# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Yue, Shantang' _publ_contact_author_email yuesht@scnu.edu.cn _publ_section_title ; A new family of 3D heterometallic 3d-4f organodisulfonate complexes based on the linkages of 2D [Ln(nds)(H2O)]+ layers and [Cu(ina)2]- chains ; loop_ _publ_author_name 'Wenjing Liu' 'Zhaoyang Li' 'Ning Wang' 'Xiaoxu Li' 'Zhiqiang Wei' ; Shantang Yue ; 'Yingliang Liu' # Attachment 'ce.cif' data_ce _database_code_depnum_ccdc_archive 'CCDC 768848' #TrackingRef 'ce.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H16 Ce Cu N2 O11 S2' _chemical_formula_sum 'C22 H16 Ce Cu N2 O11 S2' _chemical_formula_weight 752.18 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' Ce Ce -0.2486 2.6331 '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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5770(9) _cell_length_b 11.5117(11) _cell_length_c 12.3980(19) _cell_angle_alpha 99.6810(10) _cell_angle_beta 100.1280(10) _cell_angle_gamma 114.1460(10) _cell_volume 1183.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5608 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.83 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 738 _exptl_absorpt_coefficient_mu 3.043 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.487 _exptl_absorpt_correction_T_max 0.544 _exptl_absorpt_process_details SADABS,Bruker(2002) _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 11420 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4263 _reflns_number_gt 3910 _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 ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+1.0206P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4263 _refine_ls_number_parameters 352 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0551 _refine_ls_wR_factor_gt 0.0532 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 Ce1 Ce 0.31172(2) 0.467353(16) 0.097404(14) 0.01769(6) Uani 1 1 d . . . Cu1 Cu 0.26868(6) -0.02559(5) 0.59342(4) 0.04449(13) Uani 1 1 d . . . S2 S 0.30176(9) 0.22333(7) -0.14935(6) 0.02158(17) Uani 1 1 d . . . S1 S 0.21404(10) 0.71833(9) 0.27867(7) 0.02898(19) Uani 1 1 d . . . O3 O 0.1810(3) 0.2788(2) 0.1766(2) 0.0432(7) Uani 1 1 d . . . O2 O 0.3785(3) 0.4501(2) 0.30652(19) 0.0327(6) Uani 1 1 d . . . O1 O 0.2299(3) 0.6144(2) 0.2027(2) 0.0395(6) Uani 1 1 d . . . O4 O 0.2357(3) 0.2857(2) -0.07438(18) 0.0274(5) Uani 1 1 d . . . O9 O 0.1197(3) 0.7685(2) 0.2150(2) 0.0372(6) Uani 1 1 d . . . O10 O 0.3635(3) 0.8194(3) 0.3517(2) 0.0516(7) Uani 1 1 d . . . O5 O 0.5362(3) 0.4127(2) 0.1062(2) 0.0317(5) Uani 1 1 d . . . O7 O 0.4451(3) 0.3210(2) -0.16764(19) 0.0275(5) Uani 1 1 d . . . O8 O 0.1864(3) 0.1360(2) -0.25412(19) 0.0337(6) Uani 1 1 d . . . N1 N 0.2556(3) 0.0843(3) 0.4997(2) 0.0294(6) Uani 1 1 d . . . N2 N 0.7157(4) 0.1450(3) 0.3243(2) 0.0328(7) Uani 1 1 d . . . C20 C -0.1350(4) 0.5606(4) 0.4286(3) 0.0380(9) Uani 1 1 d . . . H20 H -0.2349 0.5558 0.4262 0.046 Uiso 1 1 calc R . . C19 C -0.0472(4) 0.6299(4) 0.3639(3) 0.0363(9) Uani 1 1 d . . . H19 H -0.0864 0.6728 0.3192 0.044 Uiso 1 1 calc R . . C18 C 0.1024(4) 0.6351(3) 0.3661(3) 0.0304(8) Uani 1 1 d . . . C22 C 0.1635(4) 0.5741(4) 0.4327(3) 0.0328(8) Uani 1 1 d . . . H22 H 0.2629 0.5790 0.4329 0.039 Uiso 1 1 calc R . . C21 C -0.0764(4) 0.4964(4) 0.4987(3) 0.0306(8) Uani 1 1 d . . . C8 C 0.5677(4) 0.2478(4) 0.2448(3) 0.0392(9) Uani 1 1 d . . . H8 H 0.4777 0.2615 0.2379 0.047 Uiso 1 1 calc R . . C11 C 0.5896(5) 0.1683(4) 0.3105(3) 0.0457(10) Uani 1 1 d . . . H11 H 0.5126 0.1291 0.3470 0.055 Uiso 1 1 calc R . . C10 C 0.8251(4) 0.2041(4) 0.2720(3) 0.0376(9) Uani 1 1 d . . . H10 H 0.9150 0.1901 0.2814 0.045 Uiso 1 1 calc R . . C9 C 0.8109(4) 0.2848(4) 0.2048(3) 0.0334(8) Uani 1 1 d . . . H9 H 0.8902 0.3241 0.1701 0.040 Uiso 1 1 calc R . . C3 C 0.4982(4) 0.1161(3) -0.0875(3) 0.0251(7) Uani 1 1 d . . . H3 H 0.5581 0.1630 -0.1310 0.030 Uiso 1 1 calc R . . C2 C 0.5469(4) 0.0354(3) -0.0329(3) 0.0259(7) Uani 1 1 d . . . C1 C 0.6868(4) 0.0237(3) -0.0412(3) 0.0319(8) Uani 1 1 d . . . H1 H 0.7491 0.0705 -0.0835 0.038 Uiso 1 1 calc R . . C5 C 0.2691(4) 0.0550(3) -0.0119(3) 0.0306(8) Uani 1 1 d . . . H5 H 0.1774 0.0622 -0.0057 0.037 Uiso 1 1 calc R . . C4 C 0.3633(4) 0.1257(3) -0.0766(3) 0.0240(7) Uani 1 1 d . . . C13 C 0.3505(4) 0.2149(3) 0.5362(3) 0.0299(8) Uani 1 1 d . . . H13 H 0.4128 0.2507 0.6112 0.036 Uiso 1 1 calc R . . C14 C 0.3593(4) 0.2978(3) 0.4669(3) 0.0269(7) Uani 1 1 d . . . H14 H 0.4280 0.3876 0.4943 0.032 Uiso 1 1 calc R . . C16 C 0.2647(4) 0.2461(3) 0.3559(3) 0.0229(7) Uani 1 1 d . . . C15 C 0.1639(4) 0.1119(3) 0.3191(3) 0.0285(7) Uani 1 1 d . . . H15 H 0.0969 0.0744 0.2455 0.034 Uiso 1 1 calc R . . C12 C 0.1639(4) 0.0349(3) 0.3925(3) 0.0312(8) Uani 1 1 d . . . H12 H 0.0973 -0.0555 0.3665 0.037 Uiso 1 1 calc R . . C7 C 0.6786(4) 0.3070(3) 0.1892(3) 0.0222(7) Uani 1 1 d . . . C6 C 0.6524(4) 0.3877(3) 0.1111(3) 0.0219(7) Uani 1 1 d . . . C17 C 0.2744(4) 0.3320(3) 0.2756(3) 0.0256(7) Uani 1 1 d . . . O6 O 0.7472(3) 0.4228(2) 0.05054(19) 0.0301(5) Uani 1 1 d . . . O1W O 0.0165(3) 0.3703(2) 0.00973(19) 0.0312(5) Uani 1 1 d D . . H2W H -0.0269 0.3225 -0.0554 0.047 Uiso 1 1 d RD . . H1W H -0.0478 0.3950 0.0262 0.047 Uiso 1 1 d RD . . 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 Ce1 0.02104(10) 0.01930(10) 0.01892(10) 0.01049(7) 0.00748(7) 0.01210(8) Cu1 0.0586(3) 0.0415(3) 0.0436(3) 0.0319(2) 0.0113(2) 0.0256(3) S2 0.0225(4) 0.0186(4) 0.0239(4) 0.0058(3) 0.0054(3) 0.0099(3) S1 0.0323(5) 0.0336(5) 0.0271(4) 0.0084(4) 0.0105(4) 0.0195(4) O3 0.0413(15) 0.0422(16) 0.0320(14) 0.0237(12) -0.0040(12) 0.0060(13) O2 0.0447(15) 0.0236(13) 0.0313(13) 0.0148(10) 0.0107(11) 0.0139(12) O1 0.0578(17) 0.0455(16) 0.0386(14) 0.0157(12) 0.0299(13) 0.0370(14) O4 0.0298(13) 0.0274(12) 0.0293(12) 0.0052(10) 0.0071(10) 0.0184(11) O9 0.0456(15) 0.0447(15) 0.0341(14) 0.0142(12) 0.0127(12) 0.0303(13) O10 0.0370(15) 0.0520(18) 0.0502(17) 0.0124(14) 0.0034(13) 0.0092(14) O5 0.0328(13) 0.0306(13) 0.0399(14) 0.0113(11) 0.0059(11) 0.0228(11) O7 0.0269(12) 0.0234(12) 0.0339(13) 0.0120(10) 0.0096(10) 0.0106(10) O8 0.0322(13) 0.0299(13) 0.0296(13) 0.0019(11) 0.0033(11) 0.0093(11) N1 0.0359(16) 0.0288(16) 0.0294(16) 0.0151(13) 0.0080(13) 0.0177(14) N2 0.0435(18) 0.0332(17) 0.0338(16) 0.0227(14) 0.0142(14) 0.0221(15) C20 0.036(2) 0.056(2) 0.038(2) 0.0162(19) 0.0172(17) 0.0315(19) C19 0.040(2) 0.050(2) 0.036(2) 0.0168(18) 0.0165(17) 0.0315(19) C18 0.0332(19) 0.038(2) 0.0256(18) 0.0058(15) 0.0110(15) 0.0206(17) C22 0.0333(19) 0.044(2) 0.0299(19) 0.0097(16) 0.0135(16) 0.0240(18) C21 0.0327(19) 0.039(2) 0.0291(18) 0.0085(16) 0.0114(15) 0.0234(17) C8 0.042(2) 0.052(2) 0.057(2) 0.037(2) 0.0340(19) 0.035(2) C11 0.060(3) 0.056(3) 0.056(3) 0.046(2) 0.042(2) 0.037(2) C10 0.035(2) 0.049(2) 0.047(2) 0.0301(19) 0.0137(17) 0.0279(19) C9 0.0300(19) 0.041(2) 0.046(2) 0.0293(18) 0.0195(17) 0.0213(17) C3 0.0280(17) 0.0193(16) 0.0324(18) 0.0097(14) 0.0134(15) 0.0118(14) C2 0.0289(18) 0.0201(17) 0.0324(18) 0.0090(14) 0.0137(15) 0.0116(15) C1 0.0306(19) 0.0297(19) 0.047(2) 0.0206(17) 0.0222(17) 0.0166(16) C5 0.0282(18) 0.0300(19) 0.044(2) 0.0173(16) 0.0170(16) 0.0170(16) C4 0.0257(17) 0.0161(16) 0.0290(18) 0.0062(13) 0.0060(14) 0.0089(14) C13 0.036(2) 0.0309(19) 0.0234(17) 0.0094(15) 0.0055(15) 0.0155(16) C14 0.0327(19) 0.0210(17) 0.0277(18) 0.0088(14) 0.0086(15) 0.0120(15) C16 0.0250(17) 0.0278(18) 0.0251(17) 0.0142(14) 0.0115(14) 0.0160(15) C15 0.0316(19) 0.0280(18) 0.0253(17) 0.0102(15) 0.0042(15) 0.0129(16) C12 0.0323(19) 0.0251(18) 0.036(2) 0.0128(16) 0.0064(16) 0.0117(16) C7 0.0291(17) 0.0195(16) 0.0231(16) 0.0098(13) 0.0096(14) 0.0132(14) C6 0.0250(17) 0.0180(16) 0.0209(16) 0.0049(13) 0.0005(13) 0.0104(14) C17 0.0297(18) 0.0313(19) 0.0271(18) 0.0179(15) 0.0138(15) 0.0183(16) O6 0.0318(13) 0.0345(13) 0.0311(13) 0.0213(11) 0.0118(11) 0.0156(11) O1W 0.0242(12) 0.0405(14) 0.0322(13) 0.0118(11) 0.0078(10) 0.0169(11) _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 Ce1 O1 2.426(2) . ? Ce1 O7 2.459(2) 2_665 ? Ce1 O5 2.465(2) . ? Ce1 O4 2.480(2) . ? Ce1 O3 2.484(2) . ? Ce1 O6 2.506(2) 2_665 ? Ce1 O1W 2.520(2) . ? Ce1 O2 2.620(2) . ? Cu1 N1 1.882(3) . ? Cu1 N2 1.881(3) 2_656 ? S2 O8 1.437(2) . ? S2 O7 1.460(2) . ? S2 O4 1.461(2) . ? S2 C4 1.766(3) . ? S1 O10 1.432(3) . ? S1 O9 1.451(2) . ? S1 O1 1.470(2) . ? S1 C18 1.776(3) . ? O3 C17 1.263(4) . ? O2 C17 1.253(4) . ? O5 C6 1.253(4) . ? O7 Ce1 2.459(2) 2_665 ? N1 C12 1.337(4) . ? N1 C13 1.341(4) . ? N2 C11 1.330(5) . ? N2 C10 1.336(4) . ? N2 Cu1 1.881(3) 2_656 ? C20 C19 1.375(5) . ? C20 C21 1.414(5) . ? C20 H20 0.9300 . ? C19 C18 1.404(5) . ? C19 H19 0.9300 . ? C18 C22 1.371(5) . ? C22 C21 1.415(5) 2_566 ? C22 H22 0.9300 . ? C21 C22 1.415(5) 2_566 ? C21 C21 1.427(6) 2_566 ? C8 C7 1.375(4) . ? C8 C11 1.376(5) . ? C8 H8 0.9300 . ? C11 H11 0.9300 . ? C10 C9 1.378(5) . ? C10 H10 0.9300 . ? C9 C7 1.380(4) . ? C9 H9 0.9300 . ? C3 C4 1.369(4) . ? C3 C2 1.412(4) . ? C3 H3 0.9300 . ? C2 C1 1.419(4) . ? C2 C2 1.421(6) 2_655 ? C1 C5 1.360(5) 2_655 ? C1 H1 0.9300 . ? C5 C1 1.360(5) 2_655 ? C5 C4 1.411(4) . ? C5 H5 0.9300 . ? C13 C14 1.376(4) . ? C13 H13 0.9300 . ? C14 C16 1.383(4) . ? C14 H14 0.9300 . ? C16 C15 1.383(4) . ? C16 C17 1.505(4) . ? C15 C12 1.373(4) . ? C15 H15 0.9300 . ? C12 H12 0.9300 . ? C7 C6 1.508(4) . ? C6 O6 1.262(4) . ? O6 Ce1 2.506(2) 2_665 ? O1W H2W 0.8206 . ? O1W H1W 0.8182 . ? 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 Ce1 O7 76.36(8) . 2_665 ? O1 Ce1 O5 141.34(9) . . ? O7 Ce1 O5 73.73(7) 2_665 . ? O1 Ce1 O4 145.80(8) . . ? O7 Ce1 O4 128.12(7) 2_665 . ? O5 Ce1 O4 72.86(7) . . ? O1 Ce1 O3 95.90(9) . . ? O7 Ce1 O3 135.11(7) 2_665 . ? O5 Ce1 O3 88.47(8) . . ? O4 Ce1 O3 81.92(8) . . ? O1 Ce1 O6 79.53(8) . 2_665 ? O7 Ce1 O6 81.31(7) 2_665 2_665 ? O5 Ce1 O6 118.81(8) . 2_665 ? O4 Ce1 O6 81.39(7) . 2_665 ? O3 Ce1 O6 141.59(8) . 2_665 ? O1 Ce1 O1W 75.23(8) . . ? O7 Ce1 O1W 142.01(7) 2_665 . ? O5 Ce1 O1W 141.59(8) . . ? O4 Ce1 O1W 71.53(7) . . ? O3 Ce1 O1W 72.79(8) . . ? O6 Ce1 O1W 69.16(7) 2_665 . ? O1 Ce1 O2 75.82(8) . . ? O7 Ce1 O2 84.46(7) 2_665 . ? O5 Ce1 O2 77.42(8) . . ? O4 Ce1 O2 124.42(7) . . ? O3 Ce1 O2 51.14(7) . . ? O6 Ce1 O2 153.84(8) 2_665 . ? O1W Ce1 O2 112.06(7) . . ? N1 Cu1 N2 174.65(13) . 