# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 #TrackingRef '- complexes.cif' _database_code_depnum_ccdc_archive 'CCDC 832847' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H74 Br6 Eu2 N6 O26 S2' _chemical_formula_weight 2334.90 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 12.839(4) _cell_length_b 12.860(4) _cell_length_c 16.021(5) _cell_angle_alpha 76.149(4) _cell_angle_beta 87.883(4) _cell_angle_gamma 88.339(4) _cell_volume 2566.0(14) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2145 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 20.22 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1148 _exptl_absorpt_coefficient_mu 3.653 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.361 _exptl_absorpt_correction_T_max 0.448 _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 '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 18846 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.1230 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.30 _reflns_number_total 9169 _reflns_number_gt 5896 _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. ; _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^)+(0.0778P)^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 9169 _refine_ls_number_parameters 525 _refine_ls_number_restraints 219 _refine_ls_R_factor_all 0.1028 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1567 _refine_ls_wR_factor_gt 0.1417 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O12 O 0.6920(5) -0.2735(5) 1.0273(4) 0.0493(17) Uani 1 1 d D . . C33 C 0.7508(8) -0.2743(8) 0.9678(7) 0.059(3) Uani 1 1 d D . . H33 H 0.7510 -0.2135 0.9227 0.071 Uiso 1 1 calc R . . N2 N 0.8182(7) -0.3568(7) 0.9598(7) 0.071(3) Uani 1 1 d D . . C34 C 0.8805(11) -0.3537(11) 0.8809(11) 0.131(7) Uani 1 1 d D . . H34A H 0.8818 -0.4232 0.8686 0.197 Uiso 1 1 calc R . . H34B H 0.9503 -0.3335 0.8883 0.197 Uiso 1 1 calc R . . H34C H 0.8502 -0.3023 0.8340 0.197 Uiso 1 1 calc R . . C35 C 0.8206(12) -0.4511(10) 1.0271(10) 0.125(6) Uani 1 1 d D . . H35A H 0.7697 -0.4446 1.0711 0.187 Uiso 1 1 calc R . . H35B H 0.8887 -0.4609 1.0510 0.187 Uiso 1 1 calc R . . H35C H 0.8051 -0.5117 1.0048 0.187 Uiso 1 1 calc R . . O13 O 0.5635(5) -0.2872(5) 1.1776(4) 0.0544(17) Uani 1 1 d DU . . C36 C 0.6314(10) -0.3464(10) 1.2134(9) 0.103(3) Uani 1 1 d DU . . H36 H 0.7005 -0.3357 1.1943 0.124 Uiso 1 1 calc R . . N3 N 0.6053(11) -0.4359(10) 1.2873(8) 0.121(4) Uani 1 1 d DU . . C37 C 0.6951(16) -0.5002(16) 1.3241(14) 0.196(8) Uani 1 1 d DU . . H37A H 0.7556 -0.4563 1.3155 0.294 Uiso 1 1 calc R . . H37B H 0.7067 -0.5582 1.2965 0.294 Uiso 1 1 calc R . . H37C H 0.6821 -0.5284 1.3846 0.294 Uiso 1 1 calc R . . C38 C 0.4987(12) -0.4301(13) 1.3064(10) 0.123(5) Uani 1 1 d DU . . H38A H 0.4649 -0.4893 1.2928 0.184 Uiso 1 1 calc R . . H38B H 0.4699 -0.3641 1.2731 0.184 Uiso 1 1 calc R . . H38C H 0.4879 -0.4330 1.3665 0.184 Uiso 1 1 calc R . . C23 C 0.8586(4) -0.0080(4) 1.1558(3) 0.0308(19) Uani 1 1 d G . . C18 C 0.9323(4) 0.0544(4) 1.1022(2) 0.033(2) Uani 1 1 d G . . C19 C 1.0127(4) 0.0985(4) 1.1372(3) 0.041(2) Uani 1 1 d G . . H19 H 1.0620 0.1402 1.1013 0.049 Uiso 1 1 calc R . . C20 C 1.0194(4) 0.0801(4) 1.2260(4) 0.046(3) Uani 1 1 d G . . H20 H 1.0732 0.1096 1.2495 0.055 Uiso 1 1 calc R . . C21 C 0.9457(5) 0.0177(5) 1.2797(3) 0.044(2) Uani 1 1 d G . . C22 C 0.8653(4) -0.0264(4) 1.2446(3) 0.045(2) Uani 1 1 d G . . H22 H 0.8160 -0.0681 1.2805 0.054 Uiso 1 1 calc R . . C31 C 0.6560(6) 0.1821(6) 1.1096(5) 0.0311(19) Uani 1 1 d . . . C26 C 0.7397(7) 0.2477(6) 1.0871(5) 0.0309(19) Uani 1 1 d . . . C27 C 0.7941(7) 0.2761(7) 1.1512(6) 0.040(2) Uani 1 1 d . . . H27 H 0.8508 0.3208 1.1359 0.048 Uiso 1 1 calc R . . C28 C 0.7668(8) 0.2404(8) 1.2358(7) 0.051(3) Uani 1 1 d . . . H28 H 0.8030 0.2617 1.2778 0.062 Uiso 1 1 calc R . . C29 C 0.6823(8) 0.1703(8) 1.2586(6) 0.048(3) Uani 1 1 d . . . C30 C 0.6298(7) 0.1412(7) 1.1962(6) 0.040(2) Uani 1 1 d . . . H30 H 0.5756 0.0932 1.2114 0.047 Uiso 1 1 calc R . . C5 C 0.9686(10) 0.3670(10) 0.6863(8) 0.077(2) Uani 1 1 d U . . C4 C 0.8822(10) 0.4193(10) 0.6481(9) 0.087(3) Uani 1 1 d U . . H4 H 0.8346 0.4547 0.6774 0.105 Uiso 1 1 calc R . . C3 C 0.8688(11) 0.4162(11) 0.5571(9) 0.093(3) Uani 1 1 d U . . H3 H 0.8136 0.4525 0.5261 0.111 Uiso 1 1 calc R . . C2 C 0.9398(11) 0.3588(11) 0.5206(9) 0.088(2) Uani 1 1 d U . . C7 C 1.0148(11) 0.3113(11) 0.5592(9) 0.092(3) Uani 1 1 d U . . H7 H 1.0606 0.2742 0.5298 0.111 Uiso 1 1 calc R . . C6 C 1.0358(11) 0.3097(11) 0.6454(9) 0.087(2) Uani 1 1 d U . . H6 H 1.0925 0.2715 0.6729 0.105 Uiso 1 1 calc R . . Eu1 Eu 0.58963(3) -0.12697(3) 1.06006(3) 0.02550(14) Uani 1 1 d . . . Br2 Br 0.94632(9) 0.00281(12) 1.39933(7) 0.0772(4) Uani 1 1 d . . . S1 S 0.99605(19) 0.37637(19) 0.79051(16) 0.0457(6) Uani 1 1 d . . . O4 O 0.9171(4) 0.0815(4) 1.0161(4) 0.0399(15) Uani 1 1 d . . . O3 O 0.7757(4) 0.1846(4) 0.7836(3) 0.0344(14) Uani 1 1 d . . . O11 O 0.5699(4) 0.0622(4) 1.0420(3) 0.0305(13) Uani 1 1 d . . . O9 O 0.6974(5) -0.0995(5) 1.1758(4) 0.0453(16) Uani 1 1 d . . . O6 O 0.6389(4) -0.0652(4) 0.9100(3) 0.0356(14) Uani 1 1 d . . . O8 O 0.7698(4) -0.0668(5) 1.0473(4) 0.0436(16) Uani 1 1 d . . . C8 C 0.8731(6) 0.2245(6) 0.8968(5) 0.0283(19) Uani 1 1 d . . . C10 C 0.7530(6) 0.1130(6) 0.7355(5) 0.0314(19) Uani 1 1 d . . . O7 O 0.5623(4) 0.0945(4) 0.8560(4) 0.0372(14) Uani 1 1 d . . . O2 O 1.0047(5) 0.4875(5) 0.7863(4) 0.0599(19) Uani 1 1 d . . . C14 C 0.6683(7) -0.0456(7) 0.7209(5) 0.036(2) Uani 1 1 d . . . H14 H 0.6254 -0.1034 0.7431 0.043 Uiso 1 1 calc R . . C9 C 0.8641(6) 0.1518(6) 0.8375(5) 0.032(2) Uani 1 1 d . . . H9A H 0.9272 0.1543 0.8020 0.039 Uiso 1 1 calc R . . H9B H 0.8555 0.0787 0.8707 0.039 Uiso 1 1 calc R . . C15 C 0.6846(6) 0.0301(6) 0.7690(5) 0.0293(19) Uani 1 1 d . . . N1 N 0.8970(5) 0.3374(5) 0.8539(4) 0.0361(17) Uani 1 1 d . . . H1 H 0.8544 0.3862 0.8637 0.043 Uiso 1 1 calc R . . C24 C 0.7712(7) -0.0619(6) 1.1236(6) 0.034(2) Uani 1 1 d . . . C17 C 0.9563(7) 0.1790(6) 0.9653(6) 0.038(2) Uani 1 1 d . . . H17A H 1.0223 0.1665 0.9375 0.045 Uiso 1 1 calc R . . H17B H 0.9669 0.2290 1.0008 0.045 Uiso 1 1 calc R . . C25 C 0.7662(6) 0.2279(6) 0.9435(5) 0.0311(19) Uani 1 1 d . . . H25A H 0.7139 0.2593 0.9021 0.037 Uiso 1 1 calc R . . H25B H 0.7455 0.1558 0.9717 0.037 Uiso 1 1 calc R . . C32 C 0.5829(6) 0.1572(6) 1.0454(5) 0.0293(19) Uani 1 1 d . . . O10 O 0.5341(4) 0.2331(4) 0.9986(4) 0.0345(14) Uani 1 1 d . . . C11 C 0.7974(7) 0.1221(7) 0.6559(6) 0.042(2) Uani 1 1 d . . . H11 H 0.8415 0.1790 0.6339 0.050 Uiso 1 1 calc R . . Br3 Br 0.64413(12) 0.11814(13) 1.37539(7) 0.0945(5) Uani 1 1 d . . . O1 O 1.0820(5) 0.3056(5) 0.8180(5) 0.064(2) Uani 1 1 d . . . O5 O 0.7731(4) 0.2907(4) 1.0062(4) 0.0390(15) Uani 1 1 d . . . C1 C 0.9116(13) 0.3526(13) 0.4287(10) 0.127(4) Uani 1 1 d U . . H1A H 0.8642 0.4104 0.4051 0.190 Uiso 1 1 calc R . . H1B H 0.8793 0.2855 0.4311 0.190 Uiso 1 1 calc R . . H1C H 0.9738 0.3582 0.3929 0.190 Uiso 1 1 calc R . . C12 C 0.7799(8) 0.0503(8) 0.6060(6) 0.051(3) Uani 1 1 d . . . H12 H 0.8101 0.0589 0.5512 0.062 Uiso 1 1 calc R . . C13 C 0.7160(8) -0.0344(8) 0.6408(5) 0.047(2) Uani 1 1 d . . . Br1 Br 0.69285(13) -0.13765(12) 0.57781(9) 0.0958(5) Uani 1 1 d . . . C16 C 0.6233(7) 0.0196(7) 0.8520(5) 0.033(2) 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 O12 0.051(4) 0.037(4) 0.064(5) -0.024(3) 0.018(4) 0.008(3) C33 0.056(7) 0.037(6) 0.092(9) -0.029(6) -0.007(7) 0.003(5) N2 0.048(6) 0.045(5) 0.128(9) -0.038(6) 0.020(6) -0.009(4) C34 0.080(10) 0.104(11) 0.23(2) -0.095(13) 0.089(12) -0.021(9) C35 0.141(14) 0.064(9) 0.173(17) -0.032(10) -0.067(13) 0.044(9) O13 0.069(4) 0.036(3) 0.055(4) -0.005(3) -0.013(3) 0.012(3) C36 0.112(6) 0.096(6) 