# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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 _database_code_depnum_ccdc_archive 'CCDC 757992' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H36 Eu4 N6 O36 S2 Zn, 5H2O' _chemical_formula_sum 'C40 H46 Eu4 N6 O41 S2 Zn' _chemical_formula_weight 2004.16 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' Zn Zn 0.2839 1.4301 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0516(8) _cell_length_b 12.4783(10) _cell_length_c 12.7662(10) _cell_angle_alpha 105.8680(10) _cell_angle_beta 98.2301(10) _cell_angle_gamma 115.6490(11) _cell_volume 1455.50(19) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5136 _cell_measurement_theta_min 1.74 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 970 _exptl_absorpt_coefficient_mu 4.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3274 _exptl_absorpt_correction_T_max 0.4161 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _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 AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7505 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.20 _reflns_number_total 5136 _reflns_number_gt 4346 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0357P)^2^+1.7396P] 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 5136 _refine_ls_number_parameters 440 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0653 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 C1 C 0.4018(5) 0.0130(4) 0.1233(4) 0.0179(10) Uani 1 1 d . . . C2 C 0.3751(5) -0.1048(5) 0.0491(4) 0.0234(11) Uani 1 1 d . . . H2 H 0.2894 -0.1596 -0.0080 0.028 Uiso 1 1 calc R . . C3 C 0.4771(6) -0.1390(5) 0.0613(5) 0.0285(13) Uani 1 1 d . . . H3 H 0.4612 -0.2179 0.0135 0.034 Uiso 1 1 calc R . . C4 C 0.6042(6) -0.0537(5) 0.1463(5) 0.0281(12) Uani 1 1 d . . . H4 H 0.6757 -0.0739 0.1561 0.034 Uiso 1 1 calc R . . C5 C 0.6227(5) 0.0613(5) 0.2157(4) 0.0209(11) Uani 1 1 d . . . C6 C 0.7554(5) 0.1590(5) 0.3099(4) 0.0203(11) Uani 1 1 d . . . C7 C 0.2992(5) 0.0619(5) 0.1163(4) 0.0208(11) Uani 1 1 d . . . C8 C 0.8535(5) 0.5293(5) 0.2014(4) 0.0212(11) Uani 1 1 d . . . C9 C 0.8285(6) 0.5068(5) 0.0869(5) 0.0271(12) Uani 1 1 d . . . H9 H 0.7454 0.4370 0.0342 0.032 Uiso 1 1 calc R . . C10 C 0.9290(6) 0.5897(5) 0.0506(5) 0.0334(14) Uani 1 1 d . . . H10 H 0.9143 0.5769 -0.0264 0.040 Uiso 1 1 calc R . . C11 C 1.0511(6) 0.6912(5) 0.1317(5) 0.0314(13) Uani 1 1 d . . . H11 H 1.1198 0.7489 0.1102 0.038 Uiso 1 1 calc R . . C12 C 1.0705(5) 0.7065(5) 0.2456(5) 0.0230(11) Uani 1 1 d . . . C13 C 1.1999(6) 0.8159(5) 0.3409(5) 0.0327(14) Uani 1 1 d . . . C14 C 0.7505(5) 0.4519(4) 0.2515(4) 0.0186(11) Uani 1 1 d . . . C15 C 0.0247(6) -0.0138(6) 0.2356(5) 0.0361(14) Uani 1 1 d . . . H15 H 0.1098 0.0612 0.2551 0.043 Uiso 1 1 calc R . . C16 C -0.0131(7) -0.0595(6) 0.3203(5) 0.0378(15) Uani 1 1 d . . . H16 H 0.0473 -0.0173 0.3946 0.045 Uiso 1 1 calc R . . C17 C -0.1412(7) -0.1682(6) 0.2930(5) 0.0346(14) Uani 1 1 d . A . C18 C -0.2263(6) -0.2310(6) 0.1796(5) 0.0336(14) Uani 1 1 d . . . H18 H -0.3132 -0.3046 0.1584 0.040 Uiso 1 1 calc R . . C19 C -0.1797(6) -0.1825(5) 0.0998(5) 0.0303(13) Uani 1 1 d . . . H19 H -0.2354 -0.2266 0.0239 0.036 Uiso 1 1 calc R . . C20 C -0.1885(8) -0.2188(7) 0.3823(7) 0.0499(19) Uani 1 1 d . . . Eu1 Eu 0.55615(2) 0.29746(2) 0.35122(2) 0.01656(8) Uani 1 1 d . . . Eu2 Eu 1.01082(2) 0.66984(2) 0.49045(2) 0.01743(8) Uani 1 1 d . . . N1 N 0.5236(4) 0.0949(4) 0.2059(3) 0.0171(9) Uani 1 1 d . . . N2 N 0.9732(4) 0.6276(4) 0.2801(3) 0.0200(9) Uani 1 1 d . . . N3 N -0.0574(5) -0.0742(4) 0.1265(4) 0.0257(10) Uani 1 1 d . . . O1 O 0.8545(4) 0.1386(3) 0.3311(3) 0.0318(9) Uani 1 1 d . . . O2 O 0.7615(3) 0.2638(3) 0.3679(3) 0.0207(8) Uani 1 1 d . . . O3 O 0.3374(4) 0.1698(3) 0.1924(3) 0.0266(8) Uani 1 1 d . . . O4 O 0.1860(4) -0.0062(3) 0.0373(3) 0.0273(8) Uani 1 1 d . . . O5 O 1.2885(5) 0.8986(4) 0.3168(4) 0.0556(14) Uani 1 1 d . . . O6 O 1.2037(4) 0.8113(4) 0.4399(3) 0.0420(11) Uani 1 1 d . . . O7 O 0.7807(3) 0.4932(3) 0.3608(3) 0.0202(7) Uani 1 1 d . . . O8 O 0.6385(4) 0.3531(3) 0.1897(3) 0.0288(9) Uani 1 1 d . . . O9 O -0.0980(5) -0.2150(4) 0.4566(3) 0.0362(10) Uani 1 1 d . . . O10 O -0.281(4) -0.211(7) 0.409(4) 0.052(12) Uani 0.39(7) 1 d P A 1 O10' O -0.330(3) -0.288(4) 0.360(3) 0.052(7) Uani 0.61(7) 1 d P A 2 O11 O 0.9289(3) 0.4970(3) 0.5765(3) 0.0219(8) Uani 1 1 d . . . O12 O 0.8470(4) 0.6443(3) 0.6140(3) 0.0301(9) Uani 1 1 d . . . O13 O 0.8430(4) 0.5303(4) 0.7413(3) 0.0349(10) Uani 1 1 d . . . O14 O 0.6802(4) 0.4188(3) 0.5517(3) 0.0316(9) Uani 1 1 d . . . O1W O 0.5028(4) 0.1379(3) 0.4360(3) 0.0365(10) Uani 1 1 d . . . H1A H 0.5657 0.1269 0.4703 0.055 Uiso 1 1 d R . . H1B H 0.4352 0.0644 0.3914 0.055 Uiso 1 1 d R . . O2W O 0.4966(4) 0.4597(4) 0.3328(4) 0.0503(13) Uani 1 1 d . . . H2A H 0.4310 0.4777 0.3224 0.075 Uiso 1 1 d R . . H2B H 0.5723 0.5236 0.3375 0.075 Uiso 1 1 d R . . O4W O 0.1054(4) 0.1962(3) 0.1249(3) 0.0350(9) Uani 1 1 d . . . H4B H 0.0884 0.2510 0.1653 0.052 Uiso 1 1 d R . . H4A H 0.1871 0.2203 0.1647 0.052 Uiso 1 1 d R . . O5W O 0.6284(8) 0.3595(7) 0.8078(5) 0.146(4) Uani 1 1 d . . . H5A H 0.6608 0.3127 0.8223 0.219 Uiso 1 1 d R . . H5B H 0.6727 0.3953 0.7669 0.219 Uiso 1 1 d R . . O7W O 0.4358(12) 0.0959(11) 0.6216(10) 0.077(3) Uani 0.50 1 d P . . H7A H 0.3840 0.0472 0.5533 0.115 Uiso 0.50 1 d PR . . H7B H 0.4045 0.1457 0.6477 0.115 Uiso 0.50 1 d PR . . S1 S 0.82261(13) 0.52156(12) 0.62422(10) 0.0199(3) Uani 1 1 d . . . Zn3 Zn 0.0000 0.0000 0.0000 0.02112(19) Uani 1 2 d S . . O3W O 0.3681(5) 0.2909(5) 0.4346(4) 0.0595(15) Uani 1 1 d . . . H3A H 0.3309 0.2353 0.4635 0.089 Uiso 1 1 d R . . H3B H 0.3100 0.3156 0.4175 0.089 Uiso 1 1 d R . . O6W O 0.5495(7) 0.5275(8) 0.9080(7) 0.144(4) Uani 1 1 d . . . H6A H 0.5260 0.5829 0.9035 0.216 Uiso 1 1 d R . . H6B H 0.6379 0.5669 0.9396 0.216 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.011(2) 0.020(2) 0.018(3) 0.009(2) 0.004(2) 0.003(2) C2 0.019(3) 0.022(3) 0.017(3) 0.005(2) 0.000(2) 0.003(2) C3 0.033(3) 0.021(3) 0.020(3) -0.002(2) 0.002(2) 0.011(2) C4 0.026(3) 0.021(3) 0.031(3) 0.003(2) 0.001(3) 0.014(2) C5 0.018(3) 0.019(3) 0.019(3) 0.004(2) 0.000(2) 0.007(2) C6 0.021(3) 0.025(3) 0.016(3) 0.006(2) 0.004(2) 0.013(2) C7 0.018(3) 0.025(3) 0.016(3) 0.007(2) 0.004(2) 0.008(2) C8 0.022(3) 0.020(3) 0.018(3) 0.006(2) 0.005(2) 0.009(2) C9 0.026(3) 0.027(3) 0.020(3) 0.006(2) 0.003(2) 0.008(2) C10 0.042(4) 0.039(3) 0.019(3) 0.013(3) 0.011(3) 0.019(3) C11 0.035(3) 0.029(3) 0.029(3) 0.017(3) 0.016(3) 0.010(3) C12 0.023(3) 0.019(3) 0.026(3) 0.010(2) 0.008(2) 0.009(2) C13 0.032(3) 0.026(3) 0.028(3) 0.007(3) 0.010(3) 0.006(3) C14 0.016(2) 0.016(2) 0.021(3) 0.005(2) 0.003(2) 0.008(2) C15 0.040(4) 0.031(3) 0.031(3) 0.016(3) 0.005(3) 0.012(3) C16 0.062(4) 0.039(3) 0.027(3) 0.017(3) 0.021(3) 0.033(3) C17 0.054(4) 0.045(4) 0.044(4) 0.033(3) 0.033(3) 0.042(3) C18 0.034(3) 0.040(3) 0.043(4) 0.026(3) 0.018(3) 0.024(3) C19 0.027(3) 0.038(3) 0.034(3) 0.018(3) 0.013(3) 0.019(3) C20 0.070(5) 0.072(5) 0.069(5) 0.058(4) 0.049(4) 0.059(4) Eu1 0.01481(13) 0.01680(14) 0.01482(14) 0.00436(10) 0.00198(10) 0.00683(11) Eu2 0.01520(14) 0.01674(14) 0.01399(14) 0.00360(11) 0.00058(10) 0.00508(11) N1 0.018(2) 0.017(2) 0.012(2) 0.0040(17) 0.0022(17) 0.0063(18) N2 0.022(2) 0.016(2) 0.019(2) 0.0056(18) 0.0037(19) 0.0081(18) N3 0.028(2) 0.027(2) 0.024(2) 0.010(2) 0.008(2) 0.015(2) O1 0.027(2) 0.028(2) 0.029(2) -0.0058(17) -0.0079(17) 0.0182(17) O2 0.0161(17) 0.0171(17) 0.0214(19) 0.0021(15) -0.0006(15) 0.0070(14) O3 0.0198(18) 0.026(2) 0.025(2) 0.0008(17) -0.0014(16) 0.0113(16) O4 0.0184(19) 0.028(2) 0.025(2) 0.0016(17) -0.0033(16) 0.0111(16) O5 0.049(3) 0.036(2) 0.039(3) 0.015(2) 0.014(2) -0.014(2) O6 0.032(2) 0.036(2) 0.022(2) 0.0076(18) 0.0010(18) -0.0089(18) O7 0.0211(18) 0.0217(18) 0.0123(17) 0.0067(15) 0.0018(15) 0.0067(15) O8 0.028(2) 0.0221(19) 0.0152(18) 0.0027(16) 0.0010(17) -0.0006(17) O9 0.063(3) 0.034(2) 0.030(2) 0.0176(19) 0.021(2) 0.033(2) O10 0.034(13) 0.10(3) 0.060(17) 0.06(2) 0.033(13) 0.041(19) O10' 0.038(8) 0.076(17) 0.070(13) 0.056(13) 0.026(9) 0.031(10) O11 0.0209(18) 0.0213(18) 0.0185(18) 0.0049(15) 0.0055(15) 0.0080(15) O12 0.028(2) 0.027(2) 0.038(2) 0.0120(18) 0.0112(18) 0.0151(17) O13 0.036(2) 0.046(2) 0.018(2) 0.0124(18) 0.0071(18) 0.016(2) O14 0.0192(19) 0.033(2) 0.022(2) 0.0039(17) 0.0036(16) 0.0000(16) O1W 0.041(2) 0.0206(19) 0.041(2) 0.0136(18) 0.012(2) 0.0092(18) O2W 0.032(2) 0.035(2) 0.098(4) 0.034(3) 0.022(3) 0.022(2) O4W 0.038(2) 0.032(2) 0.027(2) 0.0026(18) 0.0000(18) 0.0183(19) O5W 