Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Qi-Bing Bo' _publ_contact_author_address ; Department of Chemistry University of Jinan Jinan 250022 CHINA ; _publ_contact_author_email 'CHM BOQB@UJN.EDU.CN' _publ_section_title ; A new family of 3D 3d-4f heterometallic frameworks comprising 1D inorganic lanthanide ladders and organic CuI-bipyridine chains ; loop_ _publ_author_name Q.B.Bo 'W. Forsling' 'Zhong-Xi Sun.' # Attachment 'Sm-Cu.cif' data_061122d _database_code_depnum_ccdc_archive 'CCDC 630338' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H30 Cu2 N6 O20 S2 Sm2' _chemical_formula_weight 1334.54 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' Sm Sm -0.1638 3.4418 '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' Cu Cu 0.3201 1.2651 '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 6.3467(16) _cell_length_b 12.237(3) _cell_length_c 13.363(4) _cell_angle_alpha 97.447(3) _cell_angle_beta 93.032(3) _cell_angle_gamma 95.620(3) _cell_volume 1021.9(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3711 _cell_measurement_theta_min 2,435 _cell_measurement_theta_max 28.205 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.57 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 650 _exptl_absorpt_coefficient_mu 4.051 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1879 _exptl_absorpt_correction_T_max 0.3482 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 5170 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0772 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3471 _reflns_number_gt 3037 _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^)+(0.1236P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3471 _refine_ls_number_parameters 299 _refine_ls_number_restraints 198 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.1782 _refine_ls_wR_factor_gt 0.1701 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.095 _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 O8 O 0.0564(9) 0.6753(5) 0.4970(5) 0.0165(14) Uani 1 1 d U . . O7 O 0.0093(10) 0.5428(5) 0.3524(5) 0.0207(14) Uani 1 1 d . . . Sm1 Sm 0.68260(6) 0.62180(3) 0.42820(3) 0.0126(2) Uani 1 1 d . . . Cu1 Cu 0.7459(4) 0.76889(16) 0.05788(15) 0.0675(6) Uani 1 1 d . . . N1 N 0.7152(11) 0.8300(6) 0.4667(6) 0.0156(16) Uani 1 1 d . . . N2 N 0.486(3) 0.6730(12) 0.0373(10) 0.073(3) Uani 1 1 d U . . N3 N 1.016(2) 0.8450(12) 0.0324(9) 0.068(2) Uani 1 1 d U . . O1 O 0.7552(10) 0.7206(6) 0.2900(5) 0.0230(15) Uani 1 1 d . . . O2 O 0.7339(16) 0.8703(7) 0.2122(6) 0.046(2) Uani 1 1 d . . . O3 O 0.6467(11) 0.6970(6) 0.5998(5) 0.0273(16) Uani 1 1 d . . . O4 O 0.624(2) 0.8335(9) 0.7224(8) 0.073(3) Uani 1 1 d U . . O5 O 0.3284(10) 0.6757(5) 0.3746(5) 0.0207(15) Uani 1 1 d . . . O6 O 0.3042(10) 0.5343(5) 0.4760(5) 0.0200(15) Uani 1 1 d . . . O9 O 0.5631(12) 0.4623(6) 0.2999(5) 0.0297(17) Uani 1 1 d . . . H18 H 0.5022 0.4066 0.3242 0.045 Uiso 1 1 d R . . H19 H 0.6892 0.4458 0.2889 0.045 Uiso 1 1 d R . . O10 O 0.8425(19) 0.2919(9) 0.2843(8) 0.074(3) Uani 1 1 d . . . H20 H 0.8844 0.2879 0.3459 0.111 Uiso 1 1 d R . . H21 H 0.8018 0.3571 0.2865 0.111 Uiso 1 1 d R . . S1 S 0.1724(3) 0.60709(17) 0.42337(16) 0.0123(5) Uani 1 1 d . . . C1 C 0.7459(15) 0.8228(8) 0.2895(8) 0.022(2) Uani 1 1 d . . . C2 C 0.7421(14) 0.8904(7) 0.3916(8) 0.018(2) Uani 1 1 d . . . C3 C 0.7617(17) 1.0052(9) 0.4096(10) 0.031(3) Uani 1 1 d . . . H3 H 0.7750 1.0465 0.3561 0.038 Uiso 1 1 calc R . . C4 C 0.7613(16) 1.0572(9) 0.5060(10) 0.035(3) Uani 1 1 d . . . H4 H 0.7794 1.1341 0.5195 0.042 Uiso 1 1 calc R . . C5 C 0.7332(15) 0.9930(8) 0.5844(9) 0.028(3) Uani 1 1 d . . . H5 H 0.7341 1.0267 0.6510 0.034 Uiso 1 1 calc R . . C6 C 0.7039(14) 0.8777(8) 0.5617(8) 0.022(2) Uani 1 1 d . . . C7 C 0.6579(18) 0.7974(8) 0.6342(8) 0.026(2) Uani 1 1 d . . . C8 C 0.379(3) 0.6445(16) 0.1125(13) 0.085(3) Uani 1 1 d U . . H8 H 0.4356 0.6706 0.1779 0.102 Uiso 1 1 calc R . . C9 C 0.180(4) 0.5758(16) 0.1013(13) 0.084(3) Uani 1 1 d U . . H9 H 0.1084 0.5603 0.1577 0.101 Uiso 1 1 calc R . . C10 C 0.099(3) 0.5347(14) 0.0081(11) 0.073(3) Uani 1 1 d U . . C11 C 0.214(3) 0.5652(17) -0.0706(12) 0.082(3) Uani 1 1 d U . . H11 H 0.1662 0.5373 -0.1368 0.099 Uiso 1 1 calc R . . C12 C 0.399(3) 0.6368(16) -0.0524(12) 0.082(3) Uani 1 1 d U . . H12 H 0.4642 0.6604 -0.1077 0.099 Uiso 1 1 calc R . . C13 C 1.142(3) 0.8951(17) 0.1068(13) 0.081(3) Uani 1 1 d U . . H13 H 1.1045 0.8870 0.1719 0.097 Uiso 1 1 calc R . . C14 C 1.329(3) 0.9599(17) 0.0973(12) 0.079(3) Uani 1 1 d U . . H14 H 1.4069 0.9980 0.1544 0.095 Uiso 1 1 calc R . . C15 C 1.397(3) 0.9672(14) 0.0067(11) 0.067(3) Uani 1 1 d U . . C16 C 1.273(3) 0.9115(16) -0.0721(13) 0.079(3) Uani 1 1 d U . . H16 H 1.3172 0.9130 -0.1372 0.095 Uiso 1 1 calc R . . C17 C 1.087(3) 0.8536(16) -0.0592(12) 0.078(3) Uani 1 1 d U . . H17 H 1.0049 0.8184 -0.1160 0.094 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O8 0.010(3) 0.017(3) 0.022(3) -0.005(3) 0.008(3) 0.005(2) O7 0.020(3) 0.021(3) 0.020(4) 0.000(3) 0.002(3) 0.001(3) Sm1 0.0114(3) 0.0132(3) 0.0140(3) 0.0028(2) 0.00540(19) 0.00185(19) Cu1 0.1006(16) 0.0526(11) 0.0482(12) -0.0048(9) -0.0195(11) 0.0311(11) N1 0.012(4) 0.011(4) 0.022(4) -0.001(3) 0.007(3) -0.002(3) N2 0.110(6) 0.076(5) 0.027(4) -0.005(4) -0.020(4) 0.011(5) N3 0.082(5) 0.090(6) 0.029(4) -0.011(4) -0.007(4) 0.026(5) O1 0.022(4) 0.032(4) 0.018(4) 0.007(3) 0.012(3) 0.008(3) O2 0.070(6) 0.044(5) 0.025(5) 0.018(4) 0.008(4) -0.009(4) O3 0.034(4) 0.026(4) 0.020(4) -0.003(3) 0.016(3) -0.003(3) O4 0.119(8) 0.062(6) 0.034(5) -0.008(4) 0.026(5) 0.003(6) O5 0.010(3) 0.025(4) 0.031(4) 0.015(3) 0.008(3) 0.005(3) O6 0.015(3) 0.025(4) 0.023(4) 0.010(3) 0.006(3) 0.007(3) O9 0.030(4) 0.035(4) 0.020(4) -0.007(3) 0.007(3) -0.009(3) O10 0.105(9) 0.081(8) 0.041(6) 0.003(6) 0.010(6) 0.048(7) S1 0.0095(11) 0.0156(11) 0.0128(12) 0.0026(9) 0.0057(9) 0.0028(9) C1 0.022(5) 0.021(5) 0.026(6) 0.016(4) 0.010(4) 0.003(4) C2 0.008(4) 0.018(5) 0.029(6) 0.006(4) 0.003(4) 0.000(3) C3 0.028(6) 0.020(5) 0.046(7) 0.005(5) 0.000(5) 0.004(4) C4 0.022(6) 0.017(5) 0.063(9) 0.000(5) 0.004(5) -0.001(4) C5 0.018(5) 0.024(5) 0.040(7) -0.014(5) -0.002(5) 0.011(4) C6 0.011(4) 0.018(5) 0.035(6) -0.003(4) 0.006(4) 0.001(4) C7 0.041(6) 0.024(5) 0.015(5) -0.003(4) 0.016(4) 0.004(5) C8 0.126(7) 0.087(6) 0.032(5) -0.003(5) -0.025(5) -0.008(6) C9 0.124(7) 0.085(6) 0.032(5) -0.003(5) -0.022(5) -0.007(6) C10 0.111(7) 0.076(6) 0.026(5) -0.003(5) -0.026(5) 0.012(5) C11 0.112(7) 0.095(6) 0.030(5) -0.011(5) -0.019(5) 0.004(6) C12 0.112(7) 0.096(6) 0.030(5) -0.010(5) -0.015(5) 0.003(6) C13 0.087(6) 0.112(6) 0.037(5) -0.016(5) -0.001(5) 0.017(6) C14 0.086(6) 0.109(6) 0.035(5) -0.017(5) -0.006(5) 0.014(5) C15 0.084(6) 0.085(6) 0.030(5) -0.012(5) -0.011(5) 0.028(5) C16 0.099(6) 0.097(6) 0.035(5) -0.010(5) -0.009(5) 0.005(6) C17 0.096(6) 0.097(6) 0.035(5) -0.008(5) -0.011(5) 0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O8 S1 1.480(6) . ? O8 Sm1 2.492(6) 1_455 ? O7 S1 1.461(7) . ? O7 Sm1 2.573(6) 1_455 ? Sm1 O1 2.375(7) . ? Sm1 O3 2.389(7) . ? Sm1 O6 2.439(6) 2_666 ? Sm1 O9 2.455(7) . ? Sm1 O8 2.492(6) 1_655 ? Sm1 O5 2.499(6) . ? Sm1 N1 2.519(7) . ? Sm1 O7 2.573(7) 1_655 ? Sm1 O6 2.675(7) . ? Sm1 S1 3.135(2) 1_655 ? Cu1 N2 1.912(16) . ? Cu1 N3 1.939(16) . ? Cu1 O2 2.274(9) . ? N1 C2 1.330(12) . ? N1 C6 1.335(13) . ? N2 C12 1.298(19) . ? N2 C8 1.31(2) . ? N3 C13 1.29(2) . ? N3 C17 1.34(2) . ? O1 C1 1.258(12) . ? O2 C1 1.251(13) . ? O3 C7 1.249(12) . ? O4 C7 1.242(13) . ? O5 S1 1.469(7) . ? O6 S1 1.495(6) . ? O6 Sm1 2.439(6) 2_666 ? O9 H18 0.8600 . ? O9 H19 0.8602 . ? O10 H20 0.8600 . ? O10 H21 0.8600 . ? S1 Sm1 3.135(2) 1_455 ? C1 C2 1.505(14) . ? C2 C3 1.386(14) . ? C3 C4 1.361(17) . ? C3 H3 0.9300 . ? C4 C5 1.397(17) . ? C4 H4 0.9300 . ? C5 C6 1.397(14) . ? C5 H5 0.9300 . ? C6 C7 1.485(14) . ? C8 C9 1.44(3) . ? C8 H8 0.9300 . ? C9 C10 1.34(2) . ? C9 H9 0.9300 . ? C10 C11 1.38(3) . ? C10 C10 1.44(4) 2_565 ? C11 C12 1.38(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.38(3) . ? C13 H13 0.9300 . ? C14 C15 1.32(2) . ? C14 H14 0.9300 . ? C15 C16 1.35(2) . ? C15 C15 1.50(4) 2_875 ? C16 C17 1.35(3) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 O8 Sm1 101.1(3) . 1_455 ? S1 O7 Sm1 98.2(3) . 1_455 ? O1 Sm1 O3 127.5(2) . . ? O1 Sm1 O6 154.7(2) . 2_666 ? O3 Sm1 O6 74.8(2) . 2_666 ? O1 Sm1 O9 86.0(2) . . ? O3 Sm1 O9 142.8(2) . . ? O6 Sm1 O9 77.4(2) 2_666 . ? O1 Sm1 O8 89.0(2) . 1_655 ? O3 Sm1 O8 76.5(2) . 1_655 ? O6 Sm1 O8 85.1(2) 2_666 1_655 ? O9 Sm1 O8 125.1(2) . 1_655 ? O1 Sm1 O5 76.5(2) . . ? O3 Sm1 O5 91.4(2) . . ? O6 Sm1 O5 118.7(2) 2_666 . ? O9 Sm1 O5 80.6(2) . . ? O8 Sm1 O5 149.9(2) 1_655 . ? O1 Sm1 N1 64.0(2) . . ? O3 Sm1 N1 63.6(2) . . ? O6 Sm1 N1 136.9(2) 2_666 . ? O9 Sm1 N1 144.7(3) . . ? O8 Sm1 N1 75.2(2) 1_655 . ? O5 Sm1 N1 74.7(2) . . ? O1 Sm1 O7 74.7(2) . 1_655 ? O3 Sm1 O7 127.6(2) . 1_655 ? O6 Sm1 O7 81.8(2) 2_666 1_655 ? O9 Sm1 O7 71.0(2) . 1_655 ? O8 Sm1 O7 55.1(2) 1_655 1_655 ? O5 Sm1 O7 140.6(2) . 1_655 ? N1 Sm1 O7 114.6(2) . 1_655 ? O1 Sm1 O6 127.3(2) . . ? O3 Sm1 O6 74.0(2) . . ? O6 Sm1 O6 65.4(2) 2_666 . ? O9 Sm1 O6 72.2(2) . . ? O8 Sm1 O6 142.6(2) 1_655 . ? O5 Sm1 O6 53.4(2) . . ? N1 Sm1 O6 110.5(2) . . ? O7 Sm1 O6 134.9(2) 1_655 . ? O1 Sm1 S1 80.37(16) . 1_655 ? O3 Sm1 S1 102.52(18) . 1_655 ? O6 Sm1 S1 83.18(15) 2_666 1_655 ? O9 Sm1 S1 98.16(18) . 1_655 ? O8 Sm1 S1 27.60(14) 1_655 1_655 ? O5 Sm1 S1 156.84(16) . 1_655 ? N1 Sm1 S1 94.87(17) . 1_655 ? O7 Sm1 S1 27.47(15) 1_655 1_655 ? O6 Sm1 S1 148.32(14) . 1_655 ? N2 Cu1 N3 160.8(6) . . ? N2 Cu1 O2 105.6(5) . . ? N3 Cu1 O2 93.4(4) . . ? C2 N1 C6 121.2(8) . . ? C2 N1 Sm1 119.2(6) . . ? C6 N1 Sm1 119.6(6) . . ? C12 N2 C8 115.6(18) . . ? C12 N2 Cu1 122.0(14) . . ? C8 N2 Cu1 122.3(12) . . ? C13 N3 C17 114.4(17) . . ? C13 N3 Cu1 120.2(13) . . ? C17 N3 Cu1 125.3(12) . . ? C1 O1 Sm1 125.7(6) . . ? C1 O2 Cu1 118.9(8) . . ? C7 O3 Sm1 126.3(7) . . ? S1 O5 Sm1 105.7(3) . . ? S1 O6 Sm1 148.2(4) . 2_666 ? S1 O6 Sm1 97.1(3) . . ? Sm1 O6 Sm1 114.6(2) 2_666 . ? Sm1 O9 H18 113.8 . . ? Sm1 O9 H19 94.4 . . ? H18 O9 H19 105.3 . . ? H20 O10 H21 104.0 . . ? O7 S1 O5 113.5(4) . . ? O7 S1 O8 105.6(4) . . ? O5 S1 O8 111.6(4) . . ? O7 S1 O6 111.9(4) . . ? O5 S1 O6 103.7(4) . . ? O8 S1 O6 110.6(4) . . ? O7 S1 Sm1 54.3(3) . 1_455 ? O5 S1 Sm1 128.0(3) . 1_455 ? O8 S1 Sm1 51.3(2) . 1_455 ? O6 S1 Sm1 128.2(3) . 1_455 ? O2 C1 O1 125.6(10) . . ? O2 C1 C2 118.8(9) . . ? O1 C1 C2 115.6(8) . . ? N1 C2 C3 121.0(10) . . ? N1 C2 C1 113.9(8) . . ? C3 C2 C1 125.1(9) . . ? C4 C3 C2 119.6(11) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 118.9(10) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C6 C5 C4 119.2(11) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? N1 C6 C5 119.8(10) . . ? N1 C6 C7 113.8(8) . . ? C5 C6 C7 126.4(10) . . ? O4 C7 O3 124.5(10) . . ? O4 C7 C6 118.8(9) . . ? O3 C7 C6 116.7(9) . . ? N2 C8 C9 124.6(16) . . ? N2 C8 H8 117.7 . . ? C9 C8 H8 117.7 . . ? C10 C9 C8 118.5(19) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C9 C10 C11 116.4(18) . . ? C9 C10 C10 121(2) . 2_565 ? C11 C10 C10 122.5(17) . 2_565 ? C10 C11 C12 121.0(15) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? N2 C12 C11 123.8(19) . . ? N2 C12 H12 118.1 . . ? C11 C12 H12 118.1 . . ? N3 C13 C14 125.1(18) . . ? N3 C13 H13 117.4 . . ? C14 C13 H13 117.4 . . ? C15 C14 C13 119.4(16) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 116.5(19) . . ? C14 C15 C15 121.1(18) . 2_875 ? C16 C15 C15 122.4(19) . 2_875 ? C15 C16 C17 121.8(18) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? N3 C17 C16 122.5(16) . . ? N3 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? 