2_656 ? O8 S2 O7 112.48(14) . . ? O8 S2 O4 112.86(14) . . ? O7 S2 O4 111.50(13) . . ? O8 S2 C4 107.01(14) . . ? O7 S2 C4 105.91(14) . . ? O4 S2 C4 106.54(14) . . ? O10 S1 O9 113.73(17) . . ? O10 S1 O1 112.92(17) . . ? O9 S1 O1 110.85(15) . . ? O10 S1 C18 107.46(17) . . ? O9 S1 C18 107.01(16) . . ? O1 S1 C18 104.18(15) . . ? C17 O3 Ce1 96.0(2) . . ? C17 O2 Ce1 89.86(19) . . ? S1 O1 Ce1 168.59(17) . . ? S2 O4 Ce1 142.69(13) . . ? C6 O5 Ce1 178.7(2) . . ? S2 O7 Ce1 150.00(14) . 2_665 ? C12 N1 C13 118.0(3) . . ? C12 N1 Cu1 121.7(2) . . ? C13 N1 Cu1 120.0(2) . . ? C11 N2 C10 117.0(3) . . ? C11 N2 Cu1 120.9(2) . 2_656 ? C10 N2 Cu1 122.0(2) . 2_656 ? C19 C20 C21 121.2(3) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C19 C18 119.4(3) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C22 C18 C19 121.3(3) . . ? C22 C18 S1 118.7(3) . . ? C19 C18 S1 120.0(3) . . ? C18 C22 C21 120.5(3) . 2_566 ? C18 C22 H22 119.7 . . ? C21 C22 H22 119.7 2_566 . ? C22 C21 C20 122.4(3) 2_566 . ? C22 C21 C21 118.7(4) 2_566 2_566 ? C20 C21 C21 118.9(4) . 2_566 ? C7 C8 C11 120.1(3) . . ? C7 C8 H8 119.9 . . ? C11 C8 H8 119.9 . . ? N2 C11 C8 123.0(3) . . ? N2 C11 H11 118.5 . . ? C8 C11 H11 118.5 . . ? N2 C10 C9 123.1(3) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? C10 C9 C7 119.7(3) . . ? C10 C9 H9 120.2 . . ? C7 C9 H9 120.2 . . ? C4 C3 C2 120.3(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C2 C1 122.0(3) . . ? C3 C2 C2 118.7(4) . 2_655 ? C1 C2 C2 119.3(4) . 2_655 ? C5 C1 C2 120.9(3) 2_655 . ? C5 C1 H1 119.5 2_655 . ? C2 C1 H1 119.5 . . ? C1 C5 C4 119.6(3) 2_655 . ? C1 C5 H5 120.2 2_655 . ? C4 C5 H5 120.2 . . ? C3 C4 C5 121.2(3) . . ? C3 C4 S2 119.3(2) . . ? C5 C4 S2 119.4(2) . . ? N1 C13 C14 122.4(3) . . ? N1 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C13 C14 C16 119.3(3) . . ? C13 C14 H14 120.4 . . ? C16 C14 H14 120.4 . . ? C15 C16 C14 118.3(3) . . ? C15 C16 C17 120.5(3) . . ? C14 C16 C17 121.2(3) . . ? C12 C15 C16 119.2(3) . . ? C12 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? N1 C12 C15 122.8(3) . . ? N1 C12 H12 118.6 . . ? C15 C12 H12 118.6 . . ? C8 C7 C9 117.0(3) . . ? C8 C7 C6 121.1(3) . . ? C9 C7 C6 121.9(3) . . ? O5 C6 O6 123.3(3) . . ? O5 C6 C7 119.2(3) . . ? O6 C6 C7 117.4(3) . . ? O2 C17 O3 122.6(3) . . ? O2 C17 C16 119.6(3) . . ? O3 C17 C16 117.7(3) . . ? C6 O6 Ce1 118.38(19) . 2_665 ? Ce1 O1W H2W 122.4 . . ? Ce1 O1W H1W 129.9 . . ? H2W O1W H1W 104.7 . . ? 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 Ce1 O3 C17 -70.2(2) . . . . ? O7 Ce1 O3 C17 6.4(3) 2_665 . . . ? O5 Ce1 O3 C17 71.3(2) . . . . ? O4 Ce1 O3 C17 144.2(2) . . . . ? O6 Ce1 O3 C17 -150.76(18) 2_665 . . . ? O1W Ce1 O3 C17 -142.7(2) . . . . ? O2 Ce1 O3 C17 -3.72(18) . . . . ? O1 Ce1 O2 C17 113.6(2) . . . . ? O7 Ce1 O2 C17 -169.11(19) 2_665 . . . ? O5 Ce1 O2 C17 -94.58(19) . . . . ? O4 Ce1 O2 C17 -35.8(2) . . . . ? O3 Ce1 O2 C17 3.73(18) . . . . ? O6 Ce1 O2 C17 133.7(2) 2_665 . . . ? O1W Ce1 O2 C17 46.3(2) . . . . ? O10 S1 O1 Ce1 3.1(8) . . . . ? O9 S1 O1 Ce1 132.0(8) . . . . ? C18 S1 O1 Ce1 -113.2(8) . . . . ? O7 Ce1 O1 S1 -24.2(8) 2_665 . . . ? O5 Ce1 O1 S1 15.9(9) . . . . ? O4 Ce1 O1 S1 -164.8(7) . . . . ? O3 Ce1 O1 S1 110.9(8) . . . . ? O6 Ce1 O1 S1 -107.7(8) 2_665 . . . ? O1W Ce1 O1 S1 -178.7(8) . . . . ? O2 Ce1 O1 S1 63.4(8) . . . . ? O8 S2 O4 Ce1 -165.88(19) . . . . ? O7 S2 O4 Ce1 -38.1(3) . . . . ? C4 S2 O4 Ce1 77.0(2) . . . . ? O1 Ce1 O4 S2 157.20(18) . . . . ? O7 Ce1 O4 S2 28.8(3) 2_665 . . . ? O5 Ce1 O4 S2 -23.3(2) . . . . ? O3 Ce1 O4 S2 -114.2(2) . . . . ? O6 Ce1 O4 S2 100.5(2) 2_665 . . . ? O1W Ce1 O4 S2 171.3(2) . . . . ? O2 Ce1 O4 S2 -84.1(2) . . . . ? O1 Ce1 O5 C6 -50(9) . . . . ? O7 Ce1 O5 C6 -9(9) 2_665 . . . ? O4 Ce1 O5 C6 131(9) . . . . ? O3 Ce1 O5 C6 -147(9) . . . . ? O6 Ce1 O5 C6 61(9) 2_665 . . . ? O1W Ce1 O5 C6 153(9) . . . . ? O2 Ce1 O5 C6 -97(9) . . . . ? O8 S2 O7 Ce1 160.9(2) . . . 2_665 ? O4 S2 O7 Ce1 32.9(3) . . . 2_665 ? C4 S2 O7 Ce1 -82.6(3) . . . 2_665 ? N2 Cu1 N1 C12 47.2(15) 2_656 . . . ? N2 Cu1 N1 C13 -126.6(13) 2_656 . . . ? C21 C20 C19 C18 1.1(6) . . . . ? C20 C19 C18 C22 -1.0(5) . . . . ? C20 C19 C18 S1 177.4(3) . . . . ? O10 S1 C18 C22 -59.7(3) . . . . ? O9 S1 C18 C22 177.8(3) . . . . ? O1 S1 C18 C22 60.3(3) . . . . ? O10 S1 C18 C19 121.9(3) . . . . ? O9 S1 C18 C19 -0.6(3) . . . . ? O1 S1 C18 C19 -118.1(3) . . . . ? C19 C18 C22 C21 0.2(5) . . . 2_566 ? S1 C18 C22 C21 -178.3(3) . . . 2_566 ? C19 C20 C21 C22 179.1(3) . . . 2_566 ? C19 C20 C21 C21 -0.4(6) . . . 2_566 ? C10 N2 C11 C8 0.8(6) . . . . ? Cu1 N2 C11 C8 -175.5(3) 2_656 . . . ? C7 C8 C11 N2 0.3(7) . . . . ? C11 N2 C10 C9 -0.9(6) . . . . ? Cu1 N2 C10 C9 175.4(3) 2_656 . . . ? N2 C10 C9 C7 -0.1(6) . . . . ? C4 C3 C2 C1 -179.4(3) . . . . ? C4 C3 C2 C2 0.2(6) . . . 2_655 ? C3 C2 C1 C5 -179.8(3) . . . 2_655 ? C2 C2 C1 C5 0.6(6) 2_655 . . 2_655 ? C2 C3 C4 C5 -0.6(5) . . . . ? C2 C3 C4 S2 -178.0(2) . . . . ? C1 C5 C4 C3 0.3(5) 2_655 . . . ? C1 C5 C4 S2 177.8(3) 2_655 . . . ? O8 S2 C4 C3 95.4(3) . . . . ? O7 S2 C4 C3 -24.8(3) . . . . ? O4 S2 C4 C3 -143.6(3) . . . . ? O8 S2 C4 C5 -82.1(3) . . . . ? O7 S2 C4 C5 157.7(3) . . . . ? O4 S2 C4 C5 38.9(3) . . . . ? C12 N1 C13 C14 -1.7(5) . . . . ? Cu1 N1 C13 C14 172.3(3) . . . . ? N1 C13 C14 C16 1.4(5) . . . . ? C13 C14 C16 C15 0.2(5) . . . . ? C13 C14 C16 C17 -177.8(3) . . . . ? C14 C16 C15 C12 -1.5(5) . . . . ? C17 C16 C15 C12 176.5(3) . . . . ? C13 N1 C12 C15 0.3(5) . . . . ? Cu1 N1 C12 C15 -173.6(3) . . . . ? C16 C15 C12 N1 1.3(5) . . . . ? C11 C8 C7 C9 -1.3(6) . . . . ? C11 C8 C7 C6 176.2(3) . . . . ? C10 C9 C7 C8 1.2(5) . . . . ? C10 C9 C7 C6 -176.3(3) . . . . ? Ce1 O5 C6 O6 -56(9) . . . . ? Ce1 O5 C6 C7 127(9) . . . . ? C8 C7 C6 O5 7.6(5) . . . . ? C9 C7 C6 O5 -175.0(3) . . . . ? C8 C7 C6 O6 -169.9(3) . . . . ? C9 C7 C6 O6 7.5(5) . . . . ? Ce1 O2 C17 O3 -6.8(3) . . . . ? Ce1 O2 C17 C16 169.3(3) . . . . ? Ce1 O3 C17 O2 7.2(4) . . . . ? Ce1 O3 C17 C16 -169.0(2) . . . . ? C15 C16 C17 O2 -172.2(3) . . . . ? C14 C16 C17 O2 5.8(5) . . . . ? C15 C16 C17 O3 4.2(5) . . . . ? C14 C16 C17 O3 -177.9(3) . . . . ? O5 C6 O6 Ce1 -4.9(4) . . . 2_665 ? C7 C6 O6 Ce1 172.58(19) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.379 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.087 # Attachment 'dy.cif' data_dy _database_code_depnum_ccdc_archive 'CCDC 768849' #TrackingRef 'dy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H16 Cu Dy N2 O11 S2' _chemical_formula_sum 'C22 H16 Cu Dy N2 O11 S2' _chemical_formula_weight 774.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4926(14) _cell_length_b 11.3728(17) _cell_length_c 12.345(3) _cell_angle_alpha 99.253(2) _cell_angle_beta 100.231(2) _cell_angle_gamma 114.0640(10) _cell_volume 1156.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8805 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 754 _exptl_absorpt_coefficient_mu 4.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.364 _exptl_absorpt_correction_T_max 0.417 _exptl_absorpt_process_details SADABS,Bruker(2002) _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 11132 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4166 _reflns_number_gt 3964 _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^)+(0.0213P)^2^+0.7780P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4166 _refine_ls_number_parameters 352 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0209 _refine_ls_R_factor_gt 0.0196 _refine_ls_wR_factor_ref 0.0482 _refine_ls_wR_factor_gt 0.0476 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 0.309515(15) 0.466253(12) 0.095883(10) 0.01594(5) Uani 1 1 d . . . Cu1 Cu 0.25721(6) -0.02290(5) 0.59660(4) 0.04031(12) Uani 1 1 d . . . S2 S 0.30871(8) 0.23428(7) -0.14650(6) 0.01830(15) Uani 1 1 d . . . S1 S 0.21751(9) 0.71247(8) 0.27281(6) 0.02304(16) Uani 1 1 d . . . O3 O 0.1833(3) 0.2810(2) 0.16869(19) 0.0348(6) Uani 1 1 d . . . O2 O 0.3770(3) 0.4540(2) 0.30004(18) 0.0303(5) Uani 1 1 d . . . O1 O 0.2213(3) 0.6033(2) 0.19249(19) 0.0326(5) Uani 1 1 d . . . O4 O 0.2406(2) 0.2963(2) -0.07218(17) 0.0238(5) Uani 1 1 d . . . O9 O 0.1272(3) 0.7703(2) 0.21301(19) 0.0306(5) Uani 1 1 d . . . O10 O 0.3733(3) 0.8086(3) 0.3434(2) 0.0432(6) Uani 1 1 d . . . O5 O 0.5198(3) 0.4090(2) 0.11025(18) 0.0282(5) Uani 1 1 d . . . O7 O 0.4556(2) 0.3320(2) -0.16317(17) 0.0232(4) Uani 1 1 d . . . O8 O 0.1939(3) 0.1487(2) -0.25274(18) 0.0288(5) Uani 1 1 d . . . N1 N 0.2461(3) 0.0860(3) 0.4987(2) 0.0267(6) Uani 1 1 d . . . N2 N 0.7220(3) 0.1434(3) 0.3213(2) 0.0301(6) Uani 1 1 d . . . C20 C -0.1370(4) 0.5572(3) 0.4222(3) 0.0308(7) Uani 1 1 d . . . H20 H -0.2387 0.5513 0.4174 0.037 Uiso 1 1 calc R . . C19 C -0.0473(4) 0.6256(3) 0.3568(3) 0.0286(7) Uani 1 1 d . . . H19 H -0.0869 0.6671 0.3092 0.034 Uiso 1 1 calc R . . C18 C 0.1050(4) 0.6321(3) 0.3628(2) 0.0242(7) Uani 1 1 d . . . C22 C 0.1670(4) 0.5743(3) 0.4345(3) 0.0264(7) Uani 1 1 d . . . H22 H 0.2688 0.5811 0.4379 0.032 Uiso 1 1 calc R . . C21 C -0.0776(4) 0.4954(3) 0.4967(3) 0.0252(7) Uani 1 1 d . . . C8 C 0.5627(4) 0.2419(3) 0.2433(3) 0.0346(8) Uani 1 1 d . . . H8 H 0.4693 0.2519 0.2364 0.042 Uiso 1 1 calc R . . C11 C 0.5909(5) 0.1631(4) 0.3089(3) 0.0405(9) Uani 1 1 d . . . H11 H 0.5154 0.1214 0.3464 0.049 Uiso 1 1 calc R . . C10 C 0.8294(4) 0.2070(4) 0.2677(3) 0.0356(8) Uani 1 1 d . . . H10 H 0.9219 0.1955 0.2757 0.043 Uiso 1 1 calc R . . C9 C 0.8097(4) 0.2885(3) 0.2013(3) 0.0297(7) Uani 1 1 d . . . H9 H 0.8880 0.3312 0.1661 0.036 Uiso 1 1 calc R . . C3 C 0.5010(4) 0.1196(3) -0.0864(3) 0.0235(6) Uani 1 1 d . . . H3 H 0.5613 0.1667 -0.1305 0.028 Uiso 1 1 calc R . . C2 C 0.5489(4) 0.0370(3) -0.0322(3) 0.0223(6) Uani 1 1 d . . . C1 C 0.6889(4) 0.0237(3) -0.0399(3) 0.0291(7) Uani 1 1 d . . . H1 H 0.7533 0.0720 -0.0813 0.035 Uiso 1 1 calc R . . C5 C 0.2688(4) 0.0585(3) -0.0122(3) 0.0268(7) Uani 1 1 d . . . H5 H 0.1765 0.0664 -0.0063 0.032 Uiso 1 1 calc R . . C4 C 0.3663(4) 0.1312(3) -0.0747(2) 0.0207(6) Uani 1 1 d . . . C13 C 0.3404(4) 0.2184(3) 0.5345(3) 0.0270(7) Uani 1 1 d . . . H13 H 0.4003 0.2554 0.6103 0.032 Uiso 1 1 calc R . . C14 C 0.3513(4) 0.3008(3) 0.4632(3) 0.0247(7) Uani 1 1 d . . . H14 H 0.4195 0.3916 0.4903 0.030 Uiso 1 1 calc R . . C16 C 0.2602(3) 0.2479(3) 0.3506(2) 0.0214(6) Uani 1 1 d . . . C15 C 0.1607(4) 0.1121(3) 0.3143(3) 0.0263(7) Uani 1 1 d . . . H15 H 0.0963 0.0734 0.2397 0.032 Uiso 1 1 calc R . . C12 C 0.1581(4) 0.0349(3) 0.3902(3) 0.0278(7) Uani 1 1 d . . . H12 H 0.0925 -0.0565 0.3648 0.033 Uiso 1 1 calc R . . C7 C 0.6736(4) 0.3064(3) 0.1876(2) 0.0207(6) Uani 1 1 d . . . C6 C 0.6389(3) 0.3877(3) 0.1101(2) 0.0201(6) Uani 1 1 d . . . C17 C 0.2739(4) 0.3343(3) 0.2689(3) 0.0247(7) Uani 1 1 d . . . O6 O 0.7316(3) 0.4265(2) 0.04792(18) 0.0268(5) Uani 1 1 d . . . O1W O 0.0256(2) 0.3748(2) 0.00933(18) 0.0286(5) Uani 1 1 d D . . H2W H -0.0178 0.3270 -0.0558 0.043 Uiso 1 1 d RD . . H1W H -0.0387 0.3995 0.0258 0.043 Uiso 1 1 d RD . . 