.061(4) 0.088(5) -0.011(4) 0.022(4) 0.002(4) C7 0.112(6) 0.081(5) 0.124(7) 0.029(5) 0.017(6) 0.013(5) C8 0.140(7) 0.094(6) 0.128(7) 0.020(6) 0.021(6) 0.009(6) C9 0.166(8) 0.117(7) 0.141(8) 0.030(7) 0.020(7) 0.016(7) C10 0.180(9) 0.138(8) 0.153(9) 0.029(8) 0.027(8) 0.015(8) C11 0.174(9) 0.143(8) 0.148(9) 0.025(8) 0.016(8) 0.009(8) C12 0.187(9) 0.134(8) 0.158(9) 0.021(8) 0.024(9) 0.023(8) C13 0.154(7) 0.117(6) 0.142(7) 0.019(6) 0.020(6) 0.020(6) C14 0.082(5) 0.087(5) 0.081(5) 0.010(5) -0.003(5) 0.006(5) C15 0.080(5) 0.069(5) 0.081(5) 0.010(4) -0.005(4) -0.001(4) C16 0.094(6) 0.081(5) 0.105(6) 0.018(5) -0.006(5) 0.002(5) C17 0.109(7) 0.087(6) 0.124(7) 0.009(6) -0.007(6) 0.014(6) C18 0.102(7) 0.102(7) 0.116(7) 0.004(6) -0.002(6) 0.018(6) C19 0.094(6) 0.098(6) 0.108(7) 0.015(6) -0.012(6) 0.007(6) C20 0.080(5) 0.078(5) 0.095(6) 0.003(5) 0.002(5) 0.001(5) C21 0.095(6) 0.098(6) 0.099(6) -0.004(5) 0.032(5) -0.004(5) C22 0.095(6) 0.105(6) 0.107(6) 0.004(5) 0.024(5) -0.003(5) C23 0.111(6) 0.127(6) 0.126(6) -0.005(6) 0.028(6) 0.000(6) C24 0.119(7) 0.141(8) 0.141(8) 0.002(7) 0.021(7) -0.019(7) C25 0.111(8) 0.143(8) 0.135(8) 0.007(7) 0.029(7) -0.007(7) C26 0.111(8) 0.142(8) 0.137(8) 0.011(7) 0.035(7) -0.002(7) C27 0.106(7) 0.124(7) 0.124(7) 0.003(6) 0.021(6) -0.008(6) C28 0.065(4) 0.061(4) 0.069(4) 0.010(4) 0.018(4) 0.001(4) C29 0.061(4) 0.059(4) 0.079(5) 0.004(4) 0.020(4) 0.006(4) C30 0.072(4) 0.061(4) 0.067(4) 0.012(4) 0.012(4) 0.014(4) C31 0.069(4) 0.057(4) 0.074(5) 0.003(4) 0.012(4) 0.000(4) C32 0.077(5) 0.044(4) 0.069(5) 0.011(4) 0.017(4) 0.007(4) C33 0.067(4) 0.053(4) 0.082(5) 0.008(4) 0.012(4) 0.008(4) C34 0.090(5) 0.084(5) 0.097(5) 0.011(5) 0.033(5) 0.003(4) C35 0.087(5) 0.082(5) 0.098(6) 0.022(5) 0.041(5) -0.012(4) C36 0.104(6) 0.082(5) 0.110(6) 0.015(5) 0.034(5) 0.002(5) C37 0.109(7) 0.091(6) 0.118(7) 0.025(6) 0.021(6) -0.006(6) C38 0.118(7) 0.108(7) 0.118(8) -0.009(7) 0.027(6) -0.018(6) C39 0.119(7) 0.086(6) 0.123(7) 0.012(6) 0.038(6) -0.004(6) C40 0.100(6) 0.085(5) 0.112(6) 0.023(5) 0.034(5) 0.000(5) C41 0.115(6) 0.106(6) 0.080(6) 0.029(5) -0.002(5) 0.013(6) C42 0.111(6) 0.101(6) 0.097(6) 0.015(5) -0.003(5) 0.023(5) C43 0.118(6) 0.131(6) 0.111(6) 0.019(6) -0.008(6) 0.015(6) C44 0.137(8) 0.158(8) 0.141(8) 0.017(8) 0.001(8) -0.009(8) C45 0.116(8) 0.145(8) 0.132(8) 0.019(7) -0.008(7) 0.015(7) C46 0.126(8) 0.140(7) 0.135(8) 0.019(7) -0.015(7) 0.022(7) C47 0.116(7) 0.139(7) 0.119(7) 0.012(6) -0.001(6) 0.021(7) C48 0.126(6) 0.081(5) 0.104(6) 0.022(5) 0.029(6) 0.001(5) C49 0.131(6) 0.098(6) 0.102(6) 0.021(5) 0.037(5) 0.021(5) C50 0.152(7) 0.117(6) 0.116(6) 0.017(6) 0.028(6) 0.010(6) C51 0.180(9) 0.144(8) 0.134(8) -0.001(8) 0.028(8) 0.015(8) C52 0.172(9) 0.152(9) 0.128(8) 0.009(8) 0.041(7) 0.017(8) C53 0.170(8) 0.147(8) 0.129(8) 0.025(7) 0.032(7) 0.010(7) C54 0.167(7) 0.134(7) 0.128(7) 0.025(6) 0.033(7) 0.003(6) C55 0.126(12) 0.194(14) 0.206(15) 0.019(13) -0.008(11) 0.002(11) C56 0.076(7) 0.114(7) 0.143(8) -0.006(7) 0.006(7) 0.003(6) C57 0.116(11) 0.193(14) 0.196(14) 0.002(12) 0.017(11) 0.030(11) C58 0.114(16) 0.117(15) 0.108(15) 0.025(13) 0.013(13) -0.015(13) C59 0.099(15) 0.132(16) 0.099(15) 0.009(13) 0.018(12) 0.001(13) _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 O1 2.412(6) . ? Eu1 O3 2.403(7) . ? Eu1 O5 2.398(7) . ? Eu1 O2 2.414(7) . ? Eu1 O6 2.412(6) . ? Eu1 O7 2.422(8) . ? Eu1 O4 2.429(6) . ? Eu1 N1 2.693(8) . ? Eu1 N5 2.722(7) . ? Cl1 C58 1.736(16) . ? Cl2 C58 1.721(16) . ? Cl3 C58 1.701(17) . ? Cl4 C59 1.700(16) . ? Cl5 C59 1.730(16) . ? Cl6 C59 1.708(16) . ? N1 C6 1.484(12) . ? N1 C4 1.478(12) . ? N1 C2 1.471(12) . ? N2 C1 1.308(12) . ? N2 C7 1.434(16) . ? N2 H2 0.9000 . ? N3 C3 1.328(12) . ? N3 C14 1.434(13) . ? N3 H3 0.9000 . ? N4 C5 1.312(13) . ? N4 C21 1.417(14) . ? N4 H4 0.9000 . ? N5 C33 1.433(11) . ? N5 C29 1.443(11) . ? N5 C31 1.504(12) . ? N6 C28 1.298(12) . ? N6 C34 1.455(14) . ? N6 H6 0.9000 . ? N7 C30 1.341(13) . ? N7 C41 1.454(12) . ? N7 H7 0.9000 . ? N8 C32 1.288(11) . ? N8 C48 1.519(15) . ? N8 H8 0.9000 . ? N9 O10 1.218(14) . ? N9 O8 1.179(13) . ? N9 O9 1.252(14) . ? N10 O11 1.198(11) . ? N10 O13 1.212(11) . ? N10 O12 1.260(12) . ? N11 O14 1.170(13) . ? N11 O15 1.116(13) . ? N11 O16 1.222(14) . ? O1 C1 1.242(11) . ? O2 C3 1.224(10) . ? O3 C5 1.250(12) . ? O4 C28 1.230(11) . ? O5 C30 1.244(11) . ? O6 C32 1.201(10) . ? O7 C56 1.213(12) . ? O17 H61 0.8699 . ? O17 H62 0.8700 . ? O18 H63 0.8702 . ? O18 H64 0.8703 . ? O19 H65 0.8700 . ? O19 H66 0.8700 . ? O20 H67 0.8700 . ? O20 H68 0.8699 . ? O21 H69 0.8702 . ? O21 H70 0.8698 . ? C1 C2 1.500(15) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.487(13) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.502(15) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.52(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.35(2) . ? C8 C9 1.45(2) . ? C9 C10 1.40(2) . ? C9 H9 0.9300 . ? C10 C11 1.47(3) . ? C10 H10 0.9300 . ? C11 C12 1.18(2) . ? C11 H11 0.9300 . ? C12 C13 1.53(3) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.609(17) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C20 1.366(16) . ? C15 C16 1.337(15) . ? C16 C17 1.375(19) . ? C16 H16 0.9300 . ? C17 C18 1.355(19) . ? C17 H17 0.9300 . ? C18 C19 1.403(18) . ? C18 H18 0.9300 . ? C19 C20 1.308(17) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.556(18) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.333(19) . ? C22 C27 1.408(19) . ? C23 C24 1.38(2) . ? C23 H23 0.9300 . ? C24 C25 1.35(2) . ? C24 H24 0.9300 . ? C25 C26 1.26(2) . ? C25 H25 0.9300 . ? C26 C27 1.37(2) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.520(13) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.455(13) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.548(13) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.507(17) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C40 1.381(16) . ? C35 C36 1.380(17) . ? C36 C37 1.316(18) . ? C36 H36 0.9300 . ? C37 C38 1.356(19) . ? C37 H37 0.9300 . ? C38 C39 1.292(19) . ? C38 H38 0.9300 . ? C39 C40 1.358(18) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C42 1.430(18) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.45(2) . ? C42 C47 1.382(19) . ? C43 C44 1.48(2) . ? C43 H43 0.9300 . ? C44 C45 1.25(2) . ? C44 H44 0.9300 . ? C45 C46 1.32(2) . ? C45 H45 0.9300 . ? C46 C47 1.22(2) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 C49 1.409(18) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.43(2) . ? C49 C54 1.44(2) . ? C50 C51 1.56(2) . ? C50 H50 0.9300 . ? C51 C52 1.40(2) . ? C51 H51 0.9300 . ? C52 C53 1.21(2) . ? C52 H52 0.9300 . ? C53 C54 1.35(2) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C56 1.492(15) . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 C57 1.468(14) . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58 0.9800 . ? C59 H59 0.9800 . ? 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 O1 Eu1 O3 93.4(2) . . ? O1 Eu1 O5 77.4(2) . . ? O3 Eu1 O5 148.2(2) . . ? O1 Eu1 O2 127.8(2) . . ? O3 Eu1 O2 73.8(2) . . ? O5 Eu1 O2 135.4(2) . . ? O1 Eu1 O6 148.4(2) . . ? O3 Eu1 O6 78.7(2) . . ? O5 Eu1 O6 93.3(2) . . ? O2 Eu1 O6 79.6(2) . . ? O1 Eu1 O7 73.3(2) . . ? O3 Eu1 O7 72.5(3) . . ? O5 Eu1 O7 75.8(3) . . ? O2 Eu1 O7 141.1(3) . . ? O6 Eu1 O7 75.2(2) . . ? O1 Eu1 O4 80.2(2) . . ? O3 Eu1 O4 135.3(2) . . ? O5 Eu1 O4 73.7(2) . . ? O2 Eu1 O4 75.8(2) . . ? O6 Eu1 O4 126.5(2) . . ? O7 Eu1 O4 143.1(3) . . ? O1 Eu1 N1 63.3(2) . . ? O3 Eu1 N1 66.0(2) . . ? O5 Eu1 N1 131.0(2) . . ? O2 Eu1 N1 65.3(2) . . ? O6 Eu1 N1 135.4(2) . . ? O7 Eu1 N1 116.0(3) . . ? O4 Eu1 N1 71.8(2) . . ? O1 Eu1 N5 134.2(2) . . ? O3 Eu1 N5 132.2(2) . . ? O5 Eu1 N5 65.3(2) . . ? O2 Eu1 N5 72.7(2) . . ? O6 Eu1 N5 62.5(2) . . ? O7 Eu1 N5 118.6(3) . . ? O4 Eu1 N5 65.1(2) . . ? N1 Eu1 N5 125.3(2) . . ? C6 N1 C4 110.6(8) . . ? C6 N1 C2 109.7(7) . . ? C4 N1 C2 111.3(7) . . ? C6 N1 Eu1 107.9(5) . . ? C4 N1 Eu1 108.9(5) . . ? C2 N1 Eu1 108.2(6) . . ? C1 N2 C7 122.0(10) . . ? C1 N2 H2 107.8 . . ? C7 N2 H2 108.1 . . ? C3 N3 C14 121.2(9) . . ? C3 N3 H3 107.0 . . ? C14 N3 H3 111.2 . . ? C5 N4 C21 124.9(10) . . ? C5 N4 H4 104.2 . . ? C21 N4 H4 106.7 . . ? C33 N5 C29 111.7(7) . . ? C33 N5 C31 109.4(7) . . ? C29 N5 C31 110.8(7) . . ? C33 N5 Eu1 108.0(5) . . ? C29 N5 Eu1 110.1(5) . . ? C31 N5 Eu1 106.6(5) . . ? C28 N6 C34 122.6(9) . . ? C28 N6 H6 106.6 . . ? C34 N6 H6 108.5 . . ? C30 N7 C41 124.7(9) . . ? C30 N7 H7 105.4 . . ? C41 N7 H7 108.6 . . ? C32 N8 C48 121.4(9) . . ? C32 N8 H8 108.1 . . ? C48 N8 H8 109.4 . . ? O10 N9 O8 121.2(14) . . ? O10 N9 O9 118.0(13) . . ? O8 N9 O9 120.8(12) . . ? O11 N10 O13 122.5(12) . . ? O11 N10 O12 120.0(10) . . ? O13 N10 O12 117.4(10) . . ? O14 