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 O1 Sm1 N1 C2 4.3(6) . . . . ? O3 Sm1 N1 C2 -177.3(7) . . . . ? O6 Sm1 N1 C2 166.3(5) 2_666 . . . ? O9 Sm1 N1 C2 -30.4(8) . . . . ? O8 Sm1 N1 C2 100.6(6) 1_655 . . . ? O5 Sm1 N1 C2 -77.8(6) . . . . ? O7 Sm1 N1 C2 61.2(7) 1_655 . . . ? O6 Sm1 N1 C2 -118.3(6) . . . . ? S1 Sm1 N1 C2 81.1(6) 1_655 . . . ? O1 Sm1 N1 C6 -176.1(7) . . . . ? O3 Sm1 N1 C6 2.2(6) . . . . ? O6 Sm1 N1 C6 -14.1(8) 2_666 . . . ? O9 Sm1 N1 C6 149.1(6) . . . . ? O8 Sm1 N1 C6 -79.8(6) 1_655 . . . ? O5 Sm1 N1 C6 101.7(6) . . . . ? O7 Sm1 N1 C6 -119.2(6) 1_655 . . . ? O6 Sm1 N1 C6 61.3(7) . . . . ? S1 Sm1 N1 C6 -99.3(6) 1_655 . . . ? N3 Cu1 N2 C12 -21(3) . . . . ? O2 Cu1 N2 C12 152.0(15) . . . . ? N3 Cu1 N2 C8 163.1(17) . . . . ? O2 Cu1 N2 C8 -24.1(17) . . . . ? N2 Cu1 N3 C13 -164.5(16) . . . . ? O2 Cu1 N3 C13 22.5(15) . . . . ? N2 Cu1 N3 C17 17(3) . . . . ? O2 Cu1 N3 C17 -155.7(15) . . . . ? O3 Sm1 O1 C1 -13.2(9) . . . . ? O6 Sm1 O1 C1 -161.7(7) 2_666 . . . ? O9 Sm1 O1 C1 149.4(8) . . . . ? O8 Sm1 O1 C1 -85.3(8) 1_655 . . . ? O5 Sm1 O1 C1 68.1(8) . . . . ? N1 Sm1 O1 C1 -11.3(7) . . . . ? O7 Sm1 O1 C1 -139.2(8) 1_655 . . . ? O6 Sm1 O1 C1 85.4(8) . . . . ? S1 Sm1 O1 C1 -111.6(8) 1_655 . . . ? N2 Cu1 O2 C1 68.9(10) . . . . ? N3 Cu1 O2 C1 -113.5(9) . . . . ? O1 Sm1 O3 C7 1.8(10) . . . . ? O6 Sm1 O3 C7 168.4(9) 2_666 . . . ? O9 Sm1 O3 C7 -148.6(8) . . . . ? O8 Sm1 O3 C7 79.9(9) 1_655 . . . ? O5 Sm1 O3 C7 -72.2(9) . . . . ? N1 Sm1 O3 C7 -0.1(8) . . . . ? O7 Sm1 O3 C7 101.7(9) 1_655 . . . ? O6 Sm1 O3 C7 -123.4(9) . . . . ? S1 Sm1 O3 C7 89.2(8) 1_655 . . . ? O1 Sm1 O5 S1 165.0(4) . . . . ? O3 Sm1 O5 S1 -66.6(4) . . . . ? O6 Sm1 O5 S1 6.8(5) 2_666 . . . ? O9 Sm1 O5 S1 76.9(4) . . . . ? O8 Sm1 O5 S1 -131.7(4) 1_655 . . . ? N1 Sm1 O5 S1 -128.7(4) . . . . ? O7 Sm1 O5 S1 120.9(4) 1_655 . . . ? O6 Sm1 O5 S1 2.2(3) . . . . ? S1 Sm1 O5 S1 165.8(2) 1_655 . . . ? O1 Sm1 O6 S1 -23.2(4) . . . . ? O3 Sm1 O6 S1 102.2(4) . . . . ? O6 Sm1 O6 S1 -177.6(5) 2_666 . . . ? O9 Sm1 O6 S1 -93.5(4) . . . . ? O8 Sm1 O6 S1 141.3(3) 1_655 . . . ? O5 Sm1 O6 S1 -2.1(3) . . . . ? N1 Sm1 O6 S1 49.1(4) . . . . ? O7 Sm1 O6 S1 -130.2(3) 1_655 . . . ? S1 Sm1 O6 S1 -169.86(17) 1_655 . . . ? O1 Sm1 O6 Sm1 154.4(3) . . . 2_666 ? O3 Sm1 O6 Sm1 -80.3(3) . . . 2_666 ? O6 Sm1 O6 Sm1 0.0 2_666 . . 2_666 ? O9 Sm1 O6 Sm1 84.0(3) . . . 2_666 ? O8 Sm1 O6 Sm1 -41.1(5) 1_655 . . 2_666 ? O5 Sm1 O6 Sm1 175.5(4) . . . 2_666 ? N1 Sm1 O6 Sm1 -133.3(3) . . . 2_666 ? O7 Sm1 O6 Sm1 47.3(4) 1_655 . . 2_666 ? S1 Sm1 O6 Sm1 7.7(5) 1_655 . . 2_666 ? Sm1 O7 S1 O5 -120.9(3) 1_455 . . . ? Sm1 O7 S1 O8 1.7(4) 1_455 . . . ? Sm1 O7 S1 O6 122.1(3) 1_455 . . . ? Sm1 O5 S1 O7 -124.9(4) . . . . ? Sm1 O5 S1 O8 115.9(4) . . . . ? Sm1 O5 S1 O6 -3.2(4) . . . . ? Sm1 O5 S1 Sm1 172.96(10) . . . 1_455 ? Sm1 O8 S1 O7 -1.8(4) 1_455 . . . ? Sm1 O8 S1 O5 122.0(3) 1_455 . . . ? Sm1 O8 S1 O6 -123.0(3) 1_455 . . . ? Sm1 O6 S1 O7 -50.2(9) 2_666 . . . ? Sm1 O6 S1 O7 125.6(3) . . . . ? Sm1 O6 S1 O5 -172.9(7) 2_666 . . . ? Sm1 O6 S1 O5 2.9(4) . . . . ? Sm1 O6 S1 O8 67.3(8) 2_666 . . . ? Sm1 O6 S1 O8 -116.9(3) . . . . ? Sm1 O6 S1 Sm1 11.0(10) 2_666 . . 1_455 ? Sm1 O6 S1 Sm1 -173.24(11) . . . 1_455 ? Cu1 O2 C1 O1 -3.3(15) . . . . ? Cu1 O2 C1 C2 178.9(6) . . . . ? Sm1 O1 C1 O2 -162.0(8) . . . . ? Sm1 O1 C1 C2 16.0(12) . . . . ? C6 N1 C2 C3 0.7(13) . . . . ? Sm1 N1 C2 C3 -179.7(7) . . . . ? C6 N1 C2 C1 -178.6(8) . . . . ? Sm1 N1 C2 C1 1.0(9) . . . . ? O2 C1 C2 N1 168.0(9) . . . . ? O1 C1 C2 N1 -10.1(12) . . . . ? O2 C1 C2 C3 -11.3(15) . . . . ? O1 C1 C2 C3 170.6(9) . . . . ? N1 C2 C3 C4 2.5(15) . . . . ? C1 C2 C3 C4 -178.3(9) . . . . ? C2 C3 C4 C5 -2.3(15) . . . . ? C3 C4 C5 C6 -0.8(14) . . . . ? C2 N1 C6 C5 -3.9(13) . . . . ? Sm1 N1 C6 C5 176.6(7) . . . . ? C2 N1 C6 C7 175.8(8) . . . . ? Sm1 N1 C6 C7 -3.8(10) . . . . ? C4 C5 C6 N1 3.9(14) . . . . ? C4 C5 C6 C7 -175.7(9) . . . . ? Sm1 O3 C7 O4 174.8(10) . . . . ? Sm1 O3 C7 C6 -1.8(13) . . . . ? N1 C6 C7 O4 -173.2(11) . . . . ? C5 C6 C7 O4 6.4(17) . . . . ? N1 C6 C7 O3 3.6(13) . . . . ? C5 C6 C7 O3 -176.8(10) . . . . ? C12 N2 C8 C9 2(3) . . . . ? Cu1 N2 C8 C9 177.8(15) . . . . ? N2 C8 C9 C10 2(3) . . . . ? C8 C9 C10 C11 -2(3) . . . . ? C8 C9 C10 C10 180(2) . . . 2_565 ? C9 C10 C11 C12 -2(3) . . . . ? C10 C10 C11 C12 177(2) 2_565 . . . ? C8 N2 C12 C11 -5(3) . . . . ? Cu1 N2 C12 C11 178.4(15) . . . . ? C10 C11 C12 N2 6(3) . . . . ? C17 N3 C13 C14 4(3) . . . . ? Cu1 N3 C13 C14 -174.0(15) . . . . ? N3 C13 C14 C15 -5(3) . . . . ? C13 C14 C15 C16 1(3) . . . . ? C13 C14 C15 C15 -177.6(19) . . . 2_875 ? C14 C15 C16 C17 2(3) . . . . ? C15 C15 C16 C17 -179(2) 2_875 . . . ? C13 N3 C17 C16 -1(3) . . . . ? Cu1 N3 C17 C16 177.2(14) . . . . ? C15 C16 C17 N3 -2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.882 _refine_diff_density_min -3.240 _refine_diff_density_rms 0.290 # Attachment 'Eu-Cu.cif' data_061202f _database_code_depnum_ccdc_archive 'CCDC 630339' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H30 Cu2 Eu2 N6 O20 S2' _chemical_formula_weight 1337.76 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' Cu Cu 0.3201 1.2651 '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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.383(2) _cell_length_b 12.333(3) _cell_length_c 13.507(2) _cell_angle_alpha 97.427(3) _cell_angle_beta 93.019(2) _cell_angle_gamma 95.519(3) _cell_volume 1047.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4333 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 28.24 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.121 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 4.144 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2090 _exptl_absorpt_correction_T_max 0.6820 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4235 _diffrn_reflns_av_R_equivalents 0.1070 _diffrn_reflns_av_sigmaI/netI 0.0817 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2821 _reflns_number_gt 2587 _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^)+(0.1273P)^2^+54.7124P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2821 _refine_ls_number_parameters 298 _refine_ls_number_restraints 203 _refine_ls_R_factor_all 0.1051 _refine_ls_R_factor_gt 0.0960 _refine_ls_wR_factor_ref 0.2315 _refine_ls_wR_factor_gt 0.2256 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.7467(7) 0.7689(3) 0.5587(3) 0.0733(12) Uani 1 1 d . . . Eu1 Eu 0.68249(13) 0.62215(7) 0.92878(6) 0.0167(3) Uani 1 1 d D . . N1 N 0.715(3) 0.8264(13) 0.9671(13) 0.031(4) Uani 1 1 d . . . N2 N 0.482(5) 0.676(2) 0.537(2) 0.076(5) Uani 1 1 d U . . N3 N 1.018(4) 0.842(2) 0.5322(15) 0.069(5) Uani 1 1 d DU . . O1 O 0.755(2) 0.7206(11) 0.7914(11) 0.033(3) Uani 1 1 d . . . O2 O 0.739(3) 0.8714(13) 0.7135(13) 0.053(4) Uani 1 1 d . . . O3 O 0.634(2) 0.6925(10) 1.0949(8) 0.029(3) Uani 1 1 d DU . . O4 O 0.620(4) 0.8362(16) 1.2193(13) 0.079(7) Uani 1 1 d D . . O5 O 0.6979(19) 0.4684(10) 1.0234(9) 0.024(3) Uani 1 1 d . . . O6 O 0.943(2) 0.3225(10) 1.0029(11) 0.031(3) Uani 1 1 d . . . O7 O 0.672(2) 0.3230(11) 1.1244(11) 0.034(3) Uani 1 1 d . . . O8 O 0.990(2) 0.4572(10) 1.1457(11) 0.032(3) Uani 1 1 d . . . O9 O 0.564(2) 0.4633(11) 0.8021(11) 0.037(3) Uani 1 1 d . . . H18 H 0.4366 0.4425 0.8114 0.055 Uiso 1 1 d R . . H19 H 0.6033 0.4123 0.8334 0.055 Uiso 1 1 d R . . O10 O 0.840(3) 0.2967(16) 0.7814(15) 0.062(5) Uani 1 1 d U . . H20 H 0.8575 0.2817 0.8407 0.093 Uiso 1 1 d R . . H21 H 0.7300 0.3304 0.7799 0.093 Uiso 1 1 d R . . S1 S 0.8260(6) 0.3927(3) 1.0742(3) 0.0163(8) Uani 1 1 d . . . C1 C 0.741(3) 0.8201(15) 0.7894(14) 0.031(4) Uani 1 1 d . . . C2 C 0.740(3) 0.8913(16) 0.8911(15) 0.031(4) Uani 1 1 d . . . C3 C 0.764(3) 1.0053(16) 0.9082(16) 0.033(4) Uani 1 1 d . . . H3 H 0.7805 1.0469 0.8559 0.040 Uiso 1 1 calc R . . C4 C 0.763(3) 1.0567(19) 1.0103(18) 0.042(5) Uani 1 1 d . . . H4 H 0.7801 1.1330 1.0245 0.050 Uiso 1 1 calc R . . C5 C 0.737(3) 0.9920(14) 1.0894(15) 0.028(4) Uani 1 1 d . . . H5 H 0.7408 1.0246 1.1556 0.034 Uiso 1 1 calc R . . C6 C 0.705(3) 0.8790(15) 1.0646(14) 0.034(4) Uani 1 1 d D . . C7 C 0.657(4) 0.7948(12) 1.1340(11) 0.043(5) Uani 1 1 d D . . C8 C 0.393(6) 0.642(3) 0.612(3) 0.084(6) Uani 1 1 d U . . H8 H 0.4639 0.6597 0.6749 0.101 Uiso 1 1 calc R . . C9 C 0.183(6) 0.576(3) 0.605(3) 0.085(6) Uani 1 1 d U . . H9 H 0.1116 0.5630 0.6610 0.102 Uiso 1 1 calc R . . C10 C 0.098(6) 0.535(3) 0.505(2) 0.072(5) Uani 1 1 d U . . C11 C 0.212(6) 0.576(3) 0.429(3) 0.082(6) Uani 1 1 d U . . H11 H 0.1597 0.5558 0.3629 0.098 Uiso 1 1 calc R . . C12 C 0.402(6) 0.647(3) 0.447(3) 0.083(6) Uani 1 1 d U . . H12 H 0.4683 0.6734 0.3943 0.099 Uiso 1 1 calc R . . C13 C 1.150(4) 0.876(3) 0.618(2) 0.075(5) Uani 1 1 d DU . . H13 H 1.1205 0.8563 0.6801 0.090 Uiso 1 1 calc R . . C14 C 1.333(5) 0.942(3) 0.601(2) 0.075(5) Uani 1 1 d DU . . H14 H 1.4201 0.9724 0.6567 0.090 Uiso 1 1 calc R . . C15 C 1.397(4) 0.967(2) 0.5074(17) 0.064(5) Uani 1 1 d DU . . C16 C 1.258(4) 0.918(3) 0.427(2) 0.075(5) Uani 1 1 d DU . . H16 H 1.2933 0.9286 0.3623 0.090 Uiso 1 1 calc R . . C17 C 1.071(5) 0.855(3) 0.4369(19) 0.075(5) Uani 1 1 d DU . . H17 H 0.9843 0.8223 0.3814 0.090 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.102(3) 0.053(2) 0.065(2) -0.0006(17) -0.020(2) 0.033(2) Eu1 0.0143(5) 0.0133(4) 0.0250(5) 0.0075(3) 0.0028(3) 0.0063(3) N1 0.026(8) 0.025(8) 0.039(9) -0.004(7) 0.013(7) -0.001(7) N2 0.095(12) 0.068(10) 0.059(10) 0.000(9) -0.033(9) 0.010(9) N3 0.079(10) 0.068(10) 0.058(9) -0.006(8) -0.013(8) 0.028(9) O1 0.041(8) 0.027(7) 0.040(8) 0.025(6) 0.005(6) 0.013(6) O2 0.066(12) 0.036(9) 0.056(11) 0.012(8) 0.011(8) -0.009(8) O3 0.029(3) 0.029(3) 0.029(3) 0.0044(11) 0.0029(10) 0.0034(11) O4 0.14(2) 0.044(11) 0.053(12) -0.014(9) 0.022(12) 0.017(12) O5 0.020(6) 0.028(7) 0.029(7) 0.009(5) 0.002(5) 0.018(5) O6 0.018(6) 0.024(6) 0.056(9) 0.007(6) 0.026(6) 0.011(5) O7 0.027(7) 0.032(7) 0.047(8) 0.014(6) 0.018(6) 0.010(6) O8 0.021(6) 0.021(6) 0.051(8) -0.005(6) 0.000(6) 0.007(5) O9 0.042(8) 0.021(7) 0.041(8) -0.003(6) 0.001(6) -0.016(6) O10 0.062(5) 0.062(5) 0.062(5) 0.0083(12) 0.0040(11) 0.0067(11) S1 0.0104(17) 0.0125(18) 0.028(2) 0.0062(15) 0.0010(15) 0.0061(15) C1 0.043(11) 0.025(10) 0.023(9) 0.005(7) 0.001(8) -0.009(8) C2 0.041(11) 0.023(9) 0.034(10) 0.002(8) 0.006(8) 0.026(8) C3 0.029(10) 0.028(10) 0.042(11) -0.002(8) 0.006(8) 0.005(8) C4 0.031(11) 0.040(12) 0.054(14) 0.006(10) -0.013(10) 0.008(9) C5 0.035(10) 0.017(8) 0.036(10) 0.002(7) 0.018(8) 0.009(7) C6 0.047(12) 0.027(10) 0.029(10) 0.005(8) 0.005(8) 0.012(9) C7 0.048(14) 0.039(12) 0.044(13) -0.002(10) 0.009(10) 0.016(10) C8 0.107(13) 0.071(11) 0.066(11) 0.003(9) -0.033(10) -0.005(10) C9 0.107(13) 0.074(11) 0.065(11) 0.006(9) -0.025(10) -0.008(10) C10 0.096(13) 0.060(11) 0.056(10) -0.001(9) -0.027(10) 0.013(10) C11 0.097(13) 0.082(11) 0.060(10) -0.001(9) -0.023(10) 0.009(10) C12 0.098(13) 0.082(11) 0.063(10) 0.005(10) -0.024(10) 0.002(10) C13 0.077(11) 0.087(11) 0.060(10) 0.003(9) -0.006(9) 0.021(10) C14 0.075(11) 0.087(11) 0.059(10) -0.005(9) -0.015(9) 0.021(10) C15 0.071(10) 0.063(10) 0.056(9) -0.006(9) -0.017(9) 0.035(9) C16 0.088(11) 0.074(11) 0.060(10) 0.000(9) -0.014(9) 0.008(10) C17 0.087(11) 0.073(11) 0.063(10) 0.008(9) -0.012(9) 0.010(10) _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 Cu1 N2 1.93(3) . ? Cu1 N3 1.95(3) . ? Cu1 O2 2.305(18) . ? Eu1 O3 2.347(11) . ? Eu1 O1 2.387(13) . ? Eu1 O5 2.427(12) . ? Eu1 O9 2.460(13) . ? Eu1 N1 2.491(16) . ? Eu1 O6 2.515(14) 2_767 ? Eu1 O7 2.519(14) 2_667 ? Eu1 O8 2.586(12) 2_767 ? Eu1 O5 2.718(13) 2_667 ? Eu1 S1 3.162(4) 2_767 ? Eu1 S1 3.231(4) 2_667 ? Eu1 Eu1 4.3390(18) 2_667 ? Eu1 H19 2.7263 . ? N1 C2 1.39(3) . ? N1 C6 1.40(2) . ? N2 C8 1.28(5) . ? N2 C12 1.28(4) . ? N3 C17 1.372(18) . ? N3 C13 1.387(18) . ? O1 C1 1.24(2) . ? O2 C1 1.27(3) . ? O3 C7 1.295(15) . ? O4 C7 1.244(15) . ? O5 S1 1.504(12) . ? O5 Eu1 2.718(13) 2_667 ? O6 S1 1.490(12) . ? O6 Eu1 2.515(14) 2_767 ? O7 S1 1.491(14) . ? O7 Eu1 2.519(14) 2_667 ? O8 S1 1.482(14) . ? O8 Eu1 2.586(12) 2_767 ? O9 H18 0.8505 . ? O9 H19 0.8503 . ? O10 H20 0.8500 . ? O10 H21 0.8500 . ? S1 Eu1 3.162(4) 2_767 ? S1 Eu1 3.231(4) 2_667 ? C1 C2 1.53(3) . ? C2 C3 1.39(3) . ? C3 C4 1.44(3) . ? C3 H3 0.9300 . ? C4 C5 1.42(3) . ? C4 H4 0.9300 . ? C5 C6 1.38(3) . ? C5 H5 0.9300 . ? C6 C7 1.507(17) . ? C8 C9 1.49(5) . ? C8 H8 0.9300 . ? C9 C10 1.44(4) . ? C9 H9 0.9300 . ? C10 C11 1.41(5) . ? C10 C10 1.43(7) 2_566 ? C11 C12 1.42(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.406(19) . ? C13 H13 0.9300 . ? C14 C15 1.407(19) . ? C14 H14 0.9300 . ? C15 C16 1.404(18) . ? C15 C15 1.52(6) 2_876 ? C16 C17 1.385(19) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N3 160.2(11) . . ? N2 Cu1 O2 106.1(10) . . ? N3 Cu1 O2 93.5(8) . . ? O3 Eu1 O1 128.5(5) . . ? O3 Eu1 O5 74.3(4) . . ? O1 Eu1 O5 154.6(4) . . ? O3 Eu1 O9 140.9(5) . . ? O1 Eu1 O9 86.2(5) . . ? O5 Eu1 O9 77.4(5) . . ? O3 Eu1 N1 64.3(5) . . ? O1 Eu1 N1 64.2(5) . . ? O5 Eu1 N1 136.5(5) . . ? O9 Eu1 N1 145.2(6) . . ? O3 Eu1 O6 78.6(4) . 2_767 ? O1 Eu1 O6 88.6(5) . 2_767 ? O5 Eu1 O6 85.3(4) . 2_767 ? O9 Eu1 O6 125.4(5) . 2_767 ? N1 Eu1 O6 74.4(5) . 2_767 ? O3 Eu1 O7 89.7(5) . 2_667 ? O1 Eu1 O7 76.4(5) . 2_667 ? O5 Eu1 O7 119.1(4) . 2_667 ? O9 Eu1 O7 81.0(5) . 2_667 ? N1 Eu1 O7 74.7(5) . 2_667 ? O6 Eu1 O7 149.1(4) 2_767 2_667 ? O3 Eu1 O8 129.1(5) . 2_767 ? O1 Eu1 O8 75.0(5) . 2_767 ? O5 Eu1 O8 81.3(4) . 2_767 ? O9 Eu1 O8 71.1(5) . 2_767 ? N1 Eu1 O8 114.6(5) . 2_767 ? O6 Eu1 O8 55.2(4) 2_767 2_767 ? O7 Eu1 O8 140.9(5) 2_667 2_767 ? O3 Eu1 O5 72.1(4) . 2_667 ? O1 Eu1 O5 127.7(4) . 2_667 ? O5 Eu1 O5 65.1(4) . 2_667 ? O9 Eu1 O5 71.7(4) . 2_667 ? N1 Eu1 O5 111.2(4) . 2_667 ? O6 Eu1 O5 142.8(4) 2_767 2_667 ? O7 Eu1 O5 54.1(4) 2_667 2_667 ? O8 Eu1 O5 134.1(4) 2_767 2_667 ? O3 Eu1 S1 104.1(3) . 