0.129(6) 0.144(7) 0.059(4) 0.053(5) 0.019(4) -0.027(5) O7W 0.101(9) 0.103(9) 0.069(8) 0.055(7) 0.051(7) 0.065(8) S1 0.0186(6) 0.0222(6) 0.0122(6) 0.0031(5) 0.0023(5) 0.0072(5) Zn3 0.0173(4) 0.0263(4) 0.0182(4) 0.0096(4) 0.0035(3) 0.0093(4) O3W 0.048(3) 0.126(5) 0.052(3) 0.058(3) 0.033(3) 0.063(3) O6W 0.066(4) 0.156(7) 0.182(8) 0.133(7) -0.021(5) 0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.335(6) . ? C1 C2 1.388(7) . ? C1 C7 1.505(7) . ? C2 C3 1.370(7) . ? C2 H2 0.9300 . ? C3 C4 1.386(7) . ? C3 H3 0.9300 . ? C4 C5 1.373(7) . ? C4 H4 0.9300 . ? C5 N1 1.333(6) . ? C5 C6 1.492(7) . ? C6 O1 1.237(6) . ? C6 O2 1.282(6) . ? C6 Eu2 2.845(5) 2_766 ? C7 O4 1.247(6) . ? C7 O3 1.269(6) . ? C8 N2 1.344(6) . ? C8 C9 1.373(7) . ? C8 C14 1.494(7) . ? C9 C10 1.390(7) . ? C9 H9 0.9300 . ? C10 C11 1.379(8) . ? C10 H10 0.9300 . ? C11 C12 1.385(7) . ? C11 H11 0.9300 . ? C12 N2 1.333(6) . ? C12 C13 1.514(8) . ? C13 O5 1.227(7) . ? C13 O6 1.276(7) . ? C14 O8 1.242(6) . ? C14 O7 1.284(6) . ? C15 N3 1.343(7) . ? C15 C16 1.389(8) . ? C15 H15 0.9300 . ? C16 C17 1.380(8) . ? C16 H16 0.9300 . ? C17 C18 1.395(9) . ? C17 C20 1.500(8) . ? C18 C19 1.373(8) . ? C18 H18 0.9300 . ? C19 N3 1.343(7) . ? C19 H19 0.9300 . ? C20 O10 1.161(18) . ? C20 O9 1.250(8) . ? Eu1 O14 2.408(4) . ? Eu1 O1W 2.414(4) . ? Eu1 O2W 2.441(4) . ? Eu1 O3 2.447(3) . ? Eu1 O3W 2.448(4) . ? Eu1 O2 2.471(3) . ? Eu1 O8 2.517(3) . ? Eu1 N1 2.534(4) . ? Eu1 O7 2.576(3) . ? Eu1 H2B 2.8052 . ? Eu2 O9 2.321(4) 1_665 ? Eu2 O6 2.416(4) . ? Eu2 O11 2.429(3) 2_766 ? Eu2 O7 2.452(3) . ? Eu2 O1 2.468(3) 2_766 ? Eu2 O2 2.522(3) 2_766 ? Eu2 N2 2.526(4) . ? Eu2 O12 2.541(4) . ? Eu2 O11 2.563(3) . ? N3 Zn3 2.115(4) . ? O1 Eu2 2.468(3) 2_766 ? O2 Eu2 2.522(3) 2_766 ? O4 Zn3 2.082(3) . ? O9 Eu2 2.321(4) 1_445 ? O11 S1 1.504(3) . ? O11 Eu2 2.429(3) 2_766 ? O12 S1 1.482(4) . ? O13 S1 1.445(4) . ? O14 S1 1.472(4) . ? O1W H1A 0.8500 . ? O1W H1B 0.8500 . ? O2W H2A 0.8501 . ? O2W H2B 0.8500 . ? O4W Zn3 2.181(4) . ? O4W H4B 0.8457 . ? O4W H4A 0.8458 . ? O5W H5A 0.8500 . ? O5W H5B 0.8501 . ? O7W H7A 0.8500 . ? O7W H7B 0.8501 . ? Zn3 O4 2.082(3) 2 ? Zn3 N3 2.115(4) 2 ? Zn3 O4W 2.181(4) 2 ? O3W H3A 0.8500 . ? O3W H3B 0.8500 . ? O6W H6A 0.8501 . ? O6W H6B 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.5(5) . . ? N1 C1 C7 113.9(4) . . ? C2 C1 C7 123.6(4) . . ? C3 C2 C1 119.0(5) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 118.7(5) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 118.8(5) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? N1 C5 C4 123.1(5) . . ? N1 C5 C6 114.2(4) . . ? C4 C5 C6 122.7(5) . . ? O1 C6 O2 121.7(4) . . ? O1 C6 C5 121.1(4) . . ? O2 C6 C5 117.2(4) . . ? O4 C7 O3 126.3(5) . . ? O4 C7 C1 117.7(4) . . ? O3 C7 C1 116.1(4) . . ? N2 C8 C9 122.3(5) . . ? N2 C8 C14 113.4(4) . . ? C9 C8 C14 124.3(5) . . ? C8 C9 C10 119.2(5) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C11 C10 C9 118.3(5) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? C10 C11 C12 119.4(5) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? N2 C12 C11 122.1(5) . . ? N2 C12 C13 114.6(5) . . ? C11 C12 C13 123.3(5) . . ? O5 C13 O6 126.8(5) . . ? O5 C13 C12 118.3(5) . . ? O6 C13 C12 114.9(5) . . ? O8 C14 O7 121.3(4) . . ? O8 C14 C8 121.2(5) . . ? O7 C14 C8 117.5(4) . . ? N3 C15 C16 122.2(5) . . ? N3 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C17 C16 C15 119.4(6) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 118.4(5) . . ? C16 C17 C20 121.2(6) . . ? C18 C17 C20 120.4(6) . . ? C19 C18 C17 119.0(5) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? N3 C19 C18 122.9(6) . . ? N3 C19 H19 118.5 . . ? C18 C19 H19 118.5 . . ? O10 C20 O9 117.1(15) . . ? O9 C20 O10' 125.9(7) . . ? O10 C20 C17 118.2(12) . . ? O9 C20 C17 117.6(6) . . ? O10' C20 C17 115.0(10) . . ? O14 Eu1 O1W 75.44(13) . . ? O14 Eu1 O2W 92.33(15) . . ? O1W Eu1 O2W 141.21(14) . . ? O14 Eu1 O3 150.82(12) . . ? O1W Eu1 O3 95.00(13) . . ? O2W Eu1 O3 77.87(14) . . ? O14 Eu1 O3W 76.94(14) . . ? O1W Eu1 O3W 72.84(15) . . ? O2W Eu1 O3W 68.54(15) . . ? O3 Eu1 O3W 73.90(14) . . ? O14 Eu1 O2 79.21(12) . . ? O1W Eu1 O2 75.58(12) . . ? O2W Eu1 O2 139.00(12) . . ? O3 Eu1 O2 125.74(11) . . ? O3W Eu1 O2 144.20(13) . . ? O14 Eu1 O8 125.82(11) . . ? O1W Eu1 O8 142.65(13) . . ? O2W Eu1 O8 73.82(14) . . ? O3 Eu1 O8 78.16(12) . . ? O3W Eu1 O8 136.75(14) . . ? O2 Eu1 O8 79.04(12) . . ? O14 Eu1 N1 134.81(13) . . ? O1W Eu1 N1 71.70(13) . . ? O2W Eu1 N1 132.45(15) . . ? O3 Eu1 N1 63.08(12) . . ? O3W Eu1 N1 120.11(16) . . ? O2 Eu1 N1 63.27(11) . . ? O8 Eu1 N1 72.56(12) . . ? O14 Eu1 O7 74.62(11) . . ? O1W Eu1 O7 135.82(12) . . ? O2W Eu1 O7 71.58(12) . . ? O3 Eu1 O7 125.96(11) . . ? O3W Eu1 O7 129.25(15) . . ? O2 Eu1 O7 67.47(11) . . ? O8 Eu1 O7 51.21(10) . . ? N1 Eu1 O7 109.77(11) . . ? O14 Eu1 H2B 87.1 . . ? O1W Eu1 H2B 152.6 . . ? O2W Eu1 H2B 16.9 . . ? O3 Eu1 H2B 90.1 . . ? O3W Eu1 H2B 82.9 . . ? O2 Eu1 H2B 122.2 . . ? O8 Eu1 H2B 64.7 . . ? N1 Eu1 H2B 133.5 . . ? O7 Eu1 H2B 54.7 . . ? O9 Eu2 O6 86.66(15) 1_665 . ? O9 Eu2 O11 151.17(13) 1_665 2_766 ? O6 Eu2 O11 89.24(13) . 2_766 ? O9 Eu2 O7 80.01(13) 1_665 . ? O6 Eu2 O7 127.28(12) . . ? O11 Eu2 O7 79.91(11) 2_766 . ? O9 Eu2 O1 81.47(13) 1_665 2_766 ? O6 Eu2 O1 76.98(13) . 2_766 ? O11 Eu2 O1 125.24(12) 2_766 2_766 ? O7 Eu2 O1 148.09(12) . 2_766 ? O9 Eu2 O2 131.75(13) 1_665 2_766 ? O6 Eu2 O2 71.56(13) . 2_766 ? O11 Eu2 O2 72.97(11) 2_766 2_766 ? O7 Eu2 O2 146.97(11) . 2_766 ? O1 Eu2 O2 52.33(11) 2_766 2_766 ? O9 Eu2 N2 76.26(13) 1_665 . ? O6 Eu2 N2 63.68(13) . . ? O11 Eu2 N2 76.36(12) 2_766 . ? O7 Eu2 N2 63.62(11) . . ? O1 Eu2 N2 135.37(13) 2_766 . ? O2 Eu2 N2 125.18(12) 2_766 . ? O9 Eu2 O12 75.27(13) 1_665 . ? O6 Eu2 O12 148.40(13) . . ? O11 Eu2 O12 118.85(11) 2_766 . ? O7 Eu2 O12 75.40(11) . . ? O1 Eu2 O12 74.88(12) 2_766 . ? O2 Eu2 O12 101.45(12) 2_766 . ? N2 Eu2 O12 133.20(13) . . ? O9 Eu2 O11 127.25(12) 1_665 . ? O6 Eu2 O11 145.34(14) . . ? O11 Eu2 O11 64.68(12) 2_766 . ? O7 Eu2 O11 72.66(11) . . ? O1 Eu2 O11 98.99(12) 2_766 . ? O2 Eu2 O11 78.83(11) 2_766 . ? N2 Eu2 O11 125.28(11) . . ? O12 Eu2 O11 54.77(11) . . ? O9 Eu2 C6 105.68(14) 1_665 2_766 ? O6 Eu2 C6 70.49(14) . 2_766 ? O11 Eu2 C6 99.74(13) 2_766 2_766 ? O7 Eu2 C6 162.07(13) . 2_766 ? O1 Eu2 C6 25.69(12) 2_766 2_766 ? O2 Eu2 C6 26.79(12) 2_766 2_766 ? N2 Eu2 C6 133.99(13) . 2_766 ? O12 Eu2 C6 89.44(13) . 2_766 ? O11 Eu2 C6 90.87(13) . 2_766 ? O9 Eu2 Eu2 150.72(10) 1_665 2_766 ? O6 Eu2 Eu2 119.48(11) . 2_766 ? O11 Eu2 Eu2 33.32(8) 2_766 2_766 ? O7 Eu2 Eu2 73.62(8) . 2_766 ? O1 Eu2 Eu2 115.29(9) 2_766 2_766 ? O2 Eu2 Eu2 73.36(7) 2_766 2_766 ? N2 Eu2 Eu2 102.42(9) . 2_766 ? O12 Eu2 Eu2 85.83(8) . 2_766 ? O11 Eu2 Eu2 31.37(7) . 2_766 ? C6 Eu2 Eu2 96.12(10) 2_766 2_766 ? C5 N1 C1 118.0(4) . . ? C5 N1 Eu1 120.9(3) . . ? C1 N1 Eu1 120.8(3) . . ? C12 N2 C8 118.7(4) . . ? C12 N2 Eu2 120.1(3) . . ? C8 N2 Eu2 121.2(3) . . ? C15 N3 C19 118.1(5) . . ? C15 N3 Zn3 121.5(4) . . ? C19 N3 Zn3 120.4(4) . . ? C6 O1 Eu2 94.5(3) . 2_766 ? C6 O2 Eu1 123.4(3) . . ? C6 O2 Eu2 90.8(3) . 2_766 ? Eu1 O2 Eu2 141.65(14) . 2_766 ? C7 O3 Eu1 125.6(3) . . ? C7 O4 Zn3 133.9(3) . . ? C13 O6 Eu2 125.9(3) . . ? C14 O7 Eu2 123.7(3) . . ? C14 O7 Eu1 91.8(3) . . ? Eu2 O7 Eu1 142.77(14) . . ? C14 O8 Eu1 95.6(3) . . ? C20 O9 Eu2 141.9(4) . 1_445 ? S1 O11 Eu2 141.86(19) . 2_766 ? S1 O11 Eu2 99.34(17) . . ? Eu2 O11 Eu2 115.32(12) 2_766 . ? S1 O12 Eu2 100.89(17) . . ? S1 O14 Eu1 138.1(2) . . ? Eu1 O1W H1A 122.8 . . ? Eu1 O1W H1B 113.0 . . ? H1A O1W H1B 107.7 . . ? Eu1 O2W H2A 145.6 . . ? Eu1 O2W H2B 106.7 . . ? H2A O2W H2B 107.7 . . ? Zn3 O4W H4B 141.6 . . ? Zn3 O4W H4A 113.3 . . ? H4B O4W H4A 100.9 . . ? H5A O5W H5B 107.7 . . ? H7A O7W H7B 107.7 . . ? O13 S1 O14 111.0(2) . . ? O13 S1 O12 112.1(2) . . ? O14 S1 O12 109.4(2) . . ? O13 S1 O11 111.4(2) . . ? O14 S1 O11 109.0(2) . . ? O12 S1 O11 103.7(2) . . ? O4 Zn3 O4 180.00(18) . 2 ? O4 Zn3 N3 90.80(16) . 2 ? O4 Zn3 N3 89.20(16) 2 2 ? O4 Zn3 N3 89.20(16) . . ? O4 Zn3 N3 90.80(16) 2 . ? N3 Zn3 N3 180.0(2) 2 . ? O4 Zn3 O4W 90.12(14) . . ? O4 Zn3 O4W 89.88(14) 2 . ? N3 Zn3 O4W 88.83(15) 2 . ? N3 Zn3 O4W 91.17(15) . . ? O4 Zn3 O4W 89.88(14) . 2 ? O4 Zn3 O4W 90.12(14) 2 2 ? N3 Zn3 O4W 91.17(15) 2 2 ? N3 Zn3 O4W 88.83(15) . 2 ? O4W Zn3 O4W 180.0(3) . 