N11 O15 126.8(15) . . ? O14 N11 O16 119.3(13) . . ? O15 N11 O16 113.7(14) . . ? C1 O1 Eu1 124.0(7) . . ? C3 O2 Eu1 124.6(6) . . ? C5 O3 Eu1 123.8(7) . . ? C28 O4 Eu1 125.6(6) . . ? C30 O5 Eu1 124.2(6) . . ? C32 O6 Eu1 126.0(6) . . ? C56 O7 Eu1 163.6(9) . . ? H61 O17 H62 104.7 . . ? H63 O18 H64 104.2 . . ? H65 O19 H66 104.8 . . ? H67 O20 H68 104.4 . . ? H69 O21 H70 106.7 . . ? O1 C1 N2 120.5(10) . . ? O1 C1 C2 121.5(9) . . ? N2 C1 C2 117.9(9) . . ? N1 C2 C1 107.7(8) . . ? N1 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? N1 C2 H2B 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? O2 C3 N3 121.3(9) . . ? O2 C3 C4 121.6(9) . . ? N3 C3 C4 117.0(8) . . ? N1 C4 C3 111.7(7) . . ? N1 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? N1 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? O3 C5 N4 121.2(10) . . ? O3 C5 C6 120.1(10) . . ? N4 C5 C6 118.5(9) . . ? N1 C6 C5 110.8(8) . . ? N1 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? N2 C7 C8 114.0(12) . . ? N2 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? N2 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C13 C8 C9 111.3(16) . . ? C13 C8 C7 121.9(14) . . ? C9 C8 C7 126.7(14) . . ? C10 C9 C8 129.6(17) . . ? C10 C9 H9 115.2 . . ? C8 C9 H9 115.2 . . ? C9 C10 C11 112.6(18) . . ? C9 C10 H10 123.7 . . ? C11 C10 H10 123.7 . . ? C12 C11 C10 117(2) . . ? C12 C11 H11 121.6 . . ? C10 C11 H11 121.6 . . ? C11 C12 C13 127(2) . . ? C11 C12 H12 116.3 . . ? C13 C12 H12 116.3 . . ? C8 C13 C12 117.6(16) . . ? C8 C13 H13 121.2 . . ? C12 C13 H13 121.2 . . ? N3 C14 C15 110.8(9) . . ? N3 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C20 C15 C16 120.3(12) . . ? C20 C15 C14 121.4(10) . . ? C16 C15 C14 118.3(11) . . ? C15 C16 C17 120.2(14) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 119.7(13) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C19 118.5(15) . . ? C17 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? C20 C19 C18 120.7(15) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C15 120.6(12) . . ? C19 C20 H20 119.7 . . ? C15 C20 H20 119.7 . . ? N4 C21 C22 112.4(11) . . ? N4 C21 H21A 109.1 . . ? C22 C21 H21A 109.1 . . ? N4 C21 H21B 109.1 . . ? C22 C21 H21B 109.1 . . ? H21A C21 H21B 107.9 . . ? C23 C22 C27 118.2(14) . . ? C23 C22 C21 122.2(13) . . ? C27 C22 C21 119.6(12) . . ? C22 C23 C24 121.2(16) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C25 C24 C23 118.7(16) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C26 C25 C24 121.1(18) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C26 C27 123.6(18) . . ? C25 C26 H26 118.2 . . ? C27 C26 H26 118.2 . . ? C22 C27 C26 117.2(15) . . ? C22 C27 H27 121.4 . . ? C26 C27 H27 121.4 . . ? O4 C28 N6 122.5(9) . . ? O4 C28 C29 120.9(8) . . ? N6 C28 C29 116.6(9) . . ? N5 C29 C28 114.1(7) . . ? N5 C29 H29A 108.7 . . ? C28 C29 H29A 108.7 . . ? N5 C29 H29B 108.7 . . ? C28 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? O5 C30 N7 118.7(9) . . ? O5 C30 C31 122.6(9) . . ? N7 C30 C31 118.4(9) . . ? N5 C31 C30 111.5(7) . . ? N5 C31 H31A 109.3 . . ? C30 C31 H31A 109.3 . . ? N5 C31 H31B 109.3 . . ? C30 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? O6 C32 N8 124.5(9) . . ? O6 C32 C33 119.3(8) . . ? N8 C32 C33 116.1(8) . . ? N5 C33 C32 109.7(7) . . ? N5 C33 H33A 109.7 . . ? C32 C33 H33A 109.7 . . ? N5 C33 H33B 109.7 . . ? C32 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? N6 C34 C35 112.6(10) . . ? N6 C34 H34A 109.1 . . ? C35 C34 H34A 109.1 . . ? N6 C34 H34B 109.1 . . ? C35 C34 H34B 109.1 . . ? H34A C34 H34B 107.8 . . ? C40 C35 C36 115.9(12) . . ? C40 C35 C34 120.0(12) . . ? C36 C35 C34 124.1(11) . . ? C37 C36 C35 122.4(13) . . ? C37 C36 H36 118.8 . . ? C35 C36 H36 118.8 . . ? C36 C37 C38 119.1(15) . . ? C36 C37 H37 120.4 . . ? C38 C37 H37 120.4 . . ? C39 C38 C37 121.5(15) . . ? C39 C38 H38 119.3 . . ? C37 C38 H38 119.3 . . ? C38 C39 C40 120.5(14) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C35 C40 C39 120.4(14) . . ? C35 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C42 C41 N7 119.6(11) . . ? C42 C41 H41A 107.4 . . ? N7 C41 H41A 107.4 . . ? C42 C41 H41B 107.4 . . ? N7 C41 H41B 107.4 . . ? H41A C41 H41B 107.0 . . ? C41 C42 C43 127.5(12) . . ? C41 C42 C47 124.9(14) . . ? C43 C42 C47 107.4(15) . . ? C44 C43 C42 119.7(15) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C45 C44 C43 115.9(19) . . ? C45 C44 H44 122.0 . . ? C43 C44 H44 122.0 . . ? C44 C45 C46 126(2) . . ? C44 C45 H45 117.1 . . ? C46 C45 H45 117.1 . . ? C47 C46 C45 116.8(19) . . ? C47 C46 H46 121.6 . . ? C45 C46 H46 121.6 . . ? C46 C47 C42 133(2) . . ? C46 C47 H47 113.6 . . ? C42 C47 H47 113.6 . . ? C49 C48 N8 113.6(12) . . ? C49 C48 H48A 108.8 . . ? N8 C48 H48A 108.8 . . ? C49 C48 H48B 108.8 . . ? N8 C48 H48B 108.8 . . ? H48A C48 H48B 107.7 . . ? C50 C49 C54 118.7(14) . . ? C50 C49 C48 122.6(13) . . ? C54 C49 C48 118.3(14) . . ? C49 C50 C51 115.6(14) . . ? C49 C50 H50 122.2 . . ? C51 C50 H50 122.2 . . ? C52 C51 C50 109.3(17) . . ? C52 C51 H51 125.4 . . ? C50 C51 H51 125.4 . . ? C53 C52 C51 136(2) . . ? C53 C52 H52 111.8 . . ? C51 C52 H52 111.8 . . ? C52 C53 C54 115(2) . . ? C52 C53 H53 122.6 . . ? C54 C53 H53 122.6 . . ? C53 C54 C49 122.1(18) . . ? C53 C54 H54 119.0 . . ? C49 C54 H54 119.0 . . ? C56 C55 H55A 109.5 . . ? C56 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C56 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O7 C56 C55 116.1(13) . . ? O7 C56 C57 127.6(13) . . ? C55 C56 C57 114.3(13) . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? Cl3 C58 Cl1 108.7(10) . . ? Cl3 C58 Cl2 111.9(12) . . ? Cl1 C58 Cl2 108.4(10) . . ? Cl3 C58 H58 109.3 . . ? Cl1 C58 H58 109.3 . . ? Cl2 C58 H58 109.3 . . ? Cl6 C59 Cl4 110.9(11) . . ? Cl6 C59 Cl5 109.2(10) . . ? Cl4 C59 Cl5 111.8(11) . . ? Cl6 C59 H59 108.3 . . ? Cl4 C59 H59 108.3 . . ? Cl5 C59 H59 108.3 . . ? _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.904 _refine_diff_density_max 0.745 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.087 # Attachment '- 826839.cif' data_p21c _database_code_depnum_ccdc_archive 'CCDC 826839' #TrackingRef '- 826839.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H36 Eu N7 O12' _chemical_formula_weight 946.71 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.068(13) _cell_length_b 16.726(10) _cell_length_c 14.226(9) _cell_angle_alpha 90.00 _cell_angle_beta 104.205(7) _cell_angle_gamma 90.00 _cell_volume 4629(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6457 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 26.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 1.417 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7457 _exptl_absorpt_correction_T_max 0.7648 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21993 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8523 _reflns_number_gt 6212 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+0.1641P] 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 8523 _refine_ls_number_parameters 532 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0952 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 502 70 ' ' 2 1.000 0.500 0.500 502 70 ' ' _platon_squeeze_details ; ; 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 0.510617(11) 0.841854(10) 0.264247(14) 0.03465(8) Uani 1 1 d . . . C1 C 0.1641(3) 0.6774(3) -0.0403(4) 0.0703(15) Uani 1 1 d . . . H1 H 0.1903 0.7146 -0.0642 0.084 Uiso 1 1 calc R . . C2 C 0.0948(3) 0.6799(4) -0.0711(5) 0.103(2) Uani 1 1 d . . . H2 H 0.0739 0.7186 -0.1155 0.124 Uiso 1 1 calc R . . C3 C 0.0544(3) 0.6247(5) -0.0365(6) 0.118(3) Uani 1 1 d . . . H3 H 0.0068 0.6264 -0.0587 0.141 Uiso 1 1 calc R . . C4 C 0.0843(3) 0.5687(4) 0.0292(5) 0.094(2) Uani 1 1 d . . . H4 H 0.0569 0.5329 0.0527 0.112 Uiso 1 1 calc R . . C5 C 0.1554(3) 0.5643(3) 0.0617(4) 0.0620(13) Uani 1 1 d . . . C6 C 0.1868(3) 0.5054(3) 0.1291(4) 0.0688(15) Uani 1 1 d . . . H6 H 0.1598 0.4687 0.1520 0.083 Uiso 1 1 calc R . . C7 C 0.2561(3) 0.5022(3) 0.1605(4) 0.0603(13) Uani 1 1 d . . . H7 H 0.2763 0.4628 0.2045 0.072 Uiso 1 1 calc R . . C8 C 0.2977(3) 0.5570(2) 0.1277(3) 0.0484(11) Uani 1 1 d . . . H8 H 0.3452 0.5539 0.1504 0.058 Uiso 1 1 calc R . . C9 C 0.2695(2) 0.6155(2) 0.0625(3) 0.0423(10) Uani 1 1 d . . . C10 C 0.1975(2) 0.6198(3) 0.0272(3) 0.0494(11) Uani 1 1 d . . . C11 C 0.3148(2) 0.6750(2) 0.0260(3) 0.0448(11) Uani 1 1 d . . . H11A H 0.3007 0.6768 -0.0443 0.054 Uiso 1 1 calc R . . H11B H 0.3078 0.7278 0.0500 0.054 Uiso 1 1 calc R . . C12 C 0.4344(2) 0.6978(2) 0.1152(3) 0.0347(9) Uani 1 1 d . . . C13 C 0.5063(2) 0.6689(2) 0.1306(3) 0.0380(10) Uani 1 1 d . . . H13A H 0.5064 0.6113 0.1231 0.046 Uiso 1 1 calc R . . H13B