2_767 ? O1 Eu1 S1 80.7(3) . 2_767 ? O5 Eu1 S1 82.6(3) . 2_767 ? O9 Eu1 S1 98.4(4) . 2_767 ? N1 Eu1 S1 94.7(4) . 2_767 ? O6 Eu1 S1 27.5(3) 2_767 2_767 ? O7 Eu1 S1 157.1(3) 2_667 2_767 ? O8 Eu1 S1 27.6(3) 2_767 2_767 ? O5 Eu1 S1 147.5(2) 2_667 2_767 ? O3 Eu1 S1 78.8(3) . 2_667 ? O1 Eu1 S1 102.1(3) . 2_667 ? O5 Eu1 S1 92.7(3) . 2_667 ? O9 Eu1 S1 76.1(4) . 2_667 ? N1 Eu1 S1 91.8(4) . 2_667 ? O6 Eu1 S1 157.0(3) 2_767 2_667 ? O7 Eu1 S1 26.5(3) 2_667 2_667 ? O8 Eu1 S1 147.2(3) 2_767 2_667 ? O5 Eu1 S1 27.6(2) 2_667 2_667 ? S1 Eu1 S1 173.49(13) 2_767 2_667 ? O3 Eu1 Eu1 69.9(3) . 2_667 ? O1 Eu1 Eu1 152.7(4) . 2_667 ? O5 Eu1 Eu1 34.6(3) . 2_667 ? O9 Eu1 Eu1 71.4(3) . 2_667 ? N1 Eu1 Eu1 129.2(4) . 2_667 ? O6 Eu1 Eu1 117.0(3) 2_767 2_667 ? O7 Eu1 Eu1 84.5(3) 2_667 2_667 ? O8 Eu1 Eu1 110.6(3) 2_767 2_667 ? O5 Eu1 Eu1 30.5(2) 2_667 2_667 ? S1 Eu1 Eu1 117.15(7) 2_767 2_667 ? S1 Eu1 Eu1 58.10(7) 2_667 2_667 ? O3 Eu1 H19 129.6 . . ? O1 Eu1 H19 101.1 . . ? O5 Eu1 H19 60.1 . . ? O9 Eu1 H19 17.9 . . ? N1 Eu1 H19 163.0 . . ? O6 Eu1 H19 115.3 2_767 . ? O7 Eu1 H19 94.3 2_667 . ? O8 Eu1 H19 66.1 2_767 . ? O5 Eu1 H19 70.2 2_667 . ? S1 Eu1 H19 90.8 2_767 . ? S1 Eu1 H19 82.9 2_667 . ? Eu1 Eu1 H19 60.6 2_667 . ? C2 N1 C6 118.0(15) . . ? C2 N1 Eu1 120.5(12) . . ? C6 N1 Eu1 121.5(12) . . ? C8 N2 C12 121(3) . . ? C8 N2 Cu1 120(2) . . ? C12 N2 Cu1 119(3) . . ? C17 N3 C13 125(3) . . ? C17 N3 Cu1 122.0(18) . . ? C13 N3 Cu1 113.4(19) . . ? C1 O1 Eu1 126.1(13) . . ? C1 O2 Cu1 117.2(13) . . ? C7 O3 Eu1 126.9(10) . . ? S1 O5 Eu1 149.6(8) . . ? S1 O5 Eu1 95.5(6) . 2_667 ? Eu1 O5 Eu1 114.9(4) . 2_667 ? S1 O6 Eu1 101.2(7) . 2_767 ? S1 O7 Eu1 104.4(7) . 2_667 ? S1 O8 Eu1 98.3(6) . 2_767 ? Eu1 O9 H18 107.7 . . ? Eu1 O9 H19 99.1 . . ? H18 O9 H19 89.4 . . ? H20 O10 H21 106.2 . . ? O8 S1 O6 105.3(8) . . ? O8 S1 O7 112.6(9) . . ? O6 S1 O7 110.2(8) . . ? O8 S1 O5 110.4(7) . . ? O6 S1 O5 112.8(8) . . ? O7 S1 O5 105.7(8) . . ? O8 S1 Eu1 54.0(5) . 2_767 ? O6 S1 Eu1 51.3(6) . 2_767 ? O7 S1 Eu1 126.6(6) . 2_767 ? O5 S1 Eu1 127.6(5) . 2_767 ? O8 S1 Eu1 130.8(5) . 2_667 ? O6 S1 Eu1 123.7(6) . 2_667 ? O7 S1 Eu1 49.0(5) . 2_667 ? O5 S1 Eu1 56.9(5) . 2_667 ? Eu1 S1 Eu1 173.49(13) 2_767 2_667 ? O1 C1 O2 128.0(19) . . ? O1 C1 C2 116.2(17) . . ? O2 C1 C2 115.7(17) . . ? C3 C2 N1 123.0(18) . . ? C3 C2 C1 126.1(18) . . ? N1 C2 C1 110.9(15) . . ? C2 C3 C4 117(2) . . ? C2 C3 H3 121.3 . . ? C4 C3 H3 121.3 . . ? C5 C4 C3 121(2) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 117.8(18) . . ? C6 C5 H5 121.1 . . ? C4 C5 H5 121.1 . . ? C5 C6 N1 122.8(16) . . ? C5 C6 C7 127.3(16) . . ? N1 C6 C7 109.9(15) . . ? O4 C7 O3 129.0(18) . . ? O4 C7 C6 113.2(16) . . ? O3 C7 C6 117.1(13) . . ? N2 C8 C9 124(3) . . ? N2 C8 H8 117.9 . . ? C9 C8 H8 117.9 . . ? C10 C9 C8 115(3) . . ? C10 C9 H9 122.3 . . ? C8 C9 H9 122.3 . . ? C11 C10 C10 128(3) . 2_566 ? C11 C10 C9 114(3) . . ? C10 C10 C9 117(4) 2_566 . ? C10 C11 C12 124(3) . . ? C10 C11 H11 118.1 . . ? C12 C11 H11 118.1 . . ? N2 C12 C11 120(4) . . ? N2 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? N3 C13 C14 113(3) . . ? N3 C13 H13 123.3 . . ? C14 C13 H13 123.3 . . ? C13 C14 C15 126(3) . . ? C13 C14 H14 116.8 . . ? C15 C14 H14 116.8 . . ? C16 C15 C14 113(3) . . ? C16 C15 C15 122(3) . 2_876 ? C14 C15 C15 124(3) . 2_876 ? C17 C16 C15 124(3) . . ? C17 C16 H16 118.1 . . ? C15 C16 H16 118.1 . . ? N3 C17 C16 118(3) . . ? N3 C17 H17 121.2 . . ? C16 C17 H17 121.2 . . ? _diffrn_measured_fraction_theta_max 0.764 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.764 _refine_diff_density_max 3.733 _refine_diff_density_min -1.843 _refine_diff_density_rms 0.338 # Attachment 'Gd-Cu.cif' data_061202e _database_code_depnum_ccdc_archive 'CCDC 630340' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H30 Cu2 Gd2 N6 O20 S2' _chemical_formula_weight 1348.34 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' Cu Cu 0.3201 1.2651 '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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.648(3) _cell_length_b 13.225(3) _cell_length_c 14.475(3) _cell_angle_alpha 87.804(3) _cell_angle_beta 67.298(2) _cell_angle_gamma 66.926(3) _cell_volume 2036.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3670 _cell_measurement_theta_min 2.432 _cell_measurement_theta_max 28.081 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1308 _exptl_absorpt_coefficient_mu 4.439 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2513 _exptl_absorpt_correction_T_max 0.2979 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10593 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0907 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7047 _reflns_number_gt 4501 _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^)+(0.0509P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7047 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1320 _refine_ls_wR_factor_gt 0.1169 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 Cu1 Cu 0.47552(13) 0.77758(11) 0.05309(11) 0.0368(4) Uani 1 1 d . . . Cu2 Cu 1.05591(13) 1.24030(12) -0.06388(10) 0.0361(4) Uani 1 1 d . . . Gd1 Gd 0.31286(4) 0.62441(4) 0.43283(3) 0.01169(14) Uani 1 1 d . . . Gd2 Gd -0.18282(4) 0.62062(4) 0.42592(3) 0.01199(14) Uani 1 1 d . . . N1 N 0.2092(7) 0.8307(6) 0.4694(6) 0.0172(17) Uani 1 1 d . . . N2 N -0.2916(7) 0.8255(6) 0.4654(5) 0.0171(17) Uani 1 1 d . . . N3 N 0.5788(8) 0.8590(7) 0.0281(6) 0.029(2) Uani 1 1 d . . . N4 N 0.9412(7) 1.1706(7) -0.0368(6) 0.028(2) Uani 1 1 d . . . N5 N 0.4070(8) 0.6799(7) 0.0321(6) 0.027(2) Uani 1 1 d . . . N6 N 1.1302(8) 1.3348(7) -0.0449(6) 0.029(2) Uani 1 1 d . . . O1 O 0.1378(6) 0.6778(5) 0.3789(5) 0.0214(15) Uani 1 1 d . . . O2 O 0.1419(5) 0.5345(5) 0.4805(4) 0.0182(14) Uani 1 1 d . . . O3 O -0.0613(5) 0.6765(5) 0.4977(4) 0.0173(14) Uani 1 1 d . . . O4 O 0.0572(6) 0.5442(5) 0.3529(4) 0.0209(15) Uani 1 1 d . . . O5 O 0.3522(5) 0.4682(5) 0.5241(4) 0.0198(15) Uani 1 1 d . . . O6 O 0.3619(6) 0.3261(5) 0.6253(4) 0.0206(15) Uani 1 1 d . . . O7 O 0.4462(6) 0.4587(5) 0.6447(4) 0.0204(15) Uani 1 1 d . . . O8 O 0.5572(5) 0.3260(5) 0.5010(4) 0.0197(14) Uani 1 1 d . . . O9 O 0.3760(6) 0.7178(5) 0.2935(4) 0.0207(15) Uani 1 1 d . . . O10 O 0.3402(7) 0.8680(6) 0.2143(5) 0.0329(18) Uani 1 1 d . . . O11 O 0.1702(6) 0.6990(5) 0.6026(5) 0.0257(16) Uani 1 1 d . . . O12 O 0.0315(9) 0.8396(7) 0.7257(6) 0.064(3) Uani 1 1 d . . . O13 O -0.1324(6) 0.7191(5) 0.2872(5) 0.0217(15) Uani 1 1 d . . . O14 O -0.1882(7) 0.8702(6) 0.2125(5) 0.0358(19) Uani 1 1 d . . . O15 O -0.3233(6) 0.6904(5) 0.5969(4) 0.0220(15) Uani 1 1 d . . . O16 O -0.4713(9) 0.8266(7) 0.7195(6) 0.068(3) Uani 1 1 d . . . O17 O 0.3929(6) 0.4686(5) 0.3043(4) 0.0214(15) Uani 1 1 d . . . H35 H 0.3511 0.4324 0.3372 0.032 Uiso 1 1 d R . . H36 H 0.4690 0.4278 0.2930 0.032 Uiso 1 1 d R . . O18 O -0.0981(6) 0.4637(5) 0.2984(5) 0.0290(16) Uani 1 1 d . . . H37 H -0.1351 0.4200 0.3109 0.044 Uiso 1 1 d R . . H38 H -0.0315 0.4309 0.3085 0.044 Uiso 1 1 d R . . O19 O 0.6328(8) 0.2903(8) 0.2819(6) 0.063(3) Uani 1 1 d . . . H39 H 0.5972 0.2477 0.2814 0.094 Uiso 1 1 d R . . H40 H 0.6322 0.2923 0.3408 0.094 Uiso 1 1 d R . . O20 O 0.1346(9) 0.3010(8) 0.2829(6) 0.079(3) Uani 1 1 d . . . H41 H 0.1244 0.2820 0.3414 0.119 Uiso 1 1 d R . . H42 H 0.1136 0.3706 0.2901 0.119 Uiso 1 1 d R . . S1 S 0.0687(2) 0.60865(18) 0.42599(16) 0.0135(5) Uani 1 1 d . . . S2 S 0.4303(2) 0.39435(18) 0.57499(16) 0.0129(5) Uani 1 1 d . . . C1 C 0.3229(9) 0.8209(8) 0.2917(7) 0.021(2) Uani 1 1 d . . . C2 C 0.2322(9) 0.8915(8) 0.3921(7) 0.020(2) Uani 1 1 d . . . C3 C 0.1771(9) 1.0062(8) 0.4073(8) 0.025(2) Uani 1 1 d . . . H3 H 0.1913 1.0470 0.3536 0.030 Uiso 1 1 calc R . . C4 C 0.0995(10) 1.0586(8) 0.5063(8) 0.033(3) Uani 1 1 d . . . H4 H 0.0635 1.1356 0.5197 0.040 Uiso 1 1 calc R . . C5 C 0.0763(9) 0.9953(8) 0.5845(8) 0.029(2) Uani 1 1 d . . . H5 H 0.0238 1.0296 0.6504 0.035 Uiso 1 1 calc R . . C6 C 0.1322(9) 0.8805(8) 0.5633(8) 0.026(2) Uani 1 1 d . . . C7 C 0.1071(10) 0.8027(9) 0.6370(7) 0.028(2) Uani 1 1 d . . . C8 C -0.1920(9) 0.8228(9) 0.2883(7) 0.024(2) Uani 1 1 d . . . C9 C -0.2725(9) 0.8885(8) 0.3911(7) 0.020(2) Uani 1 1 d . . . C10 C -0.3284(9) 1.0041(8) 0.4118(8) 0.027(2) Uani 1 1 d . . . H10 H -0.3162 1.0473 0.3596 0.032 Uiso 1 1 calc R . . C11 C -0.4028(9) 1.0542(8) 0.5118(9) 0.032(3) Uani 1 1 d . . . H11 H -0.4382 1.1310 0.5270 0.038 Uiso 1 1 calc R . . C12 C -0.4239(9) 0.9885(8) 0.5888(8) 0.027(2) Uani 1 1 d . . . H12 H -0.4740 1.0200 0.6558 0.032 Uiso 1 1 calc R . . C13 C -0.3667(9) 0.8732(8) 0.5613(7) 0.019(2) Uani 1 1 d . . . C14 C -0.3906(9) 0.7928(9) 0.6340(7) 0.028(2) Uani 1 1 d . . . C15 C 0.5585(10) 0.9302(9) 0.1034(7) 0.035(3) Uani 1 1 d . . . H15 H 0.4927 0.9401 0.1656 0.042 Uiso 1 1 calc R . . C16 C 0.6306(10) 0.9893(9) 0.0929(7) 0.031(3) Uani 1 1 d . . . H16 H 0.6127 1.0380 0.1469 0.037 Uiso 1 1 calc R . . C17 C 0.7297(8) 0.9756(8) 0.0016(7) 0.020(2) Uani 1 1 d . . . C18 C 0.7489(10) 0.9042(9) -0.0753(7) 0.033(3) Uani 1 1 d . . . H18A H 0.8126 0.8947 -0.1387 0.039 Uiso 1 1 calc R . . C19 C 0.6750(10) 0.8465(9) -0.0598(8) 0.032(3) Uani 1 1 d . . . H19 H 0.6927 0.7966 -0.1128 0.039 Uiso 1 1 calc R . . C20 C 0.9193(10) 1.1421(9) -0.1126(8) 0.031(3) Uani 1 1 d . . . H20 H 0.9496 1.1668 -0.1744 0.037 Uiso 1 1 calc R . . C21 C 0.8530(9) 1.0770(8) -0.1032(7) 0.028(2) Uani 1 1 d . . . H21 H 0.8427 1.0559 -0.1586 0.034 Uiso 1 1 calc R . . C22 C 0.8033(9) 1.0445(8) -0.0119(7) 0.022(2) Uani 1 1 d . . . C23 C 0.8245(9) 1.0751(8) 0.0673(7) 0.025(2) Uani 1 1 d . . . H23 H 0.7930 1.0525 0.1301 0.030 Uiso 1 1 calc R . . C24 C 0.8921(9) 1.1388(8) 0.0539(7) 0.027(2) Uani 1 1 d . . . H24 H 0.9040 1.1602 0.1083 0.033 Uiso 1 1 calc R . . C25 C 0.3578(11) 0.6264(9) 0.1032(8) 0.037(3) Uani 1 1 d . . . H25 H 0.3628 0.6335 0.1648 0.045 Uiso 1 1 calc R . . C26 C 0.3005(11) 0.5620(9) 0.0936(8) 0.038(3) Uani 1 1 d . . . H26 H 0.2643 0.5300 0.1484 0.046 Uiso 1 1 calc R . . C27 C 0.2964(9) 0.5443(8) 0.0024(7) 0.026(2) Uani 1 1 d . . . C28 C 0.3458(10) 0.6000(9) -0.0737(7) 0.032(3) Uani 1 1 d . . . H28 H 0.3417 0.5938 -0.1359 0.039 Uiso 1 1 calc R . . C29 C 0.4004(10) 0.6639(9) -0.0569(8) 0.032(3) Uani 1 1 d . . . H29 H 0.4353 0.6987 -0.1098 0.038 Uiso 1 1 calc R . . C30 C 1.0878(10) 1.3924(10) 0.0459(8) 0.036(3) Uani 1 1 d . . . H30 H 1.0209 1.3858 0.0990 0.043 Uiso 1 1 calc R . . C31 C 1.1377(10) 1.4598(9) 0.0640(7) 0.033(3) Uani 1 1 d . . . H31 H 1.1053 1.4982 0.1280 0.039 Uiso 1 1 calc R . . C32 C 1.2392(9) 1.4705(8) -0.0156(7) 0.026(2) Uani 1 1 d . . . C33 C 1.2816(10) 1.4132(9) -0.1086(7) 0.032(3) Uani 1 1 d . . . H33 H 1.3468 1.4197 -0.1637 0.038 Uiso 1 1 calc R . . C34 C 1.2260(10) 1.3461(9) -0.1192(8) 0.033(3) Uani 1 1 d . . . H34 H 1.2572 1.3061 -0.1823 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0359(9) 0.0352(8) 0.0481(9) 0.0060(7) -0.0189(8) -0.0214(7) Cu2 0.0348(8) 0.0402(9) 0.0419(9) 0.0073(7) -0.0146(7) -0.0248(7) Gd1 0.0060(2) 0.0124(3) 0.0110(3) 0.00064(19) -0.0003(2) -0.0013(2) Gd2 0.0060(2) 0.0129(3) 0.0112(3) -0.00008(19) -0.0004(2) -0.0010(2) N1 0.010(4) 0.012(4) 0.025(5) -0.006(4) -0.003(4) -0.002(4) N2 0.011(4) 0.019(4) 0.013(4) 0.001(4) 0.000(3) -0.004(4) N3 0.031(5) 0.037(5) 0.021(5) 0.001(4) -0.004(4) -0.022(5) N4 0.018(5) 0.028(5) 0.039(6) 0.004(4) -0.011(4) -0.010(4) N5 0.020(5) 0.023(5) 0.034(5) 0.001(4) -0.005(4) -0.009(4) N6 0.029(5) 0.033(5) 0.032(5) 0.006(4) -0.012(5) -0.019(5) O1 0.016(4) 0.024(4) 0.028(4) 0.010(3) -0.008(3) -0.013(3) O2 0.011(3) 0.013(3) 0.026(4) 0.007(3) -0.010(3) 0.002(3) O3 0.007(3) 0.016(3) 0.018(3) -0.003(3) 0.000(3) 0.001(3) O4 0.012(3) 0.029(4) 0.017(4) -0.004(3) -0.003(3) -0.006(3) O5 0.008(3) 0.020(4) 0.024(4) 0.005(3) -0.005(3) -0.001(3) O6 0.013(3) 0.023(4) 0.024(4) 0.006(3) -0.005(3) -0.008(3) O7 0.015(4) 0.024(4) 0.022(4) 0.001(3) -0.009(3) -0.006(3) O8 0.006(3) 0.018(4) 0.025(4) -0.002(3) -0.001(3) 0.001(3) O9 0.015(4) 0.019(4) 0.018(4) 0.002(3) -0.002(3) -0.003(3) O10 0.039(5) 0.039(5) 0.025(4) 0.021(4) -0.010(4) -0.024(4) O11 0.025(4) 0.025(4) 0.017(4) -0.004(3) 0.005(3) -0.013(3) O12 0.063(7) 0.042(5) 0.030(5) -0.014(4) 0.020(5) -0.003(5) O13 0.009(3) 0.021(4) 0.023(4) 0.001(3) 0.001(3) -0.002(3) O14 0.047(5) 0.035(5) 0.023(4) 0.016(4) -0.008(4) -0.021(4) O15 0.018(4) 0.018(4) 0.012(3) -0.007(3) 0.009(3) -0.004(3) O16 0.085(7) 0.034(5) 0.026(5) -0.007(4) 0.021(5) -0.008(5) O17 0.013(3) 0.024(4) 0.013(3) -0.007(3) 0.008(3) -0.006(3) O18 0.019(4) 0.034(4) 0.026(4) -0.004(3) -0.002(3) -0.009(3) O19 0.059(6) 0.086(7) 0.033(5) -0.002(5) -0.006(5) -0.030(6) O20 0.069(7) 0.072(7) 0.042(6) -0.015(5) -0.009(5) 0.014(6) S1 0.0051(11) 0.0141(13) 0.0166(12) 0.0014(10) -0.0022(10) -0.0014(10) S2 0.0057(11) 0.0161(13) 