2 ? Eu1 O3W H3A 120.2 . . ? Eu1 O3W H3B 127.6 . . ? H3A O3W H3B 107.7 . . ? H6A O6W H6B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.031 _refine_diff_density_min -1.014 _refine_diff_density_rms 0.131 data_2 _database_code_depnum_ccdc_archive 'CCDC 757993' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C40 H36 N6 O36 S2 Tb4 Zn, 5H2O' _chemical_formula_sum 'C40 H46 N6 O41 S2 Tb4 Zn' _chemical_formula_weight 2032.00 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' Zn Zn 0.2839 1.4301 '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' 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9441(13) _cell_length_b 12.4765(15) _cell_length_c 12.7277(16) _cell_angle_alpha 105.947(2) _cell_angle_beta 98.136(2) _cell_angle_gamma 115.5680(10) _cell_volume 1438.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5052 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 978 _exptl_absorpt_coefficient_mu 5.456 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3940 _exptl_absorpt_correction_T_max 0.5482 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _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 AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7148 _diffrn_reflns_av_R_equivalents 0.0153 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.20 _reflns_number_total 5052 _reflns_number_gt 4289 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0256P)^2^+3.8587P] 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 5052 _refine_ls_number_parameters 440 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0605 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 C1 C -0.7035(5) -0.3140(5) 0.1575(5) 0.0320(12) Uani 1 1 d . . . C2 C -0.5725(5) -0.2062(4) 0.2536(4) 0.0233(10) Uani 1 1 d . . . C3 C -0.5548(6) -0.1912(5) 0.3669(4) 0.0319(12) Uani 1 1 d . . . H3 H -0.6253 -0.2482 0.3880 0.038 Uiso 1 1 calc R . . C4 C -0.4311(6) -0.0906(5) 0.4491(4) 0.0326(12) Uani 1 1 d . . . H4 H -0.4165 -0.0798 0.5259 0.039 Uiso 1 1 calc R . . C5 C -0.3293(5) -0.0062(5) 0.4144(4) 0.0275(11) Uani 1 1 d . . . H5 H -0.2460 0.0636 0.4677 0.033 Uiso 1 1 calc R . . C6 C -0.3547(5) -0.0281(4) 0.2990(4) 0.0200(10) Uani 1 1 d . . . C7 C -0.2512(5) 0.0505(4) 0.2488(4) 0.0188(10) Uani 1 1 d . . . C8 C -0.2596(5) 0.3380(5) 0.1873(4) 0.0232(10) Uani 1 1 d . . . C9 C -0.1261(5) 0.4378(4) 0.2817(4) 0.0214(10) Uani 1 1 d . . . C10 C -0.1085(5) 0.5524(5) 0.3497(4) 0.0295(12) Uani 1 1 d . . . H10 H -0.1806 0.5725 0.3385 0.035 Uiso 1 1 calc R . . C11 C 0.0189(5) 0.6382(5) 0.4356(4) 0.0298(12) Uani 1 1 d . . . H11 H 0.0341 0.7171 0.4831 0.036 Uiso 1 1 calc R . . C12 C 0.1224(5) 0.6042(5) 0.4493(4) 0.0262(11) Uani 1 1 d . . . H12 H 0.2085 0.6593 0.5068 0.031 Uiso 1 1 calc R . . C13 C 0.0957(5) 0.4859(4) 0.3754(4) 0.0200(10) Uani 1 1 d . . . C14 C 0.1982(5) 0.4367(5) 0.3833(4) 0.0225(10) Uani 1 1 d . . . C15 C 0.6794(5) 0.6841(5) 0.4009(4) 0.0282(11) Uani 1 1 d . . . H15 H 0.7351 0.7283 0.4771 0.034 Uiso 1 1 calc R . . C16 C 0.7254(6) 0.7330(5) 0.3214(5) 0.0323(12) Uani 1 1 d . . . H16 H 0.8121 0.8077 0.3435 0.039 Uiso 1 1 calc R . . C17 C 0.6425(6) 0.6711(5) 0.2081(5) 0.0305(12) Uani 1 1 d . A . C18 C 0.5143(6) 0.5614(5) 0.1799(5) 0.0343(12) Uani 1 1 d . . . H18 H 0.4542 0.5190 0.1051 0.041 Uiso 1 1 calc R . . C19 C 0.4759(6) 0.5150(5) 0.2648(5) 0.0341(12) Uani 1 1 d . . . H19 H 0.3906 0.4395 0.2447 0.041 Uiso 1 1 calc R . . C20 C 0.6903(6) 0.7245(6) 0.1198(5) 0.0378(13) Uani 1 1 d . . . N1 N -0.4745(4) -0.1261(4) 0.2194(3) 0.0206(8) Uani 1 1 d . . . N2 N -0.0262(4) 0.4039(4) 0.2928(3) 0.0200(8) Uani 1 1 d . . . N3 N 0.5568(4) 0.5747(4) 0.3735(3) 0.0258(9) Uani 1 1 d . . . O1 O -0.7948(4) -0.3977(4) 0.1795(3) 0.0513(12) Uani 1 1 d . . . O2 O -0.7059(4) -0.3072(4) 0.0584(3) 0.0376(9) Uani 1 1 d . . . O3 O -0.2809(3) 0.0085(3) 0.1394(3) 0.0202(7) Uani 1 1 d . . . O4 O -0.1387(3) 0.1501(3) 0.3103(3) 0.0301(8) Uani 1 1 d . . . O5 O -0.2636(3) 0.2345(3) 0.1309(3) 0.0202(7) Uani 1 1 d . . . O6 O -0.3600(4) 0.3580(3) 0.1650(3) 0.0350(9) Uani 1 1 d . . . O7 O 0.1611(3) 0.3292(3) 0.3076(3) 0.0290(8) Uani 1 1 d . . . O8 O 0.3122(3) 0.5051(3) 0.4633(3) 0.0296(8) Uani 1 1 d . . . O9 O -0.1777(3) 0.0823(3) -0.0497(3) 0.0292(8) Uani 1 1 d . . . O10 O -0.4301(3) 0.0024(3) -0.0764(3) 0.0219(7) Uani 1 1 d . . . O11 O -0.3453(4) -0.1429(3) -0.1116(3) 0.0291(8) Uani 1 1 d . . . O12 O -0.3399(4) -0.0301(4) -0.2396(3) 0.0362(9) Uani 1 1 d . . . O13 O 0.5982(4) 0.7183(3) 0.0442(3) 0.0320(8) Uani 1 1 d . . . O14 O 0.8239(8) 0.7817(14) 0.1340(9) 0.061(4) Uani 0.84(3) 1 d P A 1 O14' O 0.778(3) 0.699(4) 0.089(3) 0.026(9) Uani 0.16(3) 1 d PU A 2 O1W O 0.0031(4) 0.0437(4) 0.1699(4) 0.0537(12) Uani 1 1 d . . . H1A H 0.0051 -0.0207 0.1277 0.081 Uiso 1 1 d R . . H1B H -0.0293 0.0704 0.1246 0.081 Uiso 1 1 d R . . O2W O 0.1339(4) 0.2164(5) 0.0704(3) 0.0491(11) Uani 1 1 d . . . H2A H 0.1904 0.1897 0.0876 0.074 Uiso 1 1 d R . . H2B H 0.1438 0.2280 0.0089 0.074 Uiso 1 1 d R . . O3W O -0.0070(4) 0.3598(3) 0.0612(3) 0.0339(9) Uani 1 1 d . . . H3A H 0.0298 0.4325 0.1154 0.051 Uiso 1 1 d R . . H3B H -0.0955 0.3325 0.0369 0.051 Uiso 1 1 d R . . O4W O 0.3967(4) 0.3043(4) 0.3741(3) 0.0389(9) Uani 1 1 d . . . H4A H 0.4145 0.2521 0.3298 0.058 Uiso 1 1 d R . . H4B H 0.3139 0.2864 0.3392 0.058 Uiso 1 1 d R . . O5W O 0.8820(8) 0.1422(8) 0.6966(6) 0.137(3) Uani 1 1 d . . . H5A H 0.8419 0.1095 0.7414 0.206 Uiso 1 1 d R . . H5B H 0.9514 0.2152 0.7405 0.206 Uiso 1 1 d R . . O6W O 0.9493(7) 0.9648(7) 0.5874(6) 0.132(3) Uani 1 1 d . . . H6A H 0.9702 0.9191 0.6164 0.198 Uiso 1 1 d R . . H6B H 0.8962 0.9827 0.6226 0.198 Uiso 1 1 d R . . O7W O 0.069(3) 0.400(3) 0.875(2) 0.237(13) Uani 0.50 1 d P . . H7A H 0.0284 0.3980 0.9272 0.355 Uiso 0.50 1 d PR . . H7B H 0.1504 0.4093 0.9023 0.355 Uiso 0.50 1 d PR . . S1 S -0.32084(12) -0.02109(11) -0.12239(9) 0.0203(2) Uani 1 1 d . . . Tb1 Tb -0.50939(2) -0.16718(2) 0.011242(17) 0.01751(7) Uani 1 1 d . . . Tb2 Tb -0.05683(2) 0.20404(2) 0.149408(17) 0.01744(7) Uani 1 1 d . . . Zn1 Zn 0.5000 0.5000 0.5000 0.02287(17) Uani 1 2 d S . . 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 C1 0.022(3) 0.029(3) 0.035(3) 0.012(2) 0.008(2) 0.004(2) C2 0.022(2) 0.022(2) 0.025(3) 0.009(2) 0.008(2) 0.009(2) C3 0.031(3) 0.033(3) 0.030(3) 0.015(2) 0.017(2) 0.010(2) C4 0.037(3) 0.040(3) 0.021(3) 0.014(2) 0.011(2) 0.017(3) C5 0.026(3) 0.027(3) 0.022(3) 0.006(2) 0.008(2) 0.009(2) C6 0.021(2) 0.019(2) 0.017(2) 0.0060(19) 0.0055(18) 0.008(2) C7 0.015(2) 0.019(2) 0.018(2) 0.0055(19) 0.0012(18) 0.007(2) C8 0.016(2) 0.029(3) 0.021(2) 0.009(2) 0.0021(19) 0.010(2) C9 0.017(2) 0.021(2) 0.017(2) 0.0006(19) -0.0003(18) 0.007(2) C10 0.027(3) 0.028(3) 0.028(3) 0.000(2) 0.000(2) 0.018(2) C11 0.029(3) 0.021(3) 0.025(3) -0.002(2) 0.001(2) 0.009(2) C12 0.021(2) 0.025(3) 0.020(2) 0.003(2) 0.0007(19) 0.005(2) C13 0.018(2) 0.022(2) 0.023(2) 0.014(2) 0.0089(19) 0.008(2) C14 0.017(2) 0.030(3) 0.018(2) 0.010(2) 0.0046(19) 0.008(2) C15 0.027(3) 0.033(3) 0.028(3) 0.015(2) 0.009(2) 0.017(2) C16 0.026(3) 0.035(3) 0.046(3) 0.023(3) 0.015(2) 0.017(2) C17 0.037(3) 0.037(3) 0.038(3) 0.023(3) 0.021(2) 0.028(3) C18 0.041(3) 0.039(3) 0.028(3) 0.015(2) 0.010(2) 0.022(3) C19 0.035(3) 0.031(3) 0.032(3) 0.014(2) 0.011(2) 0.011(2) C20 0.045(3) 0.051(4) 0.044(3) 0.032(3) 0.021(3) 0.034(3) N1 0.0183(19) 0.017(2) 0.023(2) 0.0068(16) 0.0063(16) 0.0060(17) N2 0.0155(19) 0.023(2) 0.0169(19) 0.0050(16) 0.0010(15) 0.0080(17) N3 0.025(2) 0.029(2) 0.024(2) 0.0114(18) 0.0070(17) 0.0131(19) O1 0.043(2) 0.041(2) 0.039(2) 0.018(2) 0.0135(19) -0.008(2) O2 0.029(2) 0.036(2) 0.027(2) 0.0118(17) 0.0032(15) -0.0002(17) O3 0.0161(15) 0.0208(17) 0.0170(16) 0.0062(13) 0.0016(12) 0.0051(14) O4 0.0246(18) 0.0243(19) 0.0217(18) 0.0048(15) 0.0014(14) -0.0003(16) O5 0.0151(15) 0.0172(16) 0.0202(16) 0.0011(13) 0.0004(12) 0.0061(13) O6 0.0236(18) 0.034(2) 0.035(2) -0.0053(16) -0.0067(15) 0.0191(17) O7 0.0188(16) 0.031(2) 0.0288(19) 0.0034(16) -0.0011(14) 0.0120(15) O8 0.0190(17) 0.038(2) 0.0221(17) 0.0030(15) -0.0030(14) 0.0133(16) O9 0.0191(17) 0.0304(19) 0.0206(17) 0.0033(15) 0.0036(14) 0.0022(15) O10 0.0213(16) 0.0227(17) 0.0214(17) 0.0073(14) 0.0072(13) 0.0111(14) O11 0.0282(18) 0.0247(18) 0.039(2) 0.0120(16) 0.0127(16) 0.0160(16) O12 0.034(2) 0.053(2) 0.0180(18) 0.0121(17) 0.0082(15) 0.0188(19) O13 0.043(2) 0.034(2) 0.0279(19) 0.0153(16) 0.0117(17) 0.0239(18) O14 0.031(4) 0.099(10) 0.070(6) 0.062(7) 0.019(4) 0.028(5) O14' 0.018(11) 0.032(14) 0.031(12) 0.016(9) 0.014(7) 0.010(9) O1W 0.042(2) 0.044(3) 0.100(4) 0.041(3) 0.029(2) 0.031(2) O2W 0.044(2) 0.096(4) 0.042(2) 0.041(2) 0.025(2) 0.051(3) O3W 0.0306(19) 0.0256(19) 0.037(2) 0.0119(16) 0.0088(16) 0.0073(16) O4W 0.042(2) 0.036(2) 0.030(2) 0.0027(17) 0.0027(17) 0.0207(19) O5W 0.129(6) 0.152(7) 0.083(5) 0.066(5) 0.041(5) 0.013(5) O6W 0.085(5) 0.113(6) 0.147(7) 0.085(5) -0.033(4) 0.004(4) O7W 0.28(3) 