H 0.5271 0.6923 0.0823 0.046 Uiso 1 1 calc R . . C14 C 0.2953(3) 0.7401(3) 0.2796(4) 0.0615(13) Uani 1 1 d . . . H14 H 0.3423 0.7502 0.2948 0.074 Uiso 1 1 calc R . . C15 C 0.2519(3) 0.7857(4) 0.2126(4) 0.0833(18) Uani 1 1 d . . . H15 H 0.2694 0.8276 0.1829 0.100 Uiso 1 1 calc R . . C16 C 0.1809(4) 0.7704(5) 0.1875(5) 0.107(2) Uani 1 1 d . . . H16 H 0.1516 0.8019 0.1413 0.129 Uiso 1 1 calc R . . C17 C 0.1550(4) 0.7092(5) 0.2311(6) 0.103(2) Uani 1 1 d . . . H17 H 0.1081 0.6987 0.2132 0.123 Uiso 1 1 calc R . . C18 C 0.1973(3) 0.6627(4) 0.3014(5) 0.0777(18) Uani 1 1 d . . . C19 C 0.1698(4) 0.6033(4) 0.3471(6) 0.098(2) Uani 1 1 d . . . H19 H 0.1227 0.5938 0.3290 0.118 Uiso 1 1 calc R . . C20 C 0.2103(4) 0.5581(4) 0.4184(7) 0.110(3) Uani 1 1 d . . . H20 H 0.1910 0.5186 0.4494 0.132 Uiso 1 1 calc R . . C21 C 0.2819(3) 0.5719(3) 0.4448(5) 0.0779(16) Uani 1 1 d . . . H21 H 0.3096 0.5415 0.4939 0.093 Uiso 1 1 calc R . . C22 C 0.3119(3) 0.6306(3) 0.3984(4) 0.0570(13) Uani 1 1 d . . . C23 C 0.2693(3) 0.6780(3) 0.3255(4) 0.0596(13) Uani 1 1 d . . . C24 C 0.3880(2) 0.6456(2) 0.4355(3) 0.0456(11) Uani 1 1 d . . . H24A H 0.3947 0.7022 0.4493 0.055 Uiso 1 1 calc R . . H24B H 0.4038 0.6172 0.4964 0.055 Uiso 1 1 calc R . . C25 C 0.4760(2) 0.6709(2) 0.3458(3) 0.0342(9) Uani 1 1 d . . . C26 C 0.5304(2) 0.6361(2) 0.3021(3) 0.0396(10) Uani 1 1 d . . . H26A H 0.5718 0.6267 0.3528 0.048 Uiso 1 1 calc R . . H26B H 0.5147 0.5852 0.2722 0.048 Uiso 1 1 calc R . . C27 C 0.8776(3) 0.8436(4) 0.5769(4) 0.0854(17) Uani 1 1 d U . . H27 H 0.8651 0.8685 0.5167 0.102 Uiso 1 1 calc R . . C28 C 0.9319(3) 0.8736(5) 0.6466(5) 0.115(2) Uani 1 1 d U . . H28 H 0.9555 0.9185 0.6337 0.138 Uiso 1 1 calc R . . C29 C 0.9512(4) 0.8364(6) 0.7361(6) 0.118(2) Uani 1 1 d U . . H29 H 0.9881 0.8563 0.7832 0.142 Uiso 1 1 calc R . . C30 C 0.9170(4) 0.7719(5) 0.7554(5) 0.112(2) Uani 1 1 d U . . H30 H 0.9312 0.7476 0.8158 0.134 Uiso 1 1 calc R . . C31 C 0.8601(4) 0.7398(4) 0.6869(4) 0.0865(17) Uani 1 1 d U . . C32 C 0.8227(5) 0.6735(4) 0.7056(5) 0.112(2) Uani 1 1 d U . . H32 H 0.8357 0.6479 0.7653 0.134 Uiso 1 1 calc R . . C33 C 0.7696(5) 0.6472(4) 0.6401(5) 0.122(2) Uani 1 1 d U . . H33 H 0.7447 0.6044 0.6555 0.146 Uiso 1 1 calc R . . C34 C 0.7486(4) 0.6815(4) 0.5468(5) 0.0941(18) Uani 1 1 d U . . H34 H 0.7110 0.6611 0.5013 0.113 Uiso 1 1 calc R . . C35 C 0.7841(3) 0.7445(3) 0.5248(4) 0.0631(13) Uani 1 1 d U . . C36 C 0.8408(3) 0.7764(3) 0.5944(4) 0.0632(13) Uani 1 1 d U . . C37 C 0.7657(3) 0.7799(3) 0.4243(4) 0.0703(15) Uani 1 1 d . . . H37A H 0.7431 0.8309 0.4264 0.084 Uiso 1 1 calc R . . H37B H 0.8076 0.7899 0.4038 0.084 Uiso 1 1 calc R . . C38 C 0.6576(2) 0.7461(2) 0.3091(3) 0.0468(11) Uani 1 1 d . . . C39 C 0.6203(2) 0.6892(2) 0.2324(3) 0.0448(11) Uani 1 1 d . . . H39A H 0.6278 0.7044 0.1700 0.054 Uiso 1 1 calc R . . H39B H 0.6380 0.6355 0.2473 0.054 Uiso 1 1 calc R . . N1 N 0.54646(17) 0.69073(18) 0.2279(2) 0.0345(8) Uani 1 1 d . . . N2 N 0.38635(18) 0.65564(18) 0.0552(2) 0.0411(8) Uani 1 1 d . . . H2A H 0.3993 0.6126 0.0317 0.049 Uiso 1 1 calc R . . N3 N 0.43162(17) 0.62206(18) 0.3710(2) 0.0383(8) Uani 1 1 d . . . H3A H 0.4281 0.5741 0.3485 0.046 Uiso 1 1 calc R . . N4 N 0.7213(2) 0.7292(2) 0.3536(3) 0.0617(11) Uani 1 1 d . . . H4A H 0.7380 0.6846 0.3396 0.074 Uiso 1 1 calc R . . N5 N 0.3903(2) 0.9424(2) 0.2211(4) 0.0653(12) Uani 1 1 d . . . N6 N 0.55608(19) 0.94903(19) 0.4345(2) 0.0431(9) Uani 1 1 d . . . N7 N 0.56873(19) 0.9041(2) 0.1034(3) 0.0449(9) Uani 1 1 d . . . O1 O 0.42178(14) 0.76059(14) 0.15510(18) 0.0390(7) Uani 1 1 d . . . O2 O 0.47612(15) 0.74425(14) 0.36257(19) 0.0430(7) Uani 1 1 d . . . O3 O 0.62891(16) 0.80831(18) 0.3260(2) 0.0547(8) Uani 1 1 d . . . O4 O 0.40268(18) 0.89610(19) 0.2945(3) 0.0619(9) Uani 1 1 d . . . O5 O 0.3404(2) 0.9872(2) 0.2043(4) 0.1049(15) Uani 1 1 d . . . O6 O 0.43108(18) 0.94030(17) 0.1675(2) 0.0549(8) Uani 1 1 d . . . O7 O 0.54360(15) 0.97524(15) 0.34902(18) 0.0446(7) Uani 1 1 d . . . O8 O 0.57783(18) 0.99157(17) 0.5050(2) 0.0597(9) Uani 1 1 d . . . O9 O 0.5463(2) 0.87601(17) 0.4431(2) 0.0684(11) Uani 1 1 d . . . O10 O 0.54237(17) 0.83610(15) 0.1042(2) 0.0498(8) Uani 1 1 d . . . O11 O 0.5854(2) 0.9299(2) 0.0325(2) 0.0766(11) Uani 1 1 d . . . O12 O 0.57580(16) 0.94533(16) 0.1795(2) 0.0493(8) 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 0.05288(15) 0.01925(11) 0.03512(12) -0.00264(8) 0.01709(9) -0.00203(9) C1 0.060(4) 0.071(4) 0.075(4) 0.020(3) 0.007(3) 0.002(3) C2 0.063(4) 0.113(5) 0.124(6) 0.042(5) 0.005(4) 0.016(4) C3 0.053(4) 0.134(6) 0.160(7) 0.032(6) 0.013(5) -0.005(4) C4 0.064(4) 0.091(5) 0.126(6) 0.020(4) 0.024(4) -0.013(4) C5 0.056(3) 0.059(3) 0.075(3) -0.002(3) 0.023(3) -0.012(3) C6 0.081(4) 0.051(3) 0.084(4) 0.006(3) 0.037(3) -0.014(3) C7 0.080(4) 0.042(3) 0.065(3) 0.011(2) 0.028(3) 0.000(3) C8 0.061(3) 0.041(2) 0.044(2) 0.001(2) 0.014(2) 0.000(2) C9 0.055(3) 0.031(2) 0.042(2) -0.0034(18) 0.015(2) -0.005(2) C10 0.054(3) 0.042(2) 0.055(3) 0.001(2) 0.019(2) -0.001(2) C11 0.049(3) 0.036(2) 0.048(2) 0.0036(18) 0.009(2) -0.0051(19) C12 0.055(3) 0.0182(18) 0.035(2) -0.0011(16) 0.018(2) -0.0047(18) C13 0.057(3) 0.0192(19) 0.042(2) -0.0064(16) 0.021(2) -0.0040(18) C14 0.076(4) 0.050(3) 0.059(3) -0.014(2) 0.020(3) 0.002(3) C15 0.084(5) 0.087(4) 0.074(4) -0.014(3) 0.010(4) 0.017(4) C16 0.093(6) 0.117(6) 0.096(5) -0.029(5) -0.007(4) 0.037(5) C17 0.077(5) 0.107(6) 0.125(6) -0.048(5) 0.026(5) -0.002(5) C18 0.055(4) 0.069(4) 0.106(5) -0.036(4) 0.014(4) 0.002(3) C19 0.069(4) 0.078(5) 0.154(7) -0.026(5) 0.038(5) -0.016(4) C20 0.089(5) 0.074(5) 0.189(9) -0.017(5) 0.077(6) -0.028(4) C21 0.088(5) 0.054(3) 0.102(4) -0.007(3) 0.041(4) -0.013(3) C22 0.068(4) 0.043(3) 0.066(3) -0.019(2) 0.027(3) -0.004(2) C23 0.061(3) 0.050(3) 0.072(3) -0.027(3) 0.025(3) -0.004(2) C24 0.060(3) 0.037(2) 0.044(2) -0.0051(19) 0.021(2) -0.004(2) C25 0.048(3) 0.024(2) 0.0295(19) 0.0015(15) 0.0068(19) -0.0010(17) C26 0.047(3) 0.030(2) 0.044(2) 0.0007(18) 0.014(2) 0.0058(19) C27 0.065(3) 0.117(4) 0.070(3) 0.002(3) 0.008(3) -0.016(3) C28 0.076(4) 0.173(5) 0.089(4) -0.006(4) 0.007(4) -0.039(4) C29 0.078(4) 0.178(7) 0.086(4) -0.010(5) -0.005(4) 0.005(4) C30 0.113(5) 0.144(6) 0.067(4) 0.000(4) -0.001(4) 0.042(4) C31 0.115(4) 0.087(4) 0.057(3) 0.003(3) 0.020(3) 0.029(3) C32 0.192(6) 0.078(4) 0.068(4) 0.020(3) 0.036(4) -0.001(4) C33 0.206(7) 0.079(4) 0.088(4) 0.009(3) 0.051(5) -0.035(4) C34 0.142(5) 0.067(3) 0.081(4) 0.003(3) 0.041(4) -0.024(3) C35 0.074(3) 0.051(3) 0.068(3) 0.007(2) 0.026(3) 0.004(2) C36 0.060(3) 0.071(3) 0.060(3) 0.009(2) 0.020(2) 0.014(3) C37 0.057(3) 0.067(3) 0.076(4) 0.014(3) -0.006(3) -0.018(3) C38 0.055(3) 0.036(2) 0.048(3) 0.0056(19) 0.010(2) -0.002(2) C39 0.050(3) 0.034(2) 0.054(3) -0.001(2) 0.019(2) 0.001(2) N1 0.046(2) 0.0254(15) 0.0341(17) 0.0003(13) 0.0144(16) 0.0000(15) N2 0.055(2) 0.0263(17) 0.0421(19) -0.0058(14) 0.0113(17) -0.0017(16) N3 0.052(2) 0.0227(16) 0.0422(19) -0.0033(14) 0.0161(17) -0.0048(16) N4 0.054(3) 0.050(2) 0.075(3) -0.001(2) 0.005(2) 0.001(2) N5 0.070(3) 0.030(2) 0.094(4) -0.013(2) 0.017(3) 0.002(2) N6 0.066(3) 0.0310(18) 0.0361(19) -0.0066(15) 0.0203(18) -0.0084(17) N7 0.055(2) 0.039(2) 0.044(2) 0.0027(17) 0.0197(19) -0.0040(17) O1 0.0498(18) 0.0274(14) 0.0426(15) -0.0052(12) 0.0167(14) 0.0008(12) O2 0.070(2) 0.0207(14) 0.0463(16) -0.0036(12) 0.0289(15) -0.0041(13) O3 0.059(2) 0.0373(17) 0.063(2) -0.0099(15) 0.0053(17) -0.0005(15) O4 0.070(2) 0.0460(19) 0.082(2) -0.0129(18) 0.041(2) -0.0026(17) O5 0.077(3) 0.073(3) 0.169(4) 0.002(3) 0.038(3) 0.032(2) O6 0.062(2) 0.0381(17) 0.066(2) 0.0007(15) 0.0174(18) -0.0001(16) O7 0.073(2) 0.0279(14) 0.0330(15) 0.0020(12) 0.0141(15) -0.0061(14) O8 0.099(3) 0.0400(17) 0.0399(16) -0.0112(14) 0.0158(17) -0.0145(17) O9 0.145(3) 0.0245(15) 0.0424(17) -0.0030(13) 0.036(2) -0.0206(19) O10 0.075(2) 0.0302(16) 0.0503(17) -0.0059(12) 0.0265(16) -0.0118(14) O11 0.118(3) 0.071(2) 0.054(2) 0.0018(18) 0.045(2) -0.034(2) O12 0.075(2) 0.0319(15) 0.0443(17) -0.0065(13) 0.0205(16) -0.0086(15) _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 O2 2.361(3) . ? Eu1 O3 2.387(3) . ? Eu1 O6 2.465(3) . ? Eu1 O1 2.465(3) . ? Eu1 O4 2.482(4) . ? Eu1 O10 2.512(3) . ? Eu1 O9 2.533(3) . ? Eu1 O7 2.545(3) . ? Eu1 O12 2.633(3) . ? Eu1 N1 2.712(3) . ? C1 C2 1.353(8) . ? C1 C10 1.408(6) . ? C1 H1 0.9300 . ? C2 C3 1.394(9) . ? C2 H2 0.9300 . ? C3 C4 1.354(9) . ? C3 H3 0.9300 . ? C4 C5 1.390(8) . ? C4 H4 0.9300 . ? C5 C6 1.410(7) . ? C5 C10 1.422(6) . ? C6 C7 1.353(7) . ? C6 H6 0.9300 . ? C7 C8 1.395(6) . ? C7 H7 0.9300 . ? C8 C9 1.370(6) . ? C8 H8 0.9300 . ? C9 C10 1.410(6) . ? C9 C11 1.523(6) . ? C11 N2 