0.0137(11) 0.0030(10) -0.0028(10) -0.0026(10) C1 0.017(5) 0.025(6) 0.027(6) 0.006(5) -0.009(5) -0.015(5) C2 0.014(5) 0.021(6) 0.023(5) 0.001(5) -0.005(5) -0.009(5) C3 0.013(5) 0.014(5) 0.041(7) 0.003(5) -0.010(5) 0.000(4) C4 0.025(6) 0.013(6) 0.058(8) -0.008(5) -0.020(6) -0.001(5) C5 0.014(5) 0.025(6) 0.039(7) -0.016(5) -0.008(5) 0.000(5) C6 0.012(5) 0.025(6) 0.033(6) -0.012(5) -0.006(5) 0.000(5) C7 0.023(6) 0.027(6) 0.022(6) -0.005(5) 0.001(5) -0.008(5) C8 0.021(6) 0.028(6) 0.023(6) 0.010(5) -0.004(5) -0.016(5) C9 0.016(5) 0.022(6) 0.030(6) 0.011(5) -0.013(5) -0.012(5) C10 0.021(6) 0.022(6) 0.041(7) 0.010(5) -0.016(5) -0.010(5) C11 0.010(5) 0.013(5) 0.071(9) 0.000(6) -0.021(6) 0.000(5) C12 0.018(6) 0.017(6) 0.036(6) -0.017(5) -0.008(5) 0.000(5) C13 0.015(5) 0.015(5) 0.028(6) 0.002(4) -0.014(5) 0.000(4) C14 0.016(6) 0.035(7) 0.016(5) -0.006(5) 0.003(5) -0.004(5) C15 0.035(7) 0.051(8) 0.017(6) -0.006(5) 0.000(5) -0.026(6) C16 0.030(6) 0.040(7) 0.022(6) -0.010(5) -0.002(5) -0.020(6) C17 0.008(5) 0.029(6) 0.023(5) 0.005(5) -0.006(4) -0.008(4) C18 0.027(6) 0.042(7) 0.019(6) -0.009(5) 0.006(5) -0.018(6) C19 0.030(7) 0.039(7) 0.028(6) -0.009(5) -0.006(5) -0.017(6) C20 0.028(6) 0.037(7) 0.028(6) 0.006(5) -0.007(5) -0.018(6) C21 0.019(6) 0.034(6) 0.029(6) 0.002(5) -0.006(5) -0.012(5) C22 0.019(5) 0.019(6) 0.019(5) 0.000(4) -0.002(5) -0.005(5) C23 0.022(6) 0.028(6) 0.023(6) 0.000(5) -0.005(5) -0.013(5) C24 0.015(5) 0.036(7) 0.023(6) -0.006(5) -0.002(5) -0.008(5) C25 0.062(9) 0.042(7) 0.029(6) 0.011(6) -0.024(6) -0.037(7) C26 0.065(9) 0.042(7) 0.031(6) 0.016(6) -0.024(6) -0.042(7) C27 0.023(6) 0.031(6) 0.023(6) -0.002(5) -0.004(5) -0.014(5) C28 0.039(7) 0.041(7) 0.018(6) -0.003(5) -0.003(5) -0.025(6) C29 0.024(6) 0.039(7) 0.028(6) -0.001(5) 0.001(5) -0.018(6) C30 0.037(7) 0.058(8) 0.023(6) 0.001(6) -0.001(5) -0.039(7) C31 0.031(6) 0.049(8) 0.019(6) -0.003(5) -0.002(5) -0.024(6) C32 0.024(6) 0.029(6) 0.023(6) 0.001(5) -0.006(5) -0.013(5) C33 0.034(7) 0.045(7) 0.020(6) 0.008(5) -0.007(5) -0.024(6) C34 0.029(6) 0.041(7) 0.024(6) -0.005(5) -0.001(5) -0.018(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 Cu1 N5 1.905(7) . ? Cu1 N3 1.925(7) . ? Cu1 O10 2.309(7) . ? Cu2 N6 1.915(7) . ? Cu2 N4 1.922(7) . ? Cu2 O14 2.260(8) 2_675 ? Gd1 O9 2.359(6) . ? Gd1 O11 2.374(6) . ? Gd1 O5 2.398(6) . ? Gd1 O17 2.437(6) . ? Gd1 O1 2.466(6) . ? Gd1 O8 2.482(6) 2_666 ? Gd1 N1 2.493(7) . ? Gd1 O7 2.566(6) 2_666 ? Gd1 O2 2.714(5) . ? Gd1 S2 3.117(2) 2_666 ? Gd2 O13 2.365(6) . ? Gd2 O15 2.372(6) . ? Gd2 O2 2.410(5) 2_566 ? Gd2 O18 2.426(6) . ? Gd2 N2 2.480(7) . ? Gd2 O3 2.484(5) . ? Gd2 O6 2.487(6) 2_566 ? Gd2 O4 2.560(6) . ? Gd2 O5 2.685(5) 2_566 ? Gd2 S2 3.218(2) 2_566 ? N1 C6 1.331(11) . ? N1 C2 1.358(11) . ? N2 C9 1.341(10) . ? N2 C13 1.345(11) . ? N3 C19 1.338(12) . ? N3 C15 1.348(12) . ? N4 C20 1.331(12) . ? N4 C24 1.348(11) . ? N5 C25 1.319(12) . ? N5 C29 1.352(12) . ? N6 C34 1.331(12) . ? N6 C30 1.344(12) . ? O1 S1 1.477(5) . ? O2 S1 1.495(6) . ? O2 Gd2 2.410(5) 2_566 ? O3 S1 1.478(6) . ? O4 S1 1.467(6) . ? O5 S2 1.491(6) . ? O5 Gd2 2.685(5) 2_566 ? O6 S2 1.473(5) . ? O6 Gd2 2.487(6) 2_566 ? O7 S2 1.463(6) . ? O7 Gd1 2.566(6) 2_666 ? O8 S2 1.467(6) . ? O8 Gd1 2.482(6) 2_666 ? O9 C1 1.267(11) . ? O10 C1 1.248(10) . ? O11 C7 1.286(12) . ? O12 C7 1.240(12) . ? O13 C8 1.277(11) . ? O14 C8 1.236(10) . ? O14 Cu2 2.260(8) 2_675 ? O15 C14 1.283(12) . ? O16 C14 1.217(12) . ? O17 H35 0.8500 . ? O17 H36 0.8500 . ? O18 H37 0.8500 . ? O18 H38 0.8500 . ? O19 H39 0.8500 . ? O19 H40 0.8500 . ? O20 H41 0.8501 . ? O20 H42 0.8501 . ? S2 Gd1 3.117(2) 2_666 ? S2 Gd2 3.218(2) 2_566 ? C1 C2 1.509(13) . ? C2 C3 1.384(12) . ? C3 C4 1.397(14) . ? C3 H3 0.9300 . ? C4 C5 1.390(14) . ? C4 H4 0.9300 . ? C5 C6 1.388(13) . ? C5 H5 0.9300 . ? C6 C7 1.487(13) . ? C8 C9 1.498(13) . ? C9 C10 1.397(13) . ? C10 C11 1.398(14) . ? C10 H10 0.9300 . ? C11 C12 1.394(13) . ? C11 H11 0.9300 . ? C12 C13 1.402(12) . ? C12 H12 0.9300 . ? C13 C14 1.500(13) . ? C15 C16 1.381(12) . ? C15 H15 0.9300 . ? C16 C17 1.383(12) . ? C16 H16 0.9300 . ? C17 C18 1.372(12) . ? C17 C22 1.500(12) . ? C18 C19 1.374(12) . ? C18 H18A 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.389(12) . ? C20 H20 0.9300 . ? C21 C22 1.362(12) . ? C21 H21 0.9300 . ? C22 C23 1.381(12) . ? C23 C24 1.380(11) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.357(12) . ? C25 H25 0.9300 . ? C26 C27 1.374(13) . ? C26 H26 0.9300 . ? C27 C28 1.383(12) . ? C27 C32 1.503(13) 1_445 ? C28 C29 1.362(12) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.359(12) . ? C30 H30 0.9300 . ? C31 C32 1.409(12) . ? C31 H31 0.9300 . ? C32 C33 1.370(13) . ? C32 C27 1.503(13) 1_665 ? C33 C34 1.375(12) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Cu1 N3 161.1(4) . . ? N5 Cu1 O10 103.4(3) . . ? N3 Cu1 O10 95.3(3) . . ? N6 Cu2 N4 160.2(4) . . ? N6 Cu2 O14 107.3(3) . 2_675 ? N4 Cu2 O14 92.5(3) . 2_675 ? O9 Gd1 O11 129.2(2) . . ? O9 Gd1 O5 151.6(2) . . ? O11 Gd1 O5 76.1(2) . . ? O9 Gd1 O17 84.3(2) . . ? O11 Gd1 O17 142.52(19) . . ? O5 Gd1 O17 77.3(2) . . ? O9 Gd1 O1 77.91(19) . . ? O11 Gd1 O1 91.0(2) . . ? O5 Gd1 O1 118.74(18) . . ? O17 Gd1 O1 79.2(2) . . ? O9 Gd1 O8 88.02(19) . 2_666 ? O11 Gd1 O8 78.3(2) . 2_666 ? O5 Gd1 O8 85.12(19) . 2_666 ? O17 Gd1 O8 125.0(2) . 2_666 ? O1 Gd1 O8 150.9(2) . 2_666 ? O9 Gd1 N1 65.2(2) . . ? O11 Gd1 N1 64.1(2) . . ? O5 Gd1 N1 138.3(2) . . ? O17 Gd1 N1 143.5(2) . . ? O1 Gd1 N1 75.3(2) . . ? O8 Gd1 N1 75.7(2) 2_666 . ? O9 Gd1 O7 72.8(2) . 2_666 ? O11 Gd1 O7 129.3(2) . 2_666 ? O5 Gd1 O7 80.70(19) . 2_666 ? O17 Gd1 O7 70.56(19) . 2_666 ? O1 Gd1 O7 139.45(19) . 2_666 ? O8 Gd1 O7 55.20(19) 2_666 2_666 ? N1 Gd1 O7 115.1(2) . 2_666 ? O9 Gd1 O2 128.48(19) . . ? O11 Gd1 O2 73.65(19) . . ? O5 Gd1 O2 65.26(17) . . ? O17 Gd1 O2 71.44(19) . . ? O1 Gd1 O2 53.72(17) . . ? O8 Gd1 O2 143.06(18) 2_666 . ? N1 Gd1 O2 111.6(2) . . ? O7 Gd1 O2 133.29(18) 2_666 . ? O9 Gd1 S2 78.54(15) . 2_666 ? O11 Gd1 S2 104.27(16) . 2_666 ? O5 Gd1 S2 82.83(14) . 2_666 ? O17 Gd1 S2 98.04(15) . 2_666 ? O1 Gd1 S2 156.44(13) . 2_666 ? O8 Gd1 S2 27.50(14) 2_666 2_666 ? N1 Gd1 S2 95.12(16) . 2_666 ? O7 Gd1 S2 27.72(13) 2_666 2_666 ? O2 Gd1 S2 147.73(12) . 2_666 ? O13 Gd2 O15 129.1(2) . . ? O13 Gd2 O2 154.7(2) . 2_566 ? O15 Gd2 O2 74.0(2) . 2_566 ? O13 Gd2 O18 85.0(2) . . ? O15 Gd2 O18 141.9(2) . . ? O2 Gd2 O18 77.6(2) 2_566 . ? O13 Gd2 N2 64.7(2) . . ? O15 Gd2 N2 64.4(2) . . ? O2 Gd2 N2 136.7(2) 2_566 . ? O18 Gd2 N2 144.8(2) . . ? O13 Gd2 O3 91.14(19) . . ? O15 Gd2 O3 76.0(2) . . ? O2 Gd2 O3 84.52(18) 2_566 . ? O18 Gd2 O3 126.0(2) . . ? N2 Gd2 O3 74.7(2) . . ? O13 Gd2 O6 75.58(19) . 2_566 ? O15 Gd2 O6 90.8(2) . 2_566 ? O2 Gd2 O6 118.92(18) 2_566 2_566 ? O18 Gd2 O6 81.1(2) . 2_566 ? N2 Gd2 O6 74.5(2) . 2_566 ? O3 Gd2 O6 149.2(2) . 2_566 ? O13 Gd2 O4 76.1(2) . . ? O15 Gd2 O4 126.9(2) . . ? O2 Gd2 O4 80.92(19) 2_566 . ? O18 Gd2 O4 71.6(2) . . ? N2 Gd2 O4 114.7(2) . . ? O3 Gd2 O4 55.40(19) . . ? O6 Gd2 O4 141.96(19) 2_566 . ? O13 Gd2 O5 126.44(19) . 2_566 ? O15 Gd2 O5 72.37(19) . 2_566 ? O2 Gd2 O5 65.60(18) 2_566 2_566 ? O18 Gd2 O5 73.0(2) . 2_566 ? N2 Gd2 O5 109.9(2) . 2_566 ? O3 Gd2 O5 141.15(18) . 2_566 ? O6 Gd2 O5 53.48(17) 2_566 2_566 ? O4 Gd2 O5 135.35(19) . 2_566 ? O13 Gd2 S2 100.89(15) . 2_566 ? O15 Gd2 S2 79.78(15) . 2_566 ? O2 Gd2 S2 92.99(13) 2_566 2_566 ? O18 Gd2 S2 76.80(15) . 2_566 ? N2 Gd2 S2 91.03(16) . 2_566 ? O3 Gd2 S2 155.40(14) . 2_566 ? O6 Gd2 S2 26.13(13) 2_566 2_566 ? O4 Gd2 S2 148.37(14) . 2_566 ? O5 Gd2 S2 27.40(12) 2_566 2_566 ? C6 N1 C2 120.5(8) . . ? C6 N1 Gd1 120.5(6) . . ? C2 N1 Gd1 119.0(6) . . ? C9 N2 C13 120.1(8) . . ? C9 N2 Gd2 119.7(6) . . ? C13 N2 Gd2 120.1(5) . . ? C19 N3 C15 116.4(8) . . ? C19 N3 Cu1 124.0(7) . . ? C15 N3 Cu1 119.5(7) . . ? C20 N4 C24 118.4(8) . . ? C20 N4 Cu2 118.9(7) . . ? C24 N4 Cu2 122.3(7) . . ? C25 N5 C29 114.8(8) . . ? C25 N5 Cu1 123.3(7) . . ? C29 N5 Cu1 121.8(6) . . ? C34 N6 C30 116.8(8) . . ? C34 N6 Cu2 122.4(7) . . ? C30 N6 Cu2 120.8(6) . . ? S1 O1 Gd1 106.5(3) . . ? S1 O2 Gd2 150.8(3) . 2_566 ? S1 O2 Gd1 95.2(3) . . ? Gd2 O2 Gd1 113.8(2) 2_566 . ? S1 O3 Gd2 101.0(3) . . ? S1 O4 Gd2 98.0(3) . . ? S2 O5 Gd1 147.9(3) . . ? S2 O5 Gd2 96.6(3) . 2_566 ? Gd1 O5 Gd2 115.3(2) . 2_566 ? S2 O6 Gd2 105.9(3) . 2_566 ? S2 O7 Gd1 97.6(3) . 2_666 ? S2 O8 Gd1 101.1(3) . 2_666 ? C1 O9 Gd1 124.9(6) . . ? C1 O10 Cu1 124.2(7) . . ? C7 O11 Gd1 125.7(6) . . ? C8 O13 Gd2 124.6(6) . . ? C8 O14 Cu2 114.7(7) . 2_675 ? C14 O15 Gd2 126.4(6) . . ? Gd1 O17 H35 100.1 . . ? Gd1 O17 H36 109.6 . . ? H35 O17 H36 105.6 . . ? Gd2 O18 H37 117.0 . . ? Gd2 O18 H38 94.1 . . ? H37 O18 H38 106.3 . . ? H39 O19 H40 105.0 . . ? H41 O20 H42 105.4 . . ? O4 S1 O1 113.4(4) . . ? O4 S1 O3 105.6(3) . . ? O1 S1 O3 111.8(4) . . ? O4 S1 O2 111.2(4) . . ? O1 S1 O2 104.6(3) . . ? O3 S1 O2 110.3(3) . . ? O7 S2 O8 106.0(4) . . ? O7 S2 O6 113.5(4) . . ? O8 S2 O6 111.5(4) . . ? O7 S2 O5 111.3(4) . . ? O8 S2 O5 110.8(3) . . ? O6 S2 O5 103.8(3) . . ? O7 S2 Gd1 54.7(2) . 2_666 ? O8 S2 Gd1 51.4(2) . 2_666 ? O6 S2 Gd1 127.4(3) . 2_666 ? O5 S2 Gd1 128.7(2) . 2_666 ? O7 S2 Gd2 131.2(3) . 2_566 ? O8 S2 Gd2 122.7(3) . 2_566 ? O6 S2 Gd2 48.0(2) . 2_566 ? O5 S2 Gd2 56.0(2) . 2_566 ? Gd1 S2 Gd2 172.53(8) 2_666 2_566 ? O10 C1 O9 125.3(10) . . ? O10 C1 C2 118.1(9) . . ? O9 C1 C2 116.6(8) . . ? N1 C2 C3 121.8(9) . . ? N1 C2 C1 113.0(8) . . ? C3 C2 C1 125.1(8) . . ? C2 C3 C4 117.7(9) . . ? C2 C3 H3 121.2 . . ? C4 C3 H3 121.2 . . ? C5 C4 C3 119.8(9) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C6 C5 C4 119.4(10) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? N1 C6 C5 120.8(9) . . ? N1 C6 C7 113.8(8) . . ? C5 C6 C7 125.3(10) . . ? O12 C7 O11 124.5(9) . . ? O12 C7 C6 119.8(9) . . ? O11 C7 C6 115.7(9) . . ? O14 C8 O13 125.2(10) . . ? O14 C8 C9 119.5(9) . . ? O13 C8 C9 115.3(8) . . ? N2 C9 C10 120.9(9) . . ? N2 C9 C8 113.4(8) . . ? C10 C9 C8 125.6(8) . . ? C9 C10 C11 119.2(9) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 119.8(9) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 117.4(9) . . ? C11 C12 H12 121.3 . . ? C13 C12 H12 121.3 . . ? N2 C13 C12 122.5(8) . . ? N2 C13 C14 114.0(8) . . ? C12 C13 C14 123.4(9) . . ? O16 C14 O15 125.3(9) . . ? O16 C14 C13 120.1(10) . . ? O15 C14 C13 114.5(8) . . ? N3 C15 C16 123.2(9) . . ? N3 C15 H15 118.4 . . ? C16 C15 H15 118.4 . . ? C15 C16 C17 119.6(9) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 117.0(9) . . ? C18 C17 C22 123.2(9) . . ? C16 C17 C22 119.7(9) . . ? C17 C18 C19 120.7(9) . . ? C17 C18 H18A 119.7 . . ? C19 C18 H18A 119.7 . . ? N3 C19 C18 123.0(9) . . ? N3 C19 H19 118.5 . . ? C18 C19 H19 118.5 . . ? N4 C20 C21 122.6(9) . . ? N4 C20 H20 118.7 . . ? C21 C20 H20 118.7 . . ? C22 C21 C20 119.2(9) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 118.2(9) . . ? C21 C22 C17 120.8(9) . . ? C23 C22 C17 121.0(8) . . ? C24 C23 C22 120.3(9) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? N4 C24 C23 121.1(9) . . ? N4 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? N5 C25 C26 125.3(10) . . ? N5 C25 H25 117.3 . . ? C26 C25 H25 117.3 . . ? C25 C26 C27 119.6(9) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C26 C27 C28 116.7(8) . . ? C26 C27 C32 122.9(8) . 1_445 ? C28 C27 C32 120.4(9) . 1_445 ? C29 C28 C27 119.6(9) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? N5 C29 C28 124.0(9) . . ? N5 C29 H29 118.0 . . ? C28 C29 H29 118.0 . . ? N6 C30 C31 123.3(9) . . ? N6 C30 H30 118.3 . . ? C31 C30 H30 118.3 . . ? C30 C31 C32 119.0(10) . . ? C30 C31 H31 120.5 . . ? C32 C31 H31 120.5 . . ? C33 C32 C31 117.9(9) . . ? C33 C32 C27 122.0(9) . 1_665 ? C31 C32 C27 120.1(9) . 1_665 ? C32 C33 C34 118.8(9) . . ? C32 C33 H33 120.6 . . ? C34 C33 H33 120.6 . . ? N6 C34 C33 124.1(10) . . ? N6 C34 H34 117.9 . . ? C33 C34 H34 117.9 . . ? 