0.098(6) -0.013(5) -0.006(5) -0.004(5) N3 0.131(6) 0.116(6) 0.115(6) -0.023(5) -0.026(6) 0.020(6) C37 0.205(11) 0.187(10) 0.188(10) -0.032(8) -0.015(8) 0.014(8) C38 0.144(9) 0.131(8) 0.108(8) -0.053(7) 0.002(7) -0.039(7) C23 0.024(4) 0.037(5) 0.033(5) -0.010(4) -0.004(4) 0.003(4) C18 0.038(5) 0.028(5) 0.034(5) -0.009(4) -0.006(4) 0.007(4) C19 0.031(5) 0.036(5) 0.053(6) -0.001(4) -0.016(4) -0.005(4) C20 0.041(6) 0.045(6) 0.053(6) -0.011(5) -0.026(5) 0.003(5) C21 0.043(6) 0.061(6) 0.030(5) -0.015(5) -0.016(4) 0.005(5) C22 0.045(6) 0.049(6) 0.040(6) -0.011(5) 0.000(5) -0.002(5) C31 0.037(5) 0.034(5) 0.025(5) -0.014(4) -0.003(4) 0.008(4) C26 0.040(5) 0.022(4) 0.031(5) -0.008(4) -0.002(4) 0.005(4) C27 0.036(5) 0.047(6) 0.041(6) -0.021(5) 0.003(4) -0.006(4) C28 0.046(6) 0.057(6) 0.063(7) -0.036(6) -0.013(5) 0.011(5) C29 0.061(7) 0.057(6) 0.032(5) -0.020(5) -0.014(5) 0.018(5) C30 0.037(5) 0.041(5) 0.041(6) -0.011(4) -0.006(4) 0.001(4) C5 0.078(3) 0.077(3) 0.077(3) -0.0189(11) -0.0020(10) -0.0019(10) C4 0.088(3) 0.087(3) 0.087(3) -0.0211(11) -0.0026(10) -0.0023(10) C3 0.093(3) 0.092(3) 0.092(3) -0.0212(11) -0.0034(10) -0.0022(10) C2 0.088(3) 0.088(3) 0.087(3) -0.0208(11) -0.0024(10) -0.0023(10) C7 0.092(3) 0.092(3) 0.092(3) -0.0222(11) -0.0024(10) -0.0025(10) C6 0.087(3) 0.087(3) 0.087(3) -0.0207(11) -0.0022(10) -0.0023(10) Eu1 0.0283(2) 0.0226(2) 0.0249(2) -0.00473(16) -0.00043(17) 0.00126(16) Br2 0.0619(8) 0.1398(12) 0.0380(6) -0.0359(7) -0.0103(6) 0.0011(8) S1 0.0436(15) 0.0424(14) 0.0485(15) -0.0061(12) 0.0072(12) -0.0089(12) O4 0.045(4) 0.039(3) 0.033(3) 0.000(3) -0.007(3) -0.015(3) O3 0.034(3) 0.037(3) 0.032(3) -0.007(3) -0.001(3) 0.001(3) O11 0.030(3) 0.031(3) 0.034(3) -0.015(3) -0.002(3) 0.005(2) O9 0.040(4) 0.052(4) 0.043(4) -0.009(3) -0.006(3) -0.006(3) O6 0.044(4) 0.034(3) 0.027(3) -0.005(3) 0.003(3) 0.007(3) O8 0.037(4) 0.054(4) 0.043(4) -0.018(3) -0.001(3) -0.012(3) C8 0.030(5) 0.027(4) 0.026(4) -0.002(4) -0.001(4) -0.004(4) C10 0.031(5) 0.035(5) 0.027(5) -0.003(4) -0.002(4) 0.003(4) O7 0.039(4) 0.034(3) 0.035(3) -0.005(3) 0.016(3) 0.007(3) O2 0.070(5) 0.043(4) 0.065(5) -0.010(3) 0.017(4) -0.021(4) C14 0.051(6) 0.043(5) 0.015(4) -0.011(4) 0.005(4) -0.005(4) C9 0.033(5) 0.033(5) 0.033(5) -0.011(4) 0.002(4) -0.002(4) C15 0.034(5) 0.032(5) 0.020(4) -0.004(4) 0.002(4) 0.004(4) N1 0.040(4) 0.027(4) 0.041(4) -0.009(3) 0.002(4) -0.002(3) C24 0.034(5) 0.029(5) 0.039(6) -0.004(4) -0.012(4) 0.008(4) C17 0.035(5) 0.030(5) 0.044(6) 0.001(4) -0.010(4) -0.002(4) C25 0.034(5) 0.032(5) 0.029(5) -0.011(4) 0.000(4) 0.003(4) C32 0.030(5) 0.027(5) 0.029(5) -0.005(4) 0.005(4) 0.005(4) O10 0.038(3) 0.024(3) 0.041(4) -0.005(3) -0.009(3) 0.001(3) C11 0.048(6) 0.041(5) 0.034(5) -0.005(4) 0.007(4) -0.006(4) Br3 0.1106(11) 0.1404(13) 0.0301(6) -0.0148(7) 0.0024(7) -0.0149(10) O1 0.039(4) 0.062(5) 0.080(5) 0.002(4) 0.016(4) -0.002(4) O5 0.046(4) 0.040(3) 0.037(4) -0.021(3) 0.017(3) -0.015(3) C1 0.127(4) 0.127(4) 0.126(4) -0.0300(14) -0.0038(10) -0.0032(10) C12 0.058(7) 0.073(7) 0.027(5) -0.021(5) 0.020(5) -0.021(6) C13 0.061(7) 0.060(6) 0.023(5) -0.017(5) 0.000(5) -0.015(5) Br1 0.1321(13) 0.1085(11) 0.0689(9) -0.0643(8) 0.0276(8) -0.0416(10) C16 0.034(5) 0.038(5) 0.028(5) -0.012(4) 0.003(4) -0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _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 0.500 0.500 0.314 600 174 ' ' _platon_squeeze_details ; ; 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 O12 C33 1.196(10) . ? O12 Eu1 2.415(6) . ? C33 N2 1.376(11) . ? N2 C35 1.417(13) . ? N2 C34 1.464(14) . ? O13 C36 1.208(8) . ? O13 Eu1 2.457(6) . ? C36 N3 1.476(14) . ? N3 C38 1.396(15) . ? N3 C37 1.456(16) . ? C23 C18 1.3900 . ? C23 C22 1.3900 . ? C23 C24 1.504(9) . ? C18 O4 1.359(6) . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C21 Br2 1.881(4) . ? C31 C26 1.368(11) . ? C31 C30 1.392(11) . ? C31 C32 1.514(11) . ? C26 O5 1.341(9) . ? C26 C27 1.387(11) . ? C27 C28 1.359(13) . ? C28 C29 1.411(13) . ? C29 C30 1.355(12) . ? C29 Br3 1.882(10) . ? C5 C4 1.367(16) . ? C5 C6 1.367(16) . ? C5 S1 1.752(13) . ? C4 C3 1.484(17) . ? C3 C2 1.359(17) . ? C2 C7 1.230(16) . ? C2 C1 1.550(18) . ? C7 C6 1.411(17) . ? Eu1 O11 2.387(5) . ? Eu1 O6 2.412(5) . ? Eu1 O7 2.412(6) 2_657 ? Eu1 O8 2.446(6) . ? Eu1 O9 2.451(6) . ? Eu1 O10 2.474(5) 2_657 ? Eu1 O11 2.657(5) 2_657 ? Eu1 C32 2.925(8) 2_657 ? S1 O2 1.422(6) . ? S1 O1 1.424(7) . ? S1 N1 1.611(7) . ? O4 C17 1.415(9) . ? O3 C10 1.379(9) . ? O3 C9 1.442(9) . ? O11 C32 1.253(9) . ? O11 Eu1 2.657(5) 2_657 ? O9 C24 1.267(10) . ? O6 C16 1.268(9) . ? O8 C24 1.241(10) . ? C8 N1 1.486(9) . ? C8 C9 1.493(10) . ? C8 C25 1.543(11) . ? C8 C17 1.559(10) . ? C10 C11 1.357(11) . ? C10 C15 1.393(11) . ? O7 C16 1.235(9) . ? O7 Eu1 2.412(6) 2_657 ? C14 C13 1.379(11) . ? C14 C15 1.403(11) . ? C15 C16 1.500(11) . ? C25 O5 1.438(9) . ? C32 O10 1.247(9) . ? C32 Eu1 2.925(8) 2_657 ? O10 Eu1 2.474(5) 2_657 ? C11 C12 1.386(12) . ? C12 C13 1.377(12) . ? C13 Br1 1.886(9) . ? 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 C33 O12 Eu1 129.6(7) . . ? O12 C33 N2 126.2(10) . . ? C33 N2 C35 118.8(10) . . ? C33 N2 C34 121.9(11) . . ? C35 N2 C34 119.1(10) . . ? C36 O13 Eu1 125.9(8) . . ? O13 C36 N3 120.3(12) . . ? C38 N3 C37 137.1(15) . . ? C38 N3 C36 108.5(11) . . ? C37 N3 C36 114.1(13) . . ? C18 C23 C22 120.0 . . ? C18 C23 C24 123.6(5) . . ? C22 C23 C24 116.4(5) . . ? O4 C18 C23 118.7(4) . . ? O4 C18 C19 120.8(4) . . ? C23 C18 C19 120.0 . . ? C18 C19 C20 120.0 . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C22 C21 Br2 119.3(3) . . ? C20 C21 Br2 120.5(3) . . ? C21 C22 C23 120.0 . . ? C26 C31 C30 119.8(7) . . ? C26 C31 C32 123.6(7) . . ? C30 C31 C32 116.4(7) . . ? O5 C26 C31 125.2(7) . . ? O5 C26 C27 115.8(8) . . ? C31 C26 C27 119.1(8) . . ? C28 C27 C26 121.8(9) . . ? C27 C28 C29 118.7(9) . . ? C30 C29 C28 119.7(9) . . ? C30 C29 Br3 120.8(8) . . ? C28 C29 Br3 119.5(7) . . ? C29 C30 C31 120.9(9) . . ? C4 C5 C6 122.4(13) . . ? C4 C5 S1 118.8(11) . . ? C6 C5 S1 118.8(10) . . ? C5 C4 C3 116.0(13) . . ? C2 C3 C4 118.0(13) . . ? C7 C2 C3 122.8(16) . . ? C7 C2 C1 123.9(15) . . ? C3 C2 C1 113.1(13) . . ? C2 C7 C6 124.0(16) . . ? C5 C6 C7 116.7(13) . . ? O11 Eu1 O6 79.29(18) . . ? O11 Eu1 O7 72.40(18) . 2_657 ? O6 Eu1 O7 132.81(18) . 2_657 ? O11 Eu1 O12 147.1(2) . . ? O6 Eu1 O12 75.6(2) . . ? O7 Eu1 O12 140.4(2) 2_657 . ? O11 Eu1 O8 76.95(19) . . ? O6 Eu1 O8 70.8(2) . . ? O7 Eu1 O8 134.3(2) 2_657 . ? O12 Eu1 O8 74.9(2) . . ? O11 Eu1 O9 79.28(19) . . ? O6 Eu1 O9 122.7(2) . . ? O7 Eu1 O9 88.3(2) 2_657 . ? O12 Eu1 O9 96.8(2) . . ? O8 Eu1 O9 52.8(2) . . ? O11 Eu1 O13 136.5(2) . . ? O6 Eu1 O13 144.2(2) . . ? O7 Eu1 O13 72.2(2) 2_657 . ? O12 Eu1 O13 71.3(2) . . ? O8 Eu1 O13 112.4(2) . . ? O9 Eu1 O13 75.3(2) . . ? O11 Eu1 O10 122.52(17) . 2_657 ? O6 Eu1 O10 81.95(19) . 2_657 ? O7 Eu1 O10 82.5(2) 2_657 2_657 ? O12 Eu1 O10 74.6(2) . 2_657 ? O8 Eu1 O10 143.1(2) . 2_657 ? O9 Eu1 O10 151.63(19) . 2_657 ? O13 Eu1 O10 76.4(2) . 2_657 ? O11 Eu1 O11 72.60(18) . 2_657 ? O6 Eu1 O11 65.87(18) . 2_657 ? O7 Eu1 O11 69.97(18) 2_657 2_657 ? O12 Eu1 O11 114.6(2) . 2_657 ? O8 Eu1 O11 130.45(18) . 2_657 ? O9 Eu1 O11 148.47(19) . 2_657 ? O13 Eu1 O11 116.7(2) . 2_657 ? O10 Eu1 O11 50.17(16) 2_657 2_657 ? O11 Eu1 C32 98.0(2) . 2_657 ? O6 Eu1 C32 70.5(2) . 2_657 ? O7 Eu1 C32 76.9(2) 2_657 2_657 ? O12 Eu1 C32 93.4(2) . 2_657 ? O8 Eu1 C32 141.2(2) . 2_657 ? O9 Eu1 C32 165.1(2) . 2_657 ? O13 Eu1 C32 97.8(2) . 2_657 ? O10 Eu1 C32 24.97(18) 2_657 2_657 ? O11 Eu1 C32 25.36(18) 2_657 2_657 ? O11 Eu1 Eu1 38.55(12) . 2_657 ? O6 Eu1 Eu1 67.91(13) . 2_657 ? O7 Eu1 Eu1 66.35(13) 2_657 2_657 ? O12 Eu1 Eu1 139.87(16) . 2_657 ? O8 Eu1 Eu1 106.93(15) . 