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 0.02130(8) 0.01637(8) 0.01573(8) 0.00960(5) 0.00679(5) 0.01108(6) Cu1 0.0524(3) 0.0378(3) 0.0398(3) 0.0300(2) 0.0087(2) 0.0231(2) S2 0.0217(4) 0.0156(3) 0.0191(3) 0.0064(3) 0.0051(3) 0.0093(3) S1 0.0270(4) 0.0255(4) 0.0210(4) 0.0082(3) 0.0091(3) 0.0141(3) O3 0.0349(13) 0.0368(14) 0.0271(12) 0.0213(11) 0.0030(10) 0.0081(11) O2 0.0448(14) 0.0224(12) 0.0282(12) 0.0148(10) 0.0132(10) 0.0150(11) O1 0.0473(14) 0.0380(13) 0.0305(12) 0.0152(10) 0.0230(11) 0.0289(12) O4 0.0278(11) 0.0246(11) 0.0242(11) 0.0070(9) 0.0074(9) 0.0164(10) O9 0.0401(13) 0.0345(13) 0.0297(12) 0.0145(10) 0.0147(10) 0.0243(11) O10 0.0325(13) 0.0454(16) 0.0387(14) 0.0135(12) 0.0034(11) 0.0068(12) O5 0.0310(12) 0.0276(12) 0.0321(12) 0.0109(10) 0.0048(10) 0.0192(10) O7 0.0257(11) 0.0188(11) 0.0272(11) 0.0106(9) 0.0078(9) 0.0100(9) O8 0.0309(12) 0.0267(12) 0.0225(11) 0.0013(9) 0.0014(9) 0.0113(10) N1 0.0332(15) 0.0275(14) 0.0267(14) 0.0162(12) 0.0094(12) 0.0169(12) N2 0.0421(16) 0.0289(15) 0.0292(14) 0.0183(12) 0.0105(13) 0.0210(13) C20 0.0332(18) 0.043(2) 0.0315(18) 0.0170(15) 0.0150(15) 0.0263(16) C19 0.0342(18) 0.0372(19) 0.0268(16) 0.0144(14) 0.0116(14) 0.0243(16) C18 0.0296(16) 0.0266(16) 0.0187(15) 0.0040(12) 0.0109(13) 0.0137(14) C22 0.0294(17) 0.0349(18) 0.0240(16) 0.0112(14) 0.0125(13) 0.0195(15) C21 0.0313(17) 0.0293(17) 0.0215(15) 0.0062(13) 0.0116(13) 0.0182(14) C8 0.0390(19) 0.043(2) 0.047(2) 0.0298(18) 0.0267(17) 0.0294(17) C11 0.051(2) 0.051(2) 0.052(2) 0.042(2) 0.0367(19) 0.034(2) C10 0.0320(18) 0.043(2) 0.048(2) 0.0288(18) 0.0141(16) 0.0248(17) C9 0.0279(17) 0.0366(19) 0.0397(19) 0.0266(16) 0.0176(15) 0.0194(15) C3 0.0303(16) 0.0190(15) 0.0256(16) 0.0113(12) 0.0127(13) 0.0110(13) C2 0.0277(16) 0.0182(15) 0.0259(16) 0.0090(12) 0.0121(13) 0.0117(13) C1 0.0320(17) 0.0257(17) 0.0417(19) 0.0198(15) 0.0233(15) 0.0151(15) C5 0.0263(16) 0.0254(16) 0.0393(18) 0.0170(14) 0.0171(14) 0.0153(14) C4 0.0265(15) 0.0139(14) 0.0240(15) 0.0053(12) 0.0066(12) 0.0111(12) C13 0.0350(17) 0.0288(17) 0.0196(15) 0.0109(13) 0.0061(13) 0.0153(15) C14 0.0288(16) 0.0207(16) 0.0255(16) 0.0095(13) 0.0070(13) 0.0110(13) C16 0.0237(15) 0.0259(16) 0.0247(16) 0.0158(13) 0.0114(13) 0.0153(13) C15 0.0310(17) 0.0261(17) 0.0211(15) 0.0095(13) 0.0025(13) 0.0126(14) C12 0.0332(17) 0.0211(16) 0.0295(17) 0.0116(13) 0.0054(14) 0.0119(14) C7 0.0288(16) 0.0206(15) 0.0181(14) 0.0086(12) 0.0076(12) 0.0143(13) C6 0.0268(16) 0.0152(14) 0.0181(14) 0.0066(11) 0.0013(12) 0.0103(12) C17 0.0285(16) 0.0299(18) 0.0276(17) 0.0175(14) 0.0141(14) 0.0180(15) O6 0.0352(12) 0.0256(12) 0.0246(11) 0.0165(9) 0.0096(10) 0.0143(10) O1W 0.0254(11) 0.0370(13) 0.0269(12) 0.0104(10) 0.0076(9) 0.0163(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 Dy1 O1 2.319(2) . ? Dy1 O5 2.326(2) . ? Dy1 O7 2.342(2) 2_665 ? Dy1 O3 2.369(2) . ? Dy1 O6 2.373(2) 2_665 ? Dy1 O4 2.380(2) . ? Dy1 O1W 2.412(2) . ? Dy1 O2 2.528(2) . ? Cu1 N2 1.882(3) 2_656 ? Cu1 N1 1.884(3) . ? S2 O8 1.439(2) . ? S2 O4 1.460(2) . ? S2 O7 1.461(2) . ? S2 C4 1.773(3) . ? S1 O10 1.435(3) . ? S1 O9 1.450(2) . ? S1 O1 1.476(2) . ? S1 C18 1.779(3) . ? O3 C17 1.263(4) . ? O2 C17 1.253(4) . ? O5 C6 1.250(4) . ? O7 Dy1 2.342(2) 2_665 ? N1 C12 1.336(4) . ? N1 C13 1.345(4) . ? N2 C10 1.338(4) . ? N2 C11 1.339(4) . ? N2 Cu1 1.882(3) 2_656 ? C20 C19 1.374(4) . ? C20 C21 1.416(4) . ? C20 H20 0.9300 . ? C19 C18 1.405(4) . ? C19 H19 0.9300 . ? C18 C22 1.371(4) . ? C22 C21 1.412(4) 2_566 ? C22 H22 0.9300 . ? C21 C22 1.412(4) 2_566 ? C21 C21 1.421(6) 2_566 ? C8 C11 1.371(5) . ? C8 C7 1.381(4) . ? C8 H8 0.9300 . ? C11 H11 0.9300 . ? C10 C9 1.378(4) . ? C10 H10 0.9300 . ? C9 C7 1.374(4) . ? C9 H9 0.9300 . ? C3 C4 1.367(4) . ? C3 C2 1.408(4) . ? C3 H3 0.9300 . ? C2 C1 1.415(4) . ? C2 C2 1.428(6) 2_655 ? C1 C5 1.363(4) 2_655 ? C1 H1 0.9300 . ? C5 C1 1.363(4) 2_655 ? C5 C4 1.404(4) . ? C5 H5 0.9300 . ? C13 C14 1.372(4) . ? C13 H13 0.9300 . ? C14 C16 1.386(4) . ? C14 H14 0.9300 . ? C16 C15 1.384(4) . ? C16 C17 1.503(4) . ? C15 C12 1.380(4) . ? C15 H15 0.9300 . ? C12 H12 0.9300 . ? C7 C6 1.517(4) . ? C6 O6 1.262(4) . ? O6 Dy1 2.373(2) 2_665 ? O1W H2W 0.8193 . ? O1W H1W 0.8112 . ? 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 O5 142.56(8) . . ? O1 Dy1 O7 78.63(8) . 2_665 ? O5 Dy1 O7 74.17(7) . 2_665 ? O1 Dy1 O3 96.26(9) . . ? O5 Dy1 O3 85.76(8) . . ? O7 Dy1 O3 135.42(7) 2_665 . ? O1 Dy1 O6 81.57(8) . 2_665 ? O5 Dy1 O6 117.68(8) . 2_665 ? O7 Dy1 O6 80.03(7) 2_665 2_665 ? O3 Dy1 O6 143.66(8) . 2_665 ? O1 Dy1 O4 143.98(8) . . ? O5 Dy1 O4 73.44(7) . . ? O7 Dy1 O4 126.38(7) 2_665 . ? O3 Dy1 O4 82.63(8) . . ? O6 Dy1 O4 78.73(7) 2_665 . ? O1 Dy1 O1W 73.39(8) . . ? O5 Dy1 O1W 141.30(8) . . ? O7 Dy1 O1W 142.17(7) 2_665 . ? O3 Dy1 O1W 73.45(8) . . ? O6 Dy1 O1W 71.20(7) 2_665 . ? O4 Dy1 O1W 71.82(7) . . ? O1 Dy1 O2 75.86(8) . . ? O5 Dy1 O2 75.71(8) . . ? O7 Dy1 O2 82.96(7) 2_665 . ? O3 Dy1 O2 53.29(7) . . ? O6 Dy1 O2 153.98(7) 2_665 . ? O4 Dy1 O2 127.29(7) . . ? O1W Dy1 O2 113.47(7) . . ? N2 Cu1 N1 171.86(12) 2_656 . ? O8 S2 O4 112.62(13) . . ? O8 S2 O7 112.28(13) . . ? O4 S2 O7 112.22(12) . . ? O8 S2 C4 106.67(13) . . ? O4 S2 C4 106.80(13) . . ? O7 S2 C4 105.69(13) . . ? O10 S1 O9 113.88(15) . . ? O10 S1 O1 113.15(15) . . ? O9 S1 O1 110.42(13) . . ? O10 S1 C18 107.71(15) . . ? O9 S1 C18 106.58(14) . . ? O1 S1 C18 104.39(14) . . ? C17 O3 Dy1 95.71(19) . . ? C17 O2 Dy1 88.55(18) . . ? S1 O1 Dy1 162.45(16) . . ? S2 O4 Dy1 143.04(12) . . ? C6 O5 Dy1 172.8(2) . . ? S2 O7 Dy1 150.47(13) . 2_665 ? C12 N1 C13 118.0(3) . . ? C12 N1 Cu1 122.0(2) . . ? C13 N1 Cu1 119.7(2) . . ? C10 N2 C11 116.8(3) . . ? C10 N2 Cu1 123.0(2) . 2_656 ? C11 N2 Cu1 120.0(2) . 2_656 ? C19 C20 C21 121.2(3) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C19 C18 119.2(3) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C22 C18 C19 121.3(3) . . ? C22 C18 S1 119.1(2) . . ? C19 C18 S1 119.5(2) . . ? C18 C22 C21 120.5(3) . 2_566 ? C18 C22 H22 119.7 . . ? C21 C22 H22 119.7 2_566 . ? C22 C21 C20 122.2(3) 2_566 . ? C22 C21 C21 118.8(4) 2_566 2_566 ? C20 C21 C21 119.0(4) . 2_566 ? C11 C8 C7 119.8(3) . . ? C11 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? N2 C11 C8 123.1(3) . . ? N2 C11 H11 118.5 . . ? C8 C11 H11 118.5 . . ? N2 C10 C9 123.3(3) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? C7 C9 C10 119.4(3) . . ? C7 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C2 C1 122.5(3) . . ? C3 C2 C2 118.4(3) . 2_655 ? C1 C2 C2 119.0(3) . 2_655 ? C5 C1 C2 121.3(3) 2_655 . ? C5 C1 H1 119.4 2_655 . ? C2 C1 H1 119.4 . . ? C1 C5 C4 119.1(3) 2_655 . ? C1 C5 H5 120.4 2_655 . ? C4 C5 H5 120.4 . . ? C3 C4 C5 121.7(3) . . ? C3 C4 S2 118.9(2) . . ? C5 C4 S2 119.4(2) . . ? N1 C13 C14 122.3(3) . . ? N1 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C13 C14 C16 119.7(3) . . ? C13 C14 H14 120.2 . . ? C16 C14 H14 120.2 . . ? C15 C16 C14 118.0(3) . . ? C15 C16 C17 120.8(3) . . ? C14 C16 C17 121.1(3) . . ? C12 C15 C16 119.1(3) . . ? C12 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? N1 C12 C15 122.8(3) . . ? N1 C12 H12 118.6 . . ? C15 C12 H12 118.6 . . ? C9 C7 C8 117.6(3) . . ? C9 C7 C6 122.4(3) . . ? C8 C7 C6 119.9(3) . . ? O5 C6 O6 124.7(3) . . ? O5 C6 C7 118.3(3) . . ? O6 C6 C7 117.0(3) . . ? O2 C17 O3 122.1(3) . . ? O2 C17 C16 119.9(3) . . ? O3 C17 C16 117.9(3) . . ? C6 O6 Dy1 124.40(19) . 2_665 ? Dy1 O1W H2W 122.9 . . ? Dy1 O1W H1W 129.6 . . ? H2W O1W H1W 104.9 . . ? 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 O1 Dy1 O3 C17 -70.5(2) . . . . ? O5 Dy1 O3 C17 71.96(19) . . . . ? O7 Dy1 O3 C17 9.7(2) 2_665 . . . ? O6 Dy1 O3 C17 -154.77(17) 2_665 . . . ? O4 Dy1 O3 C17 145.8(2) . . . . ? O1W Dy1 O3 C17 -141.1(2) . . . . ? O2 Dy1 O3 C17 -3.35(17) . . . . ? O1 Dy1 O2 C17 112.52(19) . . . . ? O5 Dy1 O2 C17 -92.09(18) . . . . ? O7 Dy1 O2 C17 -167.49(18) 2_665 . . . ? O3 Dy1 O2 C17 3.36(17) . . . . ? O6 Dy1 O2 C17 143.11(19) 2_665 . . . ? O4 Dy1 O2 C17 -36.4(2) . . . . ? O1W Dy1 O2 C17 48.03(19) . . . . ? O10 S1 O1 Dy1 3.7(5) . . . . ? O9 S1 O1 Dy1 132.7(4) . . . . ? C18 S1 O1 Dy1 -113.1(5) . . . . ? O5 Dy1 O1 S1 19.3(5) . . . . ? O7 Dy1 O1 S1 -24.6(5) 2_665 . . . ? O3 Dy1 O1 S1 110.5(5) . . . . ? O6 Dy1 O1 S1 -106.1(5) 2_665 . . . ? O4 Dy1 O1 S1 -163.4(4) . . . . ? O1W Dy1 O1 S1 -178.9(5) . . . . ? O2 Dy1 O1 S1 60.9(5) . . . . ? O8 S2 O4 Dy1 -167.48(18) . . . . ? O7 S2 O4 Dy1 -39.6(2) . . . . ? C4 S2 O4 Dy1 75.8(2) . . . . ? O1 Dy1 O4 S2 157.70(17) . . . . ? O5 Dy1 O4 S2 -24.0(2) . . . . ? O7 Dy1 O4 S2 31.1(2) 2_665 . . . ? O3 Dy1 O4 S2 -111.8(2) . . . . ? O6 Dy1 O4 S2 99.6(2) 2_665 . . . ? O1W Dy1 O4 S2 173.3(2) . . . . ? O2 Dy1 O4 S2 -80.6(2) . . . . ? O1 Dy1 O5 C6 -100.2(16) . . . . ? O7 Dy1 O5 C6 -55.2(16) 2_665 . . . ? O3 Dy1 O5 C6 165.1(16) . . . . ? O6 Dy1 O5 C6 14.2(16) 2_665 . . . ? O4 Dy1 O5 C6 81.5(16) . . . . ? O1W Dy1 O5 C6 108.4(16) . . . . ? O2 Dy1 O5 C6 -141.8(16) . . . . ? O8 S2 O7 Dy1 159.7(2) . . . 2_665 ? O4 S2 O7 Dy1 31.7(3) . . . 2_665 ? C4 S2 O7 Dy1 -84.3(3) . . . 2_665 ? N2 Cu1 N1 C12 56.1(10) 2_656 . . . ? N2 Cu1 N1 C13 -117.5(8) 2_656 . . . ? C21 C20 C19 C18 1.2(5) . . . . ? C20 C19 C18 C22 -1.6(5) . . . . ? C20 C19 C18 S1 176.5(3) . . . . ? O10 S1 C18 C22 -54.0(3) . . . . ? O9 S1 C18 C22 -176.6(2) . . . . ? O1 S1 C18 C22 66.5(3) . . . . ? O10 S1 C18 C19 127.9(3) . . . . ? O9 S1 C18 C19 5.3(3) . . . . ? O1 S1 C18 C19 -111.6(3) . . . . ? C19 C18 C22 C21 1.0(5) . . . 