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 O9 Gd1 N1 C6 -175.0(7) . . . . ? O11 Gd1 N1 C6 3.2(6) . . . . ? O5 Gd1 N1 C6 -15.2(8) . . . . ? O17 Gd1 N1 C6 149.0(6) . . . . ? O1 Gd1 N1 C6 101.7(6) . . . . ? O8 Gd1 N1 C6 -80.5(6) 2_666 . . . ? O7 Gd1 N1 C6 -120.2(6) 2_666 . . . ? O2 Gd1 N1 C6 61.3(7) . . . . ? S2 Gd1 N1 C6 -100.2(6) 2_666 . . . ? O9 Gd1 N1 C2 5.1(6) . . . . ? O11 Gd1 N1 C2 -176.7(7) . . . . ? O5 Gd1 N1 C2 164.9(5) . . . . ? O17 Gd1 N1 C2 -30.9(8) . . . . ? O1 Gd1 N1 C2 -78.2(6) . . . . ? O8 Gd1 N1 C2 99.6(6) 2_666 . . . ? O7 Gd1 N1 C2 59.9(6) 2_666 . . . ? O2 Gd1 N1 C2 -118.6(6) . . . . ? S2 Gd1 N1 C2 79.9(6) 2_666 . . . ? O13 Gd2 N2 C9 2.3(6) . . . . ? O15 Gd2 N2 C9 -177.4(7) . . . . ? O2 Gd2 N2 C9 165.3(5) 2_566 . . . ? O18 Gd2 N2 C9 -31.0(8) . . . . ? O3 Gd2 N2 C9 101.1(6) . . . . ? O6 Gd2 N2 C9 -78.8(6) 2_566 . . . ? O4 Gd2 N2 C9 61.7(6) . . . . ? O5 Gd2 N2 C9 -119.5(6) 2_566 . . . ? S2 Gd2 N2 C9 -99.2(6) 2_566 . . . ? O13 Gd2 N2 C13 -175.9(7) . . . . ? O15 Gd2 N2 C13 4.4(6) . . . . ? O2 Gd2 N2 C13 -12.9(7) 2_566 . . . ? O18 Gd2 N2 C13 150.8(5) . . . . ? O3 Gd2 N2 C13 -77.1(6) . . . . ? O6 Gd2 N2 C13 103.0(6) 2_566 . . . ? O4 Gd2 N2 C13 -116.4(6) . . . . ? O5 Gd2 N2 C13 62.3(6) 2_566 . . . ? S2 Gd2 N2 C13 82.6(6) 2_566 . . . ? N5 Cu1 N3 C19 -4.7(17) . . . . ? O10 Cu1 N3 C19 -176.6(9) . . . . ? N5 Cu1 N3 C15 178.2(10) . . . . ? O10 Cu1 N3 C15 6.3(8) . . . . ? N6 Cu2 N4 C20 146.4(10) . . . . ? O14 Cu2 N4 C20 -39.3(8) 2_675 . . . ? N6 Cu2 N4 C24 -40.7(15) . . . . ? O14 Cu2 N4 C24 133.6(8) 2_675 . . . ? N3 Cu1 N5 C25 149.7(11) . . . . ? O10 Cu1 N5 C25 -38.6(10) . . . . ? N3 Cu1 N5 C29 -33.2(16) . . . . ? O10 Cu1 N5 C29 138.5(8) . . . . ? N4 Cu2 N6 C34 -172.0(9) . . . . ? O14 Cu2 N6 C34 14.0(9) 2_675 . . . ? N4 Cu2 N6 C30 8.7(16) . . . . ? O14 Cu2 N6 C30 -165.4(8) 2_675 . . . ? O9 Gd1 O1 S1 163.0(4) . . . . ? O11 Gd1 O1 S1 -67.0(4) . . . . ? O5 Gd1 O1 S1 7.6(4) . . . . ? O17 Gd1 O1 S1 76.6(3) . . . . ? O8 Gd1 O1 S1 -134.3(4) 2_666 . . . ? N1 Gd1 O1 S1 -129.8(4) . . . . ? O7 Gd1 O1 S1 118.6(3) 2_666 . . . ? O2 Gd1 O1 S1 1.8(3) . . . . ? S2 Gd1 O1 S1 161.99(17) 2_666 . . . ? O9 Gd1 O2 S1 -25.5(4) . . . . ? O11 Gd1 O2 S1 102.0(3) . . . . ? O5 Gd1 O2 S1 -176.1(4) . . . . ? O17 Gd1 O2 S1 -91.8(3) . . . . ? O1 Gd1 O2 S1 -1.7(3) . . . . ? O8 Gd1 O2 S1 144.2(3) 2_666 . . . ? N1 Gd1 O2 S1 49.3(3) . . . . ? O7 Gd1 O2 S1 -128.8(3) 2_666 . . . ? S2 Gd1 O2 S1 -167.01(13) 2_666 . . . ? O9 Gd1 O2 Gd2 151.4(2) . . . 2_566 ? O11 Gd1 O2 Gd2 -81.1(3) . . . 2_566 ? O5 Gd1 O2 Gd2 0.8(2) . . . 2_566 ? O17 Gd1 O2 Gd2 85.1(3) . . . 2_566 ? O1 Gd1 O2 Gd2 175.2(4) . . . 2_566 ? O8 Gd1 O2 Gd2 -39.0(4) 2_666 . . 2_566 ? N1 Gd1 O2 Gd2 -133.8(3) . . . 2_566 ? O7 Gd1 O2 Gd2 48.1(4) 2_666 . . 2_566 ? S2 Gd1 O2 Gd2 9.9(4) 2_666 . . 2_566 ? O13 Gd2 O3 S1 -71.6(3) . . . . ? O15 Gd2 O3 S1 158.2(3) . . . . ? O2 Gd2 O3 S1 83.4(3) 2_566 . . . ? O18 Gd2 O3 S1 13.1(4) . . . . ? N2 Gd2 O3 S1 -135.0(3) . . . . ? O6 Gd2 O3 S1 -134.7(3) 2_566 . . . ? O4 Gd2 O3 S1 0.6(2) . . . . ? O5 Gd2 O3 S1 122.1(3) 2_566 . . . ? S2 Gd2 O3 S1 168.56(14) 2_566 . . . ? O13 Gd2 O4 S1 100.6(3) . . . . ? O15 Gd2 O4 S1 -28.2(4) . . . . ? O2 Gd2 O4 S1 -90.2(3) 2_566 . . . ? O18 Gd2 O4 S1 -170.0(3) . . . . ? N2 Gd2 O4 S1 47.3(3) . . . . ? O3 Gd2 O4 S1 -0.6(2) . . . . ? O6 Gd2 O4 S1 143.6(3) 2_566 . . . ? O5 Gd2 O4 S1 -131.0(3) 2_566 . . . ? S2 Gd2 O4 S1 -171.07(12) 2_566 . . . ? O9 Gd1 O5 S2 58.7(9) . . . . ? O11 Gd1 O5 S2 -97.1(7) . . . . ? O17 Gd1 O5 S2 109.5(7) . . . . ? O1 Gd1 O5 S2 179.5(6) . . . . ? O8 Gd1 O5 S2 -18.0(7) 2_666 . . . ? N1 Gd1 O5 S2 -80.1(8) . . . . ? O7 Gd1 O5 S2 37.5(7) 2_666 . . . ? O2 Gd1 O5 S2 -175.3(8) . . . . ? S2 Gd1 O5 S2 9.6(7) 2_666 . . . ? O9 Gd1 O5 Gd2 -126.8(4) . . . 2_566 ? O11 Gd1 O5 Gd2 77.4(3) . . . 2_566 ? O17 Gd1 O5 Gd2 -75.9(3) . . . 2_566 ? O1 Gd1 O5 Gd2 -5.9(3) . . . 2_566 ? O8 Gd1 O5 Gd2 156.6(3) 2_666 . . 2_566 ? N1 Gd1 O5 Gd2 94.5(3) . . . 2_566 ? O7 Gd1 O5 Gd2 -147.9(3) 2_666 . . 2_566 ? O2 Gd1 O5 Gd2 -0.7(2) . . . 2_566 ? S2 Gd1 O5 Gd2 -175.9(2) 2_666 . . 2_566 ? O11 Gd1 O9 C1 -12.5(8) . . . . ? O5 Gd1 O9 C1 -161.6(6) . . . . ? O17 Gd1 O9 C1 148.9(7) . . . . ? O1 Gd1 O9 C1 68.7(7) . . . . ? O8 Gd1 O9 C1 -85.7(7) 2_666 . . . ? N1 Gd1 O9 C1 -10.5(6) . . . . ? O7 Gd1 O9 C1 -139.7(7) 2_666 . . . ? O2 Gd1 O9 C1 88.1(7) . . . . ? S2 Gd1 O9 C1 -111.7(7) 2_666 . . . ? N5 Cu1 O10 C1 62.3(7) . . . . ? N3 Cu1 O10 C1 -120.3(7) . . . . ? O9 Gd1 O11 C7 2.1(8) . . . . ? O5 Gd1 O11 C7 167.5(8) . . . . ? O17 Gd1 O11 C7 -146.5(7) . . . . ? O1 Gd1 O11 C7 -73.0(8) . . . . ? O8 Gd1 O11 C7 79.7(7) 2_666 . . . ? N1 Gd1 O11 C7 0.1(7) . . . . ? O7 Gd1 O11 C7 102.3(8) 2_666 . . . ? O2 Gd1 O11 C7 -124.6(8) . . . . ? S2 Gd1 O11 C7 88.8(7) 2_666 . . . ? O15 Gd2 O13 C8 -11.1(8) . . . . ? O2 Gd2 O13 C8 -163.5(6) 2_566 . . . ? O18 Gd2 O13 C8 150.0(7) . . . . ? N2 Gd2 O13 C8 -11.5(7) . . . . ? O3 Gd2 O13 C8 -83.9(7) . . . . ? O6 Gd2 O13 C8 67.9(7) 2_566 . . . ? O4 Gd2 O13 C8 -137.8(7) . . . . ? O5 Gd2 O13 C8 85.4(7) 2_566 . . . ? S2 Gd2 O13 C8 74.5(7) 2_566 . . . ? O13 Gd2 O15 C14 0.7(8) . . . . ? O2 Gd2 O15 C14 168.8(8) 2_566 . . . ? O18 Gd2 O15 C14 -147.8(7) . . . . ? N2 Gd2 O15 C14 1.0(7) . . . . ? O3 Gd2 O15 C14 80.6(7) . . . . ? O6 Gd2 O15 C14 -71.3(7) 2_566 . . . ? O4 Gd2 O15 C14 103.7(7) . . . . ? O5 Gd2 O15 C14 -122.3(8) 2_566 . . . ? S2 Gd2 O15 C14 -95.1(7) 2_566 . . . ? Gd2 O4 S1 O1 -121.9(3) . . . . ? Gd2 O4 S1 O3 0.9(3) . . . . ? Gd2 O4 S1 O2 120.6(3) . . . . ? Gd1 O1 S1 O4 -124.1(3) . . . . ? Gd1 O1 S1 O3 116.6(3) . . . . ? Gd1 O1 S1 O2 -2.7(4) . . . . ? Gd2 O3 S1 O4 -0.9(4) . . . . ? Gd2 O3 S1 O1 122.9(3) . . . . ? Gd2 O3 S1 O2 -121.2(3) . . . . ? Gd2 O2 S1 O4 -49.0(9) 2_566 . . . ? Gd1 O2 S1 O4 125.2(3) . . . . ? Gd2 O2 S1 O1 -171.8(7) 2_566 . . . ? Gd1 O2 S1 O1 2.4(4) . . . . ? Gd2 O2 S1 O3 67.9(8) 2_566 . . . ? Gd1 O2 S1 O3 -118.0(3) . . . . ? Gd1 O7 S2 O8 -2.5(3) 2_666 . . . ? Gd1 O7 S2 O6 120.2(3) 2_666 . . . ? Gd1 O7 S2 O5 -123.1(3) 2_666 . . . ? Gd1 O7 S2 Gd2 174.11(12) 2_666 . . 2_566 ? Gd1 O8 S2 O7 2.7(4) 2_666 . . . ? Gd1 O8 S2 O6 -121.3(3) 2_666 . . . ? Gd1 O8 S2 O5 123.5(3) 2_666 . . . ? Gd1 O8 S2 Gd2 -174.35(9) 2_666 . . 2_566 ? Gd2 O6 S2 O7 125.1(3) 2_566 . . . ? Gd2 O6 S2 O8 -115.2(3) 2_566 . . . ? Gd2 O6 S2 O5 4.1(4) 2_566 . . . ? Gd2 O6 S2 Gd1 -172.38(10) 2_566 . . 2_666 ? Gd1 O5 S2 O7 48.9(8) . . . . ? Gd2 O5 S2 O7 -126.1(3) 2_566 . . . ? Gd1 O5 S2 O8 -68.8(8) . . . . ? Gd2 O5 S2 O8 116.2(3) 2_566 . . . ? Gd1 O5 S2 O6 171.3(7) . . . . ? Gd2 O5 S2 O6 -3.7(4) 2_566 . . . ? Gd1 O5 S2 Gd1 -12.2(9) . . . 2_666 ? Gd2 O5 S2 Gd1 172.74(12) 2_566 . . 2_666 ? Gd1 O5 S2 Gd2 175.0(8) . . . 2_566 ? Cu1 O10 C1 O9 -0.2(12) . . . . ? Cu1 O10 C1 C2 179.4(5) . . . . ? Gd1 O9 C1 O10 -166.3(6) . . . . ? Gd1 O9 C1 C2 14.0(10) . . . . ? C6 N1 C2 C3 -0.2(13) . . . . ? Gd1 N1 C2 C3 179.7(6) . . . . ? C6 N1 C2 C1 179.2(7) . . . . ? Gd1 N1 C2 C1 -0.9(9) . . . . ? O10 C1 C2 N1 172.6(7) . . . . ? O9 C1 C2 N1 -7.8(11) . . . . ? O10 C1 C2 C3 -8.1(13) . . . . ? O9 C1 C2 C3 171.6(8) . . . . ? N1 C2 C3 C4 2.2(13) . . . . ? C1 C2 C3 C4 -177.1(8) . . . . ? C2 C3 C4 C5 -2.5(13) . . . . ? C3 C4 C5 C6 0.9(14) . . . . ? C2 N1 C6 C5 -1.5(13) . . . . ? Gd1 N1 C6 C5 178.6(6) . . . . ? C2 N1 C6 C7 174.2(8) . . . . ? Gd1 N1 C6 C7 -5.7(10) . . . . ? C4 C5 C6 N1 1.1(14) . . . . ? C4 C5 C6 C7 -174.1(9) . . . . ? Gd1 O11 C7 O12 178.7(8) . . . . ? Gd1 O11 C7 C6 -2.9(12) . . . . ? N1 C6 C7 O12 -176.0(9) . . . . ? C5 C6 C7 O12 -0.5(16) . . . . ? N1 C6 C7 O11 5.4(12) . . . . ? C5 C6 C7 O11 -179.0(9) . . . . ? Cu2 O14 C8 O13 -3.1(12) 2_675 . . . ? Cu2 O14 C8 C9 177.6(6) 2_675 . . . ? Gd2 O13 C8 O14 -161.2(7) . . . . ? Gd2 O13 C8 C9 18.1(10) . . . . ? C13 N2 C9 C10 0.9(12) . . . . ? Gd2 N2 C9 C10 -177.3(6) . . . . ? C13 N2 C9 C8 -177.1(7) . . . . ? Gd2 N2 C9 C8 4.7(9) . . . . ? O14 C8 C9 N2 165.4(8) . . . . ? O13 C8 C9 N2 -14.0(11) . . . . ? O14 C8 C9 C10 -12.5(14) . . . . ? O13 C8 C9 C10 168.1(8) . . . . ? N2 C9 C10 C11 1.4(13) . . . . ? C8 C9 C10 C11 179.1(8) . . . . ? C9 C10 C11 C12 -2.3(13) . . . . ? C10 C11 C12 C13 0.9(13) . . . . ? C9 N2 C13 C12 -2.4(13) . . . . ? Gd2 N2 C13 C12 175.8(6) . . . . ? C9 N2 C13 C14 173.3(8) . . . . ? Gd2 N2 C13 C14 -8.5(10) . . . . ? C11 C12 C13 N2 1.5(13) . . . . ? C11 C12 C13 C14 -173.9(8) . . . . ? Gd2 O15 C14 O16 172.2(9) . . . . ? Gd2 O15 C14 C13 -5.6(12) . . . . ? N2 C13 C14 O16 -169.0(10) . . . . ? C12 C13 C14 O16 6.7(15) . . . . ? N2 C13 C14 O15 8.9(12) . . . . ? C12 C13 C14 O15 -175.4(8) . . . . ? C19 N3 C15 C16 0.6(16) . . . . ? Cu1 N3 C15 C16 177.9(9) . . . . ? N3 C15 C16 C17 -0.5(17) . . . . ? C15 C16 C17 C18 1.4(15) . . . . ? C15 C16 C17 C22 176.4(10) . . . . ? C16 C17 C18 C19 -2.4(16) . . . . ? C22 C17 C18 C19 -177.2(10) . . . . ? C15 N3 C19 C18 -1.6(16) . . . . ? Cu1 N3 C19 C18 -178.8(8) . . . . ? C17 C18 C19 N3 2.6(17) . . . . ? C24 N4 C20 C21 -3.0(15) . . . . ? Cu2 N4 C20 C21 170.2(8) . . . . ? N4 C20 C21 C22 2.9(16) . . . . ? C20 C21 C22 C23 -2.0(15) . . . . ? C20 C21 C22 C17 179.1(9) . . . . ? C18 C17 C22 C21 28.0(15) . . . . ? C16 C17 C22 C21 -146.7(10) . . . . ? C18 C17 C22 C23 -150.8(10) . . . . ? C16 C17 C22 C23 34.5(14) . . . . ? C21 C22 C23 C24 1.3(15) . . . . ? C17 C22 C23 C24 -179.8(9) . . . . ? C20 N4 C24 C23 2.2(15) . . . . ? Cu2 N4 C24 C23 -170.7(7) . . . . ? C22 C23 C24 N4 -1.5(16) . . . . ? C29 N5 C25 C26 -1.9(18) . . . . ? Cu1 N5 C25 C26 175.3(10) . . . . ? N5 C25 C26 C27 3(2) . . . . ? C25 C26 C27 C28 -3.7(17) . . . . ? C25 C26 C27 C32 177.5(11) . . . 1_445 ? C26 C27 C28 C29 3.1(17) . . . . ? C32 C27 C28 C29 -178.1(10) 1_445 . . . ? C25 N5 C29 C28 1.2(16) . . . . ? Cu1 N5 C29 C28 -176.1(9) . . . . ? C27 C28 C29 N5 -2.0(17) . . . . ? C34 N6 C30 C31 -0.1(17) . . . . ? Cu2 N6 C30 C31 179.3(9) . . . . ? N6 C30 C31 C32 -0.1(17) . . . . ? C30 C31 C32 C33 1.0(16) . . . . ? C30 C31 C32 C27 -179.9(10) . . . 1_665 ? C31 C32 C33 C34 -1.8(16) . . . . ? C27 C32 C33 C34 179.1(10) 1_665 . . . ? C30 N6 C34 C33 -0.8(16) . . . . ? Cu2 N6 C34 C33 179.9(8) . . . . ? C32 C33 C34 N6 1.8(17) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.569 _refine_diff_density_min -2.448 _refine_diff_density_rms 0.266 data_070114c _database_code_depnum_ccdc_archive 'CCDC 634513' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H30 Cu2 Dy2 N6 O20 S2' _chemical_formula_weight 1358.84 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' 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' Cu Cu 0.3201 1.2651 '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 12.632(6) _cell_length_b 13.234(7) _cell_length_c 14.431(7) _cell_angle_alpha 87.700(6) _cell_angle_beta 67.347(6) _cell_angle_gamma 66.628(5) _cell_volume 2025.5(18) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4416 _cell_measurement_theta_min 2.437 _cell_measurement_theta_max 28.183 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.37 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 4.878 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1781 _exptl_absorpt_correction_T_max 0.2655 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10422 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0858 _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 -17 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6981 _reflns_number_gt 4734 _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^)+(0.1068P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6981 _refine_ls_number_parameters 595 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1817 _refine_ls_wR_factor_gt 0.1582 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.012 _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 Dy1 Dy 0.68317(4) 0.87836(3) 0.07287(3) 0.01036(18) Uani 1 1 d . . . Dy2 Dy 1.18693(4) 0.87491(3) 0.06638(3) 0.00999(18) Uani 1 1 d . . . Cu1 Cu 0.55435(14) 0.74050(12) 0.43627(12) 0.0331(4) Uani 1 1 d . . . Cu2 Cu 1.02451(14) 0.72360(12) 0.44674(12) 0.0344(4) Uani 1 1 d . . . N1 N 0.7918(7) 0.6744(6) 0.0332(6) 0.0148(18) Uani 1 1 d . . . N2 N 1.2902(7) 0.6705(6) 0.0305(6) 0.0131(18) Uani 1 1 d . . . N3 N 0.6283(9) 0.8345(8) 0.4552(7) 0.026(2) Uani 1 1 d . . . N4 N 0.4394(8) 0.6713(7) 0.4629(8) 0.028(2) Uani 1 1 d . . . N5 N 0.9211(8) 0.6420(7) 0.4712(7) 0.027(2) Uani 1 1 d . . . N6 N 1.0941(8) 0.8210(7) 0.4684(7) 0.024(2) Uani 1 1 d . . . O1 O 0.6327(7) 0.7817(6) 0.2103(6) 0.0222(17) Uani 1 1 d . . . O2 O 0.6868(8) 0.6307(7) 0.2868(6) 0.033(2) Uani 1 1 d . . . O3 O 0.8238(7) 0.8107(5) -0.0976(5) 0.0209(17) Uani 1 1 d . . . O4 O 0.9699(10) 0.6749(8) -0.2211(7) 0.056(3) Uani 1 1 d U . . O5 O 1.1256(7) 0.7838(5) 0.2041(5) 0.0181(16) Uani 1 1 d . . . O6 O 1.1594(8) 0.6332(6) 0.2853(6) 0.0300(19) Uani 1 1 d . . . O7 O 1.3278(7) 0.8037(6) -0.1023(6) 0.0239(18) Uani 1 1 d . . . O8 O 1.4690(9) 0.6630(8) -0.2269(7) 0.055(3) Uani 1 1 d U . . O9 O 0.8631(6) 0.8257(5) 0.1221(5) 0.0162(15) Uani 1 1 d . . . O10 O 0.8532(6) 0.9714(5) 0.0219(5) 0.0173(16) Uani 1 1 d . . . O11 O 0.9460(6) 0.9586(5) 0.1451(5) 0.0170(16) Uani 1 1 d . . . O12 O 1.0589(6) 0.8255(5) -0.0003(5) 0.0176(16) Uani 1 1 d . . . O13 O 0.4423(7) 0.9545(6) 0.1471(5) 0.0208(17) Uani 1 1 d . . . O14 O 0.5634(6) 0.8231(5) 0.0007(5) 0.0176(16) Uani 1 1 d . . . O15 O 0.3633(7) 0.8225(5) 0.1172(6) 0.0191(16) Uani 1 1 d . . . O16 O 0.3591(6) 0.9681(5) 0.0182(5) 0.0178(16) Uani 1 1 d . . . O17 O 0.6006(7) 1.0322(6) 0.1987(5) 0.0274(19) Uani 1 1 d U . . H35 H 0.5225 1.0631 0.2366 0.041 Uiso 1 1 d R . . H36 H 0.6242 1.0849 0.1849 0.041 Uiso 1 1 d R . . O18 O 1.1082(7) 1.0276(6) 0.1938(5) 0.0224(17) Uani 1 1 d U . . H37 H 1.0544 1.0829 0.1810 0.034 Uiso 1 1 d R . . H38 H 1.1586 