0.34(4) 0.19(2) 0.17(2) 0.13(2) 0.18(3) S1 0.0178(5) 0.0238(6) 0.0148(5) 0.0042(5) 0.0037(4) 0.0087(5) Tb1 0.01400(11) 0.01767(12) 0.01592(12) 0.00437(9) 0.00112(8) 0.00588(9) Tb2 0.01389(11) 0.01813(12) 0.01740(12) 0.00535(9) 0.00274(8) 0.00688(9) Zn1 0.0169(4) 0.0286(4) 0.0220(4) 0.0109(3) 0.0045(3) 0.0100(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.228(6) . ? C1 O2 1.284(6) . ? C1 C2 1.515(7) . ? C2 N1 1.336(6) . ? C2 C3 1.375(7) . ? C3 C4 1.383(7) . ? C3 H3 0.9300 . ? C4 C5 1.388(7) . ? C4 H4 0.9300 . ? C5 C6 1.381(7) . ? C5 H5 0.9300 . ? C6 N1 1.342(6) . ? C6 C7 1.498(6) . ? C7 O4 1.243(5) . ? C7 O3 1.282(5) . ? C8 O6 1.240(6) . ? C8 O5 1.271(6) . ? C8 C9 1.497(6) . ? C9 N2 1.336(6) . ? C9 C10 1.365(7) . ? C10 C11 1.387(7) . ? C10 H10 0.9300 . ? C11 C12 1.375(7) . ? C11 H11 0.9300 . ? C12 C13 1.392(7) . ? C12 H12 0.9300 . ? C13 N2 1.329(6) . ? C13 C14 1.497(7) . ? C14 O8 1.252(5) . ? C14 O7 1.265(6) . ? C15 N3 1.346(6) . ? C15 C16 1.366(7) . ? C15 H15 0.9300 . ? C16 C17 1.383(8) . ? C16 H16 0.9300 . ? C17 C18 1.378(8) . ? C17 C20 1.502(7) . ? C18 C19 1.394(7) . ? C18 H18 0.9300 . ? C19 N3 1.331(6) . ? C19 H19 0.9300 . ? C20 O14' 1.21(2) . ? C20 O13 1.251(6) . ? C20 O14 1.278(9) . ? N1 Tb1 2.496(4) . ? N2 Tb2 2.503(4) . ? N3 Zn1 2.110(4) . ? O2 Tb1 2.395(4) . ? O3 Tb1 2.422(3) . ? O3 Tb2 2.561(3) . ? O4 Tb2 2.491(3) . ? O5 Tb2 2.442(3) . ? O5 Tb1 2.499(3) 2_455 ? O6 Tb1 2.442(3) 2_455 ? O7 Tb2 2.424(3) . ? O8 Zn1 2.074(3) . ? O9 S1 1.471(3) . ? O9 Tb2 2.384(3) . ? O10 S1 1.504(3) . ? O10 Tb1 2.398(3) 2_455 ? O10 Tb1 2.542(3) . ? O11 S1 1.475(4) . ? O11 Tb1 2.520(3) . ? O12 S1 1.443(4) . ? O13 Tb1 2.290(4) 1_665 ? O1W Tb2 2.423(4) . ? O1W H1A 0.8461 . ? O1W H1B 0.8483 . ? O2W Tb2 2.407(4) . ? O2W H2A 0.8497 . ? O2W H2B 0.8472 . ? O3W Tb2 2.407(4) . ? O3W H3A 0.8499 . ? O3W H3B 0.8500 . ? O4W Zn1 2.182(4) . ? O4W H4A 0.8474 . ? O4W H4B 0.8510 . ? O5W H5A 0.8521 . ? O5W H5B 0.8496 . ? O6W H6A 0.8472 . ? O6W H6B 0.8480 . ? O7W H7A 0.8500 . ? O7W H7B 0.8500 . ? Tb1 O13 2.290(4) 1_445 ? Tb1 O10 2.398(3) 2_455 ? Tb1 O6 2.442(3) 2_455 ? Tb1 O5 2.499(3) 2_455 ? Zn1 O8 2.074(3) 2_666 ? Zn1 N3 2.110(4) 2_666 ? Zn1 O4W 2.182(4) 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 O1 C1 O2 126.5(5) . . ? O1 C1 C2 119.1(5) . . ? O2 C1 C2 114.5(4) . . ? N1 C2 C3 122.3(4) . . ? N1 C2 C1 114.4(4) . . ? C3 C2 C1 123.3(4) . . ? C2 C3 C4 119.5(5) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 118.6(5) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C6 C5 C4 118.5(5) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? N1 C6 C5 122.8(4) . . ? N1 C6 C7 112.9(4) . . ? C5 C6 C7 124.3(4) . . ? O4 C7 O3 121.0(4) . . ? O4 C7 C6 121.7(4) . . ? O3 C7 C6 117.2(4) . . ? O6 C8 O5 122.3(4) . . ? O6 C8 C9 120.5(4) . . ? O5 C8 C9 117.2(4) . . ? O6 C8 Tb1 60.1(2) . 2_455 ? O5 C8 Tb1 62.7(2) . 2_455 ? C9 C8 Tb1 171.6(3) . 2_455 ? N2 C9 C10 123.5(4) . . ? N2 C9 C8 113.4(4) . . ? C10 C9 C8 123.1(4) . . ? C9 C10 C11 118.7(5) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? C12 C11 C10 118.7(5) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C11 C12 C13 118.7(4) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? N2 C13 C12 122.6(4) . . ? N2 C13 C14 113.5(4) . . ? C12 C13 C14 123.8(4) . . ? O8 C14 O7 126.1(5) . . ? O8 C14 C13 117.4(4) . . ? O7 C14 C13 116.5(4) . . ? N3 C15 C16 122.8(5) . . ? N3 C15 H15 118.6 . . ? C16 C15 H15 118.6 . . ? C15 C16 C17 119.7(5) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 118.0(5) . . ? C18 C17 C20 121.5(5) . . ? C16 C17 C20 120.5(5) . . ? C17 C18 C19 119.2(5) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? N3 C19 C18 122.4(5) . . ? N3 C19 H19 118.8 . . ? C18 C19 H19 118.8 . . ? O14' C20 O13 116.7(14) . . ? O13 C20 O14 125.4(5) . . ? O14' C20 C17 112.3(13) . . ? O13 C20 C17 117.7(5) . . ? O14 C20 C17 116.7(5) . . ? C2 N1 C6 118.4(4) . . ? C2 N1 Tb1 120.2(3) . . ? C6 N1 Tb1 121.3(3) . . ? C13 N2 C9 117.8(4) . . ? C13 N2 Tb2 120.9(3) . . ? C9 N2 Tb2 121.0(3) . . ? C19 N3 C15 117.8(4) . . ? C19 N3 Zn1 121.9(3) . . ? C15 N3 Zn1 120.2(3) . . ? C1 O2 Tb1 125.6(3) . . ? C7 O3 Tb1 123.6(3) . . ? C7 O3 Tb2 91.5(2) . . ? Tb1 O3 Tb2 142.99(13) . . ? C7 O4 Tb2 95.8(3) . . ? C8 O5 Tb2 123.6(3) . . ? C8 O5 Tb1 90.4(3) . 2_455 ? Tb2 O5 Tb1 141.71(13) . 2_455 ? C8 O6 Tb1 93.8(3) . 2_455 ? C14 O7 Tb2 124.9(3) . . ? C14 O8 Zn1 133.7(3) . . ? S1 O9 Tb2 137.7(2) . . ? S1 O10 Tb1 141.50(19) . 2_455 ? S1 O10 Tb1 99.02(16) . . ? Tb1 O10 Tb1 115.50(12) 2_455 . ? S1 O11 Tb1 100.85(17) . . ? C20 O13 Tb1 140.5(4) . 1_665 ? Tb2 O1W H1A 138.6 . . ? H1A O1W H1B 105.7 . . ? Tb2 O2W H2A 126.0 . . ? Tb2 O2W H2B 126.7 . . ? H2A O2W H2B 105.3 . . ? Tb2 O3W H3A 106.4 . . ? Tb2 O3W H3B 89.4 . . ? H3A O3W H3B 107.7 . . ? Zn1 O4W H4A 141.6 . . ? Zn1 O4W H4B 107.1 . . ? H4A O4W H4B 105.3 . . ? H5A O5W H5B 105.0 . . ? H6A O6W H6B 105.9 . . ? H7A O7W H7B 107.7 . . ? O12 S1 O9 110.5(2) . . ? O12 S1 O11 112.1(2) . . ? O9 S1 O11 109.8(2) . . ? O12 S1 O10 111.2(2) . . ? O9 S1 O10 109.56(19) . . ? O11 S1 O10 103.50(19) . . ? O13 Tb1 O2 87.49(14) 1_445 . ? O13 Tb1 O10 151.65(11) 1_445 2_455 ? O2 Tb1 O10 88.90(12) . 2_455 ? O13 Tb1 O3 80.74(12) 1_445 . ? O2 Tb1 O3 128.39(11) . . ? O10 Tb1 O3 79.59(10) 2_455 . ? O13 Tb1 O6 80.14(12) 1_445 2_455 ? O2 Tb1 O6 76.61(13) . 2_455 ? O10 Tb1 O6 126.15(11) 2_455 2_455 ? O3 Tb1 O6 147.50(11) . 2_455 ? O13 Tb1 N1 76.62(12) 1_445 . ? O2 Tb1 N1 64.23(12) . . ? O10 Tb1 N1 76.51(12) 2_455 . ? O3 Tb1 N1 64.16(11) . . ? O6 Tb1 N1 134.80(13) 2_455 . ? O13 Tb1 O5 130.99(11) 1_445 2_455 ? O2 Tb1 O5 70.43(11) . 2_455 ? O10 Tb1 O5 73.34(10) 2_455 2_455 ? O3 Tb1 O5 146.87(10) . 2_455 ? O6 Tb1 O5 52.86(10) 2_455 2_455 ? N1 Tb1 O5 125.15(11) . 2_455 ? O13 Tb1 O11 75.09(12) 1_445 . ? O2 Tb1 O11 148.13(12) . . ? O10 Tb1 O11 118.86(11) 2_455 . ? O3 Tb1 O11 75.55(11) . . ? O6 Tb1 O11 74.27(12) 2_455 . ? N1 Tb1 O11 133.62(12) . . ? O5 Tb1 O11 101.10(11) 2_455 . ? O13 Tb1 O10 127.65(11) 1_445 . ? O2 Tb1 O10 143.78(12) . . ? O10 Tb1 O10 64.50(12) 2_455 . ? O3 Tb1 O10 72.98(10) . . ? O6 Tb1 O10 98.84(12) 2_455 . ? N1 Tb1 O10 126.02(11) . . ? O5 Tb1 O10 78.27(10) 2_455 . ? O11 Tb1 O10 55.05(10) . . ? O13 Tb1 C8 104.80(14) 1_445 2_455 ? O2 Tb1 C8 69.62(13) . 2_455 ? O10 Tb1 C8 100.22(12) 2_455 2_455 ? O3 Tb1 C8 161.81(12) . 2_455 ? O6 Tb1 C8 26.12(12) 2_455 2_455 ? N1 Tb1 C8 133.75(13) . 2_455 ? O5 Tb1 C8 26.89(12) 2_455 2_455 ? O11 Tb1 C8 88.99(12) . 2_455 ? O10 Tb1 C8 90.40(12) . 2_455 ? O9 Tb2 O2W 77.33(13) . . ? O9 Tb2 O3W 74.73(12) . . ? O2W Tb2 O3W 72.15(14) . . ? O9 Tb2 O1W 92.03(15) . . ? O2W Tb2 O1W 69.86(15) . . ? O3W Tb2 O1W 141.66(14) . . ? O9 Tb2 O7 150.19(11) . . ? O2W Tb2 O7 72.87(13) . . ? O3W Tb2 O7 96.51(12) . . ? O1W Tb2 O7 77.20(14) . . ? O9 Tb2 O5 79.53(11) . . ? O2W Tb2 O5 144.03(12) . . ? O3W Tb2 O5 75.42(12) . . ? O1W Tb2 O5 138.33(12) . . ? O7 Tb2 O5 126.57(11) . . ? O9 Tb2 O4 126.20(11) . . ? O2W Tb2 O4 136.85(13) . . ? O3W Tb2 O4 142.99(12) . . ? O1W Tb2 O4 73.39(14) . . ? O7 Tb2 O4 77.68(11) . . ? O5 Tb2 O4 79.11(11) . . ? O9 Tb2 N2 135.47(12) . . ? O2W Tb2 N2 118.77(14) . . ? O3W Tb2 N2 72.45(12) . . ? O1W Tb2 N2 132.08(15) . . ? O7 Tb2 N2 63.55(11) . . ? O5 Tb2 N2 63.72(11) . . ? O4 Tb2 N2 72.34(12) . . ? O9 Tb2 O3 74.65(10) . . ? O2W Tb2 O3 130.29(13) . . ? O3W Tb2 O3 135.14(11) . . ? O1W Tb2 O3 71.01(12) . . ? O7 Tb2 O3 125.51(11) . . ? O5 Tb2 O3 67.39(10) . . ? O4 Tb2 O3 51.56(10) . . ? N2 Tb2 O3 110.03(11) . . ? O9 Tb2 H1B 77.2 . . ? O2W Tb2 H1B 64.2 . . ? O3W Tb2 H1B 132.0 . . ? O1W Tb2 H1B 15.1 . . ? O7 Tb2 H1B 89.1 . . ? O5 Tb2 H1B 135.5 . . ? O4 Tb2 H1B 84.8 . . ? N2 Tb2 H1B 147.1 . . ? O3 Tb2 H1B 70.1 . . ? O9 Tb2 H3B 65.7 . . ? O2W Tb2 H3B 87.6 . . ? O3W Tb2 H3B 19.5 . . ? O1W Tb2 H3B 151.7 . . ? O7 Tb2 H3B 113.1 . . ? O5 Tb2 H3B 57.7 . . ? O4 Tb2 H3B 133.5 . . ? N2 Tb2 H3B 73.4 . . ? O3 Tb2 H3B 115.9 . . ? H1B Tb2 H3B 137.7 . . ? O8 Zn1 O8 180.000(1) . 2_666 ? O8 Zn1 N3 89.17(15) . . ? O8 Zn1 N3 90.83(15) 2_666 . ? O8 Zn1 N3 90.83(15) . 2_666 ? O8 Zn1 N3 89.17(15) 2_666 2_666 ? N3 Zn1 N3 180.0(2) . 2_666 ? O8 Zn1 O4W 89.45(14) . 2_666 ? O8 Zn1 O4W 90.55(14) 2_666 2_666 ? N3 Zn1 O4W 89.06(15) . 2_666 ? N3 Zn1 O4W 90.94(15) 2_666 2_666 ? O8 Zn1 O4W 90.55(14) . . ? O8 Zn1 O4W 89.45(14) 2_666 . ? N3 Zn1 O4W 90.94(15) . . ? N3 Zn1 O4W 89.06(15) 2_666 . ? O4W Zn1 O4W 180.0 2_666 . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.955 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.119 data_3 _database_code_depnum_ccdc_archive 'CCDC 757994' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H36 Gd4 Mn N6 O36 S2, 5H2O' _chemical_formula_sum 'C40 H46 Gd4 Mn N6 O41 S2' _chemical_formula_weight 2014.89 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' Mn Mn 0.3368 0.7283 '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' 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0202(6) _cell_length_b 12.5108(6) _cell_length_c 12.9049(11) _cell_angle_alpha 106.6032(10) _cell_angle_beta 97.7810(11) _cell_angle_gamma 115.5960(10) _cell_volume 1467.10(16) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5196 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 969 _exptl_absorpt_coefficient_mu 4.855 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5036 _exptl_absorpt_correction_T_max 0.5852 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _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 AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7636 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.20 _reflns_number_total 5196 _reflns_number_gt 4616 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0263P)^2^+1.6274P] 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 5196 _refine_ls_number_parameters 440 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0623 _refine_ls_wR_factor_gt 0.0600 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 C1 C 0.2986(5) 0.1858(5) 0.1553(4) 0.0341(12) Uani 1 1 d . . . C2 C 0.4288(5) 0.2951(4) 0.2509(4) 0.0262(10) Uani 1 1 d . . . C3 C 0.4474(5) 0.3106(5) 0.3632(4) 0.0312(11) Uani 1 1 d . . . H3 H 0.3782 0.2532 0.3841 0.037 Uiso 1 1 calc R . . C4 C 0.5697(5) 0.4122(5) 0.4439(4) 0.0336(12) Uani 1 1 d . . . H4 H 0.5845 0.4238 0.5199 0.040 Uiso 1 1 calc R . . C5 C 0.6694(5) 0.4959(4) 0.4102(4) 0.0293(11) Uani 1 1 d . . . H5 H 0.7519 0.5662 0.4631 0.035 Uiso 1 1 calc R . . C6 C 0.6444(4) 0.4734(4) 0.2957(3) 0.0199(9) Uani 1 1 d . . . C7 C 0.7485(5) 0.5517(4) 0.2467(4) 0.0219(9) Uani 1 1 d . . . C8 C 0.7418(4) 0.8406(4) 0.1877(3) 0.0220(9) Uani 1 1 d . . . C9 C 0.8737(4) 0.9395(4) 0.2822(4) 0.0219(9) Uani 1 1 d . . . C10 C 0.8913(5) 1.0538(4) 0.3530(4) 0.0300(11) Uani 1 1 d . . . H10 H 0.8194 1.0736 0.3437 0.036 Uiso 1 1 calc R . . C11 C 1.0165(5) 1.1388(4) 0.4376(4) 0.0298(11) Uani 1 1 d . . . H11 H 1.0310 1.2174 0.4855 0.036 Uiso 1 1 calc R . . C12 C 1.1205(5) 1.1057(4) 0.4504(4) 0.0249(10) Uani 1 1 d . . . H12 H 1.2057 1.1610 0.5076 0.030 Uiso 1 1 calc R . . C13 C 1.0947(4) 0.9880(4) 0.3759(4) 0.0209(9) Uani 1 1 d . . . C14 C 1.1957(5) 0.9381(4) 0.3811(4) 0.0231(10) Uani 1 1 d . . . C15 C 1.4775(6) 1.0171(5) 0.2586(4) 0.0382(13) Uani 1 1 d . . . H15 H 1.3933 0.9410 0.2384 0.046 Uiso 1 1 calc R . . C16 C 1.5151(6) 1.0627(5) 0.1750(4) 0.0374(12) Uani 1 1 d . . . H16 H 1.4552 1.0201 0.1011 0.045 Uiso 1 1 calc R . . C17 C 1.6431(5) 1.1726(5) 0.2040(4) 0.0309(11) Uani 1 1 d . A . C18 C 1.7265(6) 1.2355(5) 0.3147(5) 0.0361(12) Uani 1 1 d . . . H18 H 1.8135 1.3092 0.3359 0.043 Uiso 1 1 calc R . . C19 C 1.6792(5) 1.1874(5) 0.3942(4) 0.0312(11) Uani 1 1 d . . . H19 H 1.7341 1.2329 0.4697 0.037 Uiso 1 1 calc R . . C20 C 1.6904(7) 1.2229(6) 0.1154(5) 0.0453(15) Uani 1 1 d . . . Gd1 Gd 0.48988(2) 0.331618(18) 0.009785(16) 0.01808(7) Uani 1 1 d . . . Gd2 Gd 0.94200(2) 0.703983(18) 0.148313(16) 0.01711(7) Uani 1 1 d . . . Mn1 Mn 1.5000 1.0000 0.5000 0.0219(2) Uani 1 2 d S . . N1 N 0.5254(4) 0.3743(3) 0.2173(3) 0.0209(8) Uani 1 1 d . . . N2 N 0.9727(4) 0.9061(3) 0.2931(3) 0.0205(8) Uani 1 1 d . . . N3 N 1.5580(4) 1.0786(4) 0.3677(3) 0.0278(9) Uani 1 1 d . . . O1 O 0.2087(4) 0.1033(4) 0.1784(3) 0.0593(12) Uani 1 1 d . . . O2 O 0.2955(4) 0.1905(3) 0.0578(3) 0.0431(10) Uani 1 1 d . . . O3 O 0.7184(3) 0.5092(3) 0.1384(2) 0.0211(6) Uani 1 1 d . . . O4 O 0.8601(3) 0.6513(3) 0.3082(2) 0.0313(8) Uani 1 1 d . . . O5 O 0.5703(3) 0.5016(3) -0.0769(2) 0.0231(7) Uani 1 1 d . . . O6 O 0.6556(3) 0.3572(3) -0.1102(3) 0.0302(7) Uani 1 1 d . . . O7 O 0.6585(4) 0.4655(3) -0.2391(3) 0.0352(8) Uani 1 1 d . . . O8 O 0.8201(3) 0.5820(3) -0.0504(3) 0.0308(8) Uani 1 1 d . . . O9 O 0.6421(3) 0.8611(3) 0.1666(3) 0.0336(8) Uani 1 1 d . . . O10 O 0.7367(3) 0.7366(3) 0.1309(2) 0.0212(6) Uani 1 1 d . . . O11 O 1.1592(3) 0.8318(3) 0.3044(3) 0.0290(7) Uani 1 1 d . . . O12 O 1.3079(3) 1.0054(3) 0.4611(3) 0.0320(8) Uani 1 1 d . . . O13 O 1.5984(4) 1.2176(3) 0.0417(3) 0.0339(8) Uani 1 1 d . . . O14 O 1.831(2) 1.295(4) 0.141(3) 0.046(6) Uani 0.51(11) 1 d P A 1 O14' O 1.793(7) 1.230(10) 0.098(6) 0.078(17) Uani 0.49(11) 1 d P A 2 O1W O 0.0488(6) 0.5313(7) 0.4091(6) 0.142(3) Uani 1 1 d . . . H1A H 0.0324 0.5632 0.3626 0.212 Uiso 1 1 d R . . H1B H 0.1360 0.5543 0.4254 0.212 Uiso 1 1 d R . . O2W O 0.8702(7) 0.6383(7) 0.6917(5) 0.147(3) Uani 1 1 d . . . H2A H 0.8807 0.7097 0.7526 0.220 Uiso 1 1 d R . . H2B H 0.8316 0.5721 0.7077 0.220 Uiso 1 1 d R . . O4W O 1.0023(4) 0.5441(3) 0.1686(4) 0.0564(12) Uani 1 1 d . . . H4A H 0.9261 0.4781 0.1599 0.085 Uiso 1 1 d R . . H4B H 1.0647 0.5219 0.1627 0.085 Uiso 1 1 d R . . O5W O 1.1301(4) 0.7103(5) 0.0672(3) 0.0573(12) Uani 1 1 d . . . H5A H 1.1853 0.6806 0.0763 0.086 Uiso 1 1 d R . . H5B H 1.1729 0.7755 0.0510 0.086 Uiso 1 1 d R . . O6W O 0.9954(4) 0.8613(3) 0.0648(3) 0.0369(8) Uani 1 1 d . . . H6A H 1.0515 0.9406 0.0817 0.055 Uiso 1 1 d R . . H6B H 0.9157 0.8425 0.0247 0.055 Uiso 1 1 d R . . O7W O 1.3866(4) 0.8002(3) 0.3712(3) 0.0383(8) Uani 1 1 d . . . H7A H 1.3026 0.7801 0.3400 0.057 Uiso 1 1 d R . . H7B H 1.4005 0.7401 0.3354 0.057 Uiso 1 1 d R . . S1 S 0.67853(11) 0.47778(10) -0.12210(8) 0.0205(2) Uani 1 1 d . . . O3W O 0.0627(13) 0.8944(12) 0.8728(10) 0.102(4) Uani 0.50 1 d P . . H3A H 0.0698 0.8361 0.8898 0.153 Uiso 0.50 1 d PR . . H3B H 0.1370 0.9654 0.9131 0.153 Uiso 0.50 1 d 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 C1 0.032(3) 0.026(3) 0.032(3) 0.007(2) 0.011(2) 0.006(2) C2 0.024(2) 0.022(2) 0.032(2) 0.011(2) 0.010(2) 0.011(2) C3 0.037(3) 0.031(3) 0.032(3) 0.018(2) 0.021(2) 0.016(2) C4 0.041(3) 0.037(3) 0.027(2) 0.015(2) 0.015(2) 0.020(3) C5 0.029(3) 0.027(2) 0.025(2) 0.007(2) 0.007(2) 0.011(2) C6 0.021(2) 0.018(2) 0.019(2) 0.0043(17) 0.0055(18) 0.0108(19) C7 0.024(2) 0.019(2) 0.024(2) 0.0067(19) 0.007(2) 0.012(2) C8 0.018(2) 0.022(2) 0.018(2) 0.0019(18) 0.0006(18) 0.0074(19) C9 0.017(2) 0.022(2) 0.022(2) 0.0050(18) 0.0005(19) 0.0100(19) C10 0.028(3) 0.031(3) 0.028(2) 0.003(2) 0.001(2) 0.020(2) C11 0.033(3) 0.020(2) 0.024(2) -0.0019(19) 0.000(2) 0.012(2) C12 0.020(2) 0.022(2) 0.020(2) 0.0013(18) 0.0003(19) 0.0046(19) C13 0.012(2) 0.022(2) 0.023(2) 0.0096(19) 0.0019(18) 0.0049(18) C14 0.017(2) 0.026(2) 0.020(2) 0.0065(19) 0.0030(19) 0.0075(19) C15 0.046(3) 0.031(3) 0.036(3) 0.015(2) 0.013(3) 0.016(3) C16 0.057(4) 0.038(3) 0.028(3) 0.016(2) 0.017(3) 0.029(3) C17 0.043(3) 0.035(3) 0.043(3) 0.026(2) 0.026(3) 0.032(3) C18 0.033(3) 0.036(3) 0.053(3) 0.025(3) 0.021(3) 0.021(2) C19 0.028(3) 0.035(3) 0.038(3) 0.016(2) 0.012(2) 0.020(2) C20 0.065(4) 0.062(4) 0.055(4) 0.042(3) 0.038(3) 0.052(4) Gd1 0.01537(12) 0.01588(11) 0.01708(11) 0.00337(9) 0.00184(9) 0.00558(9) Gd2 0.01470(12) 0.01585(11) 0.01782(11) 0.00447(9) 0.00294(9) 0.00691(9) Mn1 0.0180(5) 0.0261(5) 0.0210(5) 0.0095(4) 0.0040(4) 0.0107(4) N1 0.0223(19) 0.0168(18) 0.0234(19) 0.0079(15) 0.0060(16) 0.0097(16) N2 0.0213(19) 0.0199(18) 0.0168(17) 0.0049(15) 0.0033(16) 0.0094(16) N3 0.032(2) 0.028(2) 0.028(2) 0.0146(17) 0.0120(18) 0.0165(19) O1 0.052(3) 0.040(2) 0.043(2) 0.0139(19) 0.016(2) -0.0125(19) O2 0.035(2) 0.034(2) 0.0273(18) 0.0070(16) 0.0033(16) -0.0057(16) O3 0.0228(16) 0.0189(15) 0.0159(14) 0.0052(12) 0.0055(13) 0.0067(13) O4 0.0295(18) 0.0239(17) 0.0177(15) 0.0033(13) -0.0005(14) -0.0006(15) O5 0.0207(16) 0.0227(16) 0.0231(15) 0.0050(13) 0.0077(13) 0.0104(13) O6 0.0321(19) 0.0274(17) 0.0359(18) 0.0120(15) 0.0130(16) 0.0180(15) O7 0.035(2) 0.047(2) 0.0182(16) 0.0097(15) 0.0086(15) 0.0170(17) O8 0.0197(17) 0.0337(18) 0.0227(16) 0.0045(14) 0.0034(14) 0.0045(14) O9 0.0259(18) 0.0307(18) 0.0327(18) -0.0050(15) -0.0073(15) 0.0199(16) O10 0.0181(15) 0.0146(14) 0.0240(15) 0.0012(12) 0.0005(13) 0.0079(12) O11 0.0197(16) 0.0271(17) 0.0315(18) 0.0040(15) -0.0004(14) 0.0111(14) O12 0.0177(17) 0.0372(19) 0.0285(17) 0.0014(15) -0.0036(14) 0.0130(15) O13 0.051(2) 0.0309(18) 0.0294(18) 0.0142(15) 0.0142(17) 0.0261(17) O14 0.033(7) 0.061(14) 0.054(11) 0.045(10) 0.013(8) 0.019(8) O14' 0.063(19) 0.15(5) 0.10(3) 0.10(3) 0.06(2) 0.08(3) O1W 0.071(4) 0.142(6) 0.173(7) 0.115(6) -0.023(4) 0.004(4) O2W 0.144(6) 0.144(6) 0.075(4) 0.056(4) 0.041(4) -0.003(5) O4W 0.033(2) 0.037(2) 0.115(4) 0.040(2) 0.026(2) 0.0235(19) O5W 0.050(3) 0.116(4) 0.052(2) 