2_657 ? O9 Eu1 Eu1 116.59(15) . 2_657 ? O13 Eu1 Eu1 135.98(16) . 2_657 ? O10 Eu1 Eu1 84.09(12) 2_657 2_657 ? O11 Eu1 Eu1 34.04(11) 2_657 2_657 ? C32 Eu1 Eu1 59.40(16) 2_657 2_657 ? O2 S1 O1 119.6(4) . . ? O2 S1 N1 105.6(4) . . ? O1 S1 N1 108.7(4) . . ? O2 S1 C5 106.1(5) . . ? O1 S1 C5 107.0(6) . . ? N1 S1 C5 109.5(5) . . ? C18 O4 C17 119.9(6) . . ? C10 O3 C9 113.4(6) . . ? C32 O11 Eu1 163.2(5) . . ? C32 O11 Eu1 89.4(5) . 2_657 ? Eu1 O11 Eu1 107.40(18) . 2_657 ? C24 O9 Eu1 92.4(5) . . ? C16 O6 Eu1 135.5(5) . . ? C24 O8 Eu1 93.3(5) . . ? N1 C8 C9 115.0(7) . . ? N1 C8 C25 106.1(6) . . ? C9 C8 C25 107.3(6) . . ? N1 C8 C17 109.5(6) . . ? C9 C8 C17 110.1(7) . . ? C25 C8 C17 108.6(7) . . ? C11 C10 O3 120.5(8) . . ? C11 C10 C15 119.8(8) . . ? O3 C10 C15 119.8(7) . . ? C16 O7 Eu1 138.3(5) . 2_657 ? C13 C14 C15 120.0(8) . . ? O3 C9 C8 109.8(6) . . ? C10 C15 C14 118.4(8) . . ? C10 C15 C16 123.8(7) . . ? C14 C15 C16 117.7(7) . . ? C8 N1 S1 125.7(6) . . ? O8 C24 O9 120.6(8) . . ? O8 C24 C23 121.0(8) . . ? O9 C24 C23 118.4(7) . . ? O4 C17 C8 106.5(6) . . ? O5 C25 C8 109.5(6) . . ? O10 C32 O11 121.5(7) . . ? O10 C32 C31 118.2(7) . . ? O11 C32 C31 120.2(7) . . ? O10 C32 Eu1 56.9(4) . 2_657 ? O11 C32 Eu1 65.3(4) . 2_657 ? C31 C32 Eu1 168.8(5) . 2_657 ? C32 O10 Eu1 98.2(5) . 2_657 ? C10 C11 C12 122.8(8) . . ? C26 O5 C25 118.2(6) . . ? C13 C12 C11 117.4(8) . . ? C12 C13 C14 121.5(8) . . ? C12 C13 Br1 119.5(7) . . ? C14 C13 Br1 119.0(7) . . ? O7 C16 O6 127.2(8) . . ? O7 C16 C15 116.1(7) . . ? O6 C16 C15 116.7(7) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.30 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.608 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.159 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 #TrackingRef '- complexes.cif' _database_code_depnum_ccdc_archive 'CCDC 832848' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H74 Br6 Gd2 N6 O26 S2' _chemical_formula_weight 2345.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.838(2) _cell_length_b 12.867(2) _cell_length_c 16.039(3) _cell_angle_alpha 76.149(2) _cell_angle_beta 87.850(2) _cell_angle_gamma 88.362(2) _cell_volume 2570.0(7) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3322 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 21.82 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1150 _exptl_absorpt_coefficient_mu 3.718 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.539 _exptl_absorpt_correction_T_max 0.658 _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 '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 17141 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0924 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.20 _reflns_number_total 9098 _reflns_number_gt 6460 _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. ; _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^)+(0.0363P)^2^+0.6302P] 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 9098 _refine_ls_number_parameters 575 _refine_ls_number_restraints 816 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0846 _refine_ls_goodness_of_fit_ref 0.903 _refine_ls_restrained_S_all 0.893 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.58956(2) 0.37334(2) 0.559713(17) 0.02401(9) Uani 1 1 d U . . Br1 Br 0.30706(8) 0.63823(8) 0.92180(5) 0.0949(3) Uani 1 1 d U . . Br2 Br 0.05410(6) 0.49822(8) 0.10052(5) 0.0769(3) Uani 1 1 d U . . Br3 Br 0.35611(7) 0.38295(8) 0.12438(5) 0.0946(3) Uani 1 1 d U . . C1 C 0.0884(9) 0.1468(9) 1.0712(6) 0.148(4) Uani 1 1 d U . . H1A H 0.1191 0.2144 1.0697 0.222 Uiso 1 1 calc R . . H1B H 0.1361 0.0898 1.0957 0.222 Uiso 1 1 calc R . . H1C H 0.0250 0.1400 1.1055 0.222 Uiso 1 1 calc R . . C2 C 0.0644(9) 0.1405(8) 0.9793(6) 0.092(2) Uani 1 1 d U . . C3 C 0.1333(8) 0.0829(7) 0.9399(6) 0.096(2) Uani 1 1 d U . . H3 H 0.1902 0.0474 0.9690 0.115 Uiso 1 1 calc R . . C4 C 0.1166(7) 0.0780(6) 0.8544(5) 0.077(2) Uani 1 1 d U . . H4 H 0.1620 0.0393 0.8261 0.093 Uiso 1 1 calc R . . C5 C 0.0308(6) 0.1324(5) 0.8137(4) 0.0569(17) Uani 1 1 d U . . C6 C -0.0356(6) 0.1873(6) 0.8562(5) 0.079(2) Uani 1 1 d U . . H6 H -0.0934 0.2232 0.8287 0.095 Uiso 1 1 calc R . . C7 C -0.0174(8) 0.1900(7) 0.9429(6) 0.095(2) Uani 1 1 d U . . H7 H -0.0632 0.2266 0.9726 0.114 Uiso 1 1 calc R . . C8 C 0.1279(4) 0.2756(4) 0.6028(3) 0.0276(12) Uani 1 1 d U . . C9 C 0.1350(4) 0.3493(4) 0.6630(3) 0.0330(13) Uani 1 1 d U . . H9A H 0.1428 0.4227 0.6303 0.040 Uiso 1 1 calc R . . H9B H 0.0720 0.3455 0.6988 0.040 Uiso 1 1 calc R . . C10 C 0.2467(4) 0.3883(4) 0.7643(3) 0.0317(13) Uani 1 1 d U . . C11 C 0.2004(5) 0.3777(5) 0.8443(4) 0.0432(15) Uani 1 1 d U . . H11 H 0.1553 0.3218 0.8663 0.052 Uiso 1 1 calc R . . C12 C 0.2214(5) 0.4508(5) 0.8921(4) 0.0500(17) Uani 1 1 d U . . H12 H 0.1925 0.4426 0.9473 0.060 Uiso 1 1 calc R . . C13 C 0.2844(5) 0.5347(5) 0.8578(4) 0.0425(15) Uani 1 1 d U . . C14 C 0.3316(4) 0.5464(5) 0.7784(3) 0.0384(14) Uani 1 1 d U . . H14 H 0.3744 0.6042 0.7561 0.046 Uiso 1 1 calc R . . C15 C 0.3149(4) 0.4712(4) 0.7313(3) 0.0286(12) Uani 1 1 d U . . C16 C 0.3768(4) 0.4800(4) 0.6481(3) 0.0283(12) Uani 1 1 d U . . C17 C 0.0438(4) 0.3205(4) 0.5362(3) 0.0336(13) Uani 1 1 d U . . H17A H 0.0315 0.2702 0.5014 0.040 Uiso 1 1 calc R . . H17B H -0.0214 0.3337 0.5650 0.040 Uiso 1 1 calc R . . C18 C 0.0695(4) 0.4427(4) 0.3980(4) 0.0330(13) Uani 1 1 d U . . C19 C -0.0125(4) 0.4035(4) 0.3605(4) 0.0402(15) Uani 1 1 d U . . H19 H -0.0637 0.3642 0.3959 0.048 Uiso 1 1 calc R . . C20 C -0.0199(5) 0.4212(5) 0.2727(4) 0.0428(15) Uani 1 1 d U . . H20 H -0.0742 0.3932 0.2487 0.051 Uiso 1 1 calc R . . C21 C 0.0559(5) 0.4820(5) 0.2214(4) 0.0429(15) Uani 1 1 d U . . C22 C 0.1341(4) 0.5272(5) 0.2566(4) 0.0387(14) Uani 1 1 d U . . H22 H 0.1826 0.5701 0.2206 0.046 Uiso 1 1 calc R . . C23 C 0.1417(4) 0.5099(4) 0.3444(3) 0.0280(12) Uani 1 1 d U . . C24 C 0.2300(4) 0.5617(4) 0.3766(4) 0.0305(13) Uani 1 1 d U . . C25 C 0.2331(4) 0.2719(4) 0.5573(3) 0.0332(13) Uani 1 1 d U . . H25A H 0.2539 0.3440 0.5291 0.040 Uiso 1 1 calc R . . H25B H 0.2851 0.2407 0.5989 0.040 Uiso 1 1 calc R . . C26 C 0.2596(4) 0.2516(4) 0.4120(3) 0.0310(13) Uani 1 1 d U . . C27 C 0.2067(4) 0.2233(5) 0.3477(4) 0.0382(14) Uani 1 1 d U . . H27 H 0.1503 0.1779 0.3624 0.046 Uiso 1 1 calc R . . C28 C 0.2349(5) 0.2601(5) 0.2628(4) 0.0503(17) Uani 1 1 d U . . H28 H 0.1996 0.2385 0.2205 0.060 Uiso 1 1 calc R . . C29 C 0.3168(5) 0.3301(5) 0.2411(3) 0.0422(15) Uani 1 1 d U . . C30 C 0.3705(4) 0.3601(4) 0.3044(3) 0.0351(14) Uani 1 1 d U . . H30 H 0.4243 0.4085 0.2890 0.042 Uiso 1 1 calc R . . C31 C 0.3455(4) 0.3194(4) 0.3895(3) 0.0265(12) Uani 1 1 d U . . C32 C 0.4175(4) 0.3425(4) 0.4557(3) 0.0253(12) Uani 1 1 d U . . C33 C 0.7515(5) 0.2253(5) 0.4678(5) 0.0579(18) Uani 1 1 d U . . H33 H 0.7523 0.2861 0.4226 0.069 Uiso 1 1 calc R . . C34 C 0.8775(7) 0.1477(7) 0.3820(6) 0.113(3) Uani 1 1 d U . . H34A H 0.8575 0.2098 0.3387 0.170 Uiso 1 1 calc R . . H34B H 0.8655 0.0844 0.3622 0.170 Uiso 1 1 calc R . . H34C H 0.9501 0.1510 0.3932 0.170 Uiso 1 1 calc R . . C35 C 0.8219(7) 0.0514(7) 0.5275(6) 0.106(3) Uani 1 1 d U . . H35A H 0.7775 0.0607 0.5748 0.160 Uiso 1 1 calc R . . H35B H 0.8925 0.0393 0.5458 0.160 Uiso 1 1 calc R . . H35C H 0.7994 -0.0089 0.5079 0.160 Uiso 1 1 calc R . . C36A C 0.6329(10) 0.1556(8) 0.7122(7) 0.053(3) Uani 0.616(8) 1 d PU A 1 H36A H 0.6950 0.1716 0.6777 0.063 Uiso 0.616(8) 1 d PR A 1 C37A C 0.7061(12) 0.0026(11) 0.8174(9) 0.110(5) Uani 0.616(8) 1 d PU A 1 H37A H 0.6908 -0.0709 0.8204 0.166 Uiso 0.616(8) 1 calc PR A 1 H37B H 0.7178 0.0114 0.8740 0.166 Uiso 0.616(8) 1 calc PR A 1 H37C H 0.7675 0.0223 0.7816 0.166 Uiso 0.616(8) 1 calc PR A 1 C38A C 0.5157(17) 0.0513(19) 0.8098(15) 0.100(6) Uani 