2_566 ? S1 C18 C22 C21 -177.1(2) . . . 2_566 ? C19 C20 C21 C22 179.4(3) . . . 2_566 ? C19 C20 C21 C21 -0.2(6) . . . 2_566 ? C10 N2 C11 C8 1.2(6) . . . . ? Cu1 N2 C11 C8 -175.1(3) 2_656 . . . ? C7 C8 C11 N2 -0.8(6) . . . . ? C11 N2 C10 C9 -0.6(5) . . . . ? Cu1 N2 C10 C9 175.6(3) 2_656 . . . ? N2 C10 C9 C7 -0.4(6) . . . . ? C4 C3 C2 C1 -178.8(3) . . . . ? C4 C3 C2 C2 1.8(5) . . . 2_655 ? C3 C2 C1 C5 -179.0(3) . . . 2_655 ? C2 C2 C1 C5 0.4(6) 2_655 . . 2_655 ? C2 C3 C4 C5 -2.2(5) . . . . ? C2 C3 C4 S2 -179.0(2) . . . . ? C1 C5 C4 C3 1.2(5) 2_655 . . . ? C1 C5 C4 S2 178.0(3) 2_655 . . . ? O8 S2 C4 C3 94.7(3) . . . . ? O4 S2 C4 C3 -144.6(2) . . . . ? O7 S2 C4 C3 -25.0(3) . . . . ? O8 S2 C4 C5 -82.1(3) . . . . ? O4 S2 C4 C5 38.5(3) . . . . ? O7 S2 C4 C5 158.2(2) . . . . ? C12 N1 C13 C14 -1.5(5) . . . . ? Cu1 N1 C13 C14 172.3(2) . . . . ? N1 C13 C14 C16 1.5(5) . . . . ? C13 C14 C16 C15 -0.1(4) . . . . ? C13 C14 C16 C17 -177.6(3) . . . . ? C14 C16 C15 C12 -1.1(5) . . . . ? C17 C16 C15 C12 176.3(3) . . . . ? C13 N1 C12 C15 0.1(5) . . . . ? Cu1 N1 C12 C15 -173.5(2) . . . . ? C16 C15 C12 N1 1.2(5) . . . . ? C10 C9 C7 C8 0.9(5) . . . . ? C10 C9 C7 C6 -176.2(3) . . . . ? C11 C8 C7 C9 -0.3(5) . . . . ? C11 C8 C7 C6 176.8(3) . . . . ? Dy1 O5 C6 O6 -8.6(18) . . . . ? Dy1 O5 C6 C7 173.1(15) . . . . ? C9 C7 C6 O5 -173.7(3) . . . . ? C8 C7 C6 O5 9.4(4) . . . . ? C9 C7 C6 O6 7.9(4) . . . . ? C8 C7 C6 O6 -169.1(3) . . . . ? Dy1 O2 C17 O3 -6.0(3) . . . . ? Dy1 O2 C17 C16 171.4(2) . . . . ? Dy1 O3 C17 O2 6.4(3) . . . . ? Dy1 O3 C17 C16 -171.0(2) . . . . ? C15 C16 C17 O2 -172.3(3) . . . . ? C14 C16 C17 O2 5.1(4) . . . . ? C15 C16 C17 O3 5.2(4) . . . . ? C14 C16 C17 O3 -177.4(3) . . . . ? O5 C6 O6 Dy1 -5.5(4) . . . 2_665 ? C7 C6 O6 Dy1 172.82(18) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.521 _refine_diff_density_min -0.723 _refine_diff_density_rms 0.104 # Attachment 'eu.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 768850' #TrackingRef 'eu.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H16 Cu Eu N2 O11 S2' _chemical_formula_sum 'C22 H16 Cu Eu N2 O11 S2' _chemical_formula_weight 764.03 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' Cu Cu 0.3201 1.2651 '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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5144(6) _cell_length_b 11.4162(7) _cell_length_c 12.3690(12) _cell_angle_alpha 99.4150(10) _cell_angle_beta 100.2000(10) _cell_angle_gamma 114.0100(10) _cell_volume 1165.63(15) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4143 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.78 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 3.827 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.415 _exptl_absorpt_correction_T_max 0.465 _exptl_absorpt_process_details SADABS,Bruker(2002) _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 6053 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.19 _reflns_number_total 4196 _reflns_number_gt 3851 _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^)+(0.0220P)^2^+1.6491P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4196 _refine_ls_number_parameters 352 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0563 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.31012(2) 0.466483(17) 0.096428(14) 0.01680(7) Uani 1 1 d . . . Cu1 Cu 0.26095(8) -0.02359(6) 0.59569(5) 0.04236(15) Uani 1 1 d . . . S2 S 0.30661(11) 0.23088(8) -0.14748(7) 0.01958(19) Uani 1 1 d . . . S1 S 0.21609(12) 0.71441(10) 0.27461(8) 0.0252(2) Uani 1 1 d . . . O3 O 0.1825(4) 0.2800(3) 0.1713(2) 0.0370(7) Uani 1 1 d . . . O2 O 0.3770(4) 0.4527(3) 0.3020(2) 0.0304(7) Uani 1 1 d . . . O1 O 0.2232(4) 0.6068(3) 0.1957(2) 0.0347(7) Uani 1 1 d . . . O4 O 0.2394(3) 0.2934(2) -0.0726(2) 0.0241(6) Uani 1 1 d . . . O9 O 0.1247(4) 0.7698(3) 0.2138(2) 0.0333(7) Uani 1 1 d . . . O10 O 0.3705(4) 0.8122(3) 0.3463(3) 0.0455(8) Uani 1 1 d . . . O5 O 0.5250(3) 0.4098(3) 0.1088(2) 0.0297(6) Uani 1 1 d . . . O7 O 0.4524(3) 0.3284(2) -0.1646(2) 0.0254(6) Uani 1 1 d . . . O8 O 0.1915(3) 0.1443(3) -0.2537(2) 0.0299(6) Uani 1 1 d . . . N1 N 0.2488(4) 0.0859(3) 0.4990(3) 0.0276(8) Uani 1 1 d . . . N2 N 0.7189(4) 0.1434(3) 0.3221(3) 0.0312(8) Uani 1 1 d . . . C20 C -0.1360(5) 0.5584(4) 0.4245(3) 0.0330(10) Uani 1 1 d . . . H20 H -0.2369 0.5534 0.4207 0.040 Uiso 1 1 calc R . . C19 C -0.0483(5) 0.6263(4) 0.3591(3) 0.0323(10) Uani 1 1 d . . . H19 H -0.0886 0.6674 0.3119 0.039 Uiso 1 1 calc R . . C18 C 0.1034(5) 0.6331(4) 0.3642(3) 0.0256(9) Uani 1 1 d . . . C22 C 0.1663(5) 0.5747(4) 0.4337(3) 0.0298(9) Uani 1 1 d . . . H22 H 0.2675 0.5814 0.4359 0.036 Uiso 1 1 calc R . . C21 C -0.0777(5) 0.4959(4) 0.4976(3) 0.0286(9) Uani 1 1 d . . . C8 C 0.5646(5) 0.2438(4) 0.2436(4) 0.0364(11) Uani 1 1 d . . . H8 H 0.4719 0.2546 0.2363 0.044 Uiso 1 1 calc R . . C11 C 0.5909(6) 0.1657(5) 0.3099(4) 0.0442(12) Uani 1 1 d . . . H11 H 0.5157 0.1264 0.3482 0.053 Uiso 1 1 calc R . . C10 C 0.8270(5) 0.2053(5) 0.2686(4) 0.0369(10) Uani 1 1 d . . . H10 H 0.9184 0.1925 0.2766 0.044 Uiso 1 1 calc R . . C9 C 0.8097(5) 0.2869(4) 0.2024(4) 0.0327(10) Uani 1 1 d . . . H9 H 0.8886 0.3286 0.1677 0.039 Uiso 1 1 calc R . . C3 C 0.5004(5) 0.1186(4) -0.0871(3) 0.0224(8) Uani 1 1 d . . . H3 H 0.5609 0.1656 -0.1308 0.027 Uiso 1 1 calc R . . C2 C 0.5481(5) 0.0359(3) -0.0325(3) 0.0234(8) Uani 1 1 d . . . C1 C 0.6888(5) 0.0240(4) -0.0398(4) 0.0305(9) Uani 1 1 d . . . H1 H 0.7535 0.0730 -0.0804 0.037 Uiso 1 1 calc R . . C5 C 0.2693(5) 0.0575(4) -0.0115(4) 0.0283(9) Uani 1 1 d . . . H5 H 0.1780 0.0661 -0.0045 0.034 Uiso 1 1 calc R . . C4 C 0.3653(5) 0.1295(3) -0.0758(3) 0.0222(8) Uani 1 1 d . . . C13 C 0.3438(5) 0.2176(4) 0.5350(3) 0.0291(9) Uani 1 1 d . . . H13 H 0.4047 0.2542 0.6104 0.035 Uiso 1 1 calc R . . C14 C 0.3541(5) 0.2999(4) 0.4641(3) 0.0268(9) Uani 1 1 d . . . H14 H 0.4226 0.3903 0.4910 0.032 Uiso 1 1 calc R . . C16 C 0.2617(4) 0.2473(4) 0.3524(3) 0.0206(8) Uani 1 1 d . . . C15 C 0.1617(5) 0.1118(4) 0.3157(3) 0.0273(9) Uani 1 1 d . . . H15 H 0.0972 0.0734 0.2413 0.033 Uiso 1 1 calc R . . C12 C 0.1594(5) 0.0349(4) 0.3910(3) 0.0300(9) Uani 1 1 d . . . H12 H 0.0930 -0.0561 0.3657 0.036 Uiso 1 1 calc R . . C7 C 0.6749(5) 0.3063(4) 0.1880(3) 0.0222(8) Uani 1 1 d . . . C6 C 0.6436(5) 0.3878(3) 0.1108(3) 0.0219(8) Uani 1 1 d . . . C17 C 0.2736(5) 0.3329(4) 0.2705(3) 0.0245(8) Uani 1 1 d . . . O6 O 0.7374(3) 0.4255(3) 0.0495(2) 0.0288(6) Uani 1 1 d . . . O1W O 0.0218(3) 0.3730(3) 0.0093(2) 0.0292(6) Uani 1 1 d D . . H2W H -0.0217 0.3252 -0.0558 0.044 Uiso 1 1 d RD . . H1W H -0.0425 0.3977 0.0258 0.044 Uiso 1 1 d RD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.02141(11) 0.01820(10) 0.01735(10) 0.01029(7) 0.00792(7) 0.01198(8) Cu1 0.0543(4) 0.0405(3) 0.0423(3) 0.0315(3) 0.0106(3) 0.0242(3) S2 0.0221(5) 0.0184(4) 0.0211(4) 0.0066(4) 0.0068(4) 0.0109(4) S1 0.0288(5) 0.0295(5) 0.0231(5) 0.0091(4) 0.0109(4) 0.0164(4) O3 0.0380(17) 0.0369(17) 0.0305(16) 0.0216(13) 0.0032(14) 0.0092(15) O2 0.0437(18) 0.0243(15) 0.0273(14) 0.0136(12) 0.0138(13) 0.0148(14) O1 0.0497(19) 0.0414(17) 0.0335(16) 0.0160(13) 0.0250(14) 0.0321(16) O4 0.0264(14) 0.0274(14) 0.0236(13) 0.0080(11) 0.0076(12) 0.0161(12) O9 0.0418(18) 0.0372(16) 0.0329(16) 0.0142(13) 0.0135(14) 0.0259(15) O10 0.0318(17) 0.050(2) 0.0415(18) 0.0141(15) 0.0037(15) 0.0070(16) O5 0.0315(16) 0.0294(15) 0.0338(15) 0.0093(12) 0.0045(13) 0.0204(13) O7 0.0284(15) 0.0230(14) 0.0299(14) 0.0135(11) 0.0105(12) 0.0130(12) O8 0.0292(15) 0.0287(15) 0.0244(14) 0.0021(12) 0.0014(12) 0.0101(13) N1 0.036(2) 0.0258(17) 0.0278(18) 0.0155(14) 0.0117(15) 0.0155(16) N2 0.041(2) 0.0319(19) 0.0299(18) 0.0183(15) 0.0129(16) 0.0205(17) C20 0.031(2) 0.050(3) 0.033(2) 0.014(2) 0.0160(19) 0.028(2) C19 0.035(2) 0.047(3) 0.029(2) 0.0150(19) 0.0143(19) 0.027(2) C18 0.029(2) 0.031(2) 0.0215(19) 0.0044(16) 0.0123(17) 0.0169(18) C22 0.027(2) 0.040(2) 0.026(2) 0.0092(18) 0.0111(17) 0.018(2) C21 0.034(2) 0.038(2) 0.0202(19) 0.0057(17) 0.0097(17) 0.022(2) C8 0.039(3) 0.046(3) 0.051(3) 0.032(2) 0.028(2) 0.030(2) C11 0.051(3) 0.054(3) 0.061(3) 0.042(3) 0.041(3) 0.035(3) C10 0.032(2) 0.047(3) 0.049(3) 0.027(2) 0.015(2) 0.028(2) C9 0.029(2) 0.047(3) 0.042(2) 0.032(2) 0.021(2) 0.025(2) C3 0.028(2) 0.0187(18) 0.028(2) 0.0115(16) 0.0146(17) 0.0122(17) C2 0.025(2) 0.0166(18) 0.030(2) 0.0081(16) 0.0097(17) 0.0094(17) C1 0.032(2) 0.030(2) 0.042(2) 0.0216(19) 0.023(2) 0.0163(19) C5 0.028(2) 0.028(2) 0.043(2) 0.0187(18) 0.0206(19) 0.0178(18) C4 0.025(2) 0.0167(18) 0.0266(19) 0.0083(15) 0.0090(16) 0.0094(16) C13 0.039(2) 0.032(2) 0.0191(19) 0.0090(17) 0.0084(18) 0.018(2) C14 0.031(2) 0.024(2) 0.027(2) 0.0095(16) 0.0078(17) 0.0135(18) C16 0.0222(19) 0.0251(19) 0.0244(19) 0.0135(16) 0.0133(16) 0.0147(17) C15 0.032(2) 0.028(2) 0.023(2) 0.0114(17) 0.0051(17) 0.0139(19) C12 0.037(2) 0.027(2) 0.029(2) 0.0135(17) 0.0100(19) 0.0143(19) C7 0.027(2) 0.0216(19) 0.0204(18) 0.0079(15) 0.0060(16) 0.0123(17) C6 0.027(2) 0.0183(18) 0.0204(18) 0.0061(15) 0.0023(16) 0.0114(17) C17 0.029(2) 0.032(2) 0.028(2) 0.0184(17) 0.0168(18) 0.0200(19) O6 0.0373(16) 0.0282(15) 0.0270(14) 0.0182(12) 0.0134(13) 0.0144(13) O1W 0.0235(14) 0.0363(16) 0.0294(15) 0.0079(12) 0.0063(12) 0.0155(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O1 2.357(3) . ? Eu1 O5 2.371(3) . ? Eu1 O7 2.382(3) 2_665 ? Eu1 O4 2.408(2) . ? Eu1 O3 2.409(3) . ? Eu1 O6 2.425(2) 2_665 ? Eu1 O1W 2.454(3) . ? Eu1 O2 2.556(3) . ? Cu1 N2 1.882(3) 2_656 ? Cu1 N1 1.888(3) . ? S2 O8 1.445(3) . ? S2 O7 1.461(3) . ? S2 O4 1.463(3) . ? S2 C4 1.768(4) . ? S1 O10 1.439(3) . ? S1 O9 1.447(3) . ? S1 O1 1.471(3) . ? S1 C18 1.785(4) . ? O3 C17 1.255(5) . ? O2 C17 1.259(5) . ? O5 C6 1.249(5) . ? O7 Eu1 2.382(3) 2_665 ? N1 C12 1.337(5) . ? N1 C13 1.344(5) . ? N2 C11 1.330(6) . ? N2 C10 1.341(5) . ? N2 Cu1 1.882(3) 2_656 ? C20 C19 1.366(6) . ? C20 C21 1.412(6) . ? C20 H20 0.9300 . ? C19 C18 1.403(6) . ? C19 H19 0.9300 . ? C18 C22 1.368(6) . ? C22 C21 1.416(5) 2_566 ? C22 H22 0.9300 . ? C21 C22 1.416(5) 2_566 ? C21 C21 1.432(8) 2_566 ? C8 C7 1.375(5) . ? C8 C11 1.370(6) . ? C8 H8 0.9300 . ? C11 H11 0.9300 . ? C10 C9 1.375(6) . ? C10 H10 0.9300 . ? C9 C7 1.374(6) . ? C9 H9 0.9300 . ? C3 C4 1.369(5) . ? C3 C2 1.415(5) . ? C3 H3 0.9300 . ? C2 C1 1.416(6) . ? C2 C2 1.422(7) 2_655 ? C1 C5 1.353(5) 2_655 ? C1 H1 0.9300 . ? C5 C1 1.353(5) 2_655 ? C5 C4 1.415(5) . ? C5 H5 0.9300 . ? C13 C14 1.374(5) . ? C13 H13 0.9300 . ? C14 C16 1.382(5) . ? C14 H14 0.9300 . ? C16 C15 1.387(5) . ? C16 C17 1.507(5) . ? C15 C12 1.378(5) . ? C15 H15 0.9300 . ? C12 H12 0.9300 . ? C7 C6 1.510(5) . ? C6 O6 1.261(4) . ? O6 Eu1 2.425(2) 2_665 ? O1W H2W 0.8202 . ? O1W H1W 0.8129 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Eu1 O5 142.33(10) . . ? O1 Eu1 O7 77.93(10) . 