1.431(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O1 1.249(4) . ? C12 N2 1.323(5) . ? C12 C13 1.486(6) . ? C13 N1 1.467(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.357(7) . ? C14 C23 1.394(7) . ? C14 H14 0.9300 . ? C15 C16 1.406(9) . ? C15 H15 0.9300 . ? C16 C17 1.363(10) . ? C16 H16 0.9300 . ? C17 C18 1.383(9) . ? C17 H17 0.9300 . ? C18 C19 1.373(9) . ? C18 C23 1.424(8) . ? C19 C20 1.363(10) . ? C19 H19 0.9300 . ? C20 C21 1.413(9) . ? C20 H20 0.9300 . ? C21 C22 1.398(7) . ? C21 H21 0.9300 . ? C22 C23 1.414(7) . ? C22 C24 1.509(7) . ? C24 N3 1.469(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O2 1.250(4) . ? C25 N3 1.322(5) . ? C25 C26 1.499(6) . ? C26 N1 1.489(5) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.375(8) . ? C27 C36 1.400(7) . ? C27 H27 0.9300 . ? C28 C29 1.384(10) . ? C28 H28 0.9300 . ? C29 C30 1.343(10) . ? C29 H29 0.9300 . ? C30 C31 1.413(10) . ? C30 H30 0.9300 . ? C31 C32 1.401(9) . ? C31 C36 1.417(7) . ? C32 C33 1.307(11) . ? C32 H32 0.9300 . ? C33 C34 1.412(9) . ? C33 H33 0.9300 . ? C34 C35 1.351(7) . ? C34 H34 0.9300 . ? C35 C36 1.416(7) . ? C35 C37 1.507(7) . ? C37 N4 1.444(6) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 O3 1.241(5) . ? C38 N4 1.311(6) . ? C38 C39 1.502(6) . ? C39 N1 1.468(5) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? N2 H2A 0.8600 . ? N3 H3A 0.8600 . ? N4 H4A 0.8600 . ? N5 O5 1.226(5) . ? N5 O6 1.249(5) . ? N5 O4 1.276(5) . ? N6 O8 1.220(4) . ? N6 O9 1.248(4) . ? N6 O7 1.258(4) . ? N7 O11 1.217(4) . ? N7 O10 1.255(4) . ? N7 O12 1.262(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Eu1 O3 91.67(11) . . ? O2 Eu1 O6 123.28(12) . . ? O3 Eu1 O6 144.27(11) . . ? O2 Eu1 O1 73.75(10) . . ? O3 Eu1 O1 127.03(10) . . ? O6 Eu1 O1 75.38(10) . . ? O2 Eu1 O4 75.79(11) . . ? O3 Eu1 O4 148.60(12) . . ? O6 Eu1 O4 51.64(12) . . ? O1 Eu1 O4 77.52(11) . . ? O2 Eu1 O10 133.38(9) . . ? O3 Eu1 O10 82.76(11) . . ? O6 Eu1 O10 78.06(12) . . ? O1 Eu1 O10 73.33(10) . . ? O4 Eu1 O10 126.71(11) . . ? O2 Eu1 O9 67.21(10) . . ? O3 Eu1 O9 70.91(12) . . ? O6 Eu1 O9 113.25(11) . . ? O1 Eu1 O9 137.68(10) . . ? O4 Eu1 O9 77.69(13) . . ? O10 Eu1 O9 147.86(12) . . ? O2 Eu1 O7 113.91(9) . . ? O3 Eu1 O7 84.96(10) . . ? O6 Eu1 O7 74.71(10) . . ? O1 Eu1 O7 147.72(9) . . ? O4 Eu1 O7 74.56(10) . . ? O10 Eu1 O7 111.64(9) . . ? O9 Eu1 O7 49.45(8) . . ? O2 Eu1 O12 167.52(10) . . ? O3 Eu1 O12 76.24(11) . . ? O6 Eu1 O12 68.39(12) . . ? O1 Eu1 O12 115.96(9) . . ? O4 Eu1 O12 113.08(11) . . ? O10 Eu1 O12 49.10(9) . . ? O9 Eu1 O12 105.18(10) . . ? O7 Eu1 O12 62.62(9) . . ? O2 Eu1 N1 66.33(10) . . ? O3 Eu1 N1 64.20(10) . . ? O6 Eu1 N1 133.00(10) . . ? O1 Eu1 N1 63.31(9) . . ? O4 Eu1 N1 131.10(10) . . ? O10 Eu1 N1 69.73(9) . . ? O9 Eu1 N1 112.25(10) . . ? O7 Eu1 N1 148.97(10) . . ? O12 Eu1 N1 109.91(10) . . ? C2 C1 C10 121.4(5) . . ? C2 C1 H1 119.3 . . ? C10 C1 H1 119.3 . . ? C1 C2 C3 120.4(6) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 120.3(6) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.7(6) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 121.0(5) . . ? C4 C5 C10 119.9(5) . . ? C6 C5 C10 119.1(5) . . ? C7 C6 C5 120.3(5) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 120.8(5) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C9 C8 C7 121.0(5) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 119.7(4) . . ? C8 C9 C11 121.1(4) . . ? C10 C9 C11 119.3(4) . . ? C1 C10 C9 123.6(4) . . ? C1 C10 C5 117.3(5) . . ? C9 C10 C5 119.1(4) . . ? N2 C11 C9 113.1(3) . . ? N2 C11 H11A 109.0 . . ? C9 C11 H11A 109.0 . . ? N2 C11 H11B 109.0 . . ? C9 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? O1 C12 N2 123.0(4) . . ? O1 C12 C13 120.3(3) . . ? N2 C12 C13 116.7(3) . . ? N1 C13 C12 110.3(3) . . ? N1 C13 H13A 109.6 . . ? C12 C13 H13A 109.6 . . ? N1 C13 H13B 109.6 . . ? C12 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C15 C14 C23 119.9(6) . . ? C15 C14 H14 120.0 . . ? C23 C14 H14 120.0 . . ? C14 C15 C16 120.7(7) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C17 C16 C15 119.9(7) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 121.1(7) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C19 C18 C17 120.2(7) . . ? C19 C18 C23 121.2(7) . . ? C17 C18 C23 118.6(7) . . ? C20 C19 C18 121.2(7) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 119.2(7) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C22 C21 C20 121.1(6) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 119.2(5) . . ? C21 C22 C24 117.8(5) . . ? C23 C22 C24 122.7(4) . . ? C14 C23 C22 122.2(5) . . ? C14 C23 C18 119.8(6) . . ? C22 C23 C18 118.0(5) . . ? N3 C24 C22 116.4(4) . . ? N3 C24 H24A 108.2 . . ? C22 C24 H24A 108.2 . . ? N3 C24 H24B 108.2 . . ? C22 C24 H24B 108.2 . . ? H24A C24 H24B 107.3 . . ? O2 C25 N3 121.6(4) . . ? O2 C25 C26 119.6(4) . . ? N3 C25 C26 118.7(3) . . ? N1 C26 C25 111.2(3) . . ? N1 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? N1 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C28 C27 C36 121.6(6) . . ? C28 C27 H27 119.2 . . ? C36 C27 H27 119.2 . . ? C27 C28 C29 119.5(8) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C30 C29 C28 120.5(7) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 122.1(7) . . ? C29 C30 H30 119.0 . . ? C31 C30 H30 119.0 . . ? C32 C31 C30 123.4(7) . . ? C32 C31 C36 118.8(6) . . ? C30 C31 C36 117.8(7) . . ? C33 C32 C31 120.8(7) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 122.4(7) . . ? C32 C33 H33 118.8 . . ? C34 C33 H33 118.8 . . ? C35 C34 C33 118.8(7) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? C34 C35 C36 120.7(5) . . ? C34 C35 C37 120.3(5) . . ? C36 C35 C37 118.9(5) . . ? C27 C36 C35 123.1(5) . . ? C27 C36 C31 118.5(6) . . ? C35 C36 C31 118.4(6) . . ? N4 C37 C35 113.4(4) . . ? N4 C37 H37A 108.9 . . ? C35 C37 H37A 108.9 . . ? N4 C37 H37B 108.9 . . ? C35 C37 H37B 108.9 . . ? H37A C37 H37B 107.7 . . ? O3 C38 N4 122.1(4) . . ? O3 C38 C39 120.0(4) . . ? N4 C38 C39 117.9(4) . . ? N1 C39 C38 109.8(3) . . ? N1 C39 H39A 109.7 . . ? C38 C39 H39A 109.7 . . ? N1 C39 H39B 109.7 . . ? C38 C39 H39B 109.7 . . ? H39A C39 H39B 108.2 . . ? C13 N1 C39 110.6(3) . . ? C13 N1 C26 110.6(3) . . ? C39 N1 C26 110.5(3) . . ? C13 N1 Eu1 107.6(2) . . ? C39 N1 Eu1 108.7(2) . . ? C26 N1 Eu1 108.8(2) . . ? C12 N2 C11 126.0(3) . . ? C12 N2 H2A 117.0 . . ? C11 N2 H2A 117.0 . . ? C25 N3 C24 123.3(3) . . ? C25 N3 H3A 118.4 . . ? C24 N3 H3A 118.4 . . ? C38 N4 C37 124.9(4) . . ? C38 N4 H4A 117.6 . . ? C37 N4 H4A 117.6 . . ? O5 N5 O6 121.7(5) . . ? O5 N5 O4 121.1(5) . . ? O6 N5 O4 117.2(4) . . ? O8 N6 O9 121.5(3) . . ? O8 N6 O7 122.5(3) . . ? O9 N6 O7 115.9(3) . . ? O11 N7 O10 122.1(4) . . ? O11 N7 O12 121.4(4) . . ? O10 N7 O12 116.5(3) . . ? C12 O1 Eu1 123.7(3) . . ? C25 O2 Eu1 123.5(3) . . ? C38 O3 Eu1 126.3(3) . . ? N5 O4 Eu1 94.8(3) . . ? N5 O6 Eu1 96.3(3) . . ? N6 O7 Eu1 96.9(2) . . ? N6 O9 Eu1 97.7(2) . . ? N7 O10 Eu1 100.0(2) . . ? N7 O12 Eu1 94.0(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 C1 C2 C3 -0.2(11) . . . . ? C1 C2 C3 C4 0.8(13) . . . . ? C2 C3 C4 C5 -1.3(13) . . . . ? C3 C4 C5 C6 -179.1(7) . . . . ? C3 C4 C5 C10 1.0(10) . . . . ? C4 C5 C6 C7 -179.6(6) . . . . ? C10 C5 C6 C7 0.3(8) . . . . ? C5 C6 C7 C8 0.5(8) . . . . ? C6 C7 C8 C9 -0.3(7) . . . . ? C7 C8 C9 C10 -0.7(6) . . . . ? C7 C8 C9 C11 -179.5(4) . . . . ? C2 C1 C10 C9 -179.0(6) . . . . ? C2 C1 C10 C5 -0.1(9) . . . . ? C8 C9 C10 C1 -179.6(5) . . . . ? C11 C9 C10 C1 -0.8(7) . . . . ? C8 C9 C10 C5 1.4(6) . . . . ? C11 C9 C10 C5 -179.8(4) . . . . ? C4 C5 C10 C1 -0.3(8) . . . . ? C6 C5 C10 C1 179.8(5) . . . . ? C4 C5 C10 C9 178.7(5) . . . . ? C6 C5 C10 C9 -1.2(7) . . . . ? C8 C9 C11 N2 8.5(6) . . . . ? C10 C9 C11 N2 -170.3(4) . . . . ? O1 C12 C13 N1 31.9(5) . . . . ? N2 C12 C13 N1 -150.5(3) . . . . ? C23 C14 C15 C16 -1.1(8) . . . . ? C14 C15 C16 C17 0.3(10) . . . . ? C15 C16 C17 C18 1.3(10) . . . . ? C16 C17 C18 C19 177.5(6) . . . . ? C16 C17 C18 C23 -2.1(9) . . . . ? C17 C18 C19 C20 -178.2(7) . . . . ? C23 C18 C19 C20 1.4(10) . . . . ? C18 C19 C20 C21 -0.9(11) . . . . ? C19 C20 C21 C22 -0.6(10) . . . . ? C20 C21 C22 C23 1.5(8) . . . . ? C20 C21 C22 C24 175.9(5) . . . . ? C15 C14 C23 C22 -177.5(5) . . . . ? C15 C14 C23 C18 0.3(7) . . . . ? C21 C22 C23 C14 176.9(4) . . . . ? C24 C22 C23 C14 2.8(7) . . . . ? C21 C22 C23 C18 -1.0(7) . . . . ? C24 C22 C23 C18 -175.1(4) . . . . ? C19 C18 C23 C14 -178.3(5) . . . . ? C17 C18 C23 C14 1.3(8) . . . . ? C19 C18 C23 C22 -0.4(8) . . . . ? C17 C18 C23 C22 179.2(5) . . . . ? C21 C22 C24 N3 111.5(5) . . . . ? C23 C22 C24 N3 -74.4(5) . . . . ? O2 C25 C26 N1 -38.4(5) . . . . ? N3 C25 C26 N1 145.6(3) . . . . ? C36 C27 C28 C29 0.5(12) . . . . ? C27 