0.616(8) 1 d PU A 1 H38A H 0.4685 0.0979 0.7723 0.150 Uiso 0.616(8) 1 calc PR A 1 H38B H 0.5074 0.0630 0.8666 0.150 Uiso 0.616(8) 1 calc PR A 1 H38C H 0.5008 -0.0218 0.8113 0.150 Uiso 0.616(8) 1 calc PR A 1 C36B C 0.4935(16) 0.1854(14) 0.7244(11) 0.057(5) Uani 0.384(8) 1 d PU A 2 H36B H 0.4297 0.2264 0.7106 0.069 Uiso 0.384(8) 1 d PR A 2 C37B C 0.398(2) 0.066(2) 0.8437(16) 0.120(9) Uani 0.384(8) 1 d PU A 2 H37D H 0.3682 0.1268 0.8615 0.180 Uiso 0.384(8) 1 d PR A 2 H37E H 0.4167 0.0115 0.8934 0.180 Uiso 0.384(8) 1 d PR A 2 H37F H 0.3489 0.0387 0.8114 0.180 Uiso 0.384(8) 1 d PR A 2 C38B C 0.578(3) 0.026(3) 0.819(2) 0.114(9) Uani 0.384(8) 1 d PU A 2 H38D H 0.6389 0.0611 0.7898 0.171 Uiso 0.384(8) 1 calc PR A 2 H38E H 0.5678 -0.0386 0.8005 0.171 Uiso 0.384(8) 1 calc PR A 2 H38F H 0.5870 0.0093 0.8796 0.171 Uiso 0.384(8) 1 calc PR A 2 N1 N 0.1019(3) 0.1627(3) 0.6460(3) 0.0355(11) Uani 1 1 d U . . H1 H 0.1440 0.1137 0.6358 0.043 Uiso 1 1 calc R . . N2 N 0.8163(4) 0.1445(4) 0.4599(4) 0.0650(17) Uani 1 1 d U . . N3A N 0.6162(10) 0.0726(8) 0.7799(7) 0.065(3) Uani 0.616(8) 1 d PU A 1 N3B N 0.4819(19) 0.1012(18) 0.7963(15) 0.075(6) Uani 0.384(8) 1 d PU A 2 O1 O -0.0831(3) 0.1944(4) 0.6821(3) 0.0627(13) Uani 1 1 d U . . O2 O -0.0053(3) 0.0118(3) 0.7138(3) 0.0578(12) Uani 1 1 d U . . O3 O 0.2243(3) 0.3159(3) 0.7161(2) 0.0338(9) Uani 1 1 d U . . O4 O 0.0832(3) 0.4185(3) 0.4837(2) 0.0389(10) Uani 1 1 d U . . O5 O 0.2267(3) 0.2090(3) 0.4950(2) 0.0380(10) Uani 1 1 d U . . O6 O 0.3621(3) 0.5655(3) 0.5909(2) 0.0348(9) Uani 1 1 d U . . O7 O 0.4388(3) 0.4044(3) 0.6440(2) 0.0353(9) Uani 1 1 d U . . O8 O 0.2304(3) 0.5665(3) 0.4532(2) 0.0414(10) Uani 1 1 d U . . O9 O 0.3035(3) 0.6002(3) 0.3246(2) 0.0415(10) Uani 1 1 d U . . O10 O 0.4660(3) 0.2661(3) 0.5013(2) 0.0347(9) Uani 1 1 d U . . O11 O 0.4303(3) 0.4386(3) 0.4590(2) 0.0293(8) Uani 1 1 d U . . O12 O 0.6927(3) 0.2274(3) 0.5269(3) 0.0460(11) Uani 1 1 d U . . O13 O 0.5657(4) 0.2151(3) 0.6746(3) 0.0484(11) Uani 1 1 d U . . S1 S 0.00337(13) 0.12305(13) 0.70956(10) 0.0445(4) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.02491(15) 0.02101(14) 0.02559(15) -0.00468(10) -0.00086(10) 0.00093(11) Br1 0.1292(8) 0.1061(7) 0.0714(6) -0.0646(5) 0.0267(5) -0.0424(6) Br2 0.0621(5) 0.1342(8) 0.0418(4) -0.0347(5) -0.0108(4) 0.0016(5) Br3 0.1116(7) 0.1400(8) 0.0306(4) -0.0160(5) 0.0007(4) -0.0151(6) C1 0.194(7) 0.143(7) 0.109(6) -0.027(5) -0.004(6) -0.052(6) C2 0.118(5) 0.089(5) 0.067(4) -0.010(4) 0.007(4) -0.038(4) C3 0.117(5) 0.083(4) 0.079(4) 0.002(4) -0.016(4) -0.017(4) C4 0.099(5) 0.068(4) 0.065(4) -0.013(3) -0.009(4) -0.009(4) C5 0.074(4) 0.044(3) 0.050(4) -0.008(3) 0.012(3) -0.012(3) C6 0.091(4) 0.079(4) 0.067(4) -0.019(4) 0.028(4) -0.018(4) C7 0.112(5) 0.097(5) 0.079(4) -0.026(4) 0.029(4) -0.027(4) C8 0.027(3) 0.023(3) 0.030(3) -0.002(2) 0.004(2) 0.000(2) C9 0.033(3) 0.035(3) 0.032(3) -0.009(3) -0.009(2) 0.001(3) C10 0.029(3) 0.037(3) 0.029(3) -0.008(3) 0.003(2) -0.002(3) C11 0.045(4) 0.048(4) 0.034(3) -0.007(3) 0.014(3) -0.013(3) C12 0.051(4) 0.070(4) 0.032(3) -0.019(3) 0.015(3) -0.008(4) C13 0.050(4) 0.050(4) 0.032(3) -0.018(3) 0.006(3) -0.010(3) C14 0.042(4) 0.037(3) 0.038(3) -0.012(3) 0.006(3) -0.006(3) C15 0.031(3) 0.030(3) 0.024(3) -0.006(2) 0.005(2) 0.005(2) C16 0.023(3) 0.032(3) 0.031(3) -0.009(3) 0.002(2) -0.010(3) C17 0.025(3) 0.033(3) 0.042(3) -0.007(3) -0.002(2) -0.009(3) C18 0.034(3) 0.031(3) 0.037(3) -0.013(3) -0.012(3) 0.007(3) C19 0.035(3) 0.036(3) 0.049(4) -0.006(3) -0.010(3) -0.001(3) C20 0.040(4) 0.043(4) 0.050(4) -0.017(3) -0.020(3) 0.001(3) C21 0.034(4) 0.060(4) 0.037(4) -0.017(3) -0.011(3) 0.004(3) C22 0.027(3) 0.051(4) 0.038(3) -0.010(3) -0.001(3) -0.003(3) C23 0.027(3) 0.025(3) 0.032(3) -0.006(2) -0.006(2) 0.003(2) C24 0.032(3) 0.025(3) 0.035(3) -0.007(3) -0.010(3) 0.007(3) C25 0.035(3) 0.030(3) 0.036(3) -0.010(3) 0.004(3) -0.005(3) C26 0.032(3) 0.024(3) 0.038(3) -0.011(2) -0.001(3) 0.006(3) C27 0.033(3) 0.043(4) 0.046(4) -0.023(3) -0.006(3) -0.003(3) C28 0.048(4) 0.060(4) 0.051(4) -0.028(3) -0.012(3) -0.001(3) C29 0.052(4) 0.051(4) 0.025(3) -0.015(3) -0.005(3) 0.016(3) C30 0.030(3) 0.041(3) 0.034(3) -0.008(3) 0.002(3) 0.001(3) C31 0.026(3) 0.023(3) 0.031(3) -0.011(2) 0.000(2) 0.009(2) C32 0.020(3) 0.026(3) 0.029(3) -0.007(2) 0.008(2) -0.003(2) C33 0.047(4) 0.037(4) 0.091(5) -0.021(4) 0.004(4) 0.001(3) C34 0.102(6) 0.100(6) 0.153(7) -0.064(5) 0.038(5) -0.009(5) C35 0.108(6) 0.078(5) 0.135(7) -0.028(5) -0.023(5) 0.025(5) C36A 0.089(8) 0.029(5) 0.039(6) -0.003(4) -0.007(5) -0.005(5) C37A 0.136(12) 0.081(9) 0.101(10) 0.003(8) -0.016(9) 0.029(9) C38A 0.124(13) 0.090(12) 0.087(10) -0.023(10) -0.014(11) -0.008(11) C36B 0.075(10) 0.044(8) 0.049(9) -0.001(7) -0.012(8) -0.010(8) C37B 0.106(14) 0.133(15) 0.106(14) 0.003(12) -0.008(12) -0.023(13) C38B 0.120(15) 0.108(14) 0.111(14) -0.020(12) -0.011(13) -0.006(13) N1 0.034(3) 0.027(3) 0.043(3) -0.006(2) 0.008(2) -0.001(2) N2 0.047(4) 0.045(3) 0.112(5) -0.040(3) 0.015(3) 0.003(3) N3A 0.098(8) 0.040(6) 0.051(6) 0.000(5) -0.003(6) 0.000(6) N3B 0.091(11) 0.066(10) 0.063(10) 0.000(9) -0.016(9) 0.002(9) O1 0.036(3) 0.065(3) 0.077(3) 0.002(3) 0.014(2) 0.002(2) O2 0.070(3) 0.039(3) 0.063(3) -0.009(2) 0.014(2) -0.021(2) O3 0.036(2) 0.033(2) 0.033(2) -0.0092(18) -0.0023(17) -0.0023(18) O4 0.048(3) 0.031(2) 0.037(2) -0.0048(18) -0.0092(19) -0.0087(19) O5 0.045(2) 0.035(2) 0.039(2) -0.0186(19) 0.0104(18) -0.0134(19) O6 0.035(2) 0.037(2) 0.028(2) -0.0013(18) 0.0052(17) 0.0055(19) O7 0.039(2) 0.028(2) 0.035(2) -0.0021(17) 0.0129(17) 0.0078(18) O8 0.033(2) 0.056(3) 0.038(2) -0.017(2) 0.0013(18) -0.009(2) O9 0.035(2) 0.053(3) 0.033(2) -0.0008(19) -0.0032(19) -0.008(2) O10 0.035(2) 0.023(2) 0.048(2) -0.0114(18) -0.0153(18) 0.0062(18) O11 0.031(2) 0.022(2) 0.037(2) -0.0108(16) 0.0011(16) -0.0026(17) O12 0.045(3) 0.033(2) 0.061(3) -0.015(2) 0.011(2) 0.006(2) O13 0.057(3) 0.037(2) 0.043(3) 0.008(2) -0.001(2) 0.001(2) S1 0.0427(10) 0.0394(10) 0.0486(10) -0.0057(8) 0.0101(8) -0.0107(8) _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_ _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 0.393 0.756 1.014 168 35 ' ' 2 0.607 0.243 -0.014 167 35 ' ' 3 0.500 1.000 0.500 548 29 ' ' _platon_squeeze_details ; ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O11 2.374(3) 2_666 ? Gd1 O7 2.399(3) . ? Gd1 O13 2.415(4) . ? Gd1 O12 2.415(4) . ? Gd1 O6 2.418(3) 2_666 ? Gd1 O9 2.442(4) 2_666 ? Gd1 O8 2.444(4) 2_666 ? Gd1 O10 2.480(3) . ? Gd1 O11 2.645(3) . ? Gd1 C24 2.794(5) 2_666 ? Gd1 Gd1 4.0613(7) 2_666 ? Br1 C13 1.900(6) . ? Br2 C21 1.901(6) . ? Br3 C29 1.887(6) . ? C1 C2 1.538(11) . ? C2 C7 1.296(11) . ? C2 C3 1.370(12) . ? C3 C4 1.413(10) . ? C4 C5 1.386(9) . ? C5 C6 1.358(9) . ? C5 S1 1.753(7) . ? C6 C7 1.427(10) . ? C8 N1 1.493(6) . ? C8 C9 1.515(7) . ? C8 C25 1.515(7) . ? C8 C17 1.548(7) . ? C9 O3 1.446(6) . ? C10 C11 1.371(7) . ? C10 O3 1.388(6) . ? C10 C15 1.390(7) . ? C11 C12 1.386(8) . ? C12 C13 1.361(8) . ? C13 C14 1.367(7) . ? C14 C15 1.388(7) . ? C15 C16 1.509(7) . ? C16 O7 1.251(6) . ? C16 O6 1.268(6) . ? C17 O4 1.432(6) . ? C18 O4 1.352(6) . ? C18 C19 1.395(7) . ? C18 C23 1.406(7) . ? C19 C20 1.379(7) . ? C20 C21 1.383(8) . ? C21 C22 1.378(7) . ? C22 C23 1.379(7) . ? C23 C24 1.499(7) . ? C24 O8 1.245(6) . ? C24 O9 1.266(6) . ? C24 Gd1 2.794(5) 2_666 ? C25 O5 1.435(6) . ? C26 O5 1.368(6) . ? C26 C27 1.381(7) . ? C26 C31 1.407(7) . ? C27 C28 1.368(8) . ? C28 C29 1.384(8) . ? C29 C30 1.381(7) . ? C30 C31 1.369(7) . ? C31 C32 1.521(7) . ? C32 O10 1.242(6) . ? C32 O11 1.265(6) . ? C33 O12 1.194(7) . ? C33 N2 1.341(7) . ? C34 N2 1.443(9) . ? C35 N2 1.412(9) . ? C36A O13 1.213(11) . ? C36A N3A 1.344(13) . ? C37A N3A 1.497(17) . ? C38A N3A 1.37(2) . ? C36B O13 1.209(19) . ? C36B N3B 1.39(3) . ? C37B N3B 1.32(3) . ? C38B N3B 1.54(4) . ? N1 S1 1.610(4) . ? O1 S1 1.434(4) . ? O2 S1 1.424(4) . ? O6 Gd1 2.418(3) 2_666 ? O8 Gd1 2.444(4) 2_666 ? O9 Gd1 2.442(4) 2_666 ? O11 Gd1 2.374(3) 2_666 ? 