1.0567 0.1900 0.034 Uiso 1 1 d R . . O19 O 0.8672(10) 0.2115(8) 0.2188(7) 0.056(3) Uani 1 1 d . . . H39 H 0.9345 0.1525 0.1944 0.084 Uiso 1 1 d R . . H40 H 0.8322 0.2187 0.1775 0.084 Uiso 1 1 d R . . O20 O 0.3665(10) 0.1982(9) 0.2179(8) 0.072(3) Uani 1 1 d . . . H41 H 0.3911 0.2221 0.1615 0.109 Uiso 1 1 d R . . H42 H 0.3539 0.1431 0.2044 0.109 Uiso 1 1 d R . . S1 S 0.9303(2) 0.89502(19) 0.07390(18) 0.0105(5) Uani 1 1 d . . . S2 S 0.4318(2) 0.89207(19) 0.07260(18) 0.0112(5) Uani 1 1 d . . . C1 C 0.6917(10) 0.6781(9) 0.2097(8) 0.018(2) Uani 1 1 d . . . C2 C 0.7730(9) 0.6131(8) 0.1070(8) 0.018(2) Uani 1 1 d . . . C3 C 0.8287(10) 0.4956(9) 0.0874(9) 0.025(3) Uani 1 1 d . . . H3 H 0.8167 0.4526 0.1398 0.031 Uiso 1 1 calc R . . C4 C 0.9015(10) 0.4470(8) -0.0119(10) 0.025(3) Uani 1 1 d . . . H4 H 0.9355 0.3703 -0.0276 0.030 Uiso 1 1 calc R . . C5 C 0.9240(10) 0.5126(9) -0.0885(9) 0.027(3) Uani 1 1 d . . . H5 H 0.9759 0.4805 -0.1553 0.032 Uiso 1 1 calc R . . C6 C 0.8669(9) 0.6276(8) -0.0626(8) 0.017(2) Uani 1 1 d . . . C7 C 0.8888(10) 0.7087(8) -0.1340(8) 0.023(3) Uani 1 1 d . . . C8 C 1.1786(10) 0.6800(9) 0.2061(9) 0.019(2) Uani 1 1 d . . . C9 C 1.2686(9) 0.6106(9) 0.1064(9) 0.020(2) Uani 1 1 d . . . C10 C 1.3258(10) 0.4939(9) 0.0901(10) 0.026(3) Uani 1 1 d . . . H10 H 1.3134 0.4523 0.1436 0.031 Uiso 1 1 calc R . . C11 C 1.4020(10) 0.4432(9) -0.0095(10) 0.030(3) Uani 1 1 d . . . H11 H 1.4383 0.3662 -0.0242 0.036 Uiso 1 1 calc R . . C12 C 1.4230(10) 0.5072(9) -0.0857(10) 0.027(3) Uani 1 1 d . . . H12 H 1.4746 0.4737 -0.1522 0.032 Uiso 1 1 calc R . . C13 C 1.3681(9) 0.6206(9) -0.0641(8) 0.020(2) Uani 1 1 d . . . C14 C 1.3913(10) 0.6998(9) -0.1385(8) 0.023(3) Uani 1 1 d . . . C15 C 0.5871(11) 0.8910(10) 0.5465(9) 0.033(3) Uani 1 1 d . . . H15 H 0.5206 0.8840 0.5999 0.039 Uiso 1 1 calc R . . C16 C 0.6385(11) 0.9594(10) 0.5655(9) 0.034(3) Uani 1 1 d . . . H16 H 0.6082 0.9954 0.6304 0.041 Uiso 1 1 calc R . . C17 C 0.7365(10) 0.9733(9) 0.4856(8) 0.023(2) Uani 1 1 d . . . C18 C 0.7812(11) 0.9144(10) 0.3925(9) 0.034(3) Uani 1 1 d . . . H18 H 0.8479 0.9194 0.3378 0.041 Uiso 1 1 calc R . . C19 C 0.7240(11) 0.8462(10) 0.3813(9) 0.036(3) Uani 1 1 d . . . H19 H 0.7553 0.8066 0.3178 0.043 Uiso 1 1 calc R . . C20 C 0.3909(10) 0.6377(9) 0.5537(9) 0.025(3) Uani 1 1 d . . . H20 H 0.4046 0.6579 0.6077 0.030 Uiso 1 1 calc R . . C21 C 0.3228(10) 0.5755(9) 0.5692(8) 0.025(3) Uani 1 1 d . . . H21 H 0.2898 0.5553 0.6330 0.030 Uiso 1 1 calc R . . C22 C 0.3032(10) 0.5426(8) 0.4893(9) 0.022(3) Uani 1 1 d . . . C23 C 0.3514(10) 0.5772(9) 0.3970(8) 0.027(3) Uani 1 1 d . . . H23 H 0.3393 0.5574 0.3419 0.032 Uiso 1 1 calc R . . C24 C 0.4182(10) 0.6420(9) 0.3869(9) 0.028(3) Uani 1 1 d . . . H24 H 0.4491 0.6657 0.3245 0.034 Uiso 1 1 calc R . . C25 C 0.8271(11) 0.6524(10) 0.5602(9) 0.035(3) Uani 1 1 d . . . H25 H 0.8125 0.6996 0.6140 0.042 Uiso 1 1 calc R . . C26 C 0.7510(11) 0.5973(9) 0.5766(9) 0.033(3) Uani 1 1 d . . . H26 H 0.6859 0.6088 0.6398 0.040 Uiso 1 1 calc R . . C27 C 0.7713(9) 0.5236(8) 0.4980(8) 0.022(2) Uani 1 1 d . . . C28 C 0.8698(11) 0.5121(9) 0.4050(9) 0.032(3) Uani 1 1 d . . . H28 H 0.8866 0.4655 0.3499 0.038 Uiso 1 1 calc R . . C29 C 0.9419(11) 0.5704(9) 0.3957(9) 0.030(3) Uani 1 1 d . . . H29 H 1.0086 0.5598 0.3338 0.036 Uiso 1 1 calc R . . C30 C 1.0983(11) 0.8361(9) 0.5588(9) 0.031(3) Uani 1 1 d . . . H30 H 1.0624 0.8018 0.6118 0.037 Uiso 1 1 calc R . . C31 C 1.1543(11) 0.9008(10) 0.5751(9) 0.031(3) Uani 1 1 d . . . H31 H 1.1584 0.9075 0.6374 0.037 Uiso 1 1 calc R . . C32 C 1.2045(10) 0.9558(9) 0.4976(9) 0.025(3) Uani 1 1 d . . . C33 C 1.1979(12) 0.9411(10) 0.4065(9) 0.037(3) Uani 1 1 d . . . H33 H 1.2299 0.9767 0.3529 0.045 Uiso 1 1 calc R . . C34 C 1.1434(12) 0.8729(10) 0.3953(9) 0.038(3) Uani 1 1 d . . . H34 H 1.1413 0.8629 0.3327 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0132(3) 0.0113(3) 0.0065(3) -0.0018(2) -0.0067(2) -0.0020(2) Dy2 0.0134(3) 0.0112(3) 0.0059(3) -0.0014(2) -0.0067(2) -0.0026(2) Cu1 0.0417(9) 0.0368(8) 0.0380(10) 0.0054(7) -0.0226(8) -0.0264(7) Cu2 0.0416(9) 0.0324(8) 0.0454(10) 0.0026(7) -0.0253(8) -0.0230(7) N1 0.013(4) 0.019(5) 0.012(5) 0.001(4) -0.008(4) -0.003(4) N2 0.012(4) 0.012(4) 0.018(5) 0.001(4) -0.010(4) -0.003(3) N3 0.039(6) 0.032(5) 0.022(6) 0.007(4) -0.017(5) -0.023(5) N4 0.024(5) 0.031(5) 0.034(6) -0.003(5) -0.010(5) -0.015(4) N5 0.024(5) 0.023(5) 0.030(6) -0.011(4) -0.009(5) -0.008(4) N6 0.031(5) 0.029(5) 0.020(5) 0.002(4) -0.013(5) -0.017(4) O1 0.026(4) 0.022(4) 0.017(4) -0.001(3) -0.007(4) -0.009(3) O2 0.049(5) 0.039(5) 0.021(5) 0.020(4) -0.021(4) -0.022(4) O3 0.028(4) 0.015(4) 0.013(4) -0.004(3) -0.004(3) -0.006(3) O4 0.070(6) 0.040(5) 0.027(5) -0.009(4) 0.006(4) -0.014(4) O5 0.026(4) 0.016(4) 0.013(4) -0.001(3) -0.010(3) -0.006(3) O6 0.041(5) 0.034(5) 0.025(5) 0.015(4) -0.016(4) -0.024(4) O7 0.034(4) 0.019(4) 0.018(4) -0.006(3) -0.006(4) -0.014(3) O8 0.061(6) 0.045(5) 0.024(5) -0.014(4) 0.006(4) -0.010(4) O9 0.021(4) 0.020(4) 0.015(4) 0.008(3) -0.013(3) -0.009(3) O10 0.019(4) 0.020(4) 0.019(4) 0.006(3) -0.016(3) -0.006(3) O11 0.018(4) 0.020(4) 0.019(4) -0.002(3) -0.015(3) -0.007(3) O12 0.015(4) 0.019(4) 0.022(4) -0.004(3) -0.015(3) -0.002(3) O13 0.027(4) 0.026(4) 0.020(4) 0.001(3) -0.019(4) -0.010(3) O14 0.021(4) 0.014(4) 0.020(4) -0.003(3) -0.015(3) -0.002(3) O15 0.023(4) 0.017(4) 0.021(4) 0.004(3) -0.012(3) -0.009(3) O16 0.018(4) 0.017(4) 0.018(4) 0.001(3) -0.013(3) -0.002(3) O17 0.028(4) 0.033(4) 0.014(4) -0.017(3) 0.005(3) -0.017(3) O18 0.025(4) 0.022(4) 0.014(4) -0.012(3) -0.002(3) -0.008(3) O19 0.061(7) 0.068(7) 0.031(6) -0.007(5) -0.021(5) -0.015(6) O20 0.074(8) 0.067(7) 0.036(7) -0.010(6) -0.014(6) 0.005(6) S1 0.0133(12) 0.0136(12) 0.0078(13) 0.0017(10) -0.0084(11) -0.0045(10) S2 0.0133(12) 0.0118(12) 0.0115(13) 0.0009(10) -0.0093(11) -0.0037(10) C1 0.020(6) 0.024(6) 0.016(6) 0.005(5) -0.011(5) -0.012(5) C2 0.020(5) 0.014(5) 0.027(7) 0.006(5) -0.017(5) -0.008(4) C3 0.020(6) 0.025(6) 0.032(7) 0.004(5) -0.015(6) -0.006(5) C4 0.022(6) 0.008(5) 0.051(8) -0.008(5) -0.024(6) 0.001(4) C5 0.021(6) 0.024(6) 0.032(7) -0.017(5) -0.013(6) -0.003(5) C6 0.014(5) 0.020(5) 0.015(6) -0.006(4) -0.009(5) -0.001(4) C7 0.018(5) 0.019(6) 0.018(6) -0.011(5) -0.003(5) 0.002(5) C8 0.018(5) 0.026(6) 0.027(7) 0.014(5) -0.020(5) -0.015(5) C9 0.016(5) 0.028(6) 0.028(7) 0.003(5) -0.018(5) -0.011(5) C10 0.021(6) 0.020(6) 0.046(8) 0.005(5) -0.022(6) -0.009(5) C11 0.017(6) 0.014(6) 0.057(9) -0.013(6) -0.023(6) 0.004(5) C12 0.017(6) 0.022(6) 0.035(7) -0.014(5) -0.013(6) 0.003(5) C13 0.015(5) 0.027(6) 0.019(6) -0.010(5) -0.011(5) -0.003(5) C14 0.018(5) 0.027(6) 0.017(6) -0.006(5) -0.007(5) -0.002(5) C15 0.033(7) 0.055(8) 0.018(6) 0.001(6) -0.001(6) -0.034(6) C16 0.040(7) 0.050(8) 0.019(7) -0.011(6) -0.002(6) -0.032(6) C17 0.030(6) 0.027(6) 0.014(6) -0.002(5) -0.004(5) -0.018(5) C18 0.038(7) 0.055(8) 0.019(7) 0.003(6) -0.009(6) -0.031(7) C19 0.050(8) 0.048(8) 0.016(7) -0.007(6) -0.010(6) -0.029(7) C20 0.022(6) 0.031(6) 0.023(7) 0.002(5) -0.014(5) -0.008(5) C21 0.027(6) 0.033(6) 0.010(6) -0.005(5) -0.004(5) -0.011(5) C22 0.020(5) 0.023(6) 0.021(6) -0.010(5) -0.007(5) -0.006(5) C23 0.028(6) 0.042(7) 0.019(6) -0.002(5) -0.015(5) -0.016(6) C24 0.030(6) 0.036(7) 0.024(7) 0.001(6) -0.011(6) -0.018(6) C25 0.046(8) 0.040(7) 0.021(7) -0.009(6) -0.008(6) -0.024(6) C26 0.038(7) 0.046(7) 0.014(6) -0.010(5) 0.002(6) -0.027(6) C27 0.017(5) 0.018(5) 0.020(6) -0.004(5) -0.001(5) -0.003(5) C28 0.043(7) 0.032(6) 0.020(7) -0.006(5) -0.002(6) -0.026(6) C29 0.033(7) 0.039(7) 0.017(6) -0.006(5) -0.003(6) -0.020(6) C30 0.036(7) 0.034(7) 0.021(7) -0.004(5) -0.003(6) -0.022(6) C31 0.041(7) 0.045(7) 0.020(7) 0.004(6) -0.017(6) -0.026(6) C32 0.026(6) 0.027(6) 0.020(6) -0.007(5) -0.009(5) -0.009(5) C33 0.063(9) 0.041(7) 0.020(7) -0.004(6) -0.014(7) -0.035(7) C34 0.070(9) 0.044(8) 0.023(7) 0.009(6) -0.024(7) -0.042(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_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O1 2.333(7) . ? Dy1 O3 2.358(7) . ? Dy1 O16 2.367(7) 2_675 ? Dy1 O17 2.384(7) . ? Dy1 O14 2.461(6) . ? Dy1 N1 2.465(8) . ? Dy1 O9 2.470(7) . ? Dy1 O13 2.562(7) . ? Dy1 O10 2.735(7) . ? Dy2 O5 2.316(7) . ? Dy2 O10 2.343(7) 2_775 ? Dy2 O7 2.345(7) . ? Dy2 O18 2.398(6) . ? Dy2 O15 2.444(7) 1_655 ? Dy2 O12 2.461(6) . ? Dy2 N2 2.465(8) . ? Dy2 O11 2.558(7) . ? Dy2 O16 2.762(7) 1_655 ? Dy2 S2 3.226(3) 1_655 ? Cu1 N3 1.907(8) . ? Cu1 N4 1.921(8) . ? Cu1 O2 2.260(9) . ? Cu2 N6 1.917(8) . ? Cu2 N5 1.931(8) . ? Cu2 O6 2.304(8) . ? N1 C2 1.318(13) . ? N1 C6 1.337(12) . ? N2 C9 1.333(14) . ? N2 C13 1.337(13) . ? N3 C19 1.328(14) . ? N3 C15 1.344(14) . ? N4 C24 1.330(14) . ? N4 C20 1.357(14) . ? N5 C25 1.337(14) . ? N5 C29 1.349(13) . ? N6 C34 1.322(14) . ? N6 C30 1.351(14) . ? O1 C1 1.274(12) . ? O2 C1 1.248(13) . ? O3 C7 1.272(12) . ? O4 C7 1.232(13) . ? O5 C8 1.272(12) . ? O6 C8 1.264(13) . ? O7 C14 1.290(12) . ? O8 C14 1.239(13) . ? O9 S1 1.469(7) . ? O10 S1 1.501(7) . ? O10 Dy2 2.343(7) 2_775 ? O11 S1 1.470(6) . ? O12 S1 1.478(7) . ? O13 S2 1.457(7) . ? O14 S2 1.488(7) . ? O15 S2 1.473(7) . ? O15 Dy2 2.444(7) 1_455 ? O16 S2 1.495(7) . ? O16 Dy1 2.367(7) 2_675 ? O16 Dy2 2.762(7) 1_455 ? O17 H35 0.8500 . ? O17 H36 0.8500 . ? O18 H37 0.8500 . ? O18 H38 0.8499 . ? O19 H39 0.8495 . ? O19 H40 0.8500 . ? O20 H41 0.8500 . ? O20 H42 0.8500 . ? S2 Dy2 3.226(3) 1_455 ? C1 C2 1.489(14) . ? C2 C3 1.416(14) . ? C3 C4 1.380(16) . ? C3 H3 0.9300 . ? C4 C5 1.390(17) . ? C4 H4 0.9300 . ? C5 C6 1.394(14) . ? C5 H5 0.9300 . ? C6 C7 1.489(15) . ? C8 C9 1.491(15) . ? C9 C10 1.405(15) . ? C10 C11 1.394(17) . ? C10 H10 0.9300 . ? C11 C12 1.370(17) . ? C11 H11 0.9300 . ? C12 C13 1.369(15) . ? C12 H12 0.9300 . ? C13 C14 1.500(16) . ? C15 C16 1.394(14) . ? C15 H15 0.9300 . ? C16 C17 1.399(15) . ? C16 H16 0.9300 . ? C17 C18 1.372(15) . ? C17 C32 1.486(14) 2_776 ? C18 C19 1.408(14) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.366(14) . ? C20 H20 0.9300 . ? C21 C22 1.388(14) . ? C21 H21 0.9300 . ? C22 C23 1.379(15) . ? C22 C27 1.482(14) 2_666 ? C23 C24 1.392(14) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.370(14) . ? C25 H25 0.9300 . ? C26 C27 1.404(14) . ? C26 H26 0.9300 . ? C27 C28 1.397(15) . ? C27 C22 1.482(14) 2_666 ? C28 C29 1.377(14) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.384(14) . ? C30 H30 0.9300 . ? C31 C32 1.392(15) . ? C31 H31 0.9300 . ? C32 C33 1.375(15) . ? C32 C17 1.486(14) 2_776 ? C33 C34 1.380(14) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Dy1 O3 129.9(2) . . ? O1 Dy1 O16 153.9(2) . 2_675 ? O3 Dy1 O16 74.0(2) . 2_675 ? O1 Dy1 O17 84.8(3) . . ? O3 Dy1 O17 141.1(2) . . ? O16 Dy1 O17 77.4(3) 2_675 . ? O1 Dy1 O14 91.2(2) . . ? O3 Dy1 O14 76.2(2) . . ? O16 Dy1 O14 84.5(2) 2_675 . ? O17 Dy1 O14 126.6(2) . . ? O1 Dy1 N1 65.0(3) . . ? O3 Dy1 N1 64.9(3) . . ? O16 Dy1 N1 137.0(3) 2_675 . ? O17 Dy1 N1 144.7(3) . . ? O14 Dy1 N1 74.4(2) . . ? O1 Dy1 O9 76.5(2) . . ? O3 Dy1 O9 90.1(2) . . ? O16 Dy1 O9 118.4(2) 2_675 . ? O17 Dy1 O9 80.9(2) . . ? O14 Dy1 O9 149.3(2) . . ? N1 Dy1 O9 74.8(2) . . ? O1 Dy1 O13 75.4(2) . . ? O3 Dy1 O13 127.5(2) . . ? O16 Dy1 O13 81.0(2) 2_675 . ? O17 Dy1 O13 71.9(2) . . ? O14 Dy1 O13 55.7(2) . . ? N1 Dy1 O13 114.3(2) . . ? O9 Dy1 O13 142.2(2) . . ? O1 Dy1 O10 127.1(2) . . ? O3 Dy1 O10 72.0(2) . . ? O16 Dy1 O10 65.0(2) 2_675 . ? O17 Dy1 O10 72.3(2) . . ? O14 Dy1 O10 140.7(2) . . ? N1 Dy1 O10 110.8(2) . . ? O9 Dy1 O10 53.5(2) . . ? O13 Dy1 O10 134.8(2) . . ? O5 Dy2 O10 151.2(2) . 2_775 ? O5 Dy2 O7 130.3(2) . . ? O10 Dy2 O7 75.7(2) 2_775 . ? O5 Dy2 O18 83.7(2) . . ? O10 Dy2 O18 77.3(3) 2_775 . ? O7 Dy2 O18 141.9(2) . . ? O5 Dy2 O15 78.7(2) . 1_655 ? O10 Dy2 O15 117.9(2) 2_775 1_655 ? O7 Dy2 O15 90.4(3) . 1_655 ? O18 Dy2 O15 79.2(2) . 1_655 ? O5 Dy2 O12 88.5(2) . . ? O10 Dy2 O12 85.2(2) 2_775 . ? O7 Dy2 O12 78.2(2) . . ? O18 Dy2 O12 125.5(2) . . ? O15 Dy2 O12 151.0(2) 1_655 . ? O5 Dy2 N2 65.3(3) . . ? O10 Dy2 N2 138.8(3) 2_775 . ? O7 Dy2 N2 65.0(3) . . ? O18 Dy2 N2 143.0(3) . . ? O15 Dy2 N2 75.5(2) 1_655 . ? O12 Dy2 N2 75.6(2) . . ? O5 Dy2 O11 72.7(2) . . ? O10 Dy2 O11 80.6(2) 2_775 . ? O7 Dy2 O11 129.6(2) . . ? O18 Dy2 O11 70.4(2) . . ? O15 Dy2 O11 139.9(2) 1_655 . ? O12 Dy2 O11 55.9(2) . . ? N2 Dy2 O11 115.2(2) . . ? O5 Dy2 O16 128.4(2) . 1_655 ? O10 Dy2 O16 64.9(2) 2_775 1_655 ? O7 Dy2 O16 73.4(2) . 1_655 ? O18 Dy2 O16 71.1(2) . 1_655 ? O15 Dy2 O16 53.2(2) 1_655 1_655 ? O12 Dy2 O16 142.8(2) . 1_655 ? N2 Dy2 O16 112.2(2) . 1_655 ? O11 Dy2 O16 132.6(2) . 1_655 ? O5 Dy2 S2 103.05(17) . 1_655 ? O10 Dy2 S2 92.36(16) 2_775 1_655 ? O7 Dy2 S2 80.78(18) . 1_655 ? O18 Dy2 S2 74.10(18) . 1_655 ? O15 Dy2 S2 25.69(16) 1_655 1_655 ? O12 Dy2 S2 158.79(17) . 