C28 C29 C30 -0.6(13) . . . . ? C28 C29 C30 C31 -0.7(13) . . . . ? C29 C30 C31 C32 -178.8(7) . . . . ? C29 C30 C31 C36 1.9(11) . . . . ? C30 C31 C32 C33 178.7(8) . . . . ? C36 C31 C32 C33 -2.1(11) . . . . ? C31 C32 C33 C34 2.4(13) . . . . ? C32 C33 C34 C35 -0.9(12) . . . . ? C33 C34 C35 C36 -0.8(9) . . . . ? C33 C34 C35 C37 176.6(6) . . . . ? C28 C27 C36 C35 179.1(6) . . . . ? C28 C27 C36 C31 0.8(9) . . . . ? C34 C35 C36 C27 -177.3(6) . . . . ? C37 C35 C36 C27 5.2(8) . . . . ? C34 C35 C36 C31 1.1(8) . . . . ? C37 C35 C36 C31 -176.5(5) . . . . ? C32 C31 C36 C27 178.8(6) . . . . ? C30 C31 C36 C27 -1.9(8) . . . . ? C32 C31 C36 C35 0.4(8) . . . . ? C30 C31 C36 C35 179.6(5) . . . . ? C34 C35 C37 N4 -14.5(8) . . . . ? C36 C35 C37 N4 163.1(5) . . . . ? O3 C38 C39 N1 -32.6(5) . . . . ? N4 C38 C39 N1 150.1(4) . . . . ? C12 C13 N1 C39 -159.7(3) . . . . ? C12 C13 N1 C26 77.5(4) . . . . ? C12 C13 N1 Eu1 -41.1(3) . . . . ? C38 C39 N1 C13 153.0(3) . . . . ? C38 C39 N1 C26 -84.2(4) . . . . ? C38 C39 N1 Eu1 35.1(4) . . . . ? C25 C26 N1 C13 -94.8(4) . . . . ? C25 C26 N1 C39 142.4(3) . . . . ? C25 C26 N1 Eu1 23.1(4) . . . . ? O2 Eu1 N1 C13 112.5(3) . . . . ? O3 Eu1 N1 C13 -143.1(3) . . . . ? O6 Eu1 N1 C13 -1.7(3) . . . . ? O1 Eu1 N1 C13 29.5(2) . . . . ? O4 Eu1 N1 C13 70.1(3) . . . . ? O10 Eu1 N1 C13 -51.5(2) . . . . ? O9 Eu1 N1 C13 163.0(2) . . . . ? O7 Eu1 N1 C13 -150.0(2) . . . . ? O12 Eu1 N1 C13 -80.3(3) . . . . ? O2 Eu1 N1 C39 -127.7(3) . . . . ? O3 Eu1 N1 C39 -23.4(2) . . . . ? O6 Eu1 N1 C39 118.1(3) . . . . ? O1 Eu1 N1 C39 149.3(3) . . . . ? O4 Eu1 N1 C39 -170.1(2) . . . . ? O10 Eu1 N1 C39 68.3(2) . . . . ? O9 Eu1 N1 C39 -77.2(3) . . . . ? O7 Eu1 N1 C39 -30.2(3) . . . . ? O12 Eu1 N1 C39 39.5(3) . . . . ? O2 Eu1 N1 C26 -7.3(2) . . . . ? O3 Eu1 N1 C26 97.0(3) . . . . ? O6 Eu1 N1 C26 -121.5(3) . . . . ? O1 Eu1 N1 C26 -90.3(2) . . . . ? O4 Eu1 N1 C26 -49.7(3) . . . . ? O10 Eu1 N1 C26 -171.3(3) . . . . ? O9 Eu1 N1 C26 43.2(3) . . . . ? O7 Eu1 N1 C26 90.2(3) . . . . ? O12 Eu1 N1 C26 159.9(2) . . . . ? O1 C12 N2 C11 1.2(6) . . . . ? C13 C12 N2 C11 -176.4(3) . . . . ? C9 C11 N2 C12 -113.7(4) . . . . ? O2 C25 N3 C24 -11.7(6) . . . . ? C26 C25 N3 C24 164.1(4) . . . . ? C22 C24 N3 C25 127.5(4) . . . . ? O3 C38 N4 C37 -1.4(7) . . . . ? C39 C38 N4 C37 175.8(4) . . . . ? C35 C37 N4 C38 113.4(5) . . . . ? N2 C12 O1 Eu1 -178.6(3) . . . . ? C13 C12 O1 Eu1 -1.2(5) . . . . ? O2 Eu1 O1 C12 -87.5(3) . . . . ? O3 Eu1 O1 C12 -8.0(3) . . . . ? O6 Eu1 O1 C12 140.7(3) . . . . ? O4 Eu1 O1 C12 -166.1(3) . . . . ? O10 Eu1 O1 C12 59.0(3) . . . . ? O9 Eu1 O1 C12 -110.7(3) . . . . ? O7 Eu1 O1 C12 163.3(2) . . . . ? O12 Eu1 O1 C12 84.1(3) . . . . ? N1 Eu1 O1 C12 -16.2(3) . . . . ? N3 C25 O2 Eu1 -149.8(3) . . . . ? C26 C25 O2 Eu1 34.3(5) . . . . ? O3 Eu1 O2 C25 -74.5(3) . . . . ? O6 Eu1 O2 C25 113.3(3) . . . . ? O1 Eu1 O2 C25 53.7(3) . . . . ? O4 Eu1 O2 C25 134.6(3) . . . . ? O10 Eu1 O2 C25 7.1(4) . . . . ? O9 Eu1 O2 C25 -143.0(3) . . . . ? O7 Eu1 O2 C25 -159.8(3) . . . . ? O12 Eu1 O2 C25 -88.7(5) . . . . ? N1 Eu1 O2 C25 -13.8(3) . . . . ? N4 C38 O3 Eu1 -173.2(3) . . . . ? C39 C38 O3 Eu1 9.5(6) . . . . ? O2 Eu1 O3 C38 70.8(4) . . . . ? O6 Eu1 O3 C38 -120.5(3) . . . . ? O1 Eu1 O3 C38 0.0(4) . . . . ? O4 Eu1 O3 C38 135.8(3) . . . . ? O10 Eu1 O3 C38 -62.7(3) . . . . ? O9 Eu1 O3 C38 136.0(4) . . . . ? O7 Eu1 O3 C38 -175.3(4) . . . . ? O12 Eu1 O3 C38 -112.3(4) . . . . ? N1 Eu1 O3 C38 8.2(3) . . . . ? O5 N5 O4 Eu1 -177.5(4) . . . . ? O6 N5 O4 Eu1 2.2(4) . . . . ? O2 Eu1 O4 N5 -158.5(3) . . . . ? O3 Eu1 O4 N5 132.4(3) . . . . ? O6 Eu1 O4 N5 -1.3(2) . . . . ? O1 Eu1 O4 N5 -82.4(2) . . . . ? O10 Eu1 O4 N5 -24.5(3) . . . . ? O9 Eu1 O4 N5 132.2(3) . . . . ? O7 Eu1 O4 N5 81.2(2) . . . . ? O12 Eu1 O4 N5 30.7(3) . . . . ? N1 Eu1 O4 N5 -118.9(2) . . . . ? O5 N5 O6 Eu1 177.5(4) . . . . ? O4 N5 O6 Eu1 -2.3(4) . . . . ? O2 Eu1 O6 N5 28.0(3) . . . . ? O3 Eu1 O6 N5 -138.5(2) . . . . ? O1 Eu1 O6 N5 86.8(2) . . . . ? O4 Eu1 O6 N5 1.3(2) . . . . ? O10 Eu1 O6 N5 162.5(3) . . . . ? O9 Eu1 O6 N5 -49.2(3) . . . . ? O7 Eu1 O6 N5 -80.9(3) . . . . ? O12 Eu1 O6 N5 -147.0(3) . . . . ? N1 Eu1 O6 N5 115.4(3) . . . . ? O8 N6 O7 Eu1 176.5(4) . . . . ? O9 N6 O7 Eu1 -2.0(4) . . . . ? O2 Eu1 O7 N6 21.6(3) . . . . ? O3 Eu1 O7 N6 -68.0(2) . . . . ? O6 Eu1 O7 N6 141.7(3) . . . . ? O1 Eu1 O7 N6 119.0(2) . . . . ? O4 Eu1 O7 N6 88.0(2) . . . . ? O10 Eu1 O7 N6 -148.1(2) . . . . ? O9 Eu1 O7 N6 1.1(2) . . . . ? O12 Eu1 O7 N6 -145.1(3) . . . . ? N1 Eu1 O7 N6 -61.8(3) . . . . ? O8 N6 O9 Eu1 -176.5(4) . . . . ? O7 N6 O9 Eu1 2.0(4) . . . . ? O2 Eu1 O9 N6 -160.8(3) . . . . ? O3 Eu1 O9 N6 98.9(3) . . . . ? O6 Eu1 O9 N6 -43.0(3) . . . . ? O1 Eu1 O9 N6 -136.6(2) . . . . ? O4 Eu1 O9 N6 -81.3(3) . . . . ? O10 Eu1 O9 N6 62.1(3) . . . . ? O7 Eu1 O9 N6 -1.2(2) . . . . ? O12 Eu1 O9 N6 29.6(3) . . . . ? N1 Eu1 O9 N6 149.1(2) . . . . ? O11 N7 O10 Eu1 -172.5(4) . . . . ? O12 N7 O10 Eu1 6.0(4) . . . . ? O2 Eu1 O10 N7 -166.9(2) . . . . ? O3 Eu1 O10 N7 -81.5(2) . . . . ? O6 Eu1 O10 N7 68.2(2) . . . . ? O1 Eu1 O10 N7 146.3(3) . . . . ? O4 Eu1 O10 N7 86.6(3) . . . . ? O9 Eu1 O10 N7 -46.7(3) . . . . ? O7 Eu1 O10 N7 0.2(3) . . . . ? O12 Eu1 O10 N7 -3.4(2) . . . . ? N1 Eu1 O10 N7 -146.6(3) . . . . ? O11 N7 O12 Eu1 172.8(4) . . . . ? O10 N7 O12 Eu1 -5.7(4) . . . . ? O2 Eu1 O12 N7 110.3(4) . . . . ? O3 Eu1 O12 N7 95.7(2) . . . . ? O6 Eu1 O12 N7 -89.4(2) . . . . ? O1 Eu1 O12 N7 -29.1(3) . . . . ? O4 Eu1 O12 N7 -116.0(2) . . . . ? O10 Eu1 O12 N7 3.4(2) . . . . ? O9 Eu1 O12 N7 161.1(2) . . . . ? O7 Eu1 O12 N7 -172.9(3) . . . . ? N1 Eu1 O12 N7 40.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.021 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.084 # Attachment '- 826840.cif' data_p21c_2 _database_code_depnum_ccdc_archive 'CCDC 826840' #TrackingRef '- 826840.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H36 N7 O12 Tb' _chemical_formula_weight 953.67 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.146(4) _cell_length_b 16.719(4) _cell_length_c 14.240(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.397(2) _cell_angle_gamma 90.00 _cell_volume 4645.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6773 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 22.36 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 1.584 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6311 _exptl_absorpt_correction_T_max 0.6654 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33230 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8630 _reflns_number_gt 6109 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^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 8630 _refine_ls_number_parameters 532 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0870 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 516 84 ' ' 2 1.000 0.500 0.500 516 84 ' ' _platon_squeeze_details ; ; 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 0.510166(10) 0.840560(10) 0.264294(14) 0.03443(8) Uani 1 1 d . . . C1 C 0.5055(2) 0.6686(2) 0.1308(3) 0.0358(10) Uani 1 1 d . . . H1A H 0.5053 0.6110 0.1234 0.043 Uiso 1 1 calc R . . H1B H 0.5262 0.6919 0.0825 0.043 Uiso 1 1 calc R . . C2 C 0.4337(2) 0.6981(2) 0.1153(3) 0.0338(9) Uani 1 1 d . . . C3 C 0.3143(2) 0.6750(2) 0.0263(3) 0.0457(11) Uani 1 1 d . . . H3A H 0.3000 0.6775 -0.0439 0.055 Uiso 1 1 calc R . . H3B H 0.3073 0.7275 0.0512 0.055 Uiso 1 1 calc R . . C4 C 0.2695(2) 0.6144(2) 0.0623(3) 0.0385(10) Uani 1 1 d . . . C5 C 0.2973(2) 0.5573(2) 0.1271(3) 0.0458(11) Uani 1 1 d . . . H5 H 0.3447 0.5545 0.1499 0.055 Uiso 1 1 calc R . . C6 C 0.2561(3) 0.5019(3) 0.1609(3) 0.0586(13) Uani 1 1 d . . . H6 H 0.2761 0.4632 0.2060 0.070 Uiso 1 1 calc R . . C7 C 0.1880(3) 0.5050(3) 0.1282(4) 0.0683(15) Uani 1 1 d . . . H7 H 0.1609 0.4679 0.1501 0.082 Uiso 1 1 calc R . . C8 C 0.1570(3) 0.5633(3) 0.0614(4) 0.0596(13) Uani 1 1 d . . . C9 C 0.0862(3) 0.5683(4) 0.0286(5) 0.096(2) Uani 1 1 d . . . H9 H 0.0589 0.5323 0.0521 0.115 Uiso 1 1 calc R . . C10 C 0.0557(3) 0.6248(5) -0.0374(6) 0.116(3) Uani 1 1 d . . . H10 H 0.0082 0.6270 -0.0587 0.139 Uiso 1 1 calc R . . C11 C 0.0959(3) 0.6789(4) -0.0725(5) 0.097(2) Uani 1 1 d . . . H11 H 0.0754 0.7173 -0.1176 0.116 Uiso 1 1 calc R . . C12 C 0.1648(3) 0.6759(3) -0.0411(4) 0.0696(15) Uani 1 1 d . . . H12 H 0.1910 0.7127 -0.0651 0.083 Uiso 1 1 calc R . . C13 C 0.1979(2) 0.6186(3) 0.0268(3) 0.0461(11) Uani 1 1 d . . . C14 C 0.5299(2) 0.6356(2) 0.3030(3) 0.0408(10) Uani 1 1 d . . . H14A H 0.5711 0.6269 0.3542 0.049 Uiso 1 1 calc R . . H14B H 0.5148 0.5842 0.2737 0.049 Uiso 1 1 calc R . . C15 C 0.4751(2) 0.6705(2) 0.3457(3) 0.0352(9) Uani 1 1 d . . . C16 C 0.3892(2) 0.6455(2) 