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 O11 Gd1 O7 72.80(11) 2_666 . ? O11 Gd1 O13 137.22(13) 2_666 . ? O7 Gd1 O13 72.44(14) . . ? O11 Gd1 O12 146.82(13) 2_666 . ? O7 Gd1 O12 140.33(13) . . ? O13 Gd1 O12 70.86(14) . . ? O11 Gd1 O6 79.29(12) 2_666 2_666 ? O7 Gd1 O6 133.05(12) . 2_666 ? O13 Gd1 O6 143.47(13) . 2_666 ? O12 Gd1 O6 75.45(13) . 2_666 ? O11 Gd1 O9 79.80(12) 2_666 2_666 ? O7 Gd1 O9 87.96(13) . 2_666 ? O13 Gd1 O9 74.82(14) . 2_666 ? O12 Gd1 O9 96.53(13) . 2_666 ? O6 Gd1 O9 123.47(12) 2_666 2_666 ? O11 Gd1 O8 77.05(12) 2_666 2_666 ? O7 Gd1 O8 134.33(13) . 2_666 ? O13 Gd1 O8 111.90(14) . 2_666 ? O12 Gd1 O8 74.67(13) . 2_666 ? O6 Gd1 O8 71.17(12) 2_666 2_666 ? O9 Gd1 O8 53.12(12) 2_666 2_666 ? O11 Gd1 O10 122.57(11) 2_666 . ? O7 Gd1 O10 82.65(12) . . ? O13 Gd1 O10 76.28(13) . . ? O12 Gd1 O10 74.56(12) . . ? O6 Gd1 O10 81.59(12) 2_666 . ? O9 Gd1 O10 151.09(12) 2_666 . ? O8 Gd1 O10 142.99(12) 2_666 . ? O11 Gd1 O11 72.08(12) 2_666 . ? O7 Gd1 O11 70.02(11) . . ? O13 Gd1 O11 117.16(13) . . ? O12 Gd1 O11 115.10(12) . . ? O6 Gd1 O11 65.78(11) 2_666 . ? O9 Gd1 O11 148.23(12) 2_666 . ? O8 Gd1 O11 130.47(12) 2_666 . ? O10 Gd1 O11 50.70(10) . . ? O11 Gd1 C24 74.46(13) 2_666 2_666 ? O7 Gd1 C24 110.76(15) . 2_666 ? O13 Gd1 C24 95.54(16) . 2_666 ? O12 Gd1 C24 87.39(14) . 2_666 ? O6 Gd1 C24 96.66(15) 2_666 2_666 ? O9 Gd1 C24 26.92(13) 2_666 2_666 ? O8 Gd1 C24 26.43(13) 2_666 2_666 ? O10 Gd1 C24 161.75(13) . 2_666 ? O11 Gd1 C24 144.48(13) . 2_666 ? O11 Gd1 Gd1 38.29(8) 2_666 2_666 ? O7 Gd1 Gd1 66.71(8) . 2_666 ? O13 Gd1 Gd1 136.58(11) . 2_666 ? O12 Gd1 Gd1 139.95(10) . 2_666 ? O6 Gd1 Gd1 67.93(8) 2_666 2_666 ? O9 Gd1 Gd1 116.75(9) 2_666 2_666 ? O8 Gd1 Gd1 106.96(9) 2_666 2_666 ? O10 Gd1 Gd1 84.39(8) . 2_666 ? O11 Gd1 Gd1 33.80(7) . 2_666 ? C24 Gd1 Gd1 111.93(10) 2_666 2_666 ? C7 C2 C3 123.5(10) . . ? C7 C2 C1 119.5(10) . . ? C3 C2 C1 117.0(10) . . ? C2 C3 C4 119.1(9) . . ? C5 C4 C3 118.2(8) . . ? C6 C5 C4 120.2(7) . . ? C6 C5 S1 119.9(6) . . ? C4 C5 S1 119.8(6) . . ? C5 C6 C7 120.4(9) . . ? C2 C7 C6 118.6(9) . . ? N1 C8 C9 114.5(4) . . ? N1 C8 C25 106.8(4) . . ? C9 C8 C25 108.3(4) . . ? N1 C8 C17 108.4(4) . . ? C9 C8 C17 108.9(4) . . ? C25 C8 C17 109.9(4) . . ? O3 C9 C8 108.3(4) . . ? C11 C10 O3 119.4(5) . . ? C11 C10 C15 120.5(5) . . ? O3 C10 C15 120.1(5) . . ? C10 C11 C12 119.6(6) . . ? C13 C12 C11 119.6(5) . . ? C12 C13 C14 121.6(5) . . ? C12 C13 Br1 119.3(4) . . ? C14 C13 Br1 119.1(5) . . ? C13 C14 C15 119.4(5) . . ? C14 C15 C10 119.2(5) . . ? C14 C15 C16 118.0(5) . . ? C10 C15 C16 122.8(5) . . ? O7 C16 O6 127.3(5) . . ? O7 C16 C15 117.0(5) . . ? O6 C16 C15 115.7(5) . . ? O4 C17 C8 106.4(4) . . ? O4 C18 C19 123.1(5) . . ? O4 C18 C23 118.2(5) . . ? C19 C18 C23 118.7(5) . . ? C20 C19 C18 122.1(6) . . ? C19 C20 C21 117.8(5) . . ? C22 C21 C20 121.2(6) . . ? C22 C21 Br2 119.9(5) . . ? C20 C21 Br2 118.8(4) . . ? C21 C22 C23 121.0(5) . . ? C22 C23 C18 118.8(5) . . ? C22 C23 C24 117.2(5) . . ? C18 C23 C24 124.0(5) . . ? O8 C24 O9 121.0(5) . . ? O8 C24 C23 120.3(5) . . ? O9 C24 C23 118.8(5) . . ? O8 C24 Gd1 60.9(3) . 2_666 ? O9 C24 Gd1 60.9(3) . 2_666 ? C23 C24 Gd1 170.9(3) . 2_666 ? O5 C25 C8 109.6(4) . . ? O5 C26 C27 117.4(5) . . ? O5 C26 C31 123.6(5) . . ? C27 C26 C31 118.9(5) . . ? C28 C27 C26 121.8(6) . . ? C27 C28 C29 118.9(5) . . ? C30 C29 C28 120.4(6) . . ? C30 C29 Br3 120.1(5) . . ? C28 C29 Br3 119.5(4) . . ? C31 C30 C29 120.8(6) . . ? C30 C31 C26 119.1(5) . . ? C30 C31 C32 118.1(5) . . ? C26 C31 C32 122.6(5) . . ? O10 C32 O11 122.6(5) . . ? O10 C32 C31 118.2(4) . . ? O11 C32 C31 119.1(5) . . ? O12 C33 N2 126.7(7) . . ? O13 C36A N3A 125.3(11) . . ? O13 C36B N3B 133.1(19) . . ? C8 N1 S1 126.9(3) . . ? C33 N2 C35 119.6(7) . . ? C33 N2 C34 121.6(7) . . ? C35 N2 C34 118.7(7) . . ? C36A N3A C38A 118.5(15) . . ? C36A N3A C37A 119.5(12) . . ? C38A N3A C37A 121.8(15) . . ? C37B N3B C36B 131(2) . . ? C37B N3B C38B 113(3) . . ? C36B N3B C38B 116(2) . . ? C10 O3 C9 112.4(4) . . ? C18 O4 C17 119.7(4) . . ? C26 O5 C25 119.2(4) . . ? C16 O6 Gd1 135.0(3) . 2_666 ? C16 O7 Gd1 138.0(3) . . ? C24 O8 Gd1 92.7(3) . 2_666 ? C24 O9 Gd1 92.2(3) . 2_666 ? C32 O10 Gd1 97.2(3) . . ? C32 O11 Gd1 163.2(3) . 2_666 ? C32 O11 Gd1 88.9(3) . . ? Gd1 O11 Gd1 107.92(12) 2_666 . ? C33 O12 Gd1 130.5(4) . . ? C36B O13 C36A 98.3(11) . . ? C36B O13 Gd1 132.1(9) . . ? C36A O13 Gd1 127.5(6) . . ? O2 S1 O1 119.8(3) . . ? O2 S1 N1 105.9(2) . . ? O1 S1 N1 108.3(2) . . ? O2 S1 C5 106.0(3) . . ? O1 S1 C5 107.0(3) . . ? N1 S1 C5 109.6(3) . . ? 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 C7 C2 C3 C4 1.3(14) . . . . ? C1 C2 C3 C4 -177.8(8) . . . . ? C2 C3 C4 C5 0.2(12) . . . . ? C3 C4 C5 C6 -1.0(11) . . . . ? C3 C4 C5 S1 -176.8(6) . . . . ? C4 C5 C6 C7 0.5(11) . . . . ? S1 C5 C6 C7 176.2(6) . . . . ? C3 C2 C7 C6 -1.9(14) . . . . ? C1 C2 C7 C6 177.2(7) . . . . ? C5 C6 C7 C2 1.0(13) . . . . ? N1 C8 C9 O3 67.3(5) . . . . ? C25 C8 C9 O3 -51.8(5) . . . . ? C17 C8 C9 O3 -171.2(4) . . . . ? O3 C10 C11 C12 -179.1(5) . . . . ? C15 C10 C11 C12 0.6(9) . . . . ? C10 C11 C12 C13 2.5(9) . . . . ? C11 C12 C13 C14 -2.9(10) . . . . ? C11 C12 C13 Br1 177.0(5) . . . . ? C12 C13 C14 C15 0.1(9) . . . . ? Br1 C13 C14 C15 -179.8(4) . . . . ? C13 C14 C15 C10 3.0(8) . . . . ? C13 C14 C15 C16 -173.7(5) . . . . ? C11 C10 C15 C14 -3.3(8) . . . . ? O3 C10 C15 C14 176.3(5) . . . . ? C11 C10 C15 C16 173.2(5) . . . . ? O3 C10 C15 C16 -7.2(8) . . . . ? C14 C15 C16 O7 116.2(6) . . . . ? C10 C15 C16 O7 -60.4(7) . . . . ? C14 C15 C16 O6 -61.7(7) . . . . ? C10 C15 C16 O6 121.7(6) . . . . ? N1 C8 C17 O4 -167.5(4) . . . . ? C9 C8 C17 O4 67.3(5) . . . . ? C25 C8 C17 O4 -51.2(5) . . . . ? O4 C18 C19 C20 -174.1(5) . . . . ? C23 C18 C19 C20 5.5(8) . . . . ? C18 C19 C20 C21 -1.5(8) . . . . ? C19 C20 C21 C22 -2.6(9) . . . . ? C19 C20 C21 Br2 175.0(4) . . . . ? C20 C21 C22 C23 2.5(9) . . . . ? Br2 C21 C22 C23 -175.0(4) . . . . ? C21 C22 C23 C18 1.6(8) . . . . ? C21 C22 C23 C24 179.5(5) . . . . ? O4 C18 C23 C22 174.1(5) . . . . ? C19 C18 C23 C22 -5.5(7) . . . . ? O4 C18 C23 C24 -3.6(7) . . . . ? C19 C18 C23 C24 176.8(5) . . . . ? C22 C23 C24 O8 166.4(5) . . . . ? C18 C23 C24 O8 -15.9(8) . . . . ? C22 C23 C24 O9 -13.5(7) . . . . ? C18 C23 C24 O9 164.2(5) . . . . ? C22 C23 C24 Gd1 -99(3) . . . 2_666 ? C18 C23 C24 Gd1 79(3) . . . 2_666 ? N1 C8 C25 O5 60.5(5) . . . . ? C9 C8 C25 O5 -175.7(4) . . . . ? C17 C8 C25 O5 -56.8(5) . . . . ? O5 C26 C27 C28 -178.8(5) . . . . ? C31 C26 C27 C28 -0.6(8) . . . . ? C26 C27 C28 C29 -1.9(9) . . . . ? C27 C28 C29 C30 1.5(9) . . . . ? C27 C28 C29 Br3 -179.4(4) . . . . ? C28 C29 C30 C31 1.6(8) . . . . ? Br3 C29 C30 C31 -177.5(4) . . . . ? C29 C30 C31 C26 -4.1(7) . . . . ? C29 C30 C31 C32 171.1(5) . . . . ? O5 C26 C31 C30 -178.3(4) . . . . ? C27 C26 C31 C30 3.6(7) . . . . ? O5 C26 C31 C32 6.7(7) . . . . ? C27 C26 C31 C32 -171.3(5) . . . . ? C30 C31 C32 O10 -114.3(5) . . . . ? C26 C31 C32 O10 60.6(6) . . . . ? C30 C31 C32 O11 61.7(6) . . . . ? C26 C31 C32 O11 -123.4(5) . . . . ? C9 C8 N1 S1 54.5(6) . . . . ? C25 C8 N1 S1 174.4(4) . . . . ? C17 C8 N1 S1 -67.3(5) . . . . ? O12 C33 N2 C35 -2.4(11) . . . . ? O12 C33 N2 C34 174.6(7) . . . . ? O13 C36A N3A C38A 1(2) . . . . ? O13 C36A N3A C37A 177.0(10) . . . . ? O13 C36B N3B C37B -173(2) . . . . ? O13 C36B N3B C38B -2(4) . . . . ? C11 C10 O3 C9 89.2(6) . . . . ? C15 C10 O3 C9 -90.5(6) . . . . ? C8 C9 O3 C10 170.8(4) . . . . ? C19 C18 O4 C17 26.2(7) . . . . ? C23 C18 O4 C17 -153.4(5) . . . . ? C8 C17 O4 C18 139.5(4) . . . . ? C27 C26 O5 C25 -145.8(5) . . . . ? C31 C26 O5 C25 36.1(7) . . . . ? C8 C25 O5 C26 127.4(5) . . . . ? O7 C16 O6 Gd1 12.8(8) . . . 