0.052(3) 0.035(2) 0.061(3) O6W 0.037(2) 0.0246(17) 0.042(2) 0.0156(16) 0.0124(17) 0.0075(16) O7W 0.039(2) 0.0315(19) 0.0322(18) -0.0014(15) 0.0021(16) 0.0187(17) S1 0.0183(5) 0.0221(5) 0.0155(5) 0.0036(4) 0.0043(4) 0.0078(5) O3W 0.131(11) 0.145(11) 0.111(9) 0.097(9) 0.078(9) 0.094(9) _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 C1 O1 1.227(6) . ? C1 O2 1.273(6) . ? C1 C2 1.521(7) . ? C2 N1 1.328(6) . ? C2 C3 1.379(6) . ? C3 C4 1.378(7) . ? C3 H3 0.9300 . ? C4 C5 1.374(7) . ? C4 H4 0.9300 . ? C5 C6 1.387(6) . ? C5 H5 0.9300 . ? C6 N1 1.341(5) . ? C6 C7 1.501(6) . ? C7 O4 1.241(5) . ? C7 O3 1.283(5) . ? C8 O9 1.245(5) . ? C8 O10 1.271(5) . ? C8 C9 1.495(6) . ? C9 N2 1.331(5) . ? C9 C10 1.372(6) . ? C10 C11 1.373(6) . ? C10 H10 0.9300 . ? C11 C12 1.382(6) . ? C11 H11 0.9300 . ? C12 C13 1.389(6) . ? C12 H12 0.9300 . ? C13 N2 1.339(5) . ? C13 C14 1.496(6) . ? C14 O12 1.249(5) . ? C14 O11 1.260(5) . ? C15 N3 1.346(6) . ? C15 C16 1.389(7) . ? C15 H15 0.9300 . ? C16 C17 1.381(7) . ? C16 H16 0.9300 . ? C17 C18 1.371(7) . ? C17 C20 1.505(7) . ? C18 C19 1.383(7) . ? C18 H18 0.9300 . ? C19 N3 1.339(6) . ? C19 H19 0.9300 . ? C20 O14' 1.160(18) . ? C20 O13 1.257(6) . ? C20 O14 1.35(2) . ? Gd1 O13 2.305(3) 1_445 ? Gd1 O2 2.409(3) . ? Gd1 O5 2.421(3) 2_665 ? Gd1 O3 2.441(3) . ? Gd1 O9 2.459(3) 2_665 ? Gd1 O10 2.511(3) 2_665 ? Gd1 N1 2.515(3) . ? Gd1 O6 2.525(3) . ? Gd1 O5 2.561(3) . ? Gd1 C8 2.829(4) 2_665 ? Gd2 O8 2.401(3) . ? Gd2 O6W 2.402(3) . ? Gd2 O11 2.427(3) . ? Gd2 O5W 2.428(4) . ? Gd2 O4W 2.432(3) . ? Gd2 O10 2.459(3) . ? Gd2 O4 2.504(3) . ? Gd2 N2 2.528(3) . ? Gd2 O3 2.564(3) . ? Mn1 O12 2.143(3) 2_876 ? Mn1 O12 2.143(3) . ? Mn1 O7W 2.222(3) . ? Mn1 O7W 2.222(3) 2_876 ? Mn1 N3 2.236(4) 2_876 ? Mn1 N3 2.236(4) . ? O5 S1 1.500(3) . ? O5 Gd1 2.421(3) 2_665 ? O6 S1 1.476(3) . ? O7 S1 1.449(3) . ? O8 S1 1.467(3) . ? O9 Gd1 2.459(3) 2_665 ? O10 Gd1 2.511(3) 2_665 ? O13 Gd1 2.305(3) 1_665 ? O1W H1A 0.8500 . ? O1W H1B 0.8500 . ? O2W H2A 0.9561 . ? O2W H2B 0.8526 . ? O4W H4A 0.8501 . ? O4W H4B 0.8501 . ? O5W H5A 0.8501 . ? O5W H5B 0.8501 . ? O6W H6A 0.8500 . ? O6W H6B 0.8500 . ? O7W H7A 0.8500 . ? O7W H7B 0.8500 . ? O3W H3A 0.8501 . ? O3W H3B 0.8500 . ? 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 C1 O2 126.8(5) . . ? O1 C1 C2 118.3(4) . . ? O2 C1 C2 114.9(4) . . ? N1 C2 C3 122.3(4) . . ? N1 C2 C1 114.3(4) . . ? C3 C2 C1 123.4(4) . . ? C4 C3 C2 119.2(4) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C5 C4 C3 119.0(4) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 118.7(4) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? N1 C6 C5 122.3(4) . . ? N1 C6 C7 113.6(4) . . ? C5 C6 C7 124.1(4) . . ? O4 C7 O3 121.5(4) . . ? O4 C7 C6 121.6(4) . . ? O3 C7 C6 116.9(4) . . ? O9 C8 O10 122.2(4) . . ? O9 C8 C9 120.5(4) . . ? O10 C8 C9 117.3(4) . . ? O9 C8 Gd1 60.2(2) . 2_665 ? O10 C8 Gd1 62.6(2) . 2_665 ? C9 C8 Gd1 172.5(3) . 2_665 ? N2 C9 C10 122.6(4) . . ? N2 C9 C8 114.0(4) . . ? C10 C9 C8 123.5(4) . . ? C9 C10 C11 119.3(4) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C10 C11 C12 119.0(4) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C11 C12 C13 118.5(4) . . ? C11 C12 H12 120.8 . . ? C13 C12 H12 120.8 . . ? N2 C13 C12 122.1(4) . . ? N2 C13 C14 113.5(4) . . ? C12 C13 C14 124.4(4) . . ? O12 C14 O11 126.2(4) . . ? O12 C14 C13 117.0(4) . . ? O11 C14 C13 116.7(4) . . ? N3 C15 C16 122.7(5) . . ? N3 C15 H15 118.6 . . ? C16 C15 H15 118.6 . . ? C17 C16 C15 118.6(5) . . ? C17 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? C18 C17 C16 119.2(4) . . ? C18 C17 C20 120.3(5) . . ? C16 C17 C20 120.5(5) . . ? C17 C18 C19 118.9(5) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? N3 C19 C18 123.1(5) . . ? N3 C19 H19 118.4 . . ? C18 C19 H19 118.4 . . ? O14' C20 O13 120(2) . . ? O13 C20 O14 126.7(8) . . ? O14' C20 C17 118.9(10) . . ? O13 C20 C17 117.3(5) . . ? O14 C20 C17 114.1(10) . . ? O13 Gd1 O2 87.10(13) 1_445 . ? O13 Gd1 O5 151.34(11) 1_445 2_665 ? O2 Gd1 O5 89.29(12) . 2_665 ? O13 Gd1 O3 80.43(11) 1_445 . ? O2 Gd1 O3 127.71(10) . . ? O5 Gd1 O3 79.41(10) 2_665 . ? O13 Gd1 O9 80.66(11) 1_445 2_665 ? O2 Gd1 O9 76.70(12) . 2_665 ? O5 Gd1 O9 125.99(10) 2_665 2_665 ? O3 Gd1 O9 147.94(10) . 2_665 ? O13 Gd1 O10 131.33(10) 1_445 2_665 ? O2 Gd1 O10 71.15(11) . 2_665 ? O5 Gd1 O10 73.43(9) 2_665 2_665 ? O3 Gd1 O10 146.88(9) . 2_665 ? O9 Gd1 O10 52.61(10) 2_665 2_665 ? O13 Gd1 N1 76.57(11) 1_445 . ? O2 Gd1 N1 63.87(11) . . ? O5 Gd1 N1 76.33(10) 2_665 . ? O3 Gd1 N1 63.85(10) . . ? O9 Gd1 N1 134.92(11) 2_665 . ? O10 Gd1 N1 125.22(11) 2_665 . ? O13 Gd1 O6 74.74(11) 1_445 . ? O2 Gd1 O6 148.46(11) . . ? O5 Gd1 O6 118.82(10) 2_665 . ? O3 Gd1 O6 75.09(10) . . ? O9 Gd1 O6 75.08(11) 2_665 . ? O10 Gd1 O6 101.74(10) 2_665 . ? N1 Gd1 O6 132.90(11) . . ? O13 Gd1 O5 127.11(11) 1_445 . ? O2 Gd1 O5 144.76(12) . . ? O5 Gd1 O5 64.90(11) 2_665 . ? O3 Gd1 O5 73.07(9) . . ? O9 Gd1 O5 98.66(11) 2_665 . ? O10 Gd1 O5 78.38(9) 2_665 . ? N1 Gd1 O5 126.08(10) . . ? O6 Gd1 O5 54.73(10) . . ? O13 Gd1 C8 105.28(12) 1_445 2_665 ? O2 Gd1 C8 70.06(12) . 2_665 ? O5 Gd1 C8 100.12(11) 2_665 2_665 ? O3 Gd1 C8 162.05(11) . 2_665 ? O9 Gd1 C8 26.05(11) 2_665 2_665 ? O10 Gd1 C8 26.70(11) 2_665 2_665 ? N1 Gd1 C8 133.78(12) . 2_665 ? O6 Gd1 C8 89.83(11) . 2_665 ? O5 Gd1 C8 90.36(11) . 2_665 ? O8 Gd2 O6W 75.13(11) . . ? O8 Gd2 O11 150.38(11) . . ? O6W Gd2 O11 95.03(11) . . ? O8 Gd2 O5W 76.88(12) . . ? O6W Gd2 O5W 72.85(13) . . ? O11 Gd2 O5W 73.52(13) . . ? O8 Gd2 O4W 93.02(14) . . ? O6W Gd2 O4W 141.56(13) . . ? O11 Gd2 O4W 77.31(12) . . ? O5W Gd2 O4W 68.84(14) . . ? O8 Gd2 O10 79.15(10) . . ? O6W Gd2 O10 75.53(11) . . ? O11 Gd2 O10 126.11(10) . . ? O5W Gd2 O10 144.18(11) . . ? O4W Gd2 O10 138.95(11) . . ? O8 Gd2 O4 126.41(10) . . ? O6W Gd2 O4 142.59(11) . . ? O11 Gd2 O4 78.01(10) . . ? O5W Gd2 O4 136.52(12) . . ? O4W Gd2 O4 73.35(13) . . ? O10 Gd2 O4 79.30(10) . . ? O8 Gd2 N2 134.95(11) . . ? O6W Gd2 N2 72.13(11) . . ? O11 Gd2 N2 63.26(11) . . ? O5W Gd2 N2 120.27(14) . . ? O4W Gd2 N2 131.59(13) . . ? O10 Gd2 N2 63.38(10) . . ? O4 Gd2 N2 71.99(11) . . ? O8 Gd2 O3 74.95(9) . . ? O6W Gd2 O3 135.89(11) . . ? O11 Gd2 O3 125.97(10) . . ? O5W Gd2 O3 129.27(13) . . ? O4W Gd2 O3 71.48(11) . . ? O10 Gd2 O3 67.55(9) . . ? O4 Gd2 O3 51.48(9) . . ? N2 Gd2 O3 109.51(10) . . ? O12 Mn1 O12 180.000(1) 2_876 . ? O12 Mn1 O7W 92.09(13) 2_876 . ? O12 Mn1 O7W 87.91(13) . . ? O12 Mn1 O7W 87.91(13) 2_876 2_876 ? O12 Mn1 O7W 92.09(13) . 2_876 ? O7W Mn1 O7W 180.00(15) . 2_876 ? O12 Mn1 N3 87.85(14) 2_876 2_876 ? O12 Mn1 N3 92.15(14) . 2_876 ? O7W Mn1 N3 88.93(13) . 2_876 ? O7W Mn1 N3 91.07(13) 2_876 2_876 ? O12 Mn1 N3 92.15(14) 2_876 . ? O12 Mn1 N3 87.85(14) . . ? O7W Mn1 N3 91.07(13) . . ? O7W Mn1 N3 88.93(13) 2_876 . ? N3 Mn1 N3 180.000(1) 2_876 . ? C2 N1 C6 118.6(4) . . ? C2 N1 Gd1 120.3(3) . . ? C6 N1 Gd1 121.1(3) . . ? C9 N2 C13 118.6(4) . . ? C9 N2 Gd2 120.7(3) . . ? C13 N2 Gd2 120.4(3) . . ? C19 N3 C15 117.4(4) . . ? C19 N3 Mn1 120.3(3) . . ? C15 N3 Mn1 122.2(3) . . ? C1 O2 Gd1 125.7(3) . . ? C7 O3 Gd1 124.0(3) . . ? C7 O3 Gd2 91.5(2) . . ? Gd1 O3 Gd2 142.74(12) . . ? C7 O4 Gd2 95.4(3) . . ? S1 O5 Gd1 141.70(17) . 2_665 ? S1 O5 Gd1 99.04(15) . . ? Gd1 O5 Gd1 115.10(11) 2_665 . ? S1 O6 Gd1 101.29(16) . . ? S1 O8 Gd2 137.67(19) . . ? C8 O9 Gd1 93.8(2) . 2_665 ? C8 O10 Gd2 123.5(3) . . ? C8 O10 Gd1 90.7(2) . 2_665 ? Gd2 O10 Gd1 141.62(12) . 2_665 ? C14 O11 Gd2 125.6(3) . . ? C14 O12 Mn1 134.1(3) . . ? C20 O13 Gd1 141.5(3) . 1_665 ? H1A O1W H1B 107.7 . . ? H2A O2W H2B 107.6 . . ? Gd2 O4W H4A 107.3 . . ? Gd2 O4W H4B 141.9 . . ? H4A O4W H4B 107.7 . . ? Gd2 O5W H5A 131.2 . . ? Gd2 O5W H5B 115.5 . . ? H5A O5W H5B 107.7 . . ? Gd2 O6W H6A 139.7 . . ? Gd2 O6W H6B 104.7 . . ? H6A O6W H6B 107.7 . . ? Mn1 O7W H7A 109.7 . . ? Mn1 O7W H7B 141.9 . . ? H7A O7W H7B 107.7 . . ? O7 S1 O8 111.09(19) . . ? O7 S1 O6 111.9(2) . . ? O8 S1 O6 109.40(19) . . ? O7 S1 O5 111.21(19) . . ? O8 S1 O5 109.42(18) . . ? O6 S1 O5 103.59(18) . . ? H3A O3W H3B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.780 _refine_diff_density_min -0.752 _refine_diff_density_rms 0.115 ####################################################################### # # 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_22 _database_code_depnum_ccdc_archive 'CCDC 807543' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H26 Dy4 Mn N6 O36 S2, 13(H2 O)' _chemical_formula_sum 'C42 H52 Dy4 Mn N6 O49 S2' _chemical_formula_weight 2193.96 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 '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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7899(15) _cell_length_b 12.0807(16) _cell_length_c 14.4380(19) _cell_angle_alpha 76.362(2) _cell_angle_beta 68.371(3) _cell_angle_gamma 65.305(2) _cell_volume 1582.