0.4361(3) 0.0467(11) Uani 1 1 d . . . H16A H 0.3960 0.7022 0.4494 0.056 Uiso 1 1 calc R . . H16B H 0.4054 0.6174 0.4971 0.056 Uiso 1 1 calc R . . C17 C 0.3124(3) 0.6301(3) 0.3991(4) 0.0553(13) Uani 1 1 d . . . C18 C 0.2833(3) 0.5715(3) 0.4452(4) 0.0748(16) Uani 1 1 d . . . H18 H 0.3108 0.5406 0.4939 0.090 Uiso 1 1 calc R . . C19 C 0.2108(4) 0.5588(4) 0.4177(6) 0.109(3) Uani 1 1 d . . . H19 H 0.1915 0.5194 0.4486 0.130 Uiso 1 1 calc R . . C20 C 0.1694(4) 0.6044(4) 0.3455(6) 0.100(2) Uani 1 1 d . . . H20 H 0.1224 0.5953 0.3277 0.119 Uiso 1 1 calc R . . C21 C 0.1975(3) 0.6633(4) 0.3000(5) 0.0741(17) Uani 1 1 d . . . C22 C 0.1551(4) 0.7094(5) 0.2298(6) 0.097(2) Uani 1 1 d . . . H22 H 0.1083 0.6990 0.2125 0.116 Uiso 1 1 calc R . . C23 C 0.1807(4) 0.7699(5) 0.1852(5) 0.106(2) Uani 1 1 d . . . H23 H 0.1515 0.8009 0.1383 0.127 Uiso 1 1 calc R . . C24 C 0.2523(3) 0.7853(4) 0.2111(4) 0.0818(17) Uani 1 1 d . . . H24 H 0.2700 0.8270 0.1815 0.098 Uiso 1 1 calc R . . C25 C 0.2954(3) 0.7395(3) 0.2791(4) 0.0585(13) Uani 1 1 d . . . H25 H 0.3423 0.7494 0.2945 0.070 Uiso 1 1 calc R . . C26 C 0.2694(3) 0.6774(3) 0.3259(4) 0.0608(14) Uani 1 1 d . . . C27 C 0.6193(2) 0.6895(2) 0.2322(3) 0.0422(10) Uani 1 1 d . . . H27A H 0.6264 0.7048 0.1697 0.051 Uiso 1 1 calc R . . H27B H 0.6375 0.6360 0.2473 0.051 Uiso 1 1 calc R . . C28 C 0.6562(2) 0.7469(3) 0.3085(3) 0.0457(11) Uani 1 1 d . . . C29 C 0.7641(3) 0.7831(3) 0.4247(4) 0.0707(15) Uani 1 1 d . . . H29A H 0.7402 0.8330 0.4278 0.085 Uiso 1 1 calc R . . H29B H 0.8055 0.7953 0.4044 0.085 Uiso 1 1 calc R . . C30 C 0.7835(3) 0.7456(3) 0.5250(4) 0.0577(13) Uani 1 1 d U . . C31 C 0.7487(3) 0.6831(3) 0.5486(4) 0.0892(19) Uani 1 1 d U . . H31 H 0.7106 0.6631 0.5037 0.107 Uiso 1 1 calc R . . C32 C 0.7699(5) 0.6479(4) 0.6411(5) 0.124(3) Uani 1 1 d U . . H32 H 0.7456 0.6045 0.6563 0.149 Uiso 1 1 calc R . . C33 C 0.8224(5) 0.6747(4) 0.7056(5) 0.115(3) Uani 1 1 d U . . H33 H 0.8352 0.6499 0.7659 0.138 Uiso 1 1 calc R . . C34 C 0.8604(4) 0.7402(4) 0.6866(4) 0.0804(17) Uani 1 1 d U . . C35 C 0.9158(4) 0.7720(5) 0.7528(5) 0.113(2) Uani 1 1 d U . . H35 H 0.9296 0.7478 0.8133 0.136 Uiso 1 1 calc R . . C36 C 0.9511(4) 0.8359(6) 0.7351(6) 0.121(3) Uani 1 1 d U . . H36 H 0.9884 0.8548 0.7823 0.145 Uiso 1 1 calc R . . C37 C 0.9311(3) 0.8737(5) 0.6444(5) 0.115(2) Uani 1 1 d U . . H37 H 0.9545 0.9184 0.6307 0.138 Uiso 1 1 calc R . . C38 C 0.8773(3) 0.8440(4) 0.5777(4) 0.0812(17) Uani 1 1 d U . . H38 H 0.8644 0.8693 0.5177 0.097 Uiso 1 1 calc R . . C39 C 0.8396(3) 0.7773(3) 0.5938(4) 0.0599(13) Uani 1 1 d U . . N1 N 0.54583(16) 0.69021(18) 0.2278(2) 0.0338(8) Uani 1 1 d . . . N2 N 0.43189(17) 0.62148(19) 0.3709(2) 0.0388(8) Uani 1 1 d . . . H2 H 0.4284 0.5735 0.3485 0.047 Uiso 1 1 calc R . . N3 N 0.38624(17) 0.65563(18) 0.0554(2) 0.0411(8) Uani 1 1 d . . . H3 H 0.3993 0.6128 0.0317 0.049 Uiso 1 1 calc R . . N4 N 0.7205(2) 0.7311(2) 0.3524(3) 0.0613(11) Uani 1 1 d . . . H4 H 0.7380 0.6874 0.3376 0.074 Uiso 1 1 calc R . . N5 N 0.3914(2) 0.9416(2) 0.2207(3) 0.0593(11) Uani 1 1 d . . . N6 N 0.55597(19) 0.9474(2) 0.4333(3) 0.0439(9) Uani 1 1 d . . . N7 N 0.56824(18) 0.9031(2) 0.1042(3) 0.0456(9) Uani 1 1 d . . . O1 O 0.42181(13) 0.76107(15) 0.15517(18) 0.0370(7) Uani 1 1 d . . . O2 O 0.47564(14) 0.74425(15) 0.36112(19) 0.0422(7) Uani 1 1 d . . . O3 O 0.62698(15) 0.80854(18) 0.3266(2) 0.0522(8) Uani 1 1 d . . . O4 O 0.40339(17) 0.89477(19) 0.2942(3) 0.0599(9) Uani 1 1 d . . . O5 O 0.43274(16) 0.93893(17) 0.1678(2) 0.0506(8) Uani 1 1 d . . . O6 O 0.34237(19) 0.9865(2) 0.2038(3) 0.0963(13) Uani 1 1 d . . . O7 O 0.54510(19) 0.87438(18) 0.4420(2) 0.0656(10) Uani 1 1 d . . . O8 O 0.54334(15) 0.97373(15) 0.34721(19) 0.0448(7) Uani 1 1 d . . . O9 O 0.57754(17) 0.99085(17) 0.5039(2) 0.0576(9) Uani 1 1 d . . . O10 O 0.57618(16) 0.94475(17) 0.1801(2) 0.0516(8) Uani 1 1 d . . . O11 O 0.54134(15) 0.83480(16) 0.1064(2) 0.0488(8) Uani 1 1 d . . . O12 O 0.5845(2) 0.9273(2) 0.0325(2) 0.0793(12) 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 Tb1 0.05223(14) 0.01955(11) 0.03359(12) -0.00259(9) 0.01457(9) -0.00145(9) C1 0.051(3) 0.022(2) 0.036(2) -0.0057(17) 0.013(2) -0.0041(18) C2 0.049(3) 0.025(2) 0.028(2) 0.0017(18) 0.011(2) -0.0051(19) C3 0.050(3) 0.042(3) 0.042(3) 0.004(2) 0.006(2) -0.005(2) C4 0.051(3) 0.031(2) 0.033(2) -0.0008(19) 0.010(2) -0.002(2) C5 0.055(3) 0.041(3) 0.039(3) -0.003(2) 0.006(2) 0.001(2) C6 0.079(4) 0.042(3) 0.058(3) 0.009(2) 0.022(3) -0.002(3) C7 0.084(4) 0.049(3) 0.078(4) 0.009(3) 0.031(3) -0.015(3) C8 0.048(3) 0.057(3) 0.073(4) -0.001(3) 0.013(3) -0.011(3) C9 0.083(5) 0.086(5) 0.118(6) 0.019(4) 0.025(4) -0.022(4) C10 0.050(4) 0.130(6) 0.162(7) 0.033(6) 0.015(4) -0.008(4) C11 0.069(4) 0.102(5) 0.111(5) 0.040(4) 0.005(4) 0.011(4) C12 0.054(3) 0.069(4) 0.081(4) 0.018(3) 0.010(3) 0.000(3) C13 0.048(3) 0.038(3) 0.052(3) 0.001(2) 0.009(2) 0.001(2) C14 0.061(3) 0.024(2) 0.039(2) 0.0014(18) 0.015(2) 0.002(2) C15 0.048(3) 0.027(2) 0.028(2) 0.0025(17) 0.004(2) -0.0014(19) C16 0.060(3) 0.037(3) 0.046(3) -0.002(2) 0.021(2) 0.000(2) C17 0.065(3) 0.038(3) 0.066(3) -0.017(2) 0.023(3) -0.004(2) C18 0.085(4) 0.046(3) 0.103(4) -0.006(3) 0.040(4) -0.016(3) C19 0.095(5) 0.080(5) 0.177(8) -0.034(5) 0.083(6) -0.040(4) C20 0.068(5) 0.085(5) 0.144(7) -0.024(5) 0.025(5) -0.012(4) C21 0.051(3) 0.070(4) 0.102(5) -0.037(4) 0.018(3) -0.005(3) C22 0.071(5) 0.100(6) 0.117(6) -0.041(5) 0.018(5) 0.005(4) C23 0.096(6) 0.107(6) 0.101(6) -0.024(5) -0.002(5) 0.034(5) C24 0.086(5) 0.079(4) 0.078(4) -0.015(4) 0.014(4) 0.010(4) C25 0.072(4) 0.051(3) 0.054(3) -0.008(3) 0.020(3) 0.001(3) C26 0.062(3) 0.052(3) 0.072(4) -0.028(3) 0.022(3) -0.001(3) C27 0.044(3) 0.033(2) 0.050(3) -0.003(2) 0.013(2) -0.0004(19) C28 0.054(3) 0.038(3) 0.044(3) 0.005(2) 0.010(2) -0.003(2) C29 0.058(3) 0.066(4) 0.074(4) 0.007(3) -0.009(3) -0.021(3) C30 0.066(3) 0.048(3) 0.058(3) 0.004(2) 0.014(3) 0.001(3) C31 0.131(5) 0.070(4) 0.073(4) -0.001(3) 0.039(4) -0.029(4) C32 0.236(9) 0.073(5) 0.077(5) 0.005(4) 0.063(5) -0.041(5) C33 0.217(8) 0.069(5) 0.055(4) 0.012(3) 0.029(5) 0.006(5) C34 0.106(5) 0.079(4) 0.052(4) -0.001(3) 0.012(3) 0.026(4) C35 0.117(6) 0.141(7) 0.064(4) -0.001(5) -0.008(5) 0.045(5) C36 0.070(5) 0.182(8) 0.095(6) -0.020(6) -0.009(4) 0.002(5) C37 0.077(5) 0.181(7) 0.079(5) -0.012(5) 0.006(4) -0.042(5) C38 0.063(4) 0.115(5) 0.060(4) 0.006(3) 0.003(3) -0.018(3) C39 0.053(3) 0.070(4) 0.057(3) 0.007(3) 0.013(3) 0.009(3) N1 0.041(2) 0.0237(17) 0.037(2) -0.0022(15) 0.0107(17) 0.0001(14) N2 0.056(2) 0.0205(17) 0.041(2) -0.0020(15) 0.0133(18) -0.0037(16) N3 0.047(2) 0.0281(19) 0.046(2) -0.0123(17) 0.0075(18) -0.0031(17) N4 0.053(3) 0.050(3) 0.072(3) -0.002(2) 0.000(2) 0.000(2) N5 0.060(3) 0.032(2) 0.083(3) -0.013(2) 0.012(3) 0.004(2) N6 0.062(2) 0.035(2) 0.040(2) -0.0068(18) 0.021(2) -0.0051(18) N7 0.058(2) 0.039(2) 0.040(2) -0.0019(18) 0.014(2) -0.0042(18) O1 0.0454(17) 0.0267(15) 0.0394(16) -0.0083(12) 0.0113(14) 0.0004(12) O2 0.070(2) 0.0188(15) 0.0429(17) -0.0036(12) 0.0240(16) -0.0038(13) O3 0.057(2) 0.0374(18) 0.058(2) -0.0091(15) 0.0056(17) -0.0009(15) O4 0.068(2) 0.044(2) 0.076(2) -0.0102(18) 0.034(2) -0.0014(17) O5 0.058(2) 0.0388(18) 0.055(2) 0.0000(15) 0.0154(17) 0.0012(15) O6 0.071(3) 0.068(3) 0.150(4) 0.004(3) 0.029(3) 0.032(2) O7 0.135(3) 0.0254(16) 0.0441(19) -0.0025(14) 0.037(2) -0.0168(19) O8 0.073(2) 0.0302(16) 0.0303(16) 0.0030(13) 0.0108(15) -0.0058(14) O9 0.093(3) 0.0399(19) 0.0385(18) -0.0150(15) 0.0139(17) -0.0136(17) O10 0.078(2) 0.0352(17) 0.0445(19) -0.0080(14) 0.0218(17) -0.0090(15) O11 0.072(2) 0.0285(17) 0.0495(18) -0.0058(14) 0.0219(17) -0.0120(15) O12 0.125(3) 0.073(3) 0.051(2) -0.0011(18) 0.044(2) -0.036(2) _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 O2 2.335(3) . ? Tb1 O3 2.361(3) . ? Tb1 O5 2.441(3) . ? Tb1 O1 2.444(3) . ? Tb1 O4 2.467(3) . ? Tb1 O11 2.483(3) . ? Tb1 O7 2.517(3) . ? Tb1 O8 2.531(3) . ? Tb1 O10 2.652(3) . ? Tb1 N1 2.700(3) . ? Tb1 N5 2.868(4) . ? Tb1 N6 2.954(4) . ? C1 N1 1.463(5) . ? C1 C2 1.491(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 O1 1.248(4) . ? C2 N3 1.318(5) . ? C3 N3 1.442(5) . ? C3 C4 1.527(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.350(5) . ? C4 C13 1.406(6) . ? C5 C6 1.406(6) . ? C5 H5 0.9300 . ? C6 C7 1.335(7) . ? C6 H6 0.9300 . ? C7 C8 1.395(7) . ? C7 H7 0.9300 . ? C8 C9 1.389(7) . ? C8 C13 1.408(6) . ? C9 C10 1.366(8) . ? C9 H9 0.9300 . ? C10 C11 1.389(8) . ? C10 H10 0.9300 . ? C11 C12 1.348(7) . ? C11 H11 0.9300 . ? C12 C13 1.407(6) . ? C12 H12 0.9300 . ? C14 N1 1.501(5) . ? C14 C15 1.505(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 O2 1.252(4) . ? C15 N2 1.309(5) . ? C16 