2_666 ? C15 C16 O6 Gd1 -169.6(3) . . . 2_666 ? O6 C16 O7 Gd1 17.6(9) . . . . ? C15 C16 O7 Gd1 -160.0(4) . . . . ? O11 Gd1 O7 C16 18.7(5) 2_666 . . . ? O13 Gd1 O7 C16 173.3(5) . . . . ? O12 Gd1 O7 C16 -163.6(5) . . . . ? O6 Gd1 O7 C16 -37.6(6) 2_666 . . . ? O9 Gd1 O7 C16 98.6(5) 2_666 . . . ? O8 Gd1 O7 C16 69.6(5) 2_666 . . . ? O10 Gd1 O7 C16 -108.8(5) . . . . ? O11 Gd1 O7 C16 -58.0(5) . . . . ? C24 Gd1 O7 C16 84.0(5) 2_666 . . . ? Gd1 Gd1 O7 C16 -21.8(5) 2_666 . . . ? O9 C24 O8 Gd1 -10.4(5) . . . 2_666 ? C23 C24 O8 Gd1 169.7(4) . . . 2_666 ? O8 C24 O9 Gd1 10.5(5) . . . 2_666 ? C23 C24 O9 Gd1 -169.7(4) . . . 2_666 ? O11 C32 O10 Gd1 -9.0(5) . . . . ? C31 C32 O10 Gd1 166.9(4) . . . . ? O11 Gd1 O10 C32 10.7(3) 2_666 . . . ? O7 Gd1 O10 C32 74.8(3) . . . . ? O13 Gd1 O10 C32 148.4(3) . . . . ? O12 Gd1 O10 C32 -138.0(3) . . . . ? O6 Gd1 O10 C32 -60.8(3) 2_666 . . . ? O9 Gd1 O10 C32 146.9(3) 2_666 . . . ? O8 Gd1 O10 C32 -103.3(3) 2_666 . . . ? O11 Gd1 O10 C32 4.6(3) . . . . ? C24 Gd1 O10 C32 -146.6(4) 2_666 . . . ? Gd1 Gd1 O10 C32 7.6(3) 2_666 . . . ? O10 C32 O11 Gd1 -169.1(8) . . . 2_666 ? C31 C32 O11 Gd1 15.1(14) . . . 2_666 ? O10 C32 O11 Gd1 8.3(5) . . . . ? C31 C32 O11 Gd1 -167.5(4) . . . . ? O11 Gd1 O11 C32 -179.2(3) 2_666 . . . ? O7 Gd1 O11 C32 -101.5(3) . . . . ? O13 Gd1 O11 C32 -44.7(3) . . . . ? O12 Gd1 O11 C32 35.7(3) . . . . ? O6 Gd1 O11 C32 94.7(3) 2_666 . . . ? O9 Gd1 O11 C32 -150.3(3) 2_666 . . . ? O8 Gd1 O11 C32 126.6(3) 2_666 . . . ? O10 Gd1 O11 C32 -4.5(3) . . . . ? C24 Gd1 O11 C32 160.4(3) 2_666 . . . ? Gd1 Gd1 O11 C32 -179.2(3) 2_666 . . . ? O11 Gd1 O11 Gd1 0.0 2_666 . . 2_666 ? O7 Gd1 O11 Gd1 77.69(14) . . . 2_666 ? O13 Gd1 O11 Gd1 134.52(14) . . . 2_666 ? O12 Gd1 O11 Gd1 -145.07(13) . . . 2_666 ? O6 Gd1 O11 Gd1 -86.06(14) 2_666 . . 2_666 ? O9 Gd1 O11 Gd1 28.9(3) 2_666 . . 2_666 ? O8 Gd1 O11 Gd1 -54.17(18) 2_666 . . 2_666 ? O10 Gd1 O11 Gd1 174.7(2) . . . 2_666 ? C24 Gd1 O11 Gd1 -20.4(3) 2_666 . . 2_666 ? N2 C33 O12 Gd1 170.5(5) . . . . ? O11 Gd1 O12 C33 -24.4(7) 2_666 . . . ? O7 Gd1 O12 C33 159.6(5) . . . . ? O13 Gd1 O12 C33 -177.1(6) . . . . ? O6 Gd1 O12 C33 17.2(6) 2_666 . . . ? O9 Gd1 O12 C33 -105.7(6) 2_666 . . . ? O8 Gd1 O12 C33 -56.8(6) 2_666 . . . ? O10 Gd1 O12 C33 102.4(6) . . . . ? O11 Gd1 O12 C33 71.1(6) . . . . ? C24 Gd1 O12 C33 -80.3(6) 2_666 . . . ? Gd1 Gd1 O12 C33 41.5(6) 2_666 . . . ? N3B C36B O13 C36A -8(2) . . . . ? N3B C36B O13 Gd1 -171.9(17) . . . . ? N3A C36A O13 C36B 9.9(14) . . . . ? N3A C36A O13 Gd1 175.0(8) . . . . ? O11 Gd1 O13 C36B 50.6(12) 2_666 . . . ? O7 Gd1 O13 C36B 13.6(12) . . . . ? O12 Gd1 O13 C36B -151.1(12) . . . . ? O6 Gd1 O13 C36B -127.3(12) 2_666 . . . ? O9 Gd1 O13 C36B 106.3(12) 2_666 . . . ? O8 Gd1 O13 C36B 145.1(12) 2_666 . . . ? O10 Gd1 O13 C36B -72.9(12) . . . . ? O11 Gd1 O13 C36B -42.0(12) . . . . ? C24 Gd1 O13 C36B 123.7(12) 2_666 . . . ? Gd1 Gd1 O13 C36B -6.8(12) 2_666 . . . ? O11 Gd1 O13 C36A -109.3(7) 2_666 . . . ? O7 Gd1 O13 C36A -146.3(7) . . . . ? O12 Gd1 O13 C36A 49.1(7) . . . . ? O6 Gd1 O13 C36A 72.8(7) 2_666 . . . ? O9 Gd1 O13 C36A -53.6(7) 2_666 . . . ? O8 Gd1 O13 C36A -14.8(7) 2_666 . . . ? O10 Gd1 O13 C36A 127.2(7) . . . . ? O11 Gd1 O13 C36A 158.1(7) . . . . ? C24 Gd1 O13 C36A -36.2(7) 2_666 . . . ? Gd1 Gd1 O13 C36A -166.6(6) 2_666 . . . ? C8 N1 S1 O2 163.3(4) . . . . ? C8 N1 S1 O1 33.7(5) . . . . ? C8 N1 S1 C5 -82.7(5) . . . . ? C6 C5 S1 O2 -119.7(6) . . . . ? C4 C5 S1 O2 56.1(6) . . . . ? C6 C5 S1 O1 9.2(7) . . . . ? C4 C5 S1 O1 -175.0(5) . . . . ? C6 C5 S1 N1 126.4(6) . . . . ? C4 C5 S1 N1 -57.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.899 _refine_diff_density_min -0.938 _refine_diff_density_rms 0.112 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 #TrackingRef '- complexes.cif' _database_code_depnum_ccdc_archive 'CCDC 832849' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H74 Br6 N6 O26 S2 Tb2' _chemical_formula_weight 2348.82 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.818(2) _cell_length_b 12.868(2) _cell_length_c 16.038(3) _cell_angle_alpha 76.169(2) _cell_angle_beta 87.766(2) _cell_angle_gamma 88.385(2) _cell_volume 2566.1(7) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3972 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 22.66 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 3.809 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.332 _exptl_absorpt_correction_T_max 0.433 _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 '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 18184 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0751 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.10 _reflns_number_total 9034 _reflns_number_gt 6781 _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. ; _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^)+(0.1000P)^2^+0.8067P] 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 9034 _refine_ls_number_parameters 537 _refine_ls_number_restraints 276 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1380 _refine_ls_wR_factor_gt 0.1280 _refine_ls_goodness_of_fit_ref 0.858 _refine_ls_restrained_S_all 0.863 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.91067(2) 0.62641(2) 0.440681(19) 0.02291(11) Uani 1 1 d . . . Br1 Br 0.80682(10) 0.63912(10) 0.92103(7) 0.0912(4) Uani 1 1 d . . . Br2 Br 0.55509(7) 0.49943(10) 0.10037(6) 0.0730(3) Uani 1 1 d . . . Br3 Br 0.85618(10) 0.38434(11) 0.12382(6) 0.0907(4) Uani 1 1 d . . . C1 C 0.5868(11) 0.1484(11) 1.0708(9) 0.120(4) Uani 1 1 d U . . H1A H 0.6079 0.2197 1.0699 0.181 Uiso 1 1 calc R . . H1B H 0.6427 0.0987 1.0910 0.181 Uiso 1 1 calc R . . H1C H 0.5265 0.1308 1.1085 0.181 Uiso 1 1 calc R . . C2 C 0.5595(9) 0.1420(9) 0.9787(7) 0.080(2) Uani 1 1 d U . . C3 C 0.6311(9) 0.0842(9) 0.9404(8) 0.086(2) Uani 1 1 d U . . H3 H 0.6875 0.0490 0.9704 0.104 Uiso 1 1 calc R . . C4 C 0.6160(8) 0.0799(9) 0.8528(7) 0.079(2) Uani 1 1 d U . . H4 H 0.6623 0.0424 0.8241 0.095 Uiso 1 1 calc R . . C5 C 0.5307(7) 0.1334(7) 0.8136(6) 0.0622(19) Uani 1 1 d U . . C6 C 0.4615(8) 0.1880(8) 0.8558(7) 0.076(2) Uani 1 1 d U . . H6 H 0.4030 0.2230 0.8289 0.091 Uiso 1 1 calc R . . C7 C 0.4819(9) 0.1892(9) 0.9411(8) 0.084(2) Uani 1 1 d U . . H7 H 0.4361 0.2265 0.9704 0.101 Uiso 1 1 calc R . . C8 C 0.6267(5) 0.2746(5) 0.6031(4) 0.0286(14) Uani 1 1 d . . . C9 C 0.6361(5) 0.3478(5) 0.6637(4) 0.0281(14) Uani 1 1 d . . . H9A H 0.6445 0.4211 0.6310 0.034 Uiso 1 1 calc R . . H9B H 0.5731 0.3448 0.6997 0.034 Uiso 1 1 calc R . . C10 C 0.7481(5) 0.3879(5) 0.7642(4) 0.0304(15) Uani 1 1 d . . . C11 C 0.7014(6) 0.3778(6) 0.8444(5) 0.0417(18) Uani 1 1 d . . . H11 H 0.6563 0.3216 0.8658 0.050 Uiso 1 1 calc R . . C12 C 0.7199(6) 0.4489(7) 0.8933(5) 0.055(2) Uani 1 1 d . . . H12 H 0.6910 0.4394 0.9486 0.066 Uiso 1 1 calc R . . C13 C 0.7830(6) 0.5351(7) 0.8582(5) 0.0458(19) Uani 1 1 d . . . C14 C 0.8318(5) 0.5452(6) 0.7775(4) 0.0373(17) Uani 1 1 d . . . H14 H 0.8754 0.6026 0.7553 0.045 Uiso 1 1 calc R . . C15 C 0.8158(5) 0.4707(5) 0.7307(4) 0.0288(14) Uani 1 1 d . . . C16 C 0.8770(5) 0.4797(5) 0.6459(4) 0.0268(14) Uani 1 1 d . . . C17 C 0.5442(5) 0.3192(5) 0.5354(4) 0.0344(16) Uani 1 1 d . . . H17A H 0.5342 0.2693 0.4998 0.041 Uiso 1 1 calc R . . H17B H 0.4778 0.3308 0.5633 0.041 Uiso 1 1 calc R . . C18 C 0.5692(5) 0.4432(5) 0.3973(4) 0.0316(15) Uani 1 1 d . . . C19 C 0.4873(5) 0.4041(5) 0.3616(5) 0.0377(17) Uani 1 1 d . . . H19 H 0.4360 0.3649 0.3972 0.045 Uiso 1 1 calc R . . C20 C 0.4802(6) 0.4225(6) 0.2726(5) 0.0416(18) Uani 1 1 d . . . H20 