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5526 _cell_measurement_theta_min 1.52 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1059 _exptl_absorpt_coefficient_mu 5.051 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3126 _exptl_absorpt_correction_T_max 0.4315 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _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 AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7910 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.20 _reflns_number_total 5526 _reflns_number_gt 4793 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0442P)^2^+5.3378P] 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 5526 _refine_ls_number_parameters 472 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 C1 C 0.1186(6) 0.1251(6) 0.7836(4) 0.0281(13) Uani 1 1 d . . . C2 C 0.1135(6) 0.2423(6) 0.7188(4) 0.0282(13) Uani 1 1 d . . . C3 C 0.0529(7) 0.3567(6) 0.7522(5) 0.0359(15) Uani 1 1 d . . . H3 H 0.0128 0.3654 0.8205 0.043 Uiso 1 1 calc R . . C4 C 0.0519(8) 0.4585(6) 0.6838(5) 0.0394(16) Uani 1 1 d . . . H4 H 0.0099 0.5364 0.7054 0.047 Uiso 1 1 calc R . . C5 C 0.1136(7) 0.4431(6) 0.5835(5) 0.0370(16) Uani 1 1 d . . . H5 H 0.1153 0.5101 0.5362 0.044 Uiso 1 1 calc R . . C6 C 0.1727(6) 0.3273(5) 0.5545(4) 0.0279(13) Uani 1 1 d . . . C7 C 0.2436(6) 0.2964(5) 0.4482(4) 0.0244(12) Uani 1 1 d . . . C8 C 0.6593(6) 0.2219(5) 0.3384(4) 0.0265(13) Uani 1 1 d . . . C9 C 0.6336(7) 0.3448(5) 0.2789(4) 0.0282(13) Uani 1 1 d . . . C10 C 0.7022(8) 0.4208(6) 0.2719(5) 0.0404(16) Uani 1 1 d . . . H10 H 0.7716 0.3975 0.3037 0.048 Uiso 1 1 calc R . . C11 C 0.6656(9) 0.5338(7) 0.2162(7) 0.055(2) Uani 1 1 d . . . H11 H 0.7061 0.5897 0.2129 0.066 Uiso 1 1 calc R . . C12 C 0.5676(9) 0.5615(7) 0.1658(6) 0.053(2) Uani 1 1 d . . . H12 H 0.5460 0.6341 0.1244 0.063 Uiso 1 1 calc R . . C13 C 0.5027(7) 0.4803(6) 0.1780(5) 0.0335(14) Uani 1 1 d . . . C14 C 0.3909(7) 0.5008(6) 0.1302(5) 0.0335(15) Uani 1 1 d . . . C15 C 0.1606(7) 0.2420(7) 0.1752(5) 0.0407(16) Uani 1 1 d . . . C16 C 0.2888(6) 0.2015(6) 0.0827(4) 0.0286(13) Uani 1 1 d . . . C17 C 0.2791(7) 0.1849(6) -0.0054(5) 0.0349(15) Uani 1 1 d . . . H17 H 0.1908 0.2000 -0.0121 0.042 Uiso 1 1 calc R . . C18 C 0.4026(7) 0.1457(6) -0.0826(5) 0.0348(15) Uani 1 1 d . . . H18 H 0.3987 0.1335 -0.1425 0.042 Uiso 1 1 calc R . . C19 C 0.5342(7) 0.1240(5) -0.0721(4) 0.0313(14) Uani 1 1 d . . . H19 H 0.6188 0.0961 -0.1239 0.038 Uiso 1 1 calc R . . C20 C 0.5356(6) 0.1451(5) 0.0180(4) 0.0269(13) Uani 1 1 d . . . C21 C 0.6646(6) 0.1292(5) 0.0434(4) 0.0273(13) Uani 1 1 d . . . Dy1 Dy 0.41608(3) 0.22635(2) 0.250074(18) 0.02190(9) Uani 1 1 d . . . Dy2 Dy 0.28830(3) 0.01895(2) 0.563072(18) 0.02177(9) Uani 1 1 d . . . Mn1 Mn 1.0000 0.0000 0.0000 0.0301(3) Uani 1 2 d S . . N1 N 0.4131(5) 0.1822(4) 0.0936(3) 0.0247(10) Uani 1 1 d . . . N2 N 0.5338(5) 0.3734(4) 0.2335(3) 0.0269(11) Uani 1 1 d . . . N3 N 0.1748(5) 0.2274(4) 0.6197(3) 0.0257(11) Uani 1 1 d . . . O1 O 0.3111(5) -0.0591(4) 0.4156(3) 0.0345(10) Uani 1 1 d . . . O2 O 0.5211(4) -0.0636(4) 0.4313(3) 0.0260(9) Uani 1 1 d . . . O3 O 0.5390(5) -0.2014(4) 0.3240(3) 0.0399(11) Uani 1 1 d . . . O4 O 0.4734(5) 0.0144(4) 0.2725(3) 0.0314(10) Uani 1 1 d . . . O5 O 0.1762(4) 0.0297(4) 0.7390(3) 0.0333(10) Uani 1 1 d . . . O6 O 0.0673(5) 0.1299(4) 0.8764(3) 0.0355(10) Uani 1 1 d . . . O7 O 0.2863(4) 0.1847(3) 0.4327(3) 0.0256(9) Uani 1 1 d . . . O8 O 0.2598(5) 0.3761(4) 0.3775(3) 0.0322(10) Uani 1 1 d . . . O9 O 0.5757(4) 0.1675(3) 0.3486(3) 0.0250(9) Uani 1 1 d . . . O10 O 0.7605(5) 0.1743(4) 0.3740(3) 0.0356(10) Uani 1 1 d . . . O11 O 0.3389(5) 0.4218(4) 0.1466(3) 0.0349(10) Uani 1 1 d . . . O12 O 0.3568(6) 0.6024(4) 0.0753(4) 0.0523(14) Uani 1 1 d . . . O13 O 0.1895(4) 0.2490(4) 0.2509(3) 0.0309(10) Uani 1 1 d . . . O14 O 0.0402(5) 0.2640(8) 0.1714(4) 0.090(3) Uani 1 1 d . . . O15 O 0.6419(4) 0.1635(4) 0.1255(3) 0.0313(10) Uani 1 1 d . . . O16 O 0.7864(4) 0.0813(4) -0.0182(3) 0.0373(11) Uani 1 1 d . . . O1W O 0.9359(5) 0.1290(4) 0.1101(3) 0.0445(12) Uani 1 1 d . . . H1A H 0.8706 0.1130 0.1597 0.067 Uiso 1 1 d R . . H1B H 0.9865 0.1472 0.1330 0.067 Uiso 1 1 d R . . O2W O 0.0527(5) 0.0759(5) 0.5654(4) 0.0480(12) Uani 1 1 d . . . H2A H 0.1131 0.0727 0.5916 0.072 Uiso 1 1 d R . . H2B H -0.0133 0.0566 0.6116 0.072 Uiso 1 1 d R . . O3W O 0.9551(6) 0.2356(6) 0.4217(4) 0.0585(15) Uani 1 1 d . . . H3A H 1.0181 0.2640 0.3821 0.088 Uiso 1 1 d R . . H3B H 0.9163 0.2212 0.3865 0.088 Uiso 1 1 d R . . O4W O 0.1665(8) 0.6439(7) -0.0039(5) 0.087(2) Uani 1 1 d . . . H4A H 0.2545 0.6272 -0.0127 0.130 Uiso 1 1 d R . . H4B H 0.1214 0.7185 0.0079 0.130 Uiso 1 1 d R . . O5W O 0.4222(18) 0.6206(10) 0.4590(8) 0.225(8) Uani 1 1 d . . . H5A H 0.3603 0.6026 0.5103 0.337 Uiso 1 1 d R . . H5B H 0.4197 0.6900 0.4647 0.337 Uiso 1 1 d R . . O6W O 0.2364(15) 0.6234(10) 0.3637(10) 0.204(7) Uani 1 1 d . . . H6A H 0.2807 0.5626 0.3291 0.305 Uiso 1 1 d R . . H6B H 0.2560 0.6840 0.3273 0.305 Uiso 1 1 d R . . O7W O 1.0000 0.5000 1.0000 0.179(7) Uani 1 2 d S . . H7A H 0.9885 0.5601 0.9552 0.269 Uiso 0.50 1 d PR . . H7B H 0.9654 0.4524 0.9923 0.269 Uiso 0.50 1 d PR . . O8W O 0.8289(14) 0.1807(18) 0.7620(10) 0.247(9) Uani 1 1 d . . . H8A H 0.8337 0.1920 0.8160 0.370 Uiso 1 1 d R . . H8B H 0.8909 0.2007 0.7137 0.370 Uiso 1 1 d R . . O9W O 0.8490(18) 0.030(3) 0.7140(12) 0.348(16) Uani 1 1 d . . . H9A H 0.8420 -0.0306 0.7507 0.522 Uiso 1 1 d R . . H9B H 0.7863 0.0602 0.6835 0.522 Uiso 1 1 d R . . S1 S 0.46285(16) -0.08090(13) 0.35728(10) 0.0262(3) 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 C1 0.020(3) 0.038(4) 0.018(3) 0.000(3) 0.000(2) -0.008(3) C2 0.026(3) 0.032(3) 0.021(3) -0.004(2) -0.001(2) -0.010(3) C3 0.041(4) 0.033(4) 0.023(3) -0.007(3) 0.000(3) -0.009(3) C4 0.050(4) 0.030(4) 0.029(3) -0.011(3) -0.004(3) -0.010(3) C5 0.046(4) 0.026(3) 0.027(3) 0.000(3) -0.004(3) -0.009(3) C6 0.029(3) 0.029(3) 0.021(3) 0.000(2) -0.006(2) -0.008(3) C7 0.026(3) 0.023(3) 0.021(3) 0.004(2) -0.008(2) -0.008(2) C8 0.029(3) 0.029(3) 0.017(3) -0.003(2) -0.005(2) -0.008(3) C9 0.037(3) 0.024(3) 0.023(3) -0.001(2) -0.008(3) -0.012(3) C10 0.046(4) 0.037(4) 0.045(4) 0.009(3) -0.022(3) -0.022(3) C11 0.061(5) 0.036(4) 0.081(6) 0.008(4) -0.033(5) -0.027(4) C12 0.065(5) 0.034(4) 0.069(5) 0.018(4) -0.034(4) -0.030(4) C13 0.035(3) 0.027(3) 0.035(3) 0.003(3) -0.011(3) -0.010(3) C14 0.032(3) 0.030(3) 0.031(3) 0.002(3) -0.010(3) -0.007(3) C15 0.034(4) 0.053(4) 0.034(4) -0.012(3) -0.007(3) -0.014(3) C16 0.028(3) 0.034(3) 0.021(3) -0.006(2) -0.006(2) -0.008(3) C17 0.039(4) 0.040(4) 0.029(3) -0.005(3) -0.012(3) -0.015(3) C18 0.048(4) 0.036(4) 0.023(3) -0.002(3) -0.011(3) -0.017(3) C19 0.037(3) 0.026(3) 0.023(3) -0.004(2) -0.003(3) -0.008(3) C20 0.032(3) 0.023(3) 0.018(3) -0.001(2) -0.001(2) -0.009(2) C21 0.025(3) 0.023(3) 0.022(3) 0.004(2) -0.003(2) -0.005(2) Dy1 0.02362(15) 0.02402(16) 0.01572(14) -0.00117(10) -0.00490(11) -0.00789(11) Dy2 0.02256(15) 0.02141(15) 0.01682(14) -0.00033(10) -0.00366(11) -0.00667(11) Mn1 0.0225(6) 0.0503(8) 0.0155(6) 0.0134(6) -0.0056(5) -0.0203(6) N1 0.025(3) 0.027(3) 0.021(2) -0.004(2) -0.006(2) -0.009(2) N2 0.030(3) 0.024(3) 0.022(2) 0.003(2) -0.005(2) -0.010(2) N3 0.025(2) 0.031(3) 0.014(2) -0.001(2) -0.0006(19) -0.009(2) O1 0.034(2) 0.042(3) 0.032(2) -0.004(2) -0.0062(19) -0.022(2) O2 0.028(2) 0.029(2) 0.0186(19) -0.0052(16) -0.0049(17) -0.0085(18) O3 0.061(3) 0.027(2) 0.030(2) -0.0086(19) -0.012(2) -0.013(2) O4 0.041(3) 0.030(2) 0.018(2) -0.0025(17) -0.0049(18) -0.0122(19) O5 0.032(2) 0.032(2) 0.020(2) 0.0007(18) 0.0017(18) -0.0070(19) O6 0.041(3) 0.039(3) 0.017(2) -0.0030(18) 0.0028(18) -0.016(2) O7 0.029(2) 0.024(2) 0.0183(19) -0.0012(16) -0.0028(16) -0.0086(17) O8 0.039(2) 0.024(2) 0.021(2) 0.0027(17) -0.0024(18) -0.0084(19) O9 0.029(2) 0.022(2) 0.024(2) 0.0028(16) -0.0075(17) -0.0124(17) O10 0.039(3) 0.035(2) 0.040(3) 0.008(2) -0.021(2) -0.018(2) O11 0.042(3) 0.036(3) 0.029(2) 0.0040(19) -0.015(2) -0.016(2) O12 0.068(4) 0.034(3) 0.058(3) 0.022(2) -0.036(3) -0.021(3) O13 0.027(2) 0.044(3) 0.021(2) -0.0062(18) -0.0047(17) -0.0122(19) O14 0.024(3) 0.189(8) 0.057(4) -0.063(4) -0.003(3) -0.023(4) O15 0.025(2) 0.041(3) 0.024(2) -0.0061(18) -0.0039(17) -0.0106(19) O16 0.024(2) 0.048(3) 0.029(2) -0.008(2) -0.0003(19) -0.007(2) O1W 0.041(3) 0.052(3) 0.037(3) -0.010(2) 0.006(2) -0.026(2) O2W 