2_665 ? O5 Eu1 O7 74.12(9) . 2_665 ? O1 Eu1 O4 144.49(10) . . ? O5 Eu1 O4 73.17(9) . . ? O7 Eu1 O4 126.89(9) 2_665 . ? O1 Eu1 O3 96.14(11) . . ? O5 Eu1 O3 86.63(10) . . ? O7 Eu1 O3 135.37(9) 2_665 . ? O4 Eu1 O3 82.47(9) . . ? O1 Eu1 O6 80.93(9) . 2_665 ? O5 Eu1 O6 118.02(9) . 2_665 ? O7 Eu1 O6 80.52(9) 2_665 2_665 ? O4 Eu1 O6 79.42(9) . 2_665 ? O3 Eu1 O6 142.92(10) . 2_665 ? O1 Eu1 O1W 73.93(10) . . ? O5 Eu1 O1W 141.32(9) . . ? O7 Eu1 O1W 142.09(9) 2_665 . ? O4 Eu1 O1W 71.73(9) . . ? O3 Eu1 O1W 73.22(9) . . ? O6 Eu1 O1W 70.46(9) 2_665 . ? O1 Eu1 O2 75.81(9) . . ? O5 Eu1 O2 76.39(9) . . ? O7 Eu1 O2 83.51(9) 2_665 . ? O4 Eu1 O2 126.47(8) . . ? O3 Eu1 O2 52.58(9) . . ? O6 Eu1 O2 154.06(9) 2_665 . ? O1W Eu1 O2 112.93(9) . . ? N2 Cu1 N1 172.76(15) 2_656 . ? O8 S2 O7 112.30(16) . . ? O8 S2 O4 113.02(17) . . ? O7 S2 O4 111.91(15) . . ? O8 S2 C4 106.55(17) . . ? O7 S2 C4 105.73(16) . . ? O4 S2 C4 106.74(16) . . ? O10 S1 O9 113.92(19) . . ? O10 S1 O1 113.2(2) . . ? O9 S1 O1 110.48(17) . . ? O10 S1 C18 107.57(18) . . ? O9 S1 C18 106.72(18) . . ? O1 S1 C18 104.24(17) . . ? C17 O3 Eu1 95.8(2) . . ? C17 O2 Eu1 88.8(2) . . ? S1 O1 Eu1 164.1(2) . . ? S2 O4 Eu1 143.12(16) . . ? C6 O5 Eu1 174.8(3) . . ? S2 O7 Eu1 150.32(16) . 2_665 ? C12 N1 C13 118.3(3) . . ? C12 N1 Cu1 121.6(3) . . ? C13 N1 Cu1 119.7(3) . . ? C11 N2 C10 116.7(3) . . ? C11 N2 Cu1 120.8(3) . 2_656 ? C10 N2 Cu1 122.4(3) . 2_656 ? C19 C20 C21 121.8(4) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C20 C19 C18 119.1(4) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C22 C18 C19 121.6(4) . . ? C22 C18 S1 118.4(3) . . ? C19 C18 S1 119.9(3) . . ? C18 C22 C21 120.2(4) . 2_566 ? C18 C22 H22 119.9 . . ? C21 C22 H22 119.9 2_566 . ? C20 C21 C22 122.8(4) . 2_566 ? C20 C21 C21 118.5(5) . 2_566 ? C22 C21 C21 118.7(5) 2_566 2_566 ? C7 C8 C11 120.2(4) . . ? C7 C8 H8 119.9 . . ? C11 C8 H8 119.9 . . ? N2 C11 C8 123.1(4) . . ? N2 C11 H11 118.5 . . ? C8 C11 H11 118.5 . . ? N2 C10 C9 123.3(4) . . ? N2 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? C7 C9 C10 119.5(4) . . ? C7 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C4 C3 C2 120.1(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C1 C2 C3 122.0(3) . . ? C1 C2 C2 119.5(4) . 2_655 ? C3 C2 C2 118.5(4) . 2_655 ? C5 C1 C2 121.0(4) 2_655 . ? C5 C1 H1 119.5 2_655 . ? C2 C1 H1 119.5 . . ? C1 C5 C4 119.5(4) 2_655 . ? C1 C5 H5 120.2 2_655 . ? C4 C5 H5 120.2 . . ? C3 C4 C5 121.3(3) . . ? C3 C4 S2 119.0(3) . . ? C5 C4 S2 119.6(3) . . ? N1 C13 C14 122.2(4) . . ? N1 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C13 C14 C16 119.5(4) . . ? C13 C14 H14 120.3 . . ? C16 C14 H14 120.3 . . ? C14 C16 C15 118.3(3) . . ? C14 C16 C17 121.3(3) . . ? C15 C16 C17 120.3(3) . . ? C12 C15 C16 119.1(4) . . ? C12 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? N1 C12 C15 122.5(4) . . ? N1 C12 H12 118.7 . . ? C15 C12 H12 118.7 . . ? C9 C7 C8 117.2(3) . . ? C9 C7 C6 122.2(3) . . ? C8 C7 C6 120.6(4) . . ? O5 C6 O6 124.3(3) . . ? O5 C6 C7 118.5(3) . . ? O6 C6 C7 117.1(3) . . ? O3 C17 O2 122.4(3) . . ? O3 C17 C16 118.1(3) . . ? O2 C17 C16 119.4(3) . . ? C6 O6 Eu1 122.2(2) . 2_665 ? Eu1 O1W H2W 122.7 . . ? Eu1 O1W H1W 129.7 . . ? H2W O1W H1W 104.8 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.575 _refine_diff_density_min -0.643 _refine_diff_density_rms 0.098 # Attachment 'gd.cif' data_gd _database_code_depnum_ccdc_archive 'CCDC 768851' #TrackingRef 'gd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H16 Cu Gd N2 O11 S2' _chemical_formula_sum 'C22 H16 Cu Gd N2 O11 S2' _chemical_formula_weight 769.31 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' Cu Cu 0.3201 1.2651 '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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4878(10) _cell_length_b 11.3999(12) _cell_length_c 12.373(2) _cell_angle_alpha 99.3880(10) _cell_angle_beta 100.1550(10) _cell_angle_gamma 113.9630(10) _cell_volume 1162.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6207 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.75 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 750 _exptl_absorpt_coefficient_mu 3.993 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.399 _exptl_absorpt_correction_T_max 0.450 _exptl_absorpt_process_details SADABS,Bruker(2002) _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 11256 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4188 _reflns_number_gt 3868 _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^)+(0.0200P)^2^+0.4204P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4188 _refine_ls_number_parameters 356 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0240 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0492 _refine_ls_wR_factor_gt 0.0481 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.028 _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 Gd1 Gd 0.309614(17) 0.466127(14) 0.096256(12) 0.01637(6) Uani 1 1 d . . . Cu1 Cu 0.26009(6) -0.02303(5) 0.59624(4) 0.04159(13) Uani 1 1 d . . . S2 S 0.30722(9) 0.23196(7) -0.14723(6) 0.01913(17) Uani 1 1 d . . . S1 S 0.21629(10) 0.71354(8) 0.27385(7) 0.02461(18) Uani 1 1 d . . . O3 O 0.1825(3) 0.2796(2) 0.1706(2) 0.0358(6) Uani 1 1 d . . . O2 O 0.3773(3) 0.4529(2) 0.30130(19) 0.0297(5) Uani 1 1 d . . . O1 O 0.2217(3) 0.6050(2) 0.1943(2) 0.0333(6) Uani 1 1 d . . . O4 O 0.2394(2) 0.2946(2) -0.07276(18) 0.0238(5) Uani 1 1 d . . . O9 O 0.1248(3) 0.7697(2) 0.21343(19) 0.0324(6) Uani 1 1 d . . . O10 O 0.3712(3) 0.8098(3) 0.3445(2) 0.0458(7) Uani 1 1 d . . . O5 O 0.5237(3) 0.4097(2) 0.10883(19) 0.0291(5) Uani 1 1 d . . . O7 O 0.4540(2) 0.3297(2) -0.16390(18) 0.0243(5) Uani 1 1 d . . . O8 O 0.1924(3) 0.1467(2) -0.25279(19) 0.0309(5) Uani 1 1 d . . . N1 N 0.2484(3) 0.0860(3) 0.4994(2) 0.0262(6) Uani 1 1 d . . . N2 N 0.7199(4) 0.1430(3) 0.3221(2) 0.0309(7) Uani 1 1 d . . . C20 C -0.1371(4) 0.5572(4) 0.4234(3) 0.0324(8) Uani 1 1 d . . . H20 H -0.2390 0.5508 0.4188 0.039 Uiso 1 1 calc R . . C19 C -0.0481(4) 0.6261(4) 0.3585(3) 0.0320(8) Uani 1 1 d . . . H19 H -0.0880 0.6678 0.3116 0.038 Uiso 1 1 calc R . . C18 C 0.1040(4) 0.6326(3) 0.3641(3) 0.0258(7) Uani 1 1 d . . . C22 C 0.1662(4) 0.5744(3) 0.4337(3) 0.0277(8) Uani 1 1 d . . . H22 H 0.2676 0.5808 0.4361 0.033 Uiso 1 1 calc R . . C21 C -0.0771(4) 0.4958(3) 0.4973(3) 0.0267(7) Uani 1 1 d . . . C8 C 0.5648(4) 0.2433(4) 0.2429(3) 0.0348(9) Uani 1 1 d . . . H8 H 0.4720 0.2544 0.2360 0.042 Uiso 1 1 calc R . . C11 C 0.5901(5) 0.1636(4) 0.3085(3) 0.0427(10) Uani 1 1 d . . . H11 H 0.5132 0.1222 0.3451 0.051 Uiso 1 1 calc R . . C10 C 0.8281(4) 0.2061(4) 0.2692(3) 0.0368(9) Uani 1 1 d . . . H10 H 0.9207 0.1946 0.2782 0.044 Uiso 1 1 calc R . . C9 C 0.8101(4) 0.2868(4) 0.2024(3) 0.0307(8) Uani 1 1 d . . . H9 H 0.8889 0.3280 0.1672 0.037 Uiso 1 1 calc R . . C3 C 0.5010(4) 0.1194(3) -0.0863(3) 0.0238(7) Uani 1 1 d . . . H3 H 0.5623 0.1674 -0.1292 0.029 Uiso 1 1 calc R . . C2 C 0.5483(4) 0.0358(3) -0.0326(3) 0.0213(7) Uani 1 1 d . . . C1 C 0.6883(4) 0.0237(3) -0.0400(3) 0.0300(8) Uani 1 1 d . . . H1 H 0.7527 0.0721 -0.0812 0.036 Uiso 1 1 calc R . . C5 C 0.2691(4) 0.0579(3) -0.0123(3) 0.0276(8) Uani 1 1 d . . . H5 H 0.1768 0.0657 -0.0062 0.033 Uiso 1 1 calc R . . C4 C 0.3651(4) 0.1301(3) -0.0753(3) 0.0212(7) Uani 1 1 d . . . C13 C 0.3431(4) 0.2180(3) 0.5353(3) 0.0274(8) Uani 1 1 d . . . H13 H 0.4037 0.2550 0.6107 0.033 Uiso 1 1 calc R . . C14 C 0.3525(4) 0.2997(3) 0.4636(3) 0.0254(7) Uani 1 1 d . . . H14 H 0.4206 0.3903 0.4904 0.031 Uiso 1 1 calc R . . C16 C 0.2610(4) 0.2473(3) 0.3515(3) 0.0209(7) Uani 1 1 d . . . C15 C 0.1624(4) 0.1119(3) 0.3158(3) 0.0265(7) Uani 1 1 d . . . H15 H 0.0981 0.0731 0.2414 0.032 Uiso 1 1 calc R . . C12 C 0.1599(4) 0.0349(3) 0.3910(3) 0.0287(8) Uani 1 1 d . . . H12 H 0.0941 -0.0562 0.3656 0.034 Uiso 1 1 calc R . . C7 C 0.6748(4) 0.3064(3) 0.1878(3) 0.0206(7) Uani 1 1 d . . . C6 C 0.6433(4) 0.3879(3) 0.1105(3) 0.0216(7) Uani 1 1 d . . . C17 C 0.2740(4) 0.3339(3) 0.2703(3) 0.0243(7) Uani 1 1 d . . . O6 O 0.7362(3) 0.4257(2) 0.04889(18) 0.0278(5) Uani 1 1 d . . . O1W O 0.0225(3) 0.3733(2) 0.00936(18) 0.0292(5) Uani 1 1 d D . . H2W H -0.0209 0.3255 -0.0558 0.044 Uiso 1 1 d RD . . H1W H -0.0418 0.3980 0.0259 0.044 Uiso 1 1 d RD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.02121(9) 0.01734(9) 0.01672(9) 0.01004(6) 0.00734(6) 0.01152(7) Cu1 0.0540(3) 0.0396(3) 0.0413(3) 0.0313(2) 0.0102(2) 0.0240(2) S2 0.0224(4) 0.0171(4) 0.0196(4) 0.0062(3) 0.0054(3) 0.0100(3) S1 0.0284(4) 0.0284(5) 0.0223(4) 0.0087(3) 0.0097(3) 0.0158(4) O3 0.0374(14) 0.0374(15) 0.0285(13) 0.0225(12) 0.0046(11) 0.0095(12) O2 0.0439(15) 0.0223(13) 0.0264(12) 0.0140(10) 0.0135(11) 0.0138(12) O1 0.0483(15) 0.0390(15) 0.0319(13) 0.0144(11) 0.0233(12) 0.0311(13) O4 0.0282(12) 0.0260(12) 0.0237(12) 0.0076(10) 0.0079(10) 0.0175(10) O9 0.0425(14) 0.0381(15) 0.0316(13) 0.0144(11) 0.0139(11) 0.0288(12) O10 0.0342(15) 0.0505(18) 0.0401(16) 0.0152(13) 0.0038(12) 0.0082(13) O5 0.0332(13) 0.0279(13) 0.0326(13) 0.0093(11) 0.0045(11) 0.0209(11) O7 0.0254(12) 0.0210(12) 0.0306(13) 0.0134(10) 0.0110(10) 0.0103(10) O8 0.0325(13) 0.0295(13) 0.0250(12) 0.0029(10) 0.0018(10) 0.0125(11) N1 0.0335(16) 0.0274(16) 0.0228(15) 0.0143(12) 0.0074(13) 0.0158(13) N2 0.0430(18) 0.0304(17) 0.0309(16) 0.0197(13) 0.0118(14) 0.0224(15) C20 0.0312(19) 0.048(2) 0.033(2) 0.0170(17) 0.0177(16) 0.0266(18) C19 0.039(2) 0.041(2) 0.0274(19) 0.0141(16) 0.0117(16) 0.0255(18) C18 0.0320(18) 0.0305(19) 0.0194(16) 0.0057(14) 0.0105(14) 0.0170(16) C22 0.0297(18) 0.036(2) 0.0272(18) 0.0104(15) 0.0142(15) 0.0205(16) C21 0.0328(19) 0.035(2) 0.0201(16) 