H 0.4251 0.3956 0.2486 0.050 Uiso 1 1 calc R . . C21 C 0.5563(6) 0.4811(6) 0.2213(5) 0.0413(18) Uani 1 1 d . . . C22 C 0.6348(5) 0.5268(6) 0.2563(5) 0.0390(17) Uani 1 1 d . . . H22 H 0.6830 0.5699 0.2200 0.047 Uiso 1 1 calc R . . C23 C 0.6431(5) 0.5097(5) 0.3441(4) 0.0297(15) Uani 1 1 d . . . C24 C 0.7310(5) 0.5632(5) 0.3768(4) 0.0303(15) Uani 1 1 d . . . C25 C 0.7343(5) 0.2713(5) 0.5573(4) 0.0305(15) Uani 1 1 d . . . H25A H 0.7557 0.3435 0.5299 0.037 Uiso 1 1 calc R . . H25B H 0.7860 0.2392 0.5989 0.037 Uiso 1 1 calc R . . C26 C 0.7606(5) 0.2521(5) 0.4120(4) 0.0279(14) Uani 1 1 d . . . C27 C 0.7068(5) 0.2228(6) 0.3491(5) 0.0383(17) Uani 1 1 d . . . H27 H 0.6512 0.1765 0.3645 0.046 Uiso 1 1 calc R . . C28 C 0.7347(7) 0.2617(7) 0.2622(5) 0.054(2) Uani 1 1 d . . . H28 H 0.6981 0.2418 0.2197 0.065 Uiso 1 1 calc R . . C29 C 0.8185(6) 0.3308(6) 0.2408(5) 0.0426(18) Uani 1 1 d . . . C30 C 0.8717(5) 0.3603(6) 0.3031(4) 0.0345(16) Uani 1 1 d . . . H30 H 0.9259 0.4085 0.2875 0.041 Uiso 1 1 calc R . . C31 C 0.8461(5) 0.3190(5) 0.3905(4) 0.0265(14) Uani 1 1 d . . . C32 C 0.9174(5) 0.3428(5) 0.4548(4) 0.0257(14) Uani 1 1 d . . . C33 C 0.7484(6) 0.7718(7) 0.5340(6) 0.054(2) Uani 1 1 d U . . H33 H 0.7482 0.7112 0.5793 0.065 Uiso 1 1 calc R . . C34 C 0.6232(9) 0.8512(9) 0.6208(8) 0.097(3) Uani 1 1 d U . . H34A H 0.5506 0.8431 0.6117 0.146 Uiso 1 1 calc R . . H34B H 0.6324 0.9169 0.6379 0.146 Uiso 1 1 calc R . . H34C H 0.6470 0.7922 0.6651 0.146 Uiso 1 1 calc R . . C35 C 0.6780(10) 0.9482(9) 0.4708(8) 0.098(3) Uani 1 1 d U . . H35A H 0.7166 0.9356 0.4216 0.147 Uiso 1 1 calc R . . H35B H 0.7071 1.0076 0.4879 0.147 Uiso 1 1 calc R . . H35C H 0.6063 0.9642 0.4566 0.147 Uiso 1 1 calc R . . C36 C 0.8745(12) 0.8429(11) 0.2888(9) 0.111(3) Uani 1 1 d U . . H36 H 0.8051 0.8314 0.3071 0.133 Uiso 1 1 calc R . . C37 C 0.7975(13) 0.9956(13) 0.1825(11) 0.150(5) Uani 1 1 d U . . H37A H 0.7796 0.9812 0.1289 0.226 Uiso 1 1 calc R . . H37B H 0.8071 1.0711 0.1748 0.226 Uiso 1 1 calc R . . H37C H 0.7424 0.9725 0.2245 0.226 Uiso 1 1 calc R . . C38 C 1.0006(11) 0.9255(11) 0.1962(9) 0.114(4) Uani 1 1 d U . . H38A H 1.0127 0.9271 0.1365 0.171 Uiso 1 1 calc R . . H38B H 1.0256 0.8584 0.2306 0.171 Uiso 1 1 calc R . . H38C H 1.0369 0.9831 0.2101 0.171 Uiso 1 1 calc R . . N1 N 0.6016(4) 0.1633(4) 0.6461(4) 0.0323(13) Uani 1 1 d . . . H1 H 0.6442 0.1145 0.6363 0.039 Uiso 1 1 calc R . . N2 N 0.6838(6) 0.8536(6) 0.5409(6) 0.0634(19) Uani 1 1 d U . . N3 N 0.8964(10) 0.9367(9) 0.2126(8) 0.113(3) Uani 1 1 d U . . O1 O 0.4177(4) 0.1932(5) 0.6823(4) 0.0615(16) Uani 1 1 d . . . O2 O 0.4938(4) 0.0106(4) 0.7132(4) 0.0559(15) Uani 1 1 d . . . O3 O 0.7243(3) 0.3146(3) 0.7162(3) 0.0323(10) Uani 1 1 d . . . O4 O 0.5829(4) 0.4193(4) 0.4837(3) 0.0386(12) Uani 1 1 d . . . O5 O 0.7276(4) 0.2090(4) 0.4935(3) 0.0383(12) Uani 1 1 d . . . O6 O 0.8622(3) 0.5656(3) 0.5890(3) 0.0308(10) Uani 1 1 d . . . O7 O 0.9393(3) 0.4047(3) 0.6432(3) 0.0347(11) Uani 1 1 d . . . O8 O 0.7315(4) 0.5659(4) 0.4537(3) 0.0400(12) Uani 1 1 d . . . O9 O 0.8045(4) 0.6003(4) 0.3254(3) 0.0403(12) Uani 1 1 d . . . O10 O 0.9668(3) 0.2679(3) 0.5010(3) 0.0332(11) Uani 1 1 d . . . O11 O 0.9297(3) 0.4390(3) 0.4587(3) 0.0286(10) Uani 1 1 d . . . O12 O 0.8067(4) 0.7714(4) 0.4731(3) 0.0439(12) Uani 1 1 d . . . O13 O 0.9375(4) 0.7837(4) 0.3265(3) 0.0473(13) Uani 1 1 d . . . S1 S 0.50297(15) 0.12304(15) 0.70956(13) 0.0412(4) 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 0.02273(17) 0.02060(17) 0.02461(18) -0.00409(12) -0.00047(12) 0.00116(11) Br1 0.1248(10) 0.1019(9) 0.0680(7) -0.0616(7) 0.0271(7) -0.0419(8) Br2 0.0579(6) 0.1295(9) 0.0379(5) -0.0317(5) -0.0095(4) 0.0017(6) Br3 0.1046(9) 0.1354(11) 0.0295(5) -0.0140(6) 0.0018(5) -0.0123(8) C1 0.121(4) 0.120(4) 0.120(4) -0.0284(13) -0.0039(10) -0.0029(10) C2 0.080(2) 0.080(2) 0.079(2) -0.0189(11) -0.0022(10) -0.0026(10) C3 0.086(2) 0.086(2) 0.086(2) -0.0192(11) -0.0037(10) -0.0023(10) C4 0.080(2) 0.079(2) 0.079(2) -0.0190(11) -0.0026(10) -0.0017(10) C5 0.063(2) 0.062(2) 0.062(2) -0.0154(10) -0.0018(10) -0.0015(10) C6 0.076(2) 0.076(2) 0.076(2) -0.0183(11) -0.0018(10) -0.0019(10) C7 0.085(2) 0.084(2) 0.084(2) -0.0203(11) -0.0017(10) -0.0021(10) C8 0.029(3) 0.022(3) 0.032(4) -0.002(3) 0.001(3) -0.003(3) C9 0.026(3) 0.028(4) 0.029(4) -0.005(3) 0.000(3) -0.002(3) C10 0.035(4) 0.031(4) 0.024(3) -0.004(3) -0.003(3) 0.004(3) C11 0.041(4) 0.046(5) 0.037(4) -0.008(4) 0.011(3) -0.015(4) C12 0.057(5) 0.083(6) 0.024(4) -0.011(4) 0.012(4) -0.017(5) C13 0.052(5) 0.061(5) 0.029(4) -0.022(4) 0.007(3) -0.008(4) C14 0.038(4) 0.043(4) 0.034(4) -0.014(3) 0.004(3) -0.008(3) C15 0.026(3) 0.034(4) 0.029(4) -0.014(3) 0.000(3) 0.006(3) C16 0.023(3) 0.033(4) 0.023(3) -0.004(3) 0.001(3) -0.001(3) C17 0.031(4) 0.033(4) 0.037(4) -0.001(3) -0.002(3) -0.005(3) C18 0.033(4) 0.029(4) 0.032(4) -0.008(3) -0.007(3) 0.007(3) C19 0.034(4) 0.034(4) 0.045(4) -0.006(3) -0.012(3) -0.001(3) C20 0.038(4) 0.048(5) 0.040(4) -0.009(4) -0.018(3) -0.004(3) C21 0.035(4) 0.055(5) 0.037(4) -0.016(4) -0.010(3) 0.005(4) C22 0.033(4) 0.050(5) 0.035(4) -0.010(3) -0.003(3) -0.006(3) C23 0.025(3) 0.033(4) 0.032(4) -0.009(3) -0.007(3) 0.006(3) C24 0.027(4) 0.025(4) 0.035(4) -0.001(3) -0.008(3) 0.004(3) C25 0.029(4) 0.033(4) 0.033(4) -0.016(3) 0.000(3) 0.001(3) C26 0.030(4) 0.024(3) 0.030(4) -0.009(3) 0.002(3) 0.001(3) C27 0.027(4) 0.040(4) 0.054(5) -0.021(4) -0.005(3) -0.001(3) C28 0.060(5) 0.063(6) 0.045(5) -0.027(4) -0.015(4) 0.010(4) C29 0.043(4) 0.056(5) 0.029(4) -0.011(4) 0.001(3) 0.011(4) C30 0.026(4) 0.043(4) 0.032(4) -0.006(3) 0.004(3) 0.004(3) C31 0.024(3) 0.024(3) 0.033(4) -0.009(3) 0.001(3) 0.010(3) C32 0.022(3) 0.023(3) 0.034(4) -0.011(3) 0.004(3) 0.001(3) C33 0.048(4) 0.042(4) 0.079(5) -0.025(4) 0.004(4) -0.004(3) C34 0.094(6) 0.085(6) 0.125(7) -0.054(5) 0.033(5) -0.010(5) C35 0.104(6) 0.074(6) 0.117(7) -0.024(5) -0.008(5) 0.017(5) C36 0.133(6) 0.103(6) 0.103(6) -0.038(5) -0.005(6) -0.012(6) C37 0.163(8) 0.139(7) 0.141(7) -0.017(6) -0.011(7) 0.010(7) C38 0.128(7) 0.127(7) 0.103(6) -0.056(6) -0.005(6) -0.034(6) N1 0.030(3) 0.027(3) 0.038(3) -0.007(3) 0.005(3) -0.001(2) N2 0.053(4) 0.049(4) 0.097(5) -0.037(3) 0.012(3) 0.000(3) N3 0.130(6) 0.107(6) 0.110(6) -0.040(5) -0.029(5) 0.024(5) O1 0.037(3) 0.063(4) 0.072(4) 0.006(3) 0.007(3) 0.000(3) O2 0.060(4) 0.042(3) 0.063(4) -0.008(3) 0.011(3) -0.019(3) O3 0.033(3) 0.033(3) 0.031(3) -0.007(2) -0.002(2) -0.002(2) O4 0.047(3) 0.034(3) 0.034(3) -0.004(2) -0.011(2) -0.010(2) O5 0.047(3) 0.031(3) 0.040(3) -0.015(2) 0.014(2) -0.013(2) O6 0.035(3) 0.033(3) 0.022(2) -0.001(2) 0.0050(19) 0.002(2) O7 0.035(3) 0.028(3) 0.037(3) 0.000(2) 0.009(2) 0.003(2) O8 0.032(3) 0.057(3) 0.034(3) -0.017(2) 0.001(2) -0.013(2) O9 0.036(3) 0.046(3) 0.036(3) -0.002(2) -0.003(2) -0.013(2) O10 0.036(3) 0.021(2) 0.043(3) -0.007(2) -0.011(2) 0.007(2) O11 0.032(2) 0.020(2) 0.035(3) -0.0066(19) -0.003(2) -0.0021(19) O12 0.040(3) 0.036(3) 0.054(3) -0.009(2) 0.008(3) 0.010(2) O13 0.051(3) 0.034(3) 0.050(3) 0.004(2) -0.011(3) 0.009(2) S1 0.0382(10) 0.0375(10) 0.0450(11) -0.0047(9) 0.0075(9) -0.0087(8) _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_ _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 -0.003 694 160 ' ' _platon_squeeze_details ; ; 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 O11 2.366(4) . ? Tb1 O6 2.384(4) . ? Tb1 O7 2.384(4) 2_766 ? Tb1 O13 2.405(5) . ? Tb1 O12 2.407(5) . ? Tb1 O9 2.429(5) . ? Tb1 O8 2.431(4) . ? Tb1 O10 2.457(4) 2_766 ? Tb1 O11 2.648(4) 2_766 ? Tb1 C24 2.776(6) . ? Tb1 C32 2.911(6) 2_766 ? Br1 C13 1.895(7) . ? Br2 C21 1.898(7) . ? Br3 C29 1.887(7) . ? C1 C2 1.552(16) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C7 1.250(14) . ? C2 