N2 1.470(5) . ? C16 C17 1.527(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.387(7) . ? C17 C26 1.419(7) . ? C18 C19 1.430(8) . ? C18 H18 0.9300 . ? C19 C20 1.381(9) . ? C19 H19 0.9300 . ? C20 C21 1.376(9) . ? C20 H20 0.9300 . ? C21 C22 1.378(9) . ? C21 C26 1.422(7) . ? C22 C23 1.360(9) . ? C22 H22 0.9300 . ? C23 C24 1.423(8) . ? C23 H23 0.9300 . ? C24 C25 1.363(7) . ? C24 H24 0.9300 . ? C25 C26 1.403(7) . ? C25 H25 0.9300 . ? C27 N1 1.467(5) . ? C27 C28 1.501(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 O3 1.245(5) . ? C28 N4 1.317(5) . ? C29 N4 1.461(6) . ? C29 C30 1.519(7) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.348(7) . ? C30 C39 1.402(7) . ? C31 C32 1.409(8) . ? C31 H31 0.9300 . ? C32 C33 1.297(10) . ? C32 H32 0.9300 . ? C33 C34 1.399(9) . ? C33 H33 0.9300 . ? C34 C35 1.376(9) . ? C34 C39 1.426(7) . ? C35 C36 1.341(9) . ? C35 H35 0.9300 . ? C36 C37 1.404(10) . ? C36 H36 0.9300 . ? C37 C38 1.346(8) . ? C37 H37 0.9300 . ? C38 C39 1.400(7) . ? C38 H38 0.9300 . ? N2 H2 0.8600 . ? N3 H3 0.8600 . ? N4 H4 0.8600 . ? N5 O6 1.216(5) . ? N5 O5 1.255(5) . ? N5 O4 1.281(5) . ? N6 O9 1.229(4) . ? N6 O7 1.252(4) . ? N6 O8 1.267(4) . ? N7 O12 1.216(4) . ? N7 O10 1.263(4) . ? N7 O11 1.268(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Tb1 O3 92.14(10) . . ? O2 Tb1 O5 123.67(10) . . ? O3 Tb1 O5 143.31(10) . . ? O2 Tb1 O1 73.96(9) . . ? O3 Tb1 O1 128.02(9) . . ? O5 Tb1 O1 75.28(10) . . ? O2 Tb1 O4 75.57(11) . . ? O3 Tb1 O4 148.10(11) . . ? O5 Tb1 O4 52.21(11) . . ? O1 Tb1 O4 77.35(10) . . ? O2 Tb1 O11 133.44(9) . . ? O3 Tb1 O11 83.02(10) . . ? O5 Tb1 O11 77.65(10) . . ? O1 Tb1 O11 73.22(9) . . ? O4 Tb1 O11 126.76(11) . . ? O2 Tb1 O7 67.11(9) . . ? O3 Tb1 O7 70.72(11) . . ? O5 Tb1 O7 113.24(10) . . ? O1 Tb1 O7 137.63(9) . . ? O4 Tb1 O7 77.39(12) . . ? O11 Tb1 O7 148.12(11) . . ? O2 Tb1 O8 114.45(9) . . ? O3 Tb1 O8 84.33(10) . . ? O5 Tb1 O8 74.20(9) . . ? O1 Tb1 O8 147.25(9) . . ? O4 Tb1 O8 74.74(10) . . ? O11 Tb1 O8 111.09(9) . . ? O7 Tb1 O8 50.05(9) . . ? O2 Tb1 O10 167.46(10) . . ? O3 Tb1 O10 75.74(10) . . ? O5 Tb1 O10 67.98(10) . . ? O1 Tb1 O10 115.95(9) . . ? O4 Tb1 O10 113.17(10) . . ? O11 Tb1 O10 49.29(9) . . ? O7 Tb1 O10 105.11(9) . . ? O8 Tb1 O10 61.90(9) . . ? O2 Tb1 N1 66.69(9) . . ? O3 Tb1 N1 64.73(10) . . ? O5 Tb1 N1 133.01(10) . . ? O1 Tb1 N1 63.78(9) . . ? O4 Tb1 N1 131.33(10) . . ? O11 Tb1 N1 69.54(9) . . ? O7 Tb1 N1 112.41(10) . . ? O8 Tb1 N1 148.95(10) . . ? O10 Tb1 N1 109.71(9) . . ? O2 Tb1 N5 100.31(12) . . ? O3 Tb1 N5 156.19(11) . . ? O5 Tb1 N5 25.78(11) . . ? O1 Tb1 N5 75.30(10) . . ? O4 Tb1 N5 26.44(11) . . ? O11 Tb1 N5 102.25(12) . . ? O7 Tb1 N5 95.44(12) . . ? O8 Tb1 N5 72.06(10) . . ? O10 Tb1 N5 90.02(12) . . ? N1 Tb1 N5 138.97(10) . . ? O2 Tb1 N6 90.84(9) . . ? O3 Tb1 N6 75.57(10) . . ? O5 Tb1 N6 94.45(10) . . ? O1 Tb1 N6 151.30(9) . . ? O4 Tb1 N6 75.31(10) . . ? O11 Tb1 N6 131.54(9) . . ? O7 Tb1 N6 24.85(9) . . ? O8 Tb1 N6 25.22(8) . . ? O10 Tb1 N6 83.15(9) . . ? N1 Tb1 N6 132.49(10) . . ? N5 Tb1 N6 83.96(11) . . ? N1 C1 C2 110.5(3) . . ? N1 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 . . ? N1 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? O1 C2 N3 124.0(4) . . ? O1 C2 C1 120.0(3) . . ? N3 C2 C1 116.0(3) . . ? N3 C3 C4 112.9(3) . . ? N3 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? N3 C3 H3B 109.0 . . ? C4 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C13 119.7(4) . . ? C5 C4 C3 121.4(4) . . ? C13 C4 C3 119.0(4) . . ? C4 C5 C6 121.4(4) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C7 C6 C5 119.8(5) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C8 120.8(5) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C9 C8 C7 121.3(5) . . ? C9 C8 C13 119.0(5) . . ? C7 C8 C13 119.7(5) . . ? C10 C9 C8 121.5(6) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 119.7(6) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 120.1(6) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 121.8(5) . . ? C11 C12 H12 119.1 . . ? C13 C12 H12 119.1 . . ? C8 C13 C12 118.0(4) . . ? C8 C13 C4 118.6(4) . . ? C12 C13 C4 123.4(4) . . ? N1 C14 C15 111.1(3) . . ? N1 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? N1 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? O2 C15 N2 123.1(4) . . ? O2 C15 C14 118.5(4) . . ? N2 C15 C14 118.2(4) . . ? N2 C16 C17 116.0(4) . . ? N2 C16 H16A 108.3 . . ? C17 C16 H16A 108.3 . . ? N2 C16 H16B 108.3 . . ? C17 C16 H16B 108.3 . . ? H16A C16 H16B 107.4 . . ? C18 C17 C26 119.3(5) . . ? C18 C17 C16 117.8(5) . . ? C26 C17 C16 122.7(4) . . ? C17 C18 C19 119.9(6) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 120.5(6) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 120.2(7) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 119.3(6) . . ? C22 C21 C26 120.2(6) . . ? C20 C21 C26 120.5(7) . . ? C23 C22 C21 121.1(7) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 119.4(7) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C25 C24 C23 120.5(6) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 120.4(5) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 118.4(6) . . ? C25 C26 C17 122.0(5) . . ? C21 C26 C17 119.6(6) . . ? N1 C27 C28 109.8(3) . . ? N1 C27 H27A 109.7 . . ? C28 C27 H27A 109.7 . . ? N1 C27 H27B 109.7 . . ? C28 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? O3 C28 N4 121.9(4) . . ? O3 C28 C27 120.2(4) . . ? N4 C28 C27 117.8(4) . . ? N4 C29 C30 112.8(4) . . ? N4 C29 H29A 109.0 . . ? C30 C29 H29A 109.0 . . ? N4 C29 H29B 109.0 . . ? C30 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? C31 C30 C39 119.8(5) . . ? C31 C30 C29 121.7(5) . . ? C39 C30 C29 118.4(4) . . ? C30 C31 C32 120.1(6) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C33 C32 C31 121.5(7) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C32 C33 C34 121.5(7) . . ? C32 C33 H33 119.2 . . ? C34 C33 H33 119.2 . . ? C35 C34 C33 124.0(7) . . ? C35 C34 C39 117.9(7) . . ? C33 C34 C39 118.1(6) . . ? C36 C35 C34 123.9(8) . . ? C36 C35 H35 118.0 . . ? C34 C35 H35 118.0 . . ? C35 C36 C37 119.1(7) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C38 C37 C36 118.7(7) . . ? C38 C37 H37 120.7 . . ? C36 C37 H37 120.7 . . ? C37 C38 C39 123.6(6) . . ? C37 C38 H38 118.2 . . ? C39 C38 H38 118.2 . . ? C38 C39 C30 124.2(5) . . ? C38 C39 C34 116.9(6) . . ? C30 C39 C34 118.9(5) . . ? C27 N1 C1 110.9(3) . . ? C27 N1 C14 111.0(3) . . ? C1 N1 C14 110.9(3) . . ? C27 N1 Tb1 108.2(2) . . ? C1 N1 Tb1 107.4(2) . . ? C14 N1 Tb1 108.4(2) . . ? C15 N2 C16 122.4(3) . . ? C15 N2 H2 118.8 . . ? C16 N2 H2 118.8 . . ? C2 N3 C3 125.5(3) . . ? C2 N3 H3 117.3 . . ? C3 N3 H3 117.3 . . ? C28 N4 C29 124.2(4) . . ? C28 N4 H4 117.9 . . ? C29 N4 H4 117.9 . . ? O6 N5 O5 122.1(5) . . ? O6 N5 O4 121.2(5) . . ? O5 N5 O4 116.8(4) . . ? O6 N5 Tb1 177.9(3) . . ? O5 N5 Tb1 57.8(2) . . ? O4 N5 Tb1 59.0(2) . . ? O9 N6 O7 121.9(4) . . ? O9 N6 O8 122.1(3) . . ? O7 N6 O8 115.9(3) . . ? O9 N6 Tb1 177.5(3) . . ? O7 N6 Tb1 57.64(19) . . ? O8 N6 Tb1 58.35(18) . . ? O12 N7 O10 122.2(4) . . ? O12 N7 O11 121.8(4) . . ? O10 N7 O11 116.1(3) . . ? C2 O1 Tb1 123.8(2) . . ? C15 O2 Tb1 124.5(2) . . ? C28 O3 Tb1 126.1(3) . . ? N5 O4 Tb1 94.5(3) . . ? N5 O5 Tb1 96.4(3) . . ? N6 O7 Tb1 97.5(2) . . ? N6 O8 Tb1 96.4(2) . . ? N7 O10 Tb1 93.1(2) . . ? N7 O11 Tb1 101.1(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 O1 32.0(5) . . . . ? N1 C1 C2 N3 -150.5(3) . . . . ? N3 C3 C4 C5 10.0(6) . . . . ? N3 C3 C4 C13 -170.1(4) . . . . ? C13 C4 C5 C6 -0.5(6) . . . . ? C3 C4 C5 C6 179.4(4) . . . . ? C4 C5 C6 C7 0.5(7) . . . . ? C5 C6 C7 C8 -0.7(8) . . . . ? C6 C7 C8 C9 -178.4(5) . . . . ? C6 C7 C8 C13 1.1(8) . . . . ? C7 C8 C9 C10 -179.4(6) . . . . ? C13 C8 C9 C10 1.0(10) . . . . ? C8 C9 C10 C11 -0.3(12) . . . . ? C9 C10 C11 C12 -0.3(12) . . . . ? C10 C11 C12 C13 0.3(10) . . . . ? C9 C8 C13 C12 -1.1(8) . . . . ? C7 C8 C13 C12 179.4(5) . . . . ? C9 C8 C13 C4 178.4(5) . . . . ? C7 C8 C13 C4 -1.1(7) . . . . ? C11 C12 C13 C8 0.5(8) . . . . ? C11 C12 C13 C4 -179.0(5) . . . . ? C5 C4 C13 C8 0.9(6) . . . . ? C3 C4 C13 C8 -179.1(4) . . . . ? C5 C4 C13 C12 -179.7(4) . . . . ? C3 C4 C13 C12 0.4(7) . . . . ? N1 C14 C15 O2 -38.6(5) . . . . ? N1 C14 C15 N2 145.9(4) . . . . ? N2 C16 C17 C18 111.0(5) . . . . ? N2 C16 C17 C26 -74.5(5) . . . . ? C26 C17 C18 C19 0.9(8) . . . . ? C16 C17 C18 C19 175.6(5) . . . . ? C17 C18 C19 C20 -0.1(9) . . . . ? C18 C19 C20 C21 -0.6(10) . . . . ? C19 C20 C21 C22 -178.5(6) . . . . ? C19 C20 C21 C26 0.5(9) . . . . ? C20 C21 C22 C23 177.8(6) . . . . ? C26 C21 C22 C23 -1.1(9) . . . . ? C21 C22 C23 C24 0.5(10) . . . . ? C22 C23 C24 C25 0.8(9) . . . . ? C23 C24 C25 C26 -1.3(8) . . . . ? C24 