0.0081(15) 0.0105(15) 0.0214(17) C8 0.040(2) 0.044(2) 0.048(2) 0.0311(19) 0.0271(18) 0.0322(19) C11 0.052(2) 0.053(3) 0.057(3) 0.044(2) 0.039(2) 0.035(2) C10 0.034(2) 0.048(2) 0.046(2) 0.031(2) 0.0156(18) 0.0271(19) C9 0.0276(18) 0.040(2) 0.038(2) 0.0249(17) 0.0148(16) 0.0203(17) C3 0.0304(18) 0.0191(17) 0.0308(18) 0.0130(14) 0.0177(15) 0.0133(15) C2 0.0262(17) 0.0158(16) 0.0271(17) 0.0087(13) 0.0114(14) 0.0114(14) C1 0.0311(19) 0.0295(19) 0.044(2) 0.0213(17) 0.0236(17) 0.0178(16) C5 0.0271(18) 0.0286(19) 0.040(2) 0.0169(16) 0.0194(16) 0.0173(16) C4 0.0271(17) 0.0156(16) 0.0235(17) 0.0082(13) 0.0075(14) 0.0107(14) C13 0.0340(19) 0.0273(19) 0.0221(17) 0.0120(15) 0.0067(15) 0.0132(16) C14 0.0308(18) 0.0192(17) 0.0272(18) 0.0098(14) 0.0090(15) 0.0102(15) C16 0.0236(16) 0.0248(17) 0.0241(17) 0.0148(14) 0.0128(14) 0.0145(14) C15 0.0309(18) 0.0278(19) 0.0192(17) 0.0073(14) 0.0010(14) 0.0135(16) C12 0.0346(19) 0.0216(18) 0.0308(19) 0.0136(15) 0.0075(16) 0.0114(16) C7 0.0255(17) 0.0201(17) 0.0197(16) 0.0093(13) 0.0070(13) 0.0115(14) C6 0.0254(17) 0.0168(16) 0.0225(17) 0.0081(13) 0.0034(14) 0.0095(14) C17 0.0311(18) 0.0288(19) 0.0272(18) 0.0168(15) 0.0160(15) 0.0199(16) O6 0.0343(13) 0.0283(13) 0.0256(12) 0.0172(11) 0.0092(11) 0.0145(11) O1W 0.0245(12) 0.0382(14) 0.0263(12) 0.0082(11) 0.0062(10) 0.0156(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O1 2.340(2) . ? Gd1 O5 2.356(2) . ? Gd1 O7 2.368(2) 2_665 ? Gd1 O4 2.399(2) . ? Gd1 O3 2.402(2) . ? Gd1 O6 2.412(2) 2_665 ? Gd1 O1W 2.439(2) . ? Gd1 O2 2.550(2) . ? Cu1 N2 1.877(3) 2_656 ? Cu1 N1 1.882(3) . ? S2 O8 1.436(2) . ? S2 O4 1.463(2) . ? S2 O7 1.463(2) . ? S2 C4 1.768(3) . ? S1 O10 1.432(3) . ? S1 O9 1.450(2) . ? S1 O1 1.475(2) . ? S1 C18 1.786(3) . ? O3 C17 1.263(4) . ? O2 C17 1.251(4) . ? O5 C6 1.253(4) . ? O7 Gd1 2.368(2) 2_665 ? N1 C12 1.339(4) . ? N1 C13 1.346(4) . ? N2 C11 1.332(4) . ? N2 C10 1.338(4) . ? N2 Cu1 1.877(3) 2_656 ? C20 C19 1.371(5) . ? C20 C21 1.413(5) . ? C20 H20 0.9300 . ? C19 C18 1.403(5) . ? C19 H19 0.9300 . ? C18 C22 1.363(5) . ? C22 C21 1.418(5) 2_566 ? C22 H22 0.9300 . ? C21 C21 1.415(6) 2_566 ? C21 C22 1.418(5) 2_566 ? C8 C7 1.369(4) . ? C8 C11 1.375(5) . ? C8 H8 0.9300 . ? C11 H11 0.9300 . ? C10 C9 1.373(5) . ? C10 H10 0.9300 . ? C9 C7 1.377(4) . ? C9 H9 0.9300 . ? C3 C4 1.370(4) . ? C3 C2 1.414(4) . ? C3 H3 0.9300 . ? C2 C1 1.407(4) . ? C2 C2 1.423(6) 2_655 ? C1 C5 1.363(5) 2_655 ? C1 H1 0.9300 . ? C5 C1 1.363(5) 2_655 ? C5 C4 1.402(4) . ? C5 H5 0.9300 . ? C13 C14 1.375(4) . ? C13 H13 0.9300 . ? C14 C16 1.385(4) . ? C14 H14 0.9300 . ? C16 C15 1.382(4) . ? C16 C17 1.506(4) . ? C15 C12 1.377(4) . ? C15 H15 0.9300 . ? C12 H12 0.9300 . ? C7 C6 1.511(4) . ? C6 O6 1.257(4) . ? O6 Gd1 2.412(2) 2_665 ? O1W H2W 0.8208 . ? O1W H1W 0.8108 . ? 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 Gd1 O5 142.49(8) . . ? O1 Gd1 O7 78.10(8) . 2_665 ? O5 Gd1 O7 74.18(8) . 2_665 ? O1 Gd1 O4 144.11(8) . . ? O5 Gd1 O4 73.39(7) . . ? O7 Gd1 O4 126.73(7) 2_665 . ? O1 Gd1 O3 96.26(9) . . ? O5 Gd1 O3 86.39(8) . . ? O7 Gd1 O3 135.41(8) 2_665 . ? O4 Gd1 O3 82.66(8) . . ? O1 Gd1 O6 81.02(8) . 2_665 ? O5 Gd1 O6 117.83(8) . 2_665 ? O7 Gd1 O6 80.25(7) 2_665 2_665 ? O4 Gd1 O6 79.05(7) . 2_665 ? O3 Gd1 O6 143.24(8) . 2_665 ? O1 Gd1 O1W 73.76(8) . . ? O5 Gd1 O1W 141.31(8) . . ? O7 Gd1 O1W 142.00(7) 2_665 . ? O4 Gd1 O1W 71.59(7) . . ? O3 Gd1 O1W 73.40(8) . . ? O6 Gd1 O1W 70.65(7) 2_665 . ? O1 Gd1 O2 75.92(8) . . ? O5 Gd1 O2 76.21(8) . . ? O7 Gd1 O2 83.33(7) 2_665 . ? O4 Gd1 O2 126.94(7) . . ? O3 Gd1 O2 52.83(7) . . ? O6 Gd1 O2 153.98(8) 2_665 . ? O1W Gd1 O2 113.26(7) . . ? N2 Cu1 N1 172.37(12) 2_656 . ? O8 S2 O4 112.61(14) . . ? O8 S2 O7 112.47(14) . . ? O4 S2 O7 111.85(13) . . ? O8 S2 C4 106.87(14) . . ? O4 S2 C4 106.70(13) . . ? O7 S2 C4 105.79(13) . . ? O10 S1 O9 114.20(16) . . ? O10 S1 O1 113.04(16) . . ? O9 S1 O1 110.35(14) . . ? O10 S1 C18 107.55(15) . . ? O9 S1 C18 106.77(15) . . ? O1 S1 C18 104.19(15) . . ? C17 O3 Gd1 95.3(2) . . ? C17 O2 Gd1 88.72(19) . . ? S1 O1 Gd1 163.28(16) . . ? S2 O4 Gd1 143.00(13) . . ? C6 O5 Gd1 174.5(2) . . ? S2 O7 Gd1 150.49(13) . 2_665 ? C12 N1 C13 118.2(3) . . ? C12 N1 Cu1 121.8(2) . . ? C13 N1 Cu1 119.7(2) . . ? C11 N2 C10 116.4(3) . . ? C11 N2 Cu1 120.7(2) . 2_656 ? C10 N2 Cu1 122.8(2) . 2_656 ? C19 C20 C21 121.4(3) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C20 C19 C18 118.9(3) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C22 C18 C19 121.6(3) . . ? C22 C18 S1 118.9(3) . . ? C19 C18 S1 119.4(3) . . ? C18 C22 C21 120.4(3) . 2_566 ? C18 C22 H22 119.8 . . ? C21 C22 H22 119.8 2_566 . ? C20 C21 C21 119.1(4) . 2_566 ? C20 C21 C22 122.3(3) . 2_566 ? C21 C21 C22 118.6(4) 2_566 2_566 ? C7 C8 C11 120.6(3) . . ? C7 C8 H8 119.7 . . ? C11 C8 H8 119.7 . . ? N2 C11 C8 122.9(3) . . ? N2 C11 H11 118.6 . . ? C8 C11 H11 118.6 . . ? N2 C10 C9 123.7(3) . . ? N2 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? C10 C9 C7 119.6(3) . . ? C10 C9 H9 120.2 . . ? C7 C9 H9 120.2 . . ? C4 C3 C2 120.3(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C1 C2 C3 122.2(3) . . ? C1 C2 C2 119.5(4) . 2_655 ? C3 C2 C2 118.3(3) . 2_655 ? C5 C1 C2 121.0(3) 2_655 . ? C5 C1 H1 119.5 2_655 . ? C2 C1 H1 119.5 . . ? C1 C5 C4 119.7(3) 2_655 . ? C1 C5 H5 120.2 2_655 . ? C4 C5 H5 120.2 . . ? C3 C4 C5 121.2(3) . . ? C3 C4 S2 118.8(2) . . ? C5 C4 S2 119.9(2) . . ? N1 C13 C14 121.8(3) . . ? N1 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C13 C14 C16 120.2(3) . . ? C13 C14 H14 119.9 . . ? C16 C14 H14 119.9 . . ? C15 C16 C14 117.6(3) . . ? C15 C16 C17 121.3(3) . . ? C14 C16 C17 121.1(3) . . ? C12 C15 C16 119.6(3) . . ? C12 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? N1 C12 C15 122.6(3) . . ? N1 C12 H12 118.7 . . ? C15 C12 H12 118.7 . . ? C8 C7 C9 116.8(3) . . ? C8 C7 C6 120.8(3) . . ? C9 C7 C6 122.3(3) . . ? O5 C6 O6 124.2(3) . . ? O5 C6 C7 118.3(3) . . ? O6 C6 C7 117.5(3) . . ? O2 C17 O3 122.8(3) . . ? O2 C17 C16 119.9(3) . . ? O3 C17 C16 117.2(3) . . ? C6 O6 Gd1 123.0(2) . 2_665 ? Gd1 O1W H2W 122.8 . . ? Gd1 O1W H1W 129.6 . . ? H2W O1W H1W 104.9 . . ? 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 O1 Gd1 O3 C17 -70.3(2) . . . . ? O5 Gd1 O3 C17 72.2(2) . . . . ? O7 Gd1 O3 C17 9.1(3) 2_665 . . . ? O4 Gd1 O3 C17 145.9(2) . . . . ? O6 Gd1 O3 C17 -153.62(18) 2_665 . . . ? O1W Gd1 O3 C17 -141.2(2) . . . . ? O2 Gd1 O3 C17 -3.22(18) . . . . ? O1 Gd1 O2 C17 112.6(2) . . . . ? O5 Gd1 O2 C17 -92.78(19) . . . . ? O7 Gd1 O2 C17 -168.07(19) 2_665 . . . ? O4 Gd1 O2 C17 -36.3(2) . . . . ? O3 Gd1 O2 C17 3.24(18) . . . . ? O6 Gd1 O2 C17 140.9(2) 2_665 . . . ? O1W Gd1 O2 C17 47.5(2) . . . . ? O10 S1 O1 Gd1 3.2(6) . . . . ? O9 S1 O1 Gd1 132.4(5) . . . . ? C18 S1 O1 Gd1 -113.3(5) . . . . ? O5 Gd1 O1 S1 18.6(6) . . . . ? O7 Gd1 O1 S1 -24.4(5) 2_665 . . . ? O4 Gd1 O1 S1 -163.1(4) . . . . ? O3 Gd1 O1 S1 110.8(5) . . . . ? O6 Gd1 O1 S1 -106.2(5) 2_665 . . . ? O1W Gd1 O1 S1 -178.5(5) . . . . ? O2 Gd1 O1 S1 61.7(5) . . . . ? O8 S2 O4 Gd1 -167.56(19) . . . . ? O7 S2 O4 Gd1 -39.7(2) . . . . ? C4 S2 O4 Gd1 75.5(2) . . . . ? O1 Gd1 O4 S2 157.91(18) . . . . ? O5 Gd1 O4 S2 -23.1(2) . . . . ? O7 Gd1 O4 S2 31.6(2) 2_665 . . . ? O3 Gd1 O4 S2 -111.5(2) . . . . ? O6 Gd1 O4 S2 100.5(2) 2_665 . . . ? O1W Gd1 O4 S2 173.6(2) . . . . ? O2 Gd1 O4 S2 -80.7(2) . . . . ? O1 Gd1 O5 C6 -92(2) . . . . ? O7 Gd1 O5 C6 -49(2) 2_665 . . . ? O4 Gd1 O5 C6 89(2) . . . . ? O3 Gd1 O5 C6 172(2) . . . . ? O6 Gd1 O5 C6 21(2) 2_665 . . . ? O1W Gd1 O5 C6 114(2) . . . . ? O2 Gd1 O5 C6 -135(2) . . . . ? O8 S2 O7 Gd1 159.2(2) . . . 2_665 ? O4 S2 O7 Gd1 31.3(3) . . . 2_665 ? C4 S2 O7 Gd1 -84.5(3) . . . 2_665 ? N2 Cu1 N1 C12 54.6(11) 2_656 . . . ? N2 Cu1 N1 C13 -118.6(9) 2_656 . . . ? C21 C20 C19 C18 1.5(5) . . . . ? C20 C19 C18 C22 -1.2(5) . . . . ? C20 C19 C18 S1 176.3(3) . . . . ? O10 S1 C18 C22 -55.0(3) . . . . ? O9 S1 C18 C22 -177.9(3) . . . . ? O1 S1 C18 C22 65.3(3) . . . . ? O10 S1 C18 C19 127.4(3) . . . . ? O9 S1 C18 C19 4.4(3) . . . . ? O1 S1 C18 C19 -112.4(3) . . . . ? C19 C18 C22 C21 0.4(5) . . . 2_566 ? S1 C18 C22 C21 -177.2(3) . . . 2_566 ? C19 C20 C21 C21 -0.9(6) . . . 2_566 ? C19 C20 C21 C22 179.2(3) . . . 2_566 ? C10 N2 C11 C8 0.9(6) . . . . ? Cu1 N2 C11 C8 -175.4(3) 2_656 . . . ? C7 C8 C11 N2 -0.2(6) . . . . ? C11 N2 C10 C9 -1.0(6) . . . . ? Cu1 N2 C10 C9 175.2(3) 2_656 . . . ? N2 C10 C9 C7 0.3(6) . . . . ? C4 C3 C2 C1 -178.9(3) . . . . ? C4 C3 C2 C2 -0.1(5) . . . 2_655 ? C3 C2 C1 C5 -179.8(3) . . . 2_655 ? C2 C2 C1 C5 1.5(6) 2_655 . . 2_655 ? C2 C3 C4 C5 -0.8(5) . . . . ? C2 C3 C4 S2 -178.2(2) . . . . ? C1 C5 C4 C3 0.5(5) 2_655 . . . ? C1 C5 C4 S2 177.9(3) 2_655 . . . ? O8 S2 C4 C3 95.4(3) . . . . ? O4 S2 C4 C3 -143.9(3) . . . . ? O7 S2 C4 C3 -24.7(3) . . . . ? O8 S2 C4 C5 -82.1(3) . . . . ? O4 S2 C4 C5 38.6(3) . . . . ? O7 S2 C4 C5 157.9(3) . . . . ? C12 N1 C13 C14 -1.1(5) . . . . ? Cu1 N1 C13 C14 172.4(3) . . . . ? N1 C13 C14 C16 1.2(5) . . . . ? C13 C14 C16 C15 -0.3(5) . . . . ? C13 C14 C16 C17 -177.7(3) . . . . ? C14 C16 C15 C12 -0.7(5) . . . . ? C17 C16 C15 C12 176.6(3) . . . . ? C13 N1 C12 C15 0.1(5) . . . . ? Cu1 N1 C12 C15 -173.3(3) . . . . ? C16 C15 C12 N1 0.9(5) . . . . ? C11 C8 C7 C9 -0.6(5) . . . . ? C11 C8 C7 C6 176.6(3) . . . . ? C10 C9 C7 C8 0.5(5) . . . . ? C10 C9 C7 C6 -176.6(3) . . . . ? Gd1 O5 C6 O6 -16(2) . . . . ? Gd1 O5 C6 C7 167(2) . . . . ? C8 C7 C6 O5 8.6(5) . . . . ? C9 C7 C6 O5 -174.4(3) . . . . ? C8 C7 C6 O6 -169.1(3) . . . . ? C9 C7 C6 O6 7.9(5) . . . . ? Gd1 O2 C17 O3 -5.8(3) . . . . ? Gd1 O2 C17 C16 171.0(3) . . . . ? Gd1 O3 C17 O2 6.2(3) . . . . ? Gd1 O3 C17 C16 -170.7(2) . . . . ? C15 C16 C17 O2 -171.9(3) . . . . ? C14 C16 C17 O2 5.4(5) . . . . ? C15 C16 C17 O3 5.1(5) . . . . ? C14 C16 C17 O3 -177.6(3) . . . . ? O5 C6 O6 Gd1 -5.0(4) . . . 2_665 ? C7 C6 O6 Gd1 172.52(19) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.377 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.090 # Attachment 'sm.cif' data_sm _database_code_depnum_ccdc_archive 'CCDC 768853' #TrackingRef 'sm.