1_655 ? N2 Dy2 S2 92.99(18) . 1_655 ? O11 Dy2 S2 144.47(15) . 1_655 ? O16 Dy2 S2 27.54(15) 1_655 1_655 ? N3 Cu1 N4 160.3(4) . . ? N3 Cu1 O2 107.1(4) . . ? N4 Cu1 O2 92.5(4) . . ? N6 Cu2 N5 161.3(4) . . ? N6 Cu2 O6 103.6(3) . . ? N5 Cu2 O6 94.9(3) . . ? C2 N1 C6 121.1(9) . . ? C2 N1 Dy1 119.2(7) . . ? C6 N1 Dy1 119.7(7) . . ? C9 N2 C13 120.5(9) . . ? C9 N2 Dy2 119.3(7) . . ? C13 N2 Dy2 120.2(7) . . ? C19 N3 C15 116.2(9) . . ? C19 N3 Cu1 122.9(8) . . ? C15 N3 Cu1 120.9(7) . . ? C24 N4 C20 117.6(9) . . ? C24 N4 Cu1 119.4(8) . . ? C20 N4 Cu1 122.5(7) . . ? C25 N5 C29 116.6(9) . . ? C25 N5 Cu2 123.7(7) . . ? C29 N5 Cu2 119.7(8) . . ? C34 N6 C30 117.5(9) . . ? C34 N6 Cu2 121.7(8) . . ? C30 N6 Cu2 120.8(7) . . ? C1 O1 Dy1 124.7(7) . . ? C1 O2 Cu1 115.6(7) . . ? C7 O3 Dy1 125.3(7) . . ? C8 O5 Dy2 125.0(7) . . ? C8 O6 Cu2 125.0(7) . . ? C14 O7 Dy2 125.7(7) . . ? S1 O9 Dy1 107.0(4) . . ? S1 O10 Dy2 149.4(4) . 2_775 ? S1 O10 Dy1 94.5(3) . . ? Dy2 O10 Dy1 116.0(3) 2_775 . ? S1 O11 Dy2 97.1(3) . . ? S1 O12 Dy2 101.1(3) . . ? S2 O13 Dy1 97.5(4) . . ? S2 O14 Dy1 100.9(3) . . ? S2 O15 Dy2 108.3(4) . 1_455 ? S2 O16 Dy1 152.0(4) . 2_675 ? S2 O16 Dy2 93.8(3) . 1_455 ? Dy1 O16 Dy2 114.1(3) 2_675 1_455 ? Dy1 O17 H35 121.4 . . ? Dy1 O17 H36 120.3 . . ? H35 O17 H36 105.4 . . ? Dy2 O18 H37 107.4 . . ? Dy2 O18 H38 116.2 . . ? H37 O18 H38 97.6 . . ? H39 O19 H40 105.2 . . ? H41 O20 H42 104.7 . . ? O9 S1 O11 114.0(4) . . ? O9 S1 O12 110.6(4) . . ? O11 S1 O12 105.9(4) . . ? O9 S1 O10 104.9(4) . . ? O11 S1 O10 110.9(4) . . ? O12 S1 O10 110.7(4) . . ? O13 S2 O15 113.6(4) . . ? O13 S2 O14 105.8(4) . . ? O15 S2 O14 111.1(4) . . ? O13 S2 O16 111.1(4) . . ? O15 S2 O16 104.7(4) . . ? O14 S2 O16 110.6(4) . . ? O13 S2 Dy2 129.9(3) . 1_455 ? O15 S2 Dy2 46.0(3) . 1_455 ? O14 S2 Dy2 123.9(3) . 1_455 ? O16 S2 Dy2 58.7(3) . 1_455 ? O2 C1 O1 124.9(10) . . ? O2 C1 C2 120.1(10) . . ? O1 C1 C2 114.9(9) . . ? N1 C2 C3 121.3(10) . . ? N1 C2 C1 114.2(8) . . ? C3 C2 C1 124.5(10) . . ? C4 C3 C2 117.9(11) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? C3 C4 C5 120.1(10) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 118.4(10) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? N1 C6 C5 121.2(10) . . ? N1 C6 C7 113.8(8) . . ? C5 C6 C7 124.9(10) . . ? O4 C7 O3 124.4(11) . . ? O4 C7 C6 119.7(9) . . ? O3 C7 C6 115.9(9) . . ? O6 C8 O5 124.7(11) . . ? O6 C8 C9 119.0(10) . . ? O5 C8 C9 116.2(9) . . ? N2 C9 C10 121.5(11) . . ? N2 C9 C8 113.1(9) . . ? C10 C9 C8 125.4(11) . . ? C11 C10 C9 117.2(11) . . ? C11 C10 H10 121.4 . . ? C9 C10 H10 121.4 . . ? C12 C11 C10 119.7(10) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C13 C12 C11 120.0(11) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? N2 C13 C12 120.9(11) . . ? N2 C13 C14 113.6(9) . . ? C12 C13 C14 125.4(10) . . ? O8 C14 O7 125.2(11) . . ? O8 C14 C13 119.6(10) . . ? O7 C14 C13 115.3(9) . . ? N3 C15 C16 123.6(10) . . ? N3 C15 H15 118.2 . . ? C16 C15 H15 118.2 . . ? C15 C16 C17 119.1(10) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C18 C17 C16 117.9(10) . . ? C18 C17 C32 120.9(10) . 2_776 ? C16 C17 C32 121.0(10) . 2_776 ? C17 C18 C19 118.7(10) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 120.7 . . ? N3 C19 C18 124.5(10) . . ? N3 C19 H19 117.7 . . ? C18 C19 H19 117.7 . . ? N4 C20 C21 122.8(10) . . ? N4 C20 H20 118.6 . . ? C21 C20 H20 118.6 . . ? C20 C21 C22 119.6(11) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 117.9(9) . . ? C23 C22 C27 120.1(10) . 2_666 ? C21 C22 C27 122.0(11) . 2_666 ? C22 C23 C24 119.5(10) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? N4 C24 C23 122.6(11) . . ? N4 C24 H24 118.7 . . ? C23 C24 H24 118.7 . . ? N5 C25 C26 123.7(10) . . ? N5 C25 H25 118.2 . . ? C26 C25 H25 118.2 . . ? C25 C26 C27 120.0(10) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C28 C27 C26 116.5(10) . . ? C28 C27 C22 120.1(10) . 2_666 ? C26 C27 C22 123.3(10) . 2_666 ? C29 C28 C27 119.5(10) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? N5 C29 C28 123.7(11) . . ? N5 C29 H29 118.1 . . ? C28 C29 H29 118.1 . . ? N6 C30 C31 122.2(11) . . ? N6 C30 H30 118.9 . . ? C31 C30 H30 118.9 . . ? C30 C31 C32 119.5(11) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C33 C32 C31 117.6(10) . . ? C33 C32 C17 122.2(11) . 2_776 ? C31 C32 C17 120.1(10) . 2_776 ? C32 C33 C34 119.4(11) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? N6 C34 C33 123.7(11) . . ? N6 C34 H34 118.1 . . ? C33 C34 H34 118.1 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 4.142 _refine_diff_density_min -5.677 _refine_diff_density_rms 0.327 # Attachment 'Tb-Cu.cif' data_070114b _database_code_depnum_ccdc_archive 'CCDC 634514' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H30 Cu2 N6 O20 S2 Tb2' _chemical_formula_weight 1351.68 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 12.624(2) _cell_length_b 13.208(3) _cell_length_c 14.457(3) _cell_angle_alpha 87.744(2) _cell_angle_beta 67.324(2) _cell_angle_gamma 66.785(2) _cell_volume 2026.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4918 _cell_measurement_theta_min 2.436 _cell_measurement_theta_max 28.203 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 4.679 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1946 _exptl_absorpt_correction_T_max 0.3439 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10584 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7019 _reflns_number_gt 5035 _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^)+(0.0758P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7019 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1282 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.68307(3) 0.87891(2) 0.07347(2) 0.01062(12) Uani 1 1 d . . . Tb2 Tb 1.18710(3) 0.87527(2) 0.06661(2) 0.01025(12) Uani 1 1 d . . . Cu1 Cu 0.55518(10) 0.74051(9) 0.43639(8) 0.0332(3) Uani 1 1 d . . . Cu2 Cu 1.02437(10) 0.72282(9) 0.44658(9) 0.0348(3) Uani 1 1 d . . . N1 N 0.7921(5) 0.6741(5) 0.0327(4) 0.0140(13) Uani 1 1 d . . . N2 N 1.2906(5) 0.6704(4) 0.0304(5) 0.0157(13) Uani 1 1 d . . . N3 N 0.6295(6) 0.8344(5) 0.4555(5) 0.0271(16) Uani 1 1 d . . . N4 N 0.4405(6) 0.6715(5) 0.4630(5) 0.0248(16) Uani 1 1 d . . . N5 N 0.9207(6) 0.6418(5) 0.4708(5) 0.0263(16) Uani 1 1 d . . . N6 N 1.0933(6) 0.8204(5) 0.4689(5) 0.0268(16) Uani 1 1 d . . . O1 O 0.6320(5) 0.7823(4) 0.2121(4) 0.0200(12) Uani 1 1 d . . . O2 O 0.6880(5) 0.6299(5) 0.2866(4) 0.0330(14) Uani 1 1 d . . . O3 O 0.8232(5) 0.8104(4) -0.0970(4) 0.0215(12) Uani 1 1 d . . . O4 O 0.9712(7) 0.6745(5) -0.2203(5) 0.062(2) Uani 1 1 d . . . O5 O 1.1254(5) 0.7829(4) 0.2048(4) 0.0181(11) Uani 1 1 d . . . O6 O 1.1600(5) 0.6319(5) 0.2854(4) 0.0313(14) Uani 1 1 d . . . O7 O 1.3287(5) 0.8027(4) -0.1024(4) 0.0238(12) Uani 1 1 d . . . O8 O 1.4674(7) 0.6634(6) -0.2255(5) 0.063(2) Uani 1 1 d . . . O9 O 0.8625(4) 0.8252(4) 0.1236(4) 0.0185(11) Uani 1 1 d . . . O10 O 0.8529(4) 0.9692(4) 0.0230(4) 0.0164(11) Uani 1 1 d . . . O11 O 0.9463(4) 0.9583(4) 0.1450(4) 0.0186(11) Uani 1 1 d . . . O12 O 1.0586(4) 0.8256(4) 0.0007(4) 0.0167(11) Uani 1 1 d . . . O13 O 0.4425(5) 0.9549(4) 0.1478(4) 0.0219(12) Uani 1 1 d . . . O14 O 0.5619(4) 0.8241(4) 0.0019(4) 0.0183(11) Uani 1 1 d . . . O15 O 0.3640(5) 0.8217(4) 0.1185(4) 0.0211(12) Uani 1 1 d . . . O16 O 0.3593(4) 0.9659(4) 0.0185(4) 0.0187(11) Uani 1 1 d . . . O17 O 0.5990(5) 1.0334(4) 0.2002(4) 0.0259(13) Uani 1 1 d . . . H35 H 0.5586 1.0734 0.1672 0.039 Uiso 1 1 d R . . H36 H 0.6442 1.0680 0.1975 0.039 Uiso 1 1 d R . . O18 O 1.1070(5) 1.0291(4) 0.1947(4) 0.0210(12) Uani 1 1 d . . . H37 H 1.0675 1.0697 0.1614 0.031 Uiso 1 1 d R . . H38 H 1.1572 1.0595 0.1875 0.031 Uiso 1 1 d R . . O19 O 0.8655(7) 0.2106(6) 0.2182(5) 0.060(2) Uani 1 1 d . . . H39 H 0.9328 0.1516 0.1939 0.090 Uiso 1 1 d R . . H40 H 0.8914 0.2606 0.2200 0.090 Uiso 1 1 d R . . O20 O 0.3655(7) 0.1976(6) 0.2180(5) 0.077(3) Uani 1 1 d . . . H41 H 0.3749 0.2133 0.1586 0.116 Uiso 1 1 d R . . H42 H 0.4270 0.1358 0.2104 0.116 Uiso 1 1 d R . . S1 S 0.93027(15) 0.89463(14) 0.07439(13) 0.0113(4) Uani 1 1 d . . . S2 S 0.43141(15) 0.89184(14) 0.07319(13) 0.0117(4) Uani 1 1 d . . . C1 C 0.6916(7) 0.6784(6) 0.2110(6) 0.0202(17) Uani 1 1 d . . . C2 C 0.7730(7) 0.6121(6) 0.1081(6) 0.0179(16) Uani 1 1 d . . . C3 C 0.8281(7) 0.4955(6) 0.0880(7) 0.0247(18) Uani 1 1 d . . . H3 H 0.8152 0.4523 0.1401 0.030 Uiso 1 1 calc R . . C4 C 0.9029(7) 0.4461(6) -0.0123(7) 0.027(2) Uani 1 1 d . . . H4 H 0.9385 0.3692 -0.0278 0.032 Uiso 1 1 calc R . . C5 C 0.9238(7) 0.5110(6) -0.0877(7) 0.0268(19) Uani 1 1 d . . . H5 H 0.9748 0.4791 -0.1546 0.032 Uiso 1 1 calc R . . C6 C 0.8663(7) 0.6264(6) -0.0616(6) 0.0193(17) Uani 1 1 d . . . C7 C 0.8896(7) 0.7088(7) -0.1350(6) 0.028(2) Uani 1 1 d . . . C8 C 1.1782(7) 0.6787(6) 0.2076(6) 0.0196(17) Uani 1 1 d . . . C9 C 1.2682(7) 0.6102(6) 0.1077(6) 0.0195(17) Uani 1 1 d . . . C10 C 1.3238(7) 0.4945(6) 0.0914(7) 0.0259(19) Uani 1 1 d . . . H10 H 1.3101 0.4531 0.1448 0.031 Uiso 1 1 calc R . . C11 C 1.4013(7) 0.4426(6) -0.0082(7) 0.032(2) Uani 1 1 d . . . H11 H 1.4378 0.3655 -0.0220 0.038 Uiso 1 1 calc R . . C12 C 1.4235(7) 0.5050(6) -0.0852(7) 0.0252(19) Uani 1 1 d . . . H12 H 1.4756 0.4708 -0.1513 0.030 Uiso 1 1 calc R . . C13 C 1.3669(7) 0.6210(6) -0.0635(6) 0.0213(17) Uani 1 1 d . . . C14 C 1.3913(7) 0.6995(6) -0.1386(6) 0.0248(18) Uani 1 1 d . . . C15 C 0.5871(8) 0.8917(7) 0.5468(6) 0.035(2) Uani 1 1 d . . . H15 H 0.5206 0.8844 0.6001 0.042 Uiso 1 1 calc R . . C16 C 0.6371(8) 0.9599(7) 0.5650(6) 0.032(2) Uani 1 1 d . . . H16 H 0.6044 0.9981 0.6293 0.039 Uiso 1 1 calc R . . C17 C 0.7377(7) 0.9720(6) 0.4862(6) 0.0241(18) Uani 1 1 d . . . C18 C 0.7802(8) 0.9142(7) 0.3926(6) 0.032(2) Uani 1 1 d . . . H18 H 0.8460 0.9206 0.3380 0.038 Uiso 1 1 calc R . . C19 C 0.7251(8) 0.8464(7) 0.3797(6) 0.035(2) Uani 1 1 d . . . H19 H 0.7555 0.8078 0.3160 0.042 Uiso 1 1 calc R . . C20 C 0.3925(7) 0.6372(6) 0.5540(6) 0.0255(19) Uani 1 1 d . . . H20 H 0.4064 0.6566 0.6080 0.031 Uiso 1 1 calc R . . C21 C 0.3239(7) 0.5746(6) 0.5680(6) 0.0265(19) Uani 1 1 d . . . H21 H 0.2909 0.5536 0.6313 0.032 Uiso 1 1 calc R . . C22 C 0.3038(7) 0.5427(6) 0.4886(6) 0.0210(17) Uani 1 1 d . . . C23 C 0.3530(7) 0.5778(6) 0.3970(6) 0.0272(19) Uani 1 1 d . . . H23 H 0.3417 0.5580 0.3416 0.033 Uiso 1 1 calc R . . C24 C 0.4186(7) 0.6420(7) 0.3875(6) 0.0277(19) Uani 1 1 d . . . H24 H 0.4492 0.6660 0.3253 0.033 Uiso 1 1 calc R . . C25 C 0.8260(8) 0.6534(7) 0.5585(7) 0.037(2) Uani 1 1 d . . . H25 H 0.8095 0.7033 0.6112 0.044 Uiso 1 1 calc R . . C26 C 0.7509(7) 0.5968(6) 0.5766(6) 0.029(2) Uani 1 1 d . . . H26 H 0.6870 0.6068 0.6400 0.034 Uiso 1 1 calc R . . C27 C 0.7726(7) 0.5234(6) 0.4971(6) 0.0212(17) Uani 1 1 d . . . C28 C 0.8707(8) 0.5109(7) 0.4057(6) 0.030(2) Uani 1 1 d . . . H28 H 0.8886 0.4629 0.3511 0.036 Uiso 1 1 calc R . . C29 C 0.9413(8) 0.5698(7) 0.3965(6) 0.034(2) Uani 1 1 d . . . H29 H 1.0079 0.5593 0.3346 0.040 Uiso 1 1 calc R . . C30 C 1.0980(8) 0.8360(7) 0.5578(6) 0.028(2) Uani 1 1 d . . . H30 H 1.0627 0.8015 0.6109 0.033 Uiso 1 1 calc R . . C31 C 1.1527(8) 0.9011(7) 0.5734(6) 0.032(2) Uani 1 1 d . . . H31 H 1.1549 0.9089 0.6362 0.038 Uiso 1 1 calc R . . C32 C 1.2051(7) 0.9557(6) 0.4968(6) 0.0236(18) Uani 1 1 d . . . C33 C 1.1965(9) 0.9409(7) 0.4065(6) 0.038(2) Uani 1 1 d . . . H33 H 1.2282 0.9768 0.3530 0.046 Uiso 1 1 calc R . . C34 C 1.1418(8) 0.8736(7) 0.3948(6) 0.035(2) Uani 1 1 d . . . H34 H 1.1382 0.8645 0.3327 0.042 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.0148(2) 0.0092(2) 0.0099(2) 0.00273(14) -0.00790(16) -0.00424(15) Tb2 0.0149(2) 0.0092(2) 0.0093(2) 0.00347(14) -0.00785(15) -0.00472(15) Cu1 0.0445(6) 0.0358(6) 0.0374(6) 0.0089(5) -0.0223(6) -0.0288(5) Cu2 0.0461(7) 0.0315(6) 0.0454(7) 0.0072(5) -0.0262(6) -0.0267(5) N1 0.013(3) 0.013(3) 0.018(3) 0.003(3) -0.010(3) -0.004(2) N2 0.018(3) 0.007(3) 0.026(4) 0.000(3) -0.012(3) -0.005(3) N3 0.038(4) 0.029(4) 0.026(4) 0.009(3) -0.013(3) -0.025(3) N4 0.027(4) 0.016(3) 0.033(4) 0.000(3) -0.010(3) -0.012(3) N5 0.033(4) 0.028(4) 0.024(4) 0.003(3) -0.011(3) -0.020(3) N6 0.033(4) 0.025(4) 0.034(4) 0.004(3) -0.020(3) -0.016(3) O1 0.022(3) 0.014(3) 0.017(3) 0.004(2) -0.005(2) -0.004(2) O2 0.045(4) 0.033(3) 0.024(3) 0.017(3) -0.015(3) -0.020(3) O3 0.030(3) 0.015(3) 0.014(3) 0.001(2) -0.005(2) -0.007(2) O4 0.085(5) 0.027(4) 0.025(4) -0.011(3) 0.014(4) -0.008(4) O5 0.024(3) 0.018(3) 0.015(3) 0.010(2) -0.011(2) -0.009(2) O6 0.043(4) 0.036(3) 0.026(3) 0.022(3) -0.020(3) -0.023(3) O7 0.028(3) 0.019(3) 0.015(3) -0.002(2) -0.001(2) -0.008(2) O8 0.073(5) 0.042(4) 0.022(4) -0.015(3) 0.019(4) -0.007(4) O9 0.021(3) 0.020(3) 0.023(3) 0.012(2) -0.013(2) -0.013(2) O10 0.018(3) 0.016(3) 0.018(3) 0.007(2) -0.012(2) -0.005(2) O11 