C25 C26 C21 0.6(7) . . . . ? C24 C25 C26 C17 -178.1(5) . . . . ? C22 C21 C26 C25 0.6(7) . . . . ? C20 C21 C26 C25 -178.4(5) . . . . ? C22 C21 C26 C17 179.3(5) . . . . ? C20 C21 C26 C17 0.3(8) . . . . ? C18 C17 C26 C25 177.6(4) . . . . ? C16 C17 C26 C25 3.2(7) . . . . ? C18 C17 C26 C21 -1.0(7) . . . . ? C16 C17 C26 C21 -175.5(4) . . . . ? N1 C27 C28 O3 -31.5(5) . . . . ? N1 C27 C28 N4 150.8(4) . . . . ? N4 C29 C30 C31 -17.6(8) . . . . ? N4 C29 C30 C39 161.9(4) . . . . ? C39 C30 C31 C32 -2.0(9) . . . . ? C29 C30 C31 C32 177.5(6) . . . . ? C30 C31 C32 C33 0.6(12) . . . . ? C31 C32 C33 C34 0.4(13) . . . . ? C32 C33 C34 C35 178.9(7) . . . . ? C32 C33 C34 C39 0.2(11) . . . . ? C33 C34 C35 C36 -178.4(8) . . . . ? C39 C34 C35 C36 0.3(11) . . . . ? C34 C35 C36 C37 0.3(13) . . . . ? C35 C36 C37 C38 -0.6(12) . . . . ? C36 C37 C38 C39 0.2(11) . . . . ? C37 C38 C39 C30 -179.9(6) . . . . ? C37 C38 C39 C34 0.3(9) . . . . ? C31 C30 C39 C38 -177.3(5) . . . . ? C29 C30 C39 C38 3.2(8) . . . . ? C31 C30 C39 C34 2.5(8) . . . . ? C29 C30 C39 C34 -177.0(5) . . . . ? C35 C34 C39 C38 -0.6(8) . . . . ? C33 C34 C39 C38 178.2(6) . . . . ? C35 C34 C39 C30 179.6(5) . . . . ? C33 C34 C39 C30 -1.6(8) . . . . ? C28 C27 N1 C1 152.5(3) . . . . ? C28 C27 N1 C14 -83.9(4) . . . . ? C28 C27 N1 Tb1 34.9(4) . . . . ? C2 C1 N1 C27 -158.8(3) . . . . ? C2 C1 N1 C14 77.5(4) . . . . ? C2 C1 N1 Tb1 -40.7(3) . . . . ? C15 C14 N1 C27 142.6(3) . . . . ? C15 C14 N1 C1 -93.8(4) . . . . ? C15 C14 N1 Tb1 23.9(4) . . . . ? O2 Tb1 N1 C27 -128.2(3) . . . . ? O3 Tb1 N1 C27 -23.9(2) . . . . ? O5 Tb1 N1 C27 116.7(2) . . . . ? O1 Tb1 N1 C27 148.8(3) . . . . ? O4 Tb1 N1 C27 -170.5(2) . . . . ? O11 Tb1 N1 C27 68.0(2) . . . . ? O7 Tb1 N1 C27 -77.7(3) . . . . ? O8 Tb1 N1 C27 -29.1(3) . . . . ? O10 Tb1 N1 C27 38.9(3) . . . . ? N5 Tb1 N1 C27 153.2(3) . . . . ? N6 Tb1 N1 C27 -60.1(3) . . . . ? O2 Tb1 N1 C1 112.0(2) . . . . ? O3 Tb1 N1 C1 -143.6(3) . . . . ? O5 Tb1 N1 C1 -3.0(3) . . . . ? O1 Tb1 N1 C1 29.1(2) . . . . ? O4 Tb1 N1 C1 69.8(3) . . . . ? O11 Tb1 N1 C1 -51.7(2) . . . . ? O7 Tb1 N1 C1 162.5(2) . . . . ? O8 Tb1 N1 C1 -148.9(2) . . . . ? O10 Tb1 N1 C1 -80.9(2) . . . . ? N5 Tb1 N1 C1 33.5(3) . . . . ? N6 Tb1 N1 C1 -179.9(2) . . . . ? O2 Tb1 N1 C14 -7.8(2) . . . . ? O3 Tb1 N1 C14 96.6(3) . . . . ? O5 Tb1 N1 C14 -122.9(2) . . . . ? O1 Tb1 N1 C14 -90.7(2) . . . . ? O4 Tb1 N1 C14 -50.1(3) . . . . ? O11 Tb1 N1 C14 -171.5(3) . . . . ? O7 Tb1 N1 C14 42.7(3) . . . . ? O8 Tb1 N1 C14 91.3(3) . . . . ? O10 Tb1 N1 C14 159.3(2) . . . . ? N5 Tb1 N1 C14 -86.4(3) . . . . ? N6 Tb1 N1 C14 60.3(3) . . . . ? O2 C15 N2 C16 -12.2(6) . . . . ? C14 C15 N2 C16 163.0(4) . . . . ? C17 C16 N2 C15 127.5(4) . . . . ? O1 C2 N3 C3 0.4(6) . . . . ? C1 C2 N3 C3 -176.9(3) . . . . ? C4 C3 N3 C2 -114.2(4) . . . . ? O3 C28 N4 C29 -0.7(7) . . . . ? C27 C28 N4 C29 176.9(4) . . . . ? C30 C29 N4 C28 113.5(5) . . . . ? O2 Tb1 N5 O6 117(11) . . . . ? O3 Tb1 N5 O6 -3(11) . . . . ? O5 Tb1 N5 O6 -86(11) . . . . ? O1 Tb1 N5 O6 -173(11) . . . . ? O4 Tb1 N5 O6 96(11) . . . . ? O11 Tb1 N5 O6 -104(11) . . . . ? O7 Tb1 N5 O6 50(11) . . . . ? O8 Tb1 N5 O6 5(11) . . . . ? O10 Tb1 N5 O6 -56(11) . . . . ? N1 Tb1 N5 O6 -177(100) . . . . ? N6 Tb1 N5 O6 27(11) . . . . ? O2 Tb1 N5 O5 -156.8(2) . . . . ? O3 Tb1 N5 O5 82.8(4) . . . . ? O1 Tb1 N5 O5 -86.5(2) . . . . ? O4 Tb1 N5 O5 -177.6(4) . . . . ? O11 Tb1 N5 O5 -17.8(2) . . . . ? O7 Tb1 N5 O5 135.6(2) . . . . ? O8 Tb1 N5 O5 90.7(2) . . . . ? O10 Tb1 N5 O5 30.4(2) . . . . ? N1 Tb1 N5 O5 -90.6(3) . . . . ? N6 Tb1 N5 O5 113.5(2) . . . . ? O2 Tb1 N5 O4 20.8(3) . . . . ? O3 Tb1 N5 O4 -99.6(4) . . . . ? O5 Tb1 N5 O4 177.6(4) . . . . ? O1 Tb1 N5 O4 91.1(2) . . . . ? O11 Tb1 N5 O4 159.8(2) . . . . ? O7 Tb1 N5 O4 -46.8(2) . . . . ? O8 Tb1 N5 O4 -91.7(2) . . . . ? O10 Tb1 N5 O4 -152.0(2) . . . . ? N1 Tb1 N5 O4 87.0(3) . . . . ? N6 Tb1 N5 O4 -68.9(2) . . . . ? O2 Tb1 N6 O9 98(6) . . . . ? O3 Tb1 N6 O9 6(6) . . . . ? O5 Tb1 N6 O9 -138(6) . . . . ? O1 Tb1 N6 O9 155(6) . . . . ? O4 Tb1 N6 O9 173(6) . . . . ? O11 Tb1 N6 O9 -61(6) . . . . ? O7 Tb1 N6 O9 81(6) . . . . ? O8 Tb1 N6 O9 -102(6) . . . . ? O10 Tb1 N6 O9 -71(6) . . . . ? N1 Tb1 N6 O9 39(7) . . . . ? N5 Tb1 N6 O9 -162(6) . . . . ? O2 Tb1 N6 O7 16.8(3) . . . . ? O3 Tb1 N6 O7 -75.2(3) . . . . ? O5 Tb1 N6 O7 140.7(3) . . . . ? O1 Tb1 N6 O7 73.5(3) . . . . ? O4 Tb1 N6 O7 91.7(3) . . . . ? O11 Tb1 N6 O7 -141.9(2) . . . . ? O8 Tb1 N6 O7 176.9(4) . . . . ? O10 Tb1 N6 O7 -152.2(3) . . . . ? N1 Tb1 N6 O7 -41.6(3) . . . . ? N5 Tb1 N6 O7 117.1(3) . . . . ? O2 Tb1 N6 O8 -160.1(2) . . . . ? O3 Tb1 N6 O8 107.9(2) . . . . ? O5 Tb1 N6 O8 -36.3(2) . . . . ? O1 Tb1 N6 O8 -103.4(3) . . . . ? O4 Tb1 N6 O8 -85.3(2) . . . . ? O11 Tb1 N6 O8 41.2(3) . . . . ? O7 Tb1 N6 O8 -176.9(4) . . . . ? O10 Tb1 N6 O8 30.9(2) . . . . ? N1 Tb1 N6 O8 141.4(2) . . . . ? N5 Tb1 N6 O8 -59.9(2) . . . . ? N3 C2 O1 Tb1 -179.1(3) . . . . ? C1 C2 O1 Tb1 -1.8(5) . . . . ? O2 Tb1 O1 C2 -87.1(3) . . . . ? O3 Tb1 O1 C2 -7.2(3) . . . . ? O5 Tb1 O1 C2 140.7(3) . . . . ? O4 Tb1 O1 C2 -165.5(3) . . . . ? O11 Tb1 O1 C2 59.4(3) . . . . ? O7 Tb1 O1 C2 -110.8(3) . . . . ? O8 Tb1 O1 C2 162.5(2) . . . . ? O10 Tb1 O1 C2 84.7(3) . . . . ? N1 Tb1 O1 C2 -15.6(3) . . . . ? N5 Tb1 O1 C2 167.4(3) . . . . ? N6 Tb1 O1 C2 -147.5(3) . . . . ? N2 C15 O2 Tb1 -150.4(3) . . . . ? C14 C15 O2 Tb1 34.4(5) . . . . ? O3 Tb1 O2 C15 -74.9(3) . . . . ? O5 Tb1 O2 C15 113.5(3) . . . . ? O1 Tb1 O2 C15 54.2(3) . . . . ? O4 Tb1 O2 C15 134.9(3) . . . . ? O11 Tb1 O2 C15 7.5(4) . . . . ? O7 Tb1 O2 C15 -143.0(3) . . . . ? O8 Tb1 O2 C15 -159.7(3) . . . . ? O10 Tb1 O2 C15 -89.5(5) . . . . ? N1 Tb1 O2 C15 -13.7(3) . . . . ? N5 Tb1 O2 C15 125.5(3) . . . . ? N6 Tb1 O2 C15 -150.5(3) . . . . ? N4 C28 O3 Tb1 -174.7(3) . . . . ? C27 C28 O3 Tb1 7.8(6) . . . . ? O2 Tb1 O3 C28 72.4(3) . . . . ? O5 Tb1 O3 C28 -119.5(3) . . . . ? O1 Tb1 O3 C28 1.1(4) . . . . ? O4 Tb1 O3 C28 138.0(3) . . . . ? O11 Tb1 O3 C28 -61.2(3) . . . . ? O7 Tb1 O3 C28 137.2(4) . . . . ? O8 Tb1 O3 C28 -173.3(3) . . . . ? O10 Tb1 O3 C28 -110.9(3) . . . . ? N1 Tb1 O3 C28 9.5(3) . . . . ? N5 Tb1 O3 C28 -165.8(4) . . . . ? N6 Tb1 O3 C28 162.7(4) . . . . ? O6 N5 O4 Tb1 -177.5(4) . . . . ? O5 N5 O4 Tb1 2.3(4) . . . . ? O2 Tb1 O4 N5 -158.8(3) . . . . ? O3 Tb1 O4 N5 131.1(3) . . . . ? O5 Tb1 O4 N5 -1.3(2) . . . . ? O1 Tb1 O4 N5 -82.4(2) . . . . ? O11 Tb1 O4 N5 -24.9(3) . . . . ? O7 Tb1 O4 N5 131.9(3) . . . . ? O8 Tb1 O4 N5 80.3(2) . . . . ? O10 Tb1 O4 N5 30.7(3) . . . . ? N1 Tb1 O4 N5 -119.2(2) . . . . ? N6 Tb1 O4 N5 106.4(2) . . . . ? O6 N5 O5 Tb1 177.5(4) . . . . ? O4 N5 O5 Tb1 -2.3(4) . . . . ? O2 Tb1 O5 N5 27.8(3) . . . . ? O3 Tb1 O5 N5 -137.9(2) . . . . ? O1 Tb1 O5 N5 86.6(2) . . . . ? O4 Tb1 O5 N5 1.3(2) . . . . ? O11 Tb1 O5 N5 162.2(2) . . . . ? O7 Tb1 O5 N5 -49.3(3) . . . . ? O8 Tb1 O5 N5 -81.4(2) . . . . ? O10 Tb1 O5 N5 -146.9(3) . . . . ? N1 Tb1 O5 N5 116.1(2) . . . . ? N6 Tb1 O5 N5 -66.2(2) . . . . ? O9 N6 O7 Tb1 -177.1(3) . . . . ? O8 N6 O7 Tb1 2.9(4) . . . . ? O2 Tb1 O7 N6 -161.7(3) . . . . ? O3 Tb1 O7 N6 97.3(3) . . . . ? O5 Tb1 O7 N6 -43.4(3) . . . . ? O1 Tb1 O7 N6 -136.9(2) . . . . ? O4 Tb1 O7 N6 -82.2(3) . . . . ? O11 Tb1 O7 N6 61.0(3) . . . . ? O8 Tb1 O7 N6 -1.7(2) . . . . ? O10 Tb1 O7 N6 28.7(3) . . . . ? N1 Tb1 O7 N6 148.0(2) . . . . ? N5 Tb1 O7 N6 -62.8(3) . . . . ? O9 N6 O8 Tb1 177.2(3) . . . . ? O7 N6 O8 Tb1 -2.9(4) . . . . ? O2 Tb1 O8 N6 21.9(2) . . . . ? O3 Tb1 O8 N6 -67.9(2) . . . . ? O5 Tb1 O8 N6 142.2(2) . . . . ? O1 Tb1 O8 N6 120.3(2) . . . . ? O4 Tb1 O8 N6 87.9(2) . . . . ? O11 Tb1 O8 N6 -148.1(2) . . . . ? O7 Tb1 O8 N6 1.7(2) . . . . ? O10 Tb1 O8 N6 -144.7(2) . . . . ? N1 Tb1 O8 N6 -63.1(3) . . . . ? N5 Tb1 O8 N6 115.3(2) . . . . ? O12 N7 O10 Tb1 173.0(4) . . . . ? O11 N7 O10 Tb1 -6.0(3) . . . . ? O2 Tb1 O10 N7 111.7(4) . . . . ? O3 Tb1 O10 N7 96.7(2) . . . . ? O5 Tb1 O10 N7 -88.9(2) . . . . ? O1 Tb1 O10 N7 -29.0(3) . . . . ? O4 Tb1 O10 N7 -115.8(2) . . . . ? O11 Tb1 O10 N7 3.6(2) . . . . ? O7 Tb1 O10 N7 161.7(2) . . . . ? O8 Tb1 O10 N7 -172.2(3) . . . . ? N1 Tb1 O10 N7 40.7(2) . . . . ? N5 Tb1 O10 N7 -102.6(2) . . . . ? N6 Tb1 O10 N7 173.5(2) . . . . ? O12 N7 O11 Tb1 -172.5(4) . . . . ? O10 N7 O11 Tb1 6.5(4) . . . . ? O2 Tb1 O11 N7 -167.2(2) . . . . ? O3 Tb1 O11 N7 -80.8(2) . . . . ? O5 Tb1 O11 N7 67.8(2) . . . . ? O1 Tb1 O11 N7 145.9(2) . . . . ? O4 Tb1 O11 N7 86.6(3) . . . . ? O7 Tb1 O11 N7 -46.6(3) . . . . ? O8 Tb1 O11 N7 0.3(3) . . . . ? O10 Tb1 O11 N7 -3.7(2) . . . . ? N1 Tb1 O11 N7 -146.4(3) . . . . ? N5 Tb1 O11 N7 75.6(2) . . . . ? N6 Tb1 O11 N7 -17.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.812 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.083