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H16 Cu N2 O11 S2 Sm' _chemical_formula_sum 'C22 H16 Cu N2 O11 S2 Sm' _chemical_formula_weight 762.42 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' Cu Cu 0.3201 1.2651 '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' S S 0.1246 0.1234 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5121(5) _cell_length_b 11.4333(6) _cell_length_c 12.3811(10) _cell_angle_alpha 99.4600(10) _cell_angle_beta 100.1680(10) _cell_angle_gamma 114.0120(10) _cell_volume 1168.14(13) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4958 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 28.05 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 746 _exptl_absorpt_coefficient_mu 3.647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.421 _exptl_absorpt_correction_T_max 0.482 _exptl_absorpt_process_details SADABS,Bruker(2002) _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 8340 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4204 _reflns_number_gt 3844 _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^)+(0.0180P)^2^+0.7126P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4204 _refine_ls_number_parameters 352 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0552 _refine_ls_wR_factor_gt 0.0536 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Sm1 Sm 0.31025(2) 0.466489(16) 0.096550(14) 0.01630(6) Uani 1 1 d . . . Cu1 Cu 0.26246(7) -0.02351(5) 0.59551(4) 0.04203(14) Uani 1 1 d . . . S2 S 0.30569(10) 0.22957(8) -0.14768(7) 0.01947(18) Uani 1 1 d . . . S1 S 0.21567(11) 0.71504(9) 0.27536(7) 0.0252(2) Uani 1 1 d . . . O3 O 0.1827(3) 0.2789(3) 0.1720(2) 0.0377(7) Uani 1 1 d . . . O2 O 0.3777(3) 0.4522(2) 0.3026(2) 0.0308(6) Uani 1 1 d . . . O1 O 0.2234(3) 0.6072(3) 0.1965(2) 0.0342(6) Uani 1 1 d . . . O4 O 0.2385(3) 0.2922(2) -0.07320(19) 0.0238(5) Uani 1 1 d . . . O9 O 0.1232(3) 0.7694(2) 0.2139(2) 0.0317(6) Uani 1 1 d . . . O10 O 0.3692(3) 0.8122(3) 0.3461(2) 0.0473(8) Uani 1 1 d . . . O5 O 0.5271(3) 0.4101(2) 0.1080(2) 0.0294(6) Uani 1 1 d . . . O7 O 0.4515(3) 0.3274(2) -0.1653(2) 0.0241(5) Uani 1 1 d . . . O8 O 0.1900(3) 0.1434(2) -0.2531(2) 0.0304(6) Uani 1 1 d . . . N1 N 0.2515(4) 0.0862(3) 0.4998(3) 0.0268(7) Uani 1 1 d . . . N2 N 0.7181(4) 0.1437(3) 0.3226(3) 0.0309(7) Uani 1 1 d . . . C20 C -0.1375(5) 0.5579(4) 0.4247(3) 0.0337(9) Uani 1 1 d . . . H20 H -0.2388 0.5519 0.4208 0.040 Uiso 1 1 calc R . . C19 C -0.0489(5) 0.6267(4) 0.3601(3) 0.0316(9) Uani 1 1 d . . . H19 H -0.0891 0.6684 0.3137 0.038 Uiso 1 1 calc R . . C18 C 0.1040(4) 0.6339(4) 0.3643(3) 0.0264(8) Uani 1 1 d . . . C22 C 0.1657(5) 0.5748(4) 0.4336(3) 0.0288(8) Uani 1 1 d . . . H22 H 0.2667 0.5809 0.4356 0.035 Uiso 1 1 calc R . . C21 C -0.0771(4) 0.4957(4) 0.4976(3) 0.0271(8) Uani 1 1 d . . . C8 C 0.5647(5) 0.2442(4) 0.2434(3) 0.0372(10) Uani 1 1 d . . . H8 H 0.4730 0.2565 0.2366 0.045 Uiso 1 1 calc R . . C11 C 0.5889(5) 0.1647(4) 0.3087(4) 0.0437(11) Uani 1 1 d . . . H11 H 0.5118 0.1235 0.3449 0.052 Uiso 1 1 calc R . . C10 C 0.8267(5) 0.2053(4) 0.2698(3) 0.0360(10) Uani 1 1 d . . . H10 H 0.9183 0.1928 0.2788 0.043 Uiso 1 1 calc R . . C9 C 0.8103(4) 0.2859(4) 0.2034(3) 0.0312(9) Uani 1 1 d . . . H9 H 0.8897 0.3269 0.1688 0.037 Uiso 1 1 calc R . . C3 C 0.5003(4) 0.1183(3) -0.0865(3) 0.0226(7) Uani 1 1 d . . . H3 H 0.5610 0.1656 -0.1299 0.027 Uiso 1 1 calc R . . C2 C 0.5482(4) 0.0363(3) -0.0319(3) 0.0236(8) Uani 1 1 d . . . C1 C 0.6877(4) 0.0234(4) -0.0401(3) 0.0300(9) Uani 1 1 d . . . H1 H 0.7509 0.0710 -0.0822 0.036 Uiso 1 1 calc R . . C5 C 0.2682(4) 0.0567(3) -0.0119(3) 0.0292(9) Uani 1 1 d . . . H5 H 0.1761 0.0644 -0.0057 0.035 Uiso 1 1 calc R . . C4 C 0.3649(4) 0.1284(3) -0.0759(3) 0.0209(7) Uani 1 1 d . . . C13 C 0.3449(5) 0.2174(4) 0.5350(3) 0.0279(8) Uani 1 1 d . . . H13 H 0.4054 0.2544 0.6105 0.033 Uiso 1 1 calc R . . C14 C 0.3550(4) 0.2991(3) 0.4647(3) 0.0251(8) Uani 1 1 d . . . H14 H 0.4239 0.3894 0.4918 0.030 Uiso 1 1 calc R . . C16 C 0.2623(4) 0.2472(3) 0.3523(3) 0.0208(7) Uani 1 1 d . . . C15 C 0.1633(4) 0.1123(4) 0.3165(3) 0.0273(8) Uani 1 1 d . . . H15 H 0.0985 0.0738 0.2422 0.033 Uiso 1 1 calc R . . C12 C 0.1609(4) 0.0354(3) 0.3912(3) 0.0288(9) Uani 1 1 d . . . H12 H 0.0941 -0.0554 0.3657 0.035 Uiso 1 1 calc R . . C7 C 0.6759(4) 0.3060(3) 0.1878(3) 0.0213(7) Uani 1 1 d . . . C6 C 0.6455(4) 0.3878(3) 0.1109(3) 0.0202(7) Uani 1 1 d . . . C17 C 0.2741(4) 0.3332(4) 0.2720(3) 0.0249(8) Uani 1 1 d . . . O6 O 0.7390(3) 0.4246(2) 0.0493(2) 0.0286(6) Uani 1 1 d . . . O1W O 0.0212(3) 0.3725(2) 0.0096(2) 0.0290(6) Uani 1 1 d D . . H2W H -0.0222 0.3247 -0.0555 0.043 Uiso 1 1 d RD . . H1W H -0.0431 0.3972 0.0261 0.043 Uiso 1 1 d RD . . 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 Sm1 0.02059(11) 0.01761(10) 0.01659(10) 0.00991(7) 0.00724(7) 0.01124(8) Cu1 0.0548(3) 0.0398(3) 0.0417(3) 0.0315(3) 0.0109(3) 0.0241(3) S2 0.0219(4) 0.0174(4) 0.0205(4) 0.0059(3) 0.0058(4) 0.0098(4) S1 0.0290(5) 0.0289(5) 0.0226(5) 0.0079(4) 0.0101(4) 0.0159(4) O3 0.0370(16) 0.0371(16) 0.0310(16) 0.0235(13) 0.0016(13) 0.0067(13) O2 0.0471(17) 0.0216(14) 0.0268(14) 0.0131(11) 0.0134(13) 0.0143(13) O1 0.0489(17) 0.0438(16) 0.0305(15) 0.0145(12) 0.0242(13) 0.0331(15) O4 0.0256(13) 0.0267(13) 0.0250(13) 0.0080(10) 0.0075(11) 0.0166(11) O9 0.0411(16) 0.0360(15) 0.0298(15) 0.0135(12) 0.0135(12) 0.0250(13) O10 0.0329(17) 0.0521(19) 0.0415(18) 0.0128(15) 0.0035(14) 0.0069(15) O5 0.0303(14) 0.0270(14) 0.0340(15) 0.0074(11) 0.0025(12) 0.0184(12) O7 0.0263(13) 0.0209(12) 0.0291(14) 0.0125(11) 0.0104(11) 0.0109(11) O8 0.0303(15) 0.0298(14) 0.0237(14) 0.0013(11) 0.0019(11) 0.0106(12) N1 0.0344(18) 0.0273(16) 0.0254(17) 0.0154(14) 0.0097(14) 0.0165(15) N2 0.042(2) 0.0302(17) 0.0303(18) 0.0193(14) 0.0120(15) 0.0207(16) C20 0.034(2) 0.049(2) 0.034(2) 0.0189(19) 0.0181(19) 0.028(2) C19 0.039(2) 0.040(2) 0.028(2) 0.0170(18) 0.0135(18) 0.025(2) C18 0.030(2) 0.032(2) 0.0219(19) 0.0064(16) 0.0113(16) 0.0174(17) C22 0.030(2) 0.037(2) 0.029(2) 0.0102(17) 0.0140(17) 0.0202(18) C21 0.032(2) 0.033(2) 0.0212(19) 0.0060(16) 0.0110(16) 0.0184(18) C8 0.045(2) 0.046(2) 0.052(3) 0.034(2) 0.032(2) 0.035(2) C11 0.052(3) 0.053(3) 0.056(3) 0.042(2) 0.038(2) 0.033(2) C10 0.034(2) 0.047(2) 0.044(3) 0.027(2) 0.012(2) 0.029(2) C9 0.027(2) 0.044(2) 0.038(2) 0.0277(19) 0.0160(18) 0.0213(19) C3 0.0262(19) 0.0188(17) 0.0266(19) 0.0099(15) 0.0138(16) 0.0097(15) C2 0.0259(19) 0.0179(17) 0.030(2) 0.0088(15) 0.0114(16) 0.0107(15) C1 0.032(2) 0.028(2) 0.042(2) 0.0231(18) 0.0221(19) 0.0153(18) C5 0.027(2) 0.0264(19) 0.044(2) 0.0145(17) 0.0165(18) 0.0155(17) C4 0.0246(19) 0.0126(16) 0.0250(19) 0.0066(14) 0.0084(15) 0.0067(15) C13 0.035(2) 0.029(2) 0.0181(18) 0.0077(15) 0.0038(16) 0.0144(18) C14 0.032(2) 0.0214(18) 0.0237(19) 0.0087(15) 0.0082(16) 0.0121(16) C16 0.0239(19) 0.0227(18) 0.0232(19) 0.0127(15) 0.0107(15) 0.0133(16) C15 0.030(2) 0.032(2) 0.0206(19) 0.0108(16) 0.0026(16) 0.0148(18) C12 0.032(2) 0.0217(19) 0.034(2) 0.0150(16) 0.0076(18) 0.0114(17) C7 0.029(2) 0.0226(18) 0.0164(17) 0.0078(14) 0.0070(15) 0.0144(16) C6 0.0244(19) 0.0170(17) 0.0181(18) 0.0050(14) 0.0028(15) 0.0091(15) C17 0.028(2) 0.032(2) 0.028(2) 0.0178(17) 0.0154(17) 0.0207(18) O6 0.0351(15) 0.0303(14) 0.0266(14) 0.0180(12) 0.0100(12) 0.0160(12) O1W 0.0237(14) 0.0364(15) 0.0280(14) 0.0083(11) 0.0082(11) 0.0142(12) _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 Sm1 O1 2.364(2) . ? Sm1 O5 2.387(2) . ? Sm1 O7 2.393(2) 2_665 ? Sm1 O4 2.422(2) . ? Sm1 O3 2.426(2) . ? Sm1 O6 2.439(2) 2_665 ? Sm1 O1W 2.458(2) . ? Sm1 O2 2.567(2) . ? Cu1 N1 1.881(3) . ? Cu1 N2 1.884(3) 2_656 ? S2 O8 1.440(3) . ? S2 O4 1.461(2) . ? S2 O7 1.465(2) . ? S2 C4 1.771(3) . ? S1 O10 1.429(3) . ? S1 O9 1.450(3) . ? S1 O1 1.477(2) . ? S1 C18 1.774(4) . ? O3 C17 1.266(4) . ? O2 C17 1.254(4) . ? O5 C6 1.248(4) . ? O7 Sm1 2.393(2) 2_665 ? N1 C13 1.339(5) . ? N1 C12 1.348(5) . ? N2 C11 1.332(5) . ? N2 C10 1.337(5) . ? N2 Cu1 1.884(3) 2_656 ? C20 C19 1.369(5) . ? C20 C21 1.419(5) . ? C20 H20 0.9300 . ? C19 C18 1.414(5) . ? C19 H19 0.9300 . ? C18 C22 1.369(5) . ? C22 C21 1.419(5) 2_566 ? C22 H22 0.9300 . ? C21 C21 1.419(7) 2_566 ? C21 C22 1.419(5) 2_566 ? C8 C11 1.371(5) . ? C8 C7 1.379(5) . ? C8 H8 0.9300 . ? C11 H11 0.9300 . ? C10 C9 1.368(5) . ? C10 H10 0.9300 . ? C9 C7 1.375(5) . ? C9 H9 0.9300 . ? C3 C4 1.365(5) . ? C3 C2 1.412(5) . ? C3 H3 0.9300 . ? C2 C2 1.415(7) 2_655 ? C2 C1 1.413(5) . ? C1 C5 1.357(5) 2_655 ? C1 H1 0.9300 . ? C5 C1 1.357(5) 2_655 ? C5 C4 1.415(5) . ? C5 H5 0.9300 . ? C13 C14 1.366(5) . ? C13 H13 0.9300 . ? C14 C16 1.391(5) . ? C14 H14 0.9300 . ? C16 C15 1.381(5) . ? C16 C17 1.496(5) . ? C15 C12 1.375(5) . ? C15 H15 0.9300 . ? C12 H12 0.9300 . ? C7 C6 1.510(4) . ? C6 O6 1.261(4) . ? O6 Sm1 2.439(2) 2_665 ? O1W H2W 0.8208 . ? O1W H1W 0.8129 . ? 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 Sm1 O5 142.35(9) . . ? O1 Sm1 O7 77.70(9) . 2_665 ? O5 Sm1 O7 74.13(8) . 2_665 ? O1 Sm1 O4 144.53(9) . . ? O5 Sm1 O4 73.11(8) . . ? O7 Sm1 O4 127.20(8) 2_665 . ? O1 Sm1 O3 96.27(9) . . ? O5 Sm1 O3 86.72(9) . . ? O7 Sm1 O3 135.21(8) 2_665 . ? O4 Sm1 O3 82.31(9) . . ? O1 Sm1 O6 80.57(8) . 2_665 ? O5 Sm1 O6 118.13(8) . 2_665 ? O7 Sm1 O6 80.59(8) 2_665 2_665 ? O4 Sm1 O6 79.80(8) . 2_665 ? O3 Sm1 O6 142.93(9) . 2_665 ? O1 Sm1 O1W 74.06(9) . . ? O5 Sm1 O1W 141.28(8) . . ? O7 Sm1 O1W 142.08(8) 2_665 . ? O4 Sm1 O1W 71.62(8) . . ? O3 Sm1 O1W 73.29(8) . . ? O6 Sm1 O1W 70.33(8) 2_665 . ? O1 Sm1 O2 75.89(8) . . ? O5 Sm1 O2 76.56(8) . . ? O7 Sm1 O2 83.51(8) 2_665 . ? O4 Sm1 O2 126.22(7) . . ? O3 Sm1 O2 52.41(8) . . ? O6 Sm1 O2 153.90(8) 2_665 . ? O1W Sm1 O2 112.89(8) . . ? N1 Cu1 N2 172.79(13) . 2_656 ? O8 S2 O4 112.57(15) . . ? O8 S2 O7 112.39(15) . . ? O4 S2 O7 111.78(14) . . ? O8 S2 C4 106.74(15) . . ? O4 S2 C4 106.93(14) . . ? O7 S2 C4 105.90(14) . . ? O10 S1 O9 114.24(17) . . ? O10 S1 O1 112.92(17) . . ? O9 S1 O1 110.33(15) . . ? O10 S1 C18 107.76(17) . . ? O9 S1 C18 106.81(16) . . ? O1 S1 C18 104.05(16) . . ? C17 O3 Sm1 95.6(2) . . ? C17 O2 Sm1 89.3(2) . . ? S1 O1 Sm1 164.43(18) . . ? S2 O4 Sm1 142.99(14) . . ? C6 O5 Sm1 175.7(2) . . ? S2 O7 Sm1 150.05(15) . 2_665 ? C13 N1 C12 117.7(3) . . ? C13 N1 Cu1 120.5(2) . . ? C12 N1 Cu1 121.6(2) . . ? C11 N2 C10 116.7(3) . . ? C11 N2 Cu1 120.9(3) . 2_656 ? C10 N2 Cu1 122.2(3) . 