0.024(3) 0.021(3) 0.017(3) 0.002(2) -0.012(2) -0.011(2) O12 0.013(2) 0.014(3) 0.020(3) 0.002(2) -0.008(2) -0.001(2) O13 0.032(3) 0.022(3) 0.019(3) 0.002(2) -0.015(2) -0.013(2) O14 0.017(3) 0.011(3) 0.024(3) 0.002(2) -0.010(2) -0.002(2) O15 0.024(3) 0.019(3) 0.028(3) 0.012(2) -0.015(3) -0.013(2) O16 0.021(3) 0.013(3) 0.024(3) 0.008(2) -0.015(2) -0.004(2) O17 0.033(3) 0.026(3) 0.021(3) -0.001(2) -0.013(3) -0.012(3) O18 0.030(3) 0.019(3) 0.015(3) 0.001(2) -0.007(2) -0.012(2) O19 0.063(5) 0.071(5) 0.037(4) 0.001(4) -0.017(4) -0.023(4) O20 0.073(6) 0.078(6) 0.034(4) -0.005(4) -0.014(4) 0.009(5) S1 0.0145(9) 0.0116(8) 0.0119(9) 0.0046(7) -0.0088(8) -0.0062(7) S2 0.0151(9) 0.0093(8) 0.0144(9) 0.0043(7) -0.0100(8) -0.0049(7) C1 0.023(4) 0.024(4) 0.017(4) 0.010(4) -0.008(3) -0.014(4) C2 0.020(4) 0.014(4) 0.031(5) 0.009(3) -0.019(4) -0.010(3) C3 0.028(4) 0.019(4) 0.039(5) 0.013(4) -0.024(4) -0.012(4) C4 0.031(4) 0.011(4) 0.052(6) 0.004(4) -0.029(4) -0.011(4) C5 0.031(4) 0.012(4) 0.041(5) -0.011(4) -0.024(4) -0.003(3) C6 0.023(4) 0.020(4) 0.024(4) 0.006(3) -0.018(4) -0.010(3) C7 0.025(4) 0.026(5) 0.019(4) -0.004(4) 0.000(4) -0.005(4) C8 0.025(4) 0.021(4) 0.026(4) 0.018(4) -0.016(4) -0.018(4) C9 0.023(4) 0.011(4) 0.030(5) 0.005(3) -0.014(4) -0.008(3) C10 0.028(4) 0.014(4) 0.045(5) 0.010(4) -0.023(4) -0.010(3) C11 0.028(5) 0.011(4) 0.065(7) -0.001(4) -0.028(5) -0.006(4) C12 0.021(4) 0.017(4) 0.038(5) -0.012(4) -0.014(4) -0.003(3) C13 0.022(4) 0.017(4) 0.031(5) -0.004(4) -0.017(4) -0.006(3) C14 0.026(4) 0.023(4) 0.023(5) 0.001(4) -0.010(4) -0.007(4) C15 0.046(5) 0.045(6) 0.023(5) 0.000(4) -0.006(4) -0.034(5) C16 0.046(5) 0.044(5) 0.014(4) 0.001(4) -0.007(4) -0.030(5) C17 0.038(5) 0.021(4) 0.023(4) 0.004(3) -0.015(4) -0.019(4) C18 0.043(5) 0.050(6) 0.019(4) 0.005(4) -0.013(4) -0.034(5) C19 0.053(6) 0.038(5) 0.023(5) -0.001(4) -0.011(4) -0.032(5) C20 0.027(4) 0.030(5) 0.021(4) -0.002(4) -0.008(4) -0.014(4) C21 0.036(5) 0.031(5) 0.023(4) 0.004(4) -0.013(4) -0.022(4) C22 0.022(4) 0.020(4) 0.020(4) -0.004(3) -0.007(4) -0.009(3) C23 0.031(5) 0.036(5) 0.025(4) 0.001(4) -0.013(4) -0.021(4) C24 0.034(5) 0.037(5) 0.022(4) 0.008(4) -0.015(4) -0.022(4) C25 0.052(6) 0.038(5) 0.027(5) -0.001(4) -0.010(5) -0.031(5) C26 0.033(5) 0.032(5) 0.022(4) -0.002(4) -0.003(4) -0.022(4) C27 0.025(4) 0.016(4) 0.022(4) 0.002(3) -0.011(4) -0.006(3) C28 0.038(5) 0.032(5) 0.018(4) -0.010(4) -0.001(4) -0.022(4) C29 0.033(5) 0.047(6) 0.021(5) -0.005(4) -0.003(4) -0.022(4) C30 0.036(5) 0.036(5) 0.022(4) 0.006(4) -0.009(4) -0.028(4) C31 0.051(5) 0.041(5) 0.018(4) 0.006(4) -0.016(4) -0.032(5) C32 0.030(4) 0.026(4) 0.017(4) -0.001(4) -0.010(4) -0.013(4) C33 0.070(7) 0.040(5) 0.025(5) 0.013(4) -0.025(5) -0.040(5) C34 0.061(6) 0.044(5) 0.025(5) 0.012(4) -0.027(5) -0.037(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O1 2.347(5) . ? Tb1 O3 2.361(5) . ? Tb1 O16 2.393(5) 2_675 ? Tb1 O17 2.394(5) . ? Tb1 O14 2.466(5) . ? Tb1 O9 2.474(5) . ? Tb1 N1 2.475(5) . ? Tb1 O13 2.560(5) . ? Tb1 O10 2.700(5) . ? Tb1 H35 2.5207 . ? Tb2 O5 2.333(5) . ? Tb2 O7 2.355(5) . ? Tb2 O10 2.372(5) 2_775 ? Tb2 O18 2.411(5) . ? Tb2 O12 2.460(5) . ? Tb2 O15 2.461(5) 1_655 ? Tb2 N2 2.470(5) . ? Tb2 O11 2.557(5) . ? Tb2 O16 2.732(5) 1_655 ? Tb2 S2 3.2140(17) 1_655 ? Tb2 H37 2.5253 . ? Cu1 N3 1.907(6) . ? Cu1 N4 1.912(6) . ? Cu1 O2 2.270(6) . ? Cu2 N6 1.912(6) . ? Cu2 N5 1.924(6) . ? Cu2 O6 2.308(6) . ? N1 C6 1.323(9) . ? N1 C2 1.341(9) . ? N2 C13 1.328(9) . ? N2 C9 1.351(9) . ? N3 C19 1.341(10) . ? N3 C15 1.348(10) . ? N4 C24 1.331(10) . ? N4 C20 1.363(10) . ? N5 C25 1.328(10) . ? N5 C29 1.341(10) . ? N6 C30 1.337(10) . ? N6 C34 1.338(10) . ? O1 C1 1.276(9) . ? O2 C1 1.241(9) . ? O3 C7 1.273(9) . ? O4 C7 1.218(9) . ? O5 C8 1.278(8) . ? O6 C8 1.248(9) . ? O7 C14 1.282(9) . ? O8 C14 1.218(9) . ? O9 S1 1.475(5) . ? O10 S1 1.491(5) . ? O10 Tb2 2.372(5) 2_775 ? O11 S1 1.467(5) . ? O12 S1 1.474(5) . ? O13 S2 1.467(5) . ? O14 S2 1.476(5) . ? O15 S2 1.469(5) . ? O15 Tb2 2.461(5) 1_455 ? O16 S2 1.484(5) . ? O16 Tb1 2.393(5) 2_675 ? O16 Tb2 2.732(5) 1_455 ? O17 H35 0.8503 . ? O17 H36 0.8503 . ? O18 H37 0.8504 . ? O18 H38 0.8503 . ? O19 H39 0.8501 . ? O19 H40 0.8501 . ? O20 H41 0.8500 . ? O20 H42 0.8500 . ? S2 Tb2 3.2140(17) 1_455 ? C1 C2 1.500(10) . ? C2 C3 1.406(10) . ? C3 C4 1.397(12) . ? C3 H3 0.9300 . ? C4 C5 1.369(11) . ? C4 H4 0.9300 . ? C5 C6 1.398(10) . ? C5 H5 0.9300 . ? C6 C7 1.523(10) . ? C8 C9 1.491(10) . ? C9 C10 1.392(10) . ? C10 C11 1.401(12) . ? C10 H10 0.9300 . ? C11 C12 1.366(12) . ? C11 H11 0.9300 . ? C12 C13 1.399(10) . ? C12 H12 0.9300 . ? C13 C14 1.501(11) . ? C15 C16 1.369(10) . ? C15 H15 0.9300 . ? C16 C17 1.403(10) . ? C16 H16 0.9300 . ? C17 C18 1.379(11) . ? C17 C32 1.480(10) 2_776 ? C18 C19 1.388(10) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.374(10) . ? C20 H20 0.9300 . ? C21 C22 1.381(10) . ? C21 H21 0.9300 . ? C22 C23 1.377(10) . ? C22 C27 1.494(10) 2_666 ? C23 C24 1.370(10) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.371(10) . ? C25 H25 0.9300 . ? C26 C27 1.403(10) . ? C26 H26 0.9300 . ? C27 C28 1.379(10) . ? C27 C22 1.494(10) 2_666 ? C28 C29 1.365(10) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.367(10) . ? C30 H30 0.9300 . ? C31 C32 1.390(10) . ? C31 H31 0.9300 . ? C32 C33 1.378(11) . ? C32 C17 1.480(10) 2_776 ? C33 C34 1.373(10) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Tb1 O3 129.86(16) . . ? O1 Tb1 O16 153.82(17) . 2_675 ? O3 Tb1 O16 74.13(17) . 2_675 ? O1 Tb1 O17 84.27(17) . . ? O3 Tb1 O17 141.82(17) . . ? O16 Tb1 O17 77.58(18) 2_675 . ? O1 Tb1 O14 91.38(17) . . ? O3 Tb1 O14 76.14(17) . . ? O16 Tb1 O14 84.36(16) 2_675 . ? O17 Tb1 O14 125.95(17) . . ? O1 Tb1 O9 75.91(16) . . ? O3 Tb1 O9 90.53(18) . . ? O16 Tb1 O9 118.96(16) 2_675 . ? O17 Tb1 O9 81.21(17) . . ? O14 Tb1 O9 149.22(16) . . ? O1 Tb1 N1 65.55(18) . . ? O3 Tb1 N1 64.31(18) . . ? O16 Tb1 N1 136.64(18) 2_675 . ? O17 Tb1 N1 144.94(19) . . ? O14 Tb1 N1 74.55(17) . . ? O9 Tb1 N1 74.67(17) . . ? O1 Tb1 O13 75.39(17) . . ? O3 Tb1 O13 127.30(17) . . ? O16 Tb1 O13 81.00(16) 2_675 . ? O17 Tb1 O13 71.44(17) . . ? O14 Tb1 O13 55.51(15) . . ? O9 Tb1 O13 141.87(16) . . ? N1 Tb1 O13 114.45(16) . . ? O1 Tb1 O10 126.63(16) . . ? O3 Tb1 O10 72.15(16) . . ? O16 Tb1 O10 65.50(16) 2_675 . ? O17 Tb1 O10 73.04(16) . . ? O14 Tb1 O10 140.89(15) . . ? O9 Tb1 O10 53.62(15) . . ? N1 Tb1 O10 110.22(16) . . ? O13 Tb1 O10 135.31(14) . . ? O1 Tb1 H35 98.1 . . ? O3 Tb1 H35 131.9 . . ? O16 Tb1 H35 60.2 2_675 . ? O17 Tb1 H35 19.7 . . ? O14 Tb1 H35 111.4 . . ? O9 Tb1 H35 98.2 . . ? N1 Tb1 H35 163.1 . . ? O13 Tb1 H35 62.0 . . ? O10 Tb1 H35 75.6 . . ? O5 Tb2 O7 129.75(17) . . ? O5 Tb2 O10 151.49(17) . 2_775 ? O7 Tb2 O10 75.88(17) . 2_775 ? O5 Tb2 O18 83.81(17) . . ? O7 Tb2 O18 142.48(16) . . ? O10 Tb2 O18 77.35(17) 2_775 . ? O5 Tb2 O12 88.26(17) . . ? O7 Tb2 O12 78.25(17) . . ? O10 Tb2 O12 85.35(16) 2_775 . ? O18 Tb2 O12 125.04(16) . . ? O5 Tb2 O15 78.26(16) . 1_655 ? O7 Tb2 O15 90.52(18) . 1_655 ? O10 Tb2 O15 118.30(16) 2_775 1_655 ? O18 Tb2 O15 79.58(17) . 1_655 ? O12 Tb2 O15 150.74(16) . 1_655 ? O5 Tb2 N2 65.21(18) . . ? O7 Tb2 N2 64.57(19) . . ? O10 Tb2 N2 138.64(19) 2_775 . ? O18 Tb2 N2 143.16(19) . . ? O12 Tb2 N2 75.60(17) . . ? O15 Tb2 N2 75.17(18) 1_655 . ? O5 Tb2 O11 72.75(16) . . ? O7 Tb2 O11 129.55(17) . . ? O10 Tb2 O11 80.77(16) 2_775 . ? O18 Tb2 O11 70.18(16) . . ? O12 Tb2 O11 55.61(15) . . ? O15 Tb2 O11 139.75(16) 1_655 . ? N2 Tb2 O11 115.16(17) . . ? O5 Tb2 O16 128.25(16) . 1_655 ? O7 Tb2 O16 73.37(16) . 1_655 ? O10 Tb2 O16 65.22(16) 2_775 1_655 ? O18 Tb2 O16 71.75(16) . 1_655 ? O12 Tb2 O16 143.02(15) . 1_655 ? O15 Tb2 O16 53.29(15) 1_655 1_655 ? N2 Tb2 O16 111.53(16) . 1_655 ? O11 Tb2 O16 133.27(14) . 1_655 ? O5 Tb2 S2 102.89(13) . 1_655 ? O7 Tb2 S2 80.92(14) . 1_655 ? O10 Tb2 S2 92.54(12) 2_775 1_655 ? O18 Tb2 S2 74.49(12) . 1_655 ? O12 Tb2 S2 158.95(11) . 1_655 ? O15 Tb2 S2 25.90(11) 1_655 1_655 ? N2 Tb2 S2 92.74(13) . 1_655 ? O11 Tb2 S2 144.67(11) . 1_655 ? O16 Tb2 S2 27.40(10) 1_655 1_655 ? O5 Tb2 H37 97.0 . . ? O7 Tb2 H37 133.1 . . ? O10 Tb2 H37 60.0 2_775 . ? O18 Tb2 H37 19.7 . . ? O12 Tb2 H37 111.0 . . ? O15 Tb2 H37 96.5 1_655 . ? N2 Tb2 H37 161.4 . . ? O11 Tb2 H37 60.9 . . ? O16 Tb2 H37 74.2 1_655 . ? S2 Tb2 H37 85.6 1_655 . ? N3 Cu1 N4 160.2(3) . . ? N3 Cu1 O2 107.2(3) . . ? N4 Cu1 O2 92.4(2) . . ? N6 Cu2 N5 161.0(3) . . ? N6 Cu2 O6 103.8(2) . . ? N5 Cu2 O6 95.0(2) . . ? C6 N1 C2 120.5(6) . . ? C6 N1 Tb1 120.9(5) . . ? C2 N1 Tb1 118.6(5) . . ? C13 N2 C9 121.0(6) . . ? C13 N2 Tb2 120.2(5) . . ? C9 N2 Tb2 118.8(5) . . ? C19 N3 C15 117.4(7) . . ? C19 N3 Cu1 122.0(6) . . ? C15 N3 Cu1 120.6(5) . . ? C24 N4 C20 117.3(6) . . ? C24 N4 Cu1 119.7(5) . . ? C20 N4 Cu1 122.4(6) . . ? C25 N5 C29 116.3(7) . . ? C25 N5 Cu2 123.6(6) . . ? C29 N5 Cu2 120.1(5) . . ? C30 N6 C34 117.5(7) . . ? C30 N6 Cu2 121.6(5) . . ? C34 N6 Cu2 120.9(6) . . ? C1 O1 Tb1 124.2(5) . . ? C1 O2 Cu1 114.5(5) . . ? C7 O3 Tb1 126.7(5) . . ? C8 O5 Tb2 125.6(5) . . ? C8 O6 Cu2 124.4(5) . . ? C14 O7 Tb2 126.3(5) . . ? S1 O9 Tb1 106.1(3) . . ? S1 O10 Tb2 148.5(3) . 2_775 ? S1 O10 Tb1 95.8(2) . . ? Tb2 O10 Tb1 115.58(18) 2_775 . ? S1 O11 Tb2 97.4(2) . . ? S1 O12 Tb2 101.4(2) . . ? S2 O13 Tb1 97.6(2) . . ? S2 O14 Tb1 101.4(2) . . ? S2 O15 Tb2 107.0(3) . 1_455 ? S2 O16 Tb1 151.4(3) . 2_675 ? S2 O16 Tb2 94.7(2) . 1_455 ? Tb1 O16 Tb2 113.71(18) 2_675 1_455 ? Tb1 O17 H35 88.6 . . ? Tb1 O17 H36 118.5 . . ? H35 O17 H36 98.8 . . ? Tb2 O18 H37 87.8 . . ? Tb2 O18 H38 114.3 . . ? H37 O18 H38 98.2 . . ? H39 O19 H40 103.7 . . ? H41 O20 H42 105.4 . . ? O11 S1 O12 105.6(3) . . ? O11 S1 O9 113.7(3) . . ? O12 S1 O9 110.9(3) . . ? O11 S1 O10 111.5(3) . . ? O12 S1 O10 111.0(3) . . ? O9 S1 O10 104.3(3) . . ? O13 S2 O15 113.3(3) . . ? O13 S2 O14 105.4(3) . . ? O15 S2 O14 111.1(3) . . ? O13 S2 O16 112.0(3) . . ? O15 S2 O16 105.0(3) . . ? O14 S2 O16 110.2(3) . . ? O13 S2 Tb2 130.1(2) . 1_455 ? O15 S2 Tb2 47.1(2) . 1_455 ? O14 S2 Tb2 124.2(2) . 1_455 ? O16 S2 Tb2 57.92(19) . 1_455 ? O2 C1 O1 125.6(7) . . ? O2 C1 C2 118.8(7) . . ? O1 C1 C2 115.6(6) . . ? N1 C2 C3 120.6(7) . . ? N1 C2 C1 114.1(6) . . ? C3 C2 C1 125.3(7) . . ? C4 C3 C2 118.3(7) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C5 C4 C3 120.0(7) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 118.3(8) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? N1 C6 C5 122.1(7) . . ? N1 C6 C7 113.2(6) . . ? C5 C6 C7 124.4(7) . . ? O4 C7 O3 126.0(8) . . ? O4 C7 C6 119.5(7) . . ? O3 C7 C6 114.4(6) . . ? O6 C8 O5 125.6(7) . . ? O6 C8 C9 119.1(7) . . ? O5 C8 C9 115.3(6) . . ? N2 C9 C10 121.1(7) . . ? N2 C9 C8 114.0(6) . . ? C10 C9 C8 124.9(7) . . ? C9 C10 C11 117.8(8) . . ? C9 C10 H10 121.1 . . ? C11 C10 H10 121.1 . . ? C12 C11 C10 120.1(7) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 119.3(8) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? N2 C13 C12 120.7(8) . . ? N2 C13 C14 114.2(6) . . ? C12 C13 C14 125.0(7) . . ? O8 C14 O7 125.4(8) . . ? O8 C14 C13 120.1(7) . . ? O7 C14 C13 114.5(7) . . ? N3 C15 C16 123.2(7) . . ? N3 C15 H15 118.4 . . ? C16 C15 H15 118.4 . . ? C15 C16 C17 119.7(7) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 117.0(7) . . ? C18 C17 C32 121.8(7) . 2_776 ? C16 C17 C32 121.2(7) . 2_776 ? C17 C18 C19 120.2(7) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? N3 C19 C18 122.5(7) . . ? N3 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? N4 C20 C21 121.8(7) . . ? N4 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C20 C21 C22 120.4(8) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C23 C22 C21 117.3(7) . . ? C23 C22 C27 121.5(7) . 2_666 ? C21 C22 C27 121.1(7) . 2_666 ? C24 C23 C22 120.1(8) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? N4 C24 C23 123.2(8) . . ? N4 C24 H24 118.4 . . ? C23 C24 H24 118.4 . . ? N5 C25 C26 124.2(8) . . ? N5 C25 H25 117.9 . . ? C26 C25 H25 117.9 . . ? C25 C26 C27 118.5(7) . . ? C25 C26 H26 120.7 . . ? C27 C26 H26 120.7 . . ? C28 C27 C26 117.6(7) . . ? C28 C27 C22 120.7(7) . 2_666 ? C26 C27 C22 121.6(7) . 2_666 ? C29 C28 C27 119.1(7) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? N5 C29 C28 124.2(8) . . ? N5 C29 H29 117.9 . . ? C28 C29 H29 117.9 . . ? N6 C30 C31 122.3(7) . . ? N6 C30 H30 118.9 . . ? C31 C30 H30 118.9 . . ? C30 C31 C32 121.0(8) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C33 C32 C31 115.9(7) . . ? C33 C32 C17 122.9(7) . 2_776 ? C31 C32 C17 121.2(7) . 2_776 ? C34 C33 C32 120.6(8) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? N6 C34 C33 122.7(8) . . ? N6 C34 H34 118.6 . . ? C33 C34 H34 118.6 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.332 _refine_diff_density_min -3.355 _refine_diff_density_rms 0.282