C3 1.381(14) . ? C3 C4 1.440(14) . ? C3 H3 0.9300 . ? C4 C5 1.367(13) . ? C4 H4 0.9300 . ? C5 C6 1.372(13) . ? C5 S1 1.756(9) . ? C6 C7 1.406(14) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 N1 1.473(8) . ? C8 C9 1.517(9) . ? C8 C25 1.542(9) . ? C8 C17 1.544(9) . ? C9 O3 1.430(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.376(9) . ? C10 C15 1.385(9) . ? C10 O3 1.399(8) . ? C11 C12 1.370(10) . ? C11 H11 0.9300 . ? C12 C13 1.385(11) . ? C12 H12 0.9300 . ? C13 C14 1.394(10) . ? C14 C15 1.377(9) . ? C14 H14 0.9300 . ? C15 C16 1.524(9) . ? C16 O7 1.242(7) . ? C16 O6 1.268(7) . ? C17 O4 1.445(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O4 1.362(8) . ? C18 C19 1.379(9) . ? C18 C23 1.410(9) . ? C19 C20 1.395(10) . ? C19 H19 0.9300 . ? C20 C21 1.371(10) . ? C20 H20 0.9300 . ? C21 C22 1.382(10) . ? C22 C23 1.381(9) . ? C22 H22 0.9300 . ? C23 C24 1.510(9) . ? C24 O8 1.241(8) . ? C24 O9 1.254(8) . ? C25 O5 1.449(7) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 O5 1.349(8) . ? C26 C27 1.373(9) . ? C26 C31 1.394(9) . ? C27 C28 1.399(11) . ? C27 H27 0.9300 . ? C28 C29 1.394(11) . ? C28 H28 0.9300 . ? C29 C30 1.362(10) . ? C30 C31 1.404(9) . ? C30 H30 0.9300 . ? C31 C32 1.495(9) . ? C32 O10 1.240(7) . ? C32 O11 1.269(7) . ? C32 Tb1 2.911(6) 2_766 ? C33 O12 1.207(9) . ? C33 N2 1.344(10) . ? C33 H33 0.9300 . ? C34 N2 1.467(12) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 N2 1.449(13) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 O13 1.176(15) . ? C36 N3 1.522(17) . ? C36 H36 0.9300 . ? C37 N3 1.494(17) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 N3 1.361(15) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? N1 S1 1.607(6) . ? N1 H1 0.8600 . ? O1 S1 1.411(6) . ? O2 S1 1.442(5) . ? O7 Tb1 2.384(4) 2_766 ? O10 Tb1 2.457(4) 2_766 ? O11 Tb1 2.648(4) 2_766 ? 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 O11 Tb1 O6 79.25(15) . . ? O11 Tb1 O7 72.78(15) . 2_766 ? O6 Tb1 O7 133.11(15) . 2_766 ? O11 Tb1 O13 136.88(17) . . ? O6 Tb1 O13 143.83(17) . . ? O7 Tb1 O13 71.81(17) 2_766 . ? O11 Tb1 O12 146.51(16) . . ? O6 Tb1 O12 75.57(16) . . ? O7 Tb1 O12 140.61(16) 2_766 . ? O13 Tb1 O12 71.45(18) . . ? O11 Tb1 O9 79.55(15) . . ? O6 Tb1 O9 123.31(15) . . ? O7 Tb1 O9 87.83(16) 2_766 . ? O13 Tb1 O9 75.32(17) . . ? O12 Tb1 O9 96.20(18) . . ? O11 Tb1 O8 76.63(16) . . ? O6 Tb1 O8 70.90(15) . . ? O7 Tb1 O8 134.13(16) 2_766 . ? O13 Tb1 O8 112.92(17) . . ? O12 Tb1 O8 74.51(17) . . ? O9 Tb1 O8 53.22(16) . . ? O11 Tb1 O10 122.72(14) . 2_766 ? O6 Tb1 O10 81.66(15) . 2_766 ? O7 Tb1 O10 82.81(16) 2_766 2_766 ? O13 Tb1 O10 75.90(17) . 2_766 ? O12 Tb1 O10 74.98(16) . 2_766 ? O9 Tb1 O10 151.21(16) . 2_766 ? O8 Tb1 O10 143.02(15) . 2_766 ? O11 Tb1 O11 72.32(15) . 2_766 ? O6 Tb1 O11 66.01(14) . 2_766 ? O7 Tb1 O11 69.95(15) 2_766 2_766 ? O13 Tb1 O11 116.29(15) . 2_766 ? O12 Tb1 O11 115.52(16) . 2_766 ? O9 Tb1 O11 148.13(15) . 2_766 ? O8 Tb1 O11 130.37(15) . 2_766 ? O10 Tb1 O11 50.60(13) 2_766 2_766 ? O11 Tb1 C24 74.53(16) . . ? O6 Tb1 C24 96.63(18) . . ? O7 Tb1 C24 110.72(18) 2_766 . ? O13 Tb1 C24 95.94(19) . . ? O12 Tb1 C24 86.76(18) . . ? O9 Tb1 C24 26.83(17) . . ? O8 Tb1 C24 26.54(17) . . ? O10 Tb1 C24 161.54(17) 2_766 . ? O11 Tb1 C24 144.83(15) 2_766 . ? O11 Tb1 C32 98.16(16) . 2_766 ? O6 Tb1 C32 70.38(16) . 2_766 ? O7 Tb1 C32 77.17(17) 2_766 2_766 ? O13 Tb1 C32 97.20(18) . 2_766 ? O12 Tb1 C32 93.83(17) . 2_766 ? O9 Tb1 C32 164.78(17) . 2_766 ? O8 Tb1 C32 141.22(16) . 2_766 ? O10 Tb1 C32 24.92(15) 2_766 2_766 ? O11 Tb1 C32 25.84(14) 2_766 2_766 ? C24 Tb1 C32 166.32(18) . 2_766 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 122.8(12) . . ? C7 C2 C1 122.7(12) . . ? C3 C2 C1 114.4(11) . . ? C2 C3 C4 118.3(11) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C5 C4 C3 117.1(10) . . ? C5 C4 H4 121.5 . . ? C3 C4 H4 121.5 . . ? C4 C5 C6 121.7(10) . . ? C4 C5 S1 119.1(8) . . ? C6 C5 S1 118.9(8) . . ? C5 C6 C7 117.9(10) . . ? C5 C6 H6 121.1 . . ? C7 C6 H6 121.1 . . ? C2 C7 C6 122.2(12) . . ? C2 C7 H7 118.9 . . ? C6 C7 H7 118.9 . . ? N1 C8 C9 114.2(5) . . ? N1 C8 C25 106.8(5) . . ? C9 C8 C25 106.8(5) . . ? N1 C8 C17 109.1(5) . . ? C9 C8 C17 110.6(5) . . ? C25 C8 C17 109.1(5) . . ? O3 C9 C8 109.3(5) . . ? O3 C9 H9A 109.8 . . ? C8 C9 H9A 109.8 . . ? O3 C9 H9B 109.8 . . ? C8 C9 H9B 109.8 . . ? H9A C9 H9B 108.3 . . ? C11 C10 C15 120.7(6) . . ? C11 C10 O3 118.9(6) . . ? C15 C10 O3 120.4(6) . . ? C12 C11 C10 121.4(7) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 118.2(7) . . ? C11 C12 H12 120.9 . . ? C13 C12 H12 120.9 . . ? C12 C13 C14 120.7(7) . . ? C12 C13 Br1 120.1(5) . . ? C14 C13 Br1 119.1(6) . . ? C15 C14 C13 120.2(7) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C10 118.6(6) . . ? C14 C15 C16 118.6(6) . . ? C10 C15 C16 122.7(6) . . ? O7 C16 O6 128.3(6) . . ? O7 C16 C15 115.7(6) . . ? O6 C16 C15 115.8(5) . . ? O4 C17 C8 106.9(5) . . ? O4 C17 H17A 110.3 . . ? C8 C17 H17A 110.3 . . ? O4 C17 H17B 110.3 . . ? C8 C17 H17B 110.3 . . ? H17A C17 H17B 108.6 . . ? O4 C18 C19 122.2(6) . . ? O4 C18 C23 117.6(6) . . ? C19 C18 C23 120.2(6) . . ? C18 C19 C20 120.9(7) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 118.5(6) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? C20 C21 C22 121.0(7) . . ? C20 C21 Br2 119.9(5) . . ? C22 C21 Br2 119.1(6) . . ? C23 C22 C21 121.3(7) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C18 117.9(6) . . ? C22 C23 C24 117.8(6) . . ? C18 C23 C24 124.4(6) . . ? O8 C24 O9 121.5(6) . . ? O8 C24 C23 120.1(6) . . ? O9 C24 C23 118.3(6) . . ? O8 C24 Tb1 61.0(3) . . ? O9 C24 Tb1 61.0(3) . . ? C23 C24 Tb1 169.8(4) . . ? O5 C25 C8 109.2(5) . . ? O5 C25 H25A 109.8 . . ? C8 C25 H25A 109.8 . . ? O5 C25 H25B 109.8 . . ? C8 C25 H25B 109.8 . . ? H25A C25 H25B 108.3 . . ? O5 C26 C27 115.8(6) . . ? O5 C26 C31 123.7(6) . . ? C27 C26 C31 120.5(6) . . ? C26 C27 C28 120.9(7) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C29 C28 C27 118.5(7) . . ? C29 C28 H28 120.7 . . ? C27 C28 H28 120.7 . . ? C30 C29 C28 120.8(7) . . ? C30 C29 Br3 120.4(6) . . ? C28 C29 Br3 118.8(6) . . ? C29 C30 C31 121.0(7) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C26 C31 C30 118.3(6) . . ? C26 C31 C32 123.8(6) . . ? C30 C31 C32 117.7(6) . . ? O10 C32 O11 121.4(6) . . ? O10 C32 C31 118.9(5) . . ? O11 C32 C31 119.7(6) . . ? O10 C32 Tb1 56.6(3) . 2_766 ? O11 C32 Tb1 65.4(3) . 2_766 ? C31 C32 Tb1 168.4(4) . 2_766 ? O12 C33 N2 124.7(9) . . ? O12 C33 H33 117.7 . . ? N2 C33 H33 117.7 . . ? N2 C34 H34A 109.5 . . ? N2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N2 C35 H35A 109.5 . . ? N2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O13 C36 N3 125.7(14) . . ? O13 C36 H36 117.1 . . ? N3 C36 H36 117.1 . . ? N3 C37 H37A 109.5 . . ? N3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N3 C38 H38A 109.5 . . ? N3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C8 N1 S1 127.0(4) . . ? C8 N1 H1 116.5 . . ? S1 N1 H1 116.5 . . ? C33 N2 C35 120.0(9) . . ? C33 N2 C34 120.8(9) . . ? C35 N2 C34 119.1(8) . . ? C38 N3 C37 145.9(14) . . ? C38 N3 C36 103.0(11) . . ? C37 N3 C36 110.7(13) . . ? C10 O3 C9 112.7(5) . . ? C18 O4 C17 118.8(5) . . ? C26 O5 C25 119.0(5) . . ? C16 O6 Tb1 134.8(4) . . ? C16 O7 Tb1 137.6(4) . 2_766 ? C24 O8 Tb1 92.4(4) . . ? C24 O9 Tb1 92.2(4) . . ? C32 O10 Tb1 98.5(4) . 2_766 ? C32 O11 Tb1 163.5(4) . . ? C32 O11 Tb1 88.8(4) . 2_766 ? Tb1 O11 Tb1 107.68(15) . 2_766 ? C33 O12 Tb1 129.4(5) . . ? C36 O13 Tb1 128.4(9) . . ? O1 S1 O2 119.3(4) . . ? O1 S1 N1 108.1(3) . . ? O2 S1 N1 106.1(3) . . ? O1 S1 C5 107.0(4) . . ? O2 S1 C5 106.9(4) . . ? N1 S1 C5 109.2(4) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.746 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.129