0.030(2) 0.057(3) 0.055(3) -0.001(2) -0.015(2) -0.015(2) O3W 0.048(3) 0.090(4) 0.045(3) -0.001(3) -0.016(3) -0.034(3) O4W 0.087(5) 0.092(5) 0.076(5) 0.010(4) -0.045(4) -0.020(4) O5W 0.39(2) 0.119(9) 0.101(8) -0.025(7) 0.047(10) -0.136(12) O6W 0.215(14) 0.096(8) 0.205(13) -0.017(8) 0.034(11) -0.052(8) O7W 0.138(13) 0.128(13) 0.23(2) 0.014(13) -0.050(13) -0.037(11) O8W 0.146(11) 0.43(3) 0.136(11) 0.003(14) 0.011(9) -0.142(15) O9W 0.233(18) 0.77(5) 0.187(15) -0.16(2) 0.031(13) -0.35(3) S1 0.0339(8) 0.0241(7) 0.0193(7) -0.0029(6) -0.0063(6) -0.0108(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O6 1.253(7) . ? C1 O5 1.259(7) . ? C1 C2 1.493(8) . ? C2 N3 1.357(7) . ? C2 C3 1.377(9) . ? C3 C4 1.384(9) . ? C3 H3 0.9300 . ? C4 C5 1.374(9) . ? C4 H4 0.9300 . ? C5 C6 1.369(9) . ? C5 H5 0.9300 . ? C6 N3 1.342(8) . ? C6 C7 1.499(8) . ? C7 O8 1.243(7) . ? C7 O7 1.276(7) . ? C8 O10 1.240(7) . ? C8 O9 1.273(7) . ? C8 C9 1.500(8) . ? C8 Dy2 2.842(6) 2_656 ? C9 N2 1.345(8) . ? C9 C10 1.368(9) . ? C10 C11 1.390(10) . ? C10 H10 0.9300 . ? C11 C12 1.385(11) . ? C11 H11 0.9300 . ? C12 C13 1.374(10) . ? C12 H12 0.9300 . ? C13 N2 1.331(8) . ? C13 C14 1.508(9) . ? C14 O11 1.236(8) . ? C14 O12 1.284(8) . ? C15 O14 1.232(8) . ? C15 O13 1.272(8) . ? C15 C16 1.522(9) . ? C16 N1 1.325(8) . ? C16 C17 1.380(8) . ? C17 C18 1.367(9) . ? C17 H17 0.9300 . ? C18 C19 1.392(9) . ? C18 H18 0.9300 . ? C19 C20 1.389(8) . ? C19 H19 0.9300 . ? C20 N1 1.346(7) . ? C20 C21 1.492(9) . ? C21 O15 1.254(7) . ? C21 O16 1.264(7) . ? Dy1 O13 2.339(4) . ? Dy1 O4 2.341(4) . ? Dy1 O15 2.370(4) . ? Dy1 O9 2.408(4) . ? Dy1 N1 2.455(5) . ? Dy1 O11 2.472(4) . ? Dy1 O8 2.497(4) . ? Dy1 N2 2.508(5) . ? Dy1 O7 2.531(4) . ? Dy2 O2W 2.329(5) . ? Dy2 O2 2.366(4) 2_656 ? Dy2 O5 2.386(4) . ? Dy2 O7 2.403(4) . ? Dy2 O1 2.418(4) . ? Dy2 O9 2.473(4) 2_656 ? Dy2 N3 2.483(5) . ? Dy2 O2 2.491(4) . ? Dy2 O10 2.495(4) 2_656 ? Mn1 O16 2.186(4) . ? Mn1 O16 2.186(4) 2_755 ? Mn1 O6 2.202(4) 2_656 ? Mn1 O6 2.202(4) 1_654 ? Mn1 O1W 2.212(5) 2_755 ? Mn1 O1W 2.212(5) . ? O1 S1 1.479(4) . ? O2 S1 1.513(4) . ? O2 Dy2 2.366(4) 2_656 ? O3 S1 1.436(4) . ? O4 S1 1.476(4) . ? O6 Mn1 2.202(4) 1_456 ? O9 Dy2 2.473(4) 2_656 ? O10 Dy2 2.495(4) 2_656 ? O1W H1A 0.8501 . ? O1W H1B 0.8500 . ? O2W H2A 0.8500 . ? O2W H2B 0.8500 . ? O3W H3A 0.8499 . ? O3W H3B 0.8500 . ? O4W H4A 0.8501 . ? O4W H4B 0.8500 . ? O5W H5A 0.8500 . ? O5W H5B 0.8500 . ? O6W H6A 0.8500 . ? O6W H6B 0.8500 . ? O7W H7A 0.8500 . ? O7W H7B 0.8500 . ? O8W H8A 0.8461 . ? O8W H8B 0.8394 . ? O9W H9A 0.8102 . ? O9W H9B 0.8490 . ? 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 O6 C1 O5 126.0(6) . . ? O6 C1 C2 117.8(6) . . ? O5 C1 C2 116.3(5) . . ? N3 C2 C3 121.1(6) . . ? N3 C2 C1 113.4(5) . . ? C3 C2 C1 125.5(5) . . ? C2 C3 C4 119.6(6) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 119.1(6) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C6 C5 C4 118.8(6) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? N3 C6 C5 123.0(5) . . ? N3 C6 C7 112.2(5) . . ? C5 C6 C7 124.8(5) . . ? O8 C7 O7 121.0(5) . . ? O8 C7 C6 121.6(5) . . ? O7 C7 C6 117.4(5) . . ? O10 C8 O9 121.6(5) . . ? O10 C8 C9 121.0(6) . . ? O9 C8 C9 117.4(5) . . ? O10 C8 Dy2 61.3(3) . 2_656 ? O9 C8 Dy2 60.4(3) . 2_656 ? C9 C8 Dy2 175.4(4) . 2_656 ? N2 C9 C10 123.3(6) . . ? N2 C9 C8 112.6(5) . . ? C10 C9 C8 124.1(6) . . ? C9 C10 C11 118.3(7) . . ? C9 C10 H10 120.9 . . ? C11 C10 H10 120.9 . . ? C12 C11 C10 118.7(7) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C13 C12 C11 119.0(7) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? N2 C13 C12 122.7(6) . . ? N2 C13 C14 112.8(6) . . ? C12 C13 C14 124.4(6) . . ? O11 C14 O12 125.2(6) . . ? O11 C14 C13 119.1(5) . . ? O12 C14 C13 115.7(6) . . ? O14 C15 O13 125.8(6) . . ? O14 C15 C16 118.7(6) . . ? O13 C15 C16 115.5(6) . . ? N1 C16 C17 122.0(6) . . ? N1 C16 C15 114.2(5) . . ? C17 C16 C15 123.9(6) . . ? C18 C17 C16 118.3(6) . . ? C18 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? C17 C18 C19 120.5(6) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 118.1(6) . . ? C20 C19 H19 120.9 . . ? C18 C19 H19 120.9 . . ? N1 C20 C19 120.6(6) . . ? N1 C20 C21 113.1(5) . . ? C19 C20 C21 126.3(5) . . ? O15 C21 O16 125.6(6) . . ? O15 C21 C20 116.4(5) . . ? O16 C21 C20 117.9(5) . . ? O13 Dy1 O4 87.88(15) . . ? O13 Dy1 O15 130.76(14) . . ? O4 Dy1 O15 79.88(15) . . ? O13 Dy1 O9 145.61(13) . . ? O4 Dy1 O9 80.44(14) . . ? O15 Dy1 O9 78.98(13) . . ? O13 Dy1 N1 66.01(14) . . ? O4 Dy1 N1 76.75(15) . . ? O15 Dy1 N1 64.78(15) . . ? O9 Dy1 N1 139.79(14) . . ? O13 Dy1 O11 75.87(15) . . ? O4 Dy1 O11 147.88(14) . . ? O15 Dy1 O11 89.91(15) . . ? O9 Dy1 O11 127.63(14) . . ? N1 Dy1 O11 71.37(15) . . ? O13 Dy1 O8 79.59(14) . . ? O4 Dy1 O8 127.58(13) . . ? O15 Dy1 O8 143.21(15) . . ? O9 Dy1 O8 82.23(14) . . ? N1 Dy1 O8 137.64(14) . . ? O11 Dy1 O8 77.03(13) . . ? O13 Dy1 N2 134.09(15) . . ? O4 Dy1 N2 138.03(15) . . ? O15 Dy1 N2 72.20(15) . . ? O9 Dy1 N2 64.12(14) . . ? N1 Dy1 N2 116.29(16) . . ? O11 Dy1 N2 63.75(15) . . ? O8 Dy1 N2 71.17(15) . . ? O13 Dy1 O7 75.76(13) . . ? O4 Dy1 O7 75.88(13) . . ? O15 Dy1 O7 143.19(13) . . ? O9 Dy1 O7 70.05(13) . . ? N1 Dy1 O7 133.21(14) . . ? O11 Dy1 O7 124.67(13) . . ? O8 Dy1 O7 51.71(13) . . ? N2 Dy1 O7 109.49(14) . . ? O2W Dy2 O2 152.08(16) . 2_656 ? O2W Dy2 O5 81.93(16) . . ? O2 Dy2 O5 91.58(14) 2_656 . ? O2W Dy2 O7 82.69(16) . . ? O2 Dy2 O7 80.17(13) 2_656 . ? O5 Dy2 O7 128.25(13) . . ? O2W Dy2 O1 75.89(16) . . ? O2 Dy2 O1 119.60(13) 2_656 . ? O5 Dy2 O1 146.10(15) . . ? O7 Dy2 O1 74.13(14) . . ? O2W Dy2 O9 126.34(15) . 2_656 ? O2 Dy2 O9 75.83(13) 2_656 2_656 ? O5 Dy2 O9 71.36(13) . 2_656 ? O7 Dy2 O9 149.54(13) . 2_656 ? O1 Dy2 O9 101.87(14) . 2_656 ? O2W Dy2 N3 77.85(17) . . ? O2 Dy2 N3 74.89(15) 2_656 . ? O5 Dy2 N3 64.31(14) . . ? O7 Dy2 N3 64.21(14) . . ? O1 Dy2 N3 132.87(15) . . ? O9 Dy2 N3 125.20(14) 2_656 . ? O2W Dy2 O2 131.66(15) . . ? O2 Dy2 O2 64.33(15) 2_656 . ? O5 Dy2 O2 144.15(13) . . ? O7 Dy2 O2 75.90(13) . . ? O1 Dy2 O2 56.81(13) . . ? O9 Dy2 O2 76.93(13) 2_656 . ? N3 Dy2 O2 126.70(14) . . ? O2W Dy2 O10 76.45(16) . 2_656 ? O2 Dy2 O10 128.18(13) 2_656 2_656 ? O5 Dy2 O10 75.17(15) . 2_656 ? O7 Dy2 O10 146.01(14) . 2_656 ? O1 Dy2 O10 74.92(14) . 2_656 ? O9 Dy2 O10 52.38(13) 2_656 2_656 ? N3 Dy2 O10 134.34(15) . 2_656 ? O2 Dy2 O10 98.41(14) . 2_656 ? O2W Dy2 C8 100.96(18) . 2_656 ? O2 Dy2 C8 102.40(16) 2_656 2_656 ? O5 Dy2 C8 70.62(15) . 2_656 ? O7 Dy2 C8 161.10(14) . 2_656 ? O1 Dy2 C8 88.67(15) . 2_656 ? O9 Dy2 C8 26.57(15) 2_656 2_656 ? N3 Dy2 C8 134.66(15) . 2_656 ? O2 Dy2 C8 88.24(15) . 2_656 ? O10 Dy2 C8 25.83(15) 2_656 2_656 ? O2 Dy2 H2A 141.8 2_656 . ? O5 Dy2 H2A 68.5 . . ? O7 Dy2 H2A 87.2 . . ? O1 Dy2 H2A 90.6 . . ? O9 Dy2 H2A 123.2 2_656 . ? N3 Dy2 H2A 67.2 . . ? O2 Dy2 H2A 146.1 . . ? O10 Dy2 H2A 79.4 2_656 . ? C8 Dy2 H2A 101.0 2_656 . ? O16 Mn1 O16 180.0(2) . 2_755 ? O16 Mn1 O6 90.69(17) . 2_656 ? O16 Mn1 O6 89.31(17) 2_755 2_656 ? O16 Mn1 O6 89.31(17) . 1_654 ? O16 Mn1 O6 90.69(17) 2_755 1_654 ? O6 Mn1 O6 180.0(3) 2_656 1_654 ? O16 Mn1 O1W 88.92(17) . 2_755 ? O16 Mn1 O1W 91.08(17) 2_755 2_755 ? O6 Mn1 O1W 90.70(17) 2_656 2_755 ? O6 Mn1 O1W 89.30(17) 1_654 2_755 ? O16 Mn1 O1W 91.08(17) . . ? O16 Mn1 O1W 88.92(17) 2_755 . ? O6 Mn1 O1W 89.30(17) 2_656 . ? O6 Mn1 O1W 90.70(17) 1_654 . ? O1W Mn1 O1W 180.0(2) 2_755 . ? C16 N1 C20 120.5(5) . . ? C16 N1 Dy1 119.2(4) . . ? C20 N1 Dy1 120.2(4) . . ? C13 N2 C9 117.9(5) . . ? C13 N2 Dy1 121.4(4) . . ? C9 N2 Dy1 120.6(4) . . ? C6 N3 C2 118.4(5) . . ? C6 N3 Dy2 121.6(4) . . ? C2 N3 Dy2 120.0(4) . . ? S1 O1 Dy2 101.8(2) . . ? S1 O2 Dy2 141.0(2) . 2_656 ? S1 O2 Dy2 97.66(19) . . ? Dy2 O2 Dy2 115.67(15) 2_656 . ? S1 O4 Dy1 137.2(2) . . ? C1 O5 Dy2 125.9(4) . . ? C1 O6 Mn1 132.2(4) . 1_456 ? C7 O7 Dy2 124.1(3) . . ? C7 O7 Dy1 92.0(3) . . ? Dy2 O7 Dy1 140.45(16) . . ? C7 O8 Dy1 94.4(3) . . ? C8 O9 Dy1 123.8(3) . . ? C8 O9 Dy2 93.1(3) . 2_656 ? Dy1 O9 Dy2 139.02(17) . 2_656 ? C8 O10 Dy2 92.9(4) . 2_656 ? C14 O11 Dy1 122.8(4) . . ? C15 O13 Dy1 124.6(4) . . ? C21 O15 Dy1 125.0(4) . . ? C21 O16 Mn1 130.9(4) . . ? H1A O1W H1B 107.7 . . ? H2A O2W H2B 107.7 . . ? H3A O3W H3B 107.7 . . ? H4A O4W H4B 107.7 . . ? H5A O5W H5B 107.7 . . ? H6A O6W H6B 107.7 . . ? H7A O7W H7B 107.7 . . ? H8A O8W H8B 109.1 . . ? H9A O9W H9B 111.6 . . ? O3 S1 O4 111.2(2) . . ? O3 S1 O1 112.8(3) . . ? O4 S1 O1 110.4(3) . . ? O3 S1 O2 111.3(3) . . ? O4 S1 O2 108.1(2) . . ? O1 S1 O2 102.6(2) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.623 _refine_diff_density_min -1.036 _refine_diff_density_rms 0.145