2_656 ? C19 C20 C21 121.0(3) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C20 C19 C18 119.7(3) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C22 C18 C19 120.8(3) . . ? C22 C18 S1 119.0(3) . . ? C19 C18 S1 120.2(3) . . ? C18 C22 C21 120.6(3) . 2_566 ? C18 C22 H22 119.7 . . ? C21 C22 H22 119.7 2_566 . ? C21 C21 C22 118.8(4) 2_566 2_566 ? C21 C21 C20 119.1(4) 2_566 . ? C22 C21 C20 122.1(3) 2_566 . ? C11 C8 C7 120.2(4) . . ? C11 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? N2 C11 C8 122.9(4) . . ? N2 C11 H11 118.6 . . ? C8 C11 H11 118.6 . . ? N2 C10 C9 123.5(3) . . ? N2 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? C10 C9 C7 119.7(3) . . ? C10 C9 H9 120.2 . . ? C7 C9 H9 120.2 . . ? C4 C3 C2 120.1(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C2 C2 118.6(4) . 2_655 ? C3 C2 C1 122.0(3) . . ? C2 C2 C1 119.3(4) 2_655 . ? C5 C1 C2 121.5(3) 2_655 . ? C5 C1 H1 119.3 2_655 . ? C2 C1 H1 119.3 . . ? C1 C5 C4 118.8(3) 2_655 . ? C1 C5 H5 120.6 2_655 . ? C4 C5 H5 120.6 . . ? C3 C4 C5 121.6(3) . . ? C3 C4 S2 119.1(3) . . ? C5 C4 S2 119.3(3) . . ? N1 C13 C14 122.7(3) . . ? N1 C13 H13 118.7 . . ? C14 C13 H13 118.7 . . ? C13 C14 C16 119.9(3) . . ? C13 C14 H14 120.0 . . ? C16 C14 H14 120.0 . . ? C15 C16 C14 117.5(3) . . ? C15 C16 C17 121.2(3) . . ? C14 C16 C17 121.3(3) . . ? C12 C15 C16 119.7(3) . . ? C12 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? N1 C12 C15 122.6(3) . . ? N1 C12 H12 118.7 . . ? C15 C12 H12 118.7 . . ? C8 C7 C9 117.0(3) . . ? C8 C7 C6 120.3(3) . . ? C9 C7 C6 122.7(3) . . ? O5 C6 O6 123.9(3) . . ? O5 C6 C7 118.9(3) . . ? O6 C6 C7 117.1(3) . . ? O2 C17 O3 122.4(3) . . ? O2 C17 C16 120.1(3) . . ? O3 C17 C16 117.3(3) . . ? C6 O6 Sm1 121.7(2) . 2_665 ? Sm1 O1W H2W 122.7 . . ? Sm1 O1W H1W 129.7 . . ? H2W O1W H1W 104.9 . . ? 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 O1 Sm1 O3 C17 -69.8(2) . . . . ? O5 Sm1 O3 C17 72.5(2) . . . . ? O7 Sm1 O3 C17 9.0(3) 2_665 . . . ? O4 Sm1 O3 C17 145.9(2) . . . . ? O6 Sm1 O3 C17 -152.49(19) 2_665 . . . ? O1W Sm1 O3 C17 -141.1(2) . . . . ? O2 Sm1 O3 C17 -3.05(19) . . . . ? O1 Sm1 O2 C17 112.7(2) . . . . ? O5 Sm1 O2 C17 -93.2(2) . . . . ? O7 Sm1 O2 C17 -168.4(2) 2_665 . . . ? O4 Sm1 O2 C17 -36.3(2) . . . . ? O3 Sm1 O2 C17 3.07(19) . . . . ? O6 Sm1 O2 C17 138.9(2) 2_665 . . . ? O1W Sm1 O2 C17 47.1(2) . . . . ? O10 S1 O1 Sm1 2.8(7) . . . . ? O9 S1 O1 Sm1 132.0(6) . . . . ? C18 S1 O1 Sm1 -113.8(6) . . . . ? O5 Sm1 O1 S1 18.5(7) . . . . ? O7 Sm1 O1 S1 -23.7(6) 2_665 . . . ? O4 Sm1 O1 S1 -163.2(5) . . . . ? O3 Sm1 O1 S1 111.2(6) . . . . ? O6 Sm1 O1 S1 -106.1(6) 2_665 . . . ? O1W Sm1 O1 S1 -178.2(6) . . . . ? O2 Sm1 O1 S1 62.6(6) . . . . ? O8 S2 O4 Sm1 -167.2(2) . . . . ? O7 S2 O4 Sm1 -39.6(3) . . . . ? C4 S2 O4 Sm1 75.9(3) . . . . ? O1 Sm1 O4 S2 157.92(19) . . . . ? O5 Sm1 O4 S2 -23.2(2) . . . . ? O7 Sm1 O4 S2 30.7(3) 2_665 . . . ? O3 Sm1 O4 S2 -112.1(2) . . . . ? O6 Sm1 O4 S2 100.6(2) 2_665 . . . ? O1W Sm1 O4 S2 173.1(2) . . . . ? O2 Sm1 O4 S2 -81.6(2) . . . . ? O1 Sm1 O5 C6 -85(3) . . . . ? O7 Sm1 O5 C6 -42(3) 2_665 . . . ? O4 Sm1 O5 C6 96(3) . . . . ? O3 Sm1 O5 C6 179(100) . . . . ? O6 Sm1 O5 C6 28(3) 2_665 . . . ? O1W Sm1 O5 C6 121(3) . . . . ? O2 Sm1 O5 C6 -129(3) . . . . ? O8 S2 O7 Sm1 160.0(2) . . . 2_665 ? O4 S2 O7 Sm1 32.2(3) . . . 2_665 ? C4 S2 O7 Sm1 -83.9(3) . . . 2_665 ? N2 Cu1 N1 C13 -117.3(11) 2_656 . . . ? N2 Cu1 N1 C12 56.9(12) 2_656 . . . ? C21 C20 C19 C18 1.2(6) . . . . ? C20 C19 C18 C22 -1.1(6) . . . . ? C20 C19 C18 S1 176.6(3) . . . . ? O10 S1 C18 C22 -56.0(3) . . . . ? O9 S1 C18 C22 -179.1(3) . . . . ? O1 S1 C18 C22 64.2(3) . . . . ? O10 S1 C18 C19 126.3(3) . . . . ? O9 S1 C18 C19 3.2(3) . . . . ? O1 S1 C18 C19 -113.6(3) . . . . ? C19 C18 C22 C21 0.3(6) . . . 2_566 ? S1 C18 C22 C21 -177.4(3) . . . 2_566 ? C19 C20 C21 C21 -0.6(7) . . . 2_566 ? C19 C20 C21 C22 179.2(4) . . . 2_566 ? C10 N2 C11 C8 0.5(7) . . . . ? Cu1 N2 C11 C8 -175.4(3) 2_656 . . . ? C7 C8 C11 N2 0.5(7) . . . . ? C11 N2 C10 C9 -0.5(6) . . . . ? Cu1 N2 C10 C9 175.3(3) 2_656 . . . ? N2 C10 C9 C7 -0.4(6) . . . . ? C4 C3 C2 C2 1.1(6) . . . 2_655 ? C4 C3 C2 C1 -179.7(3) . . . . ? C3 C2 C1 C5 -179.4(4) . . . 2_655 ? C2 C2 C1 C5 -0.2(7) 2_655 . . 2_655 ? C2 C3 C4 C5 -0.9(5) . . . . ? C2 C3 C4 S2 -178.8(3) . . . . ? C1 C5 C4 C3 0.2(5) 2_655 . . . ? C1 C5 C4 S2 178.2(3) 2_655 . . . ? O8 S2 C4 C3 95.8(3) . . . . ? O4 S2 C4 C3 -143.5(3) . . . . ? O7 S2 C4 C3 -24.2(3) . . . . ? O8 S2 C4 C5 -82.2(3) . . . . ? O4 S2 C4 C5 38.5(3) . . . . ? O7 S2 C4 C5 157.8(3) . . . . ? C12 N1 C13 C14 -2.2(5) . . . . ? Cu1 N1 C13 C14 172.2(3) . . . . ? N1 C13 C14 C16 2.0(6) . . . . ? C13 C14 C16 C15 -0.5(5) . . . . ? C13 C14 C16 C17 -178.1(3) . . . . ? C14 C16 C15 C12 -0.6(5) . . . . ? C17 C16 C15 C12 177.0(3) . . . . ? C13 N1 C12 C15 1.0(5) . . . . ? Cu1 N1 C12 C15 -173.4(3) . . . . ? C16 C15 C12 N1 0.4(6) . . . . ? C11 C8 C7 C9 -1.3(6) . . . . ? C11 C8 C7 C6 176.8(4) . . . . ? C10 C9 C7 C8 1.3(6) . . . . ? C10 C9 C7 C6 -176.8(3) . . . . ? Sm1 O5 C6 O6 -22(3) . . . . ? Sm1 O5 C6 C7 161(3) . . . . ? C8 C7 C6 O5 7.6(5) . . . . ? C9 C7 C6 O5 -174.4(3) . . . . ? C8 C7 C6 O6 -169.4(3) . . . . ? C9 C7 C6 O6 8.6(5) . . . . ? Sm1 O2 C17 O3 -5.5(3) . . . . ? Sm1 O2 C17 C16 170.3(3) . . . . ? Sm1 O3 C17 O2 5.9(4) . . . . ? Sm1 O3 C17 C16 -170.1(2) . . . . ? C15 C16 C17 O2 -171.8(3) . . . . ? C14 C16 C17 O2 5.7(5) . . . . ? C15 C16 C17 O3 4.2(5) . . . . ? C14 C16 C17 O3 -178.3(3) . . . . ? O5 C6 O6 Sm1 -4.4(5) . . . 2_665 ? C7 C6 O6 Sm1 172.4(2) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.412 _refine_diff_density_min -0.675 _refine_diff_density_rms 0.102 # Attachment 'tb.cif' data_tb _database_code_depnum_ccdc_archive 'CCDC 768854' #TrackingRef 'tb.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H16 Cu N2 O11 S2 Tb' _chemical_formula_sum 'C22 H16 Cu N2 O11 S2 Tb' _chemical_formula_weight 770.99 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' Cu Cu 0.3201 1.2651 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4951(6) _cell_length_b 11.3913(7) _cell_length_c 12.3599(13) _cell_angle_alpha 99.2940(10) _cell_angle_beta 100.2110(10) _cell_angle_gamma 113.9990(10) _cell_volume 1160.68(16) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4671 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.04 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 4.188 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.381 _exptl_absorpt_correction_T_max 0.433 _exptl_absorpt_process_details SADABS,Bruker(2002) _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 5987 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4180 _reflns_number_gt 3836 _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^)+(0.0306P)^2^+0.8648P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4180 _refine_ls_number_parameters 352 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0659 _refine_ls_wR_factor_gt 0.0649 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 0.30969(2) 0.466287(17) 0.095979(14) 0.01615(7) Uani 1 1 d . . . Cu1 Cu 0.25839(8) -0.02289(6) 0.59639(5) 0.04133(16) Uani 1 1 d . . . S2 S 0.30785(11) 0.23319(9) -0.14678(8) 0.0189(2) Uani 1 1 d . . . S1 S 0.21690(12) 0.71298(10) 0.27331(8) 0.0240(2) Uani 1 1 d . . . O3 O 0.1838(4) 0.2803(3) 0.1696(2) 0.0331(7) Uani 1 1 d . . . O2 O 0.3772(4) 0.4534(3) 0.3007(2) 0.0301(7) Uani 1 1 d . . . O1 O 0.2213(4) 0.6045(3) 0.1936(3) 0.0322(7) Uani 1 1 d . . . O4 O 0.2400(3) 0.2954(3) -0.0725(2) 0.0247(6) Uani 1 1 d . . . O9 O 0.1262(4) 0.7701(3) 0.2135(3) 0.0309(7) Uani 1 1 d . . . O10 O 0.3727(4) 0.8091(3) 0.3440(3) 0.0441(9) Uani 1 1 d . . . O5 O 0.5220(3) 0.4091(3) 0.1097(2) 0.0294(7) Uani 1 1 d . . . O7 O 0.4550(3) 0.3310(3) -0.1638(2) 0.0236(6) Uani 1 1 d . . . O8 O 0.1926(4) 0.1480(3) -0.2528(2) 0.0300(7) Uani 1 1 d . . . N1 N 0.2473(4) 0.0863(3) 0.4989(3) 0.0261(8) Uani 1 1 d . . . N2 N 0.7210(5) 0.1433(4) 0.3216(3) 0.0309(8) Uani 1 1 d . . . C20 C -0.1380(5) 0.5573(5) 0.4223(4) 0.0327(10) Uani 1 1 d . . . H20 H -0.2399 0.5509 0.4173 0.039 Uiso 1 1 calc R . . C19 C -0.0473(5) 0.6262(4) 0.3578(4) 0.0316(10) Uani 1 1 d . . . H19 H -0.0863 0.6685 0.3108 0.038 Uiso 1 1 calc R . . C18 C 0.1040(5) 0.6323(4) 0.3633(3) 0.0258(9) Uani 1 1 d . . . C22 C 0.1670(5) 0.5742(4) 0.4343(4) 0.0282(9) Uani 1 1 d . . . H22 H 0.2685 0.5807 0.4370 0.034 Uiso 1 1 calc R . . C21 C -0.0774(5) 0.4959(4) 0.4964(3) 0.0261(9) Uani 1 1 d . . . C8 C 0.5635(6) 0.2424(5) 0.2427(4) 0.0374(11) Uani 1 1 d . . . H8 H 0.4702 0.2526 0.2351 0.045 Uiso 1 1 calc R . . C11 C 0.5905(6) 0.1631(5) 0.3088(4) 0.0424(13) Uani 1 1 d . . . H11 H 0.5146 0.1218 0.3461 0.051 Uiso 1 1 calc R . . C10 C 0.8291(6) 0.2060(5) 0.2683(4) 0.0367(11) Uani 1 1 d . . . H10 H 0.9211 0.1938 0.2764 0.044 Uiso 1 1 calc R . . C9 C 0.8106(5) 0.2878(4) 0.2021(4) 0.0321(10) Uani 1 1 d . . . H9 H 0.8893 0.3302 0.1672 0.039 Uiso 1 1 calc R . . C3 C 0.5016(5) 0.1202(4) -0.0864(3) 0.0226(9) Uani 1 1 d . . . H3 H 0.5625 0.1679 -0.1297 0.027 Uiso 1 1 calc R . . C2 C 0.5489(5) 0.0369(4) -0.0324(3) 0.0227(8) Uani 1 1 d . . . C1 C 0.6890(5) 0.0240(4) -0.0393(4) 0.0300(10) Uani 1 1 d . . . H1 H 0.7541 0.0732 -0.0798 0.036 Uiso 1 1 calc R . . C5 C 0.2686(5) 0.0584(4) -0.0117(4) 0.0280(9) Uani 1 1 d . . . H5 H 0.1771 0.0671 -0.0050 0.034 Uiso 1 1 calc R . . C4 C 0.3666(5) 0.1307(4) -0.0750(3) 0.0210(8) Uani 1 1 d . . . C13 C 0.3410(5) 0.2179(4) 0.5347(4) 0.0280(9) Uani 1 1 d . . . H13 H 0.4003 0.2548 0.6105 0.034 Uiso 1 1 calc R . . C14 C 0.3525(5) 0.3006(4) 0.4634(3) 0.0249(9) Uani 1 1 d . . . H14 H 0.4215 0.3911 0.4900 0.030 Uiso 1 1 calc R . . C16 C 0.2601(5) 0.2472(4) 0.3511(3) 0.0210(8) Uani 1 1 d . . . C15 C 0.1606(5) 0.1117(4) 0.3149(3) 0.0264(9) Uani 1 1 d . . . H15 H 0.0960 0.0731 0.2405 0.032 Uiso 1 1 calc R . . C12 C 0.1585(5) 0.0347(4) 0.3905(4) 0.0299(10) Uani 1 1 d . . . H12 H 0.0929 -0.0565 0.3653 0.036 Uiso 1 1 calc R . . C7 C 0.6748(5) 0.3063(4) 0.1878(3) 0.0204(8) Uani 1 1 d . . . C6 C 0.6413(5) 0.3876(4) 0.1105(3) 0.0203(8) Uani 1 1 d . . . C17 C 0.2742(5) 0.3344(4) 0.2695(4) 0.0240(9) Uani 1 1 d . . . O6 O 0.7341(3) 0.4263(3) 0.0480(2) 0.0270(6) Uani 1 1 d . . . O1W O 0.0242(3) 0.3745(3) 0.0091(2) 0.0296(7) Uani 1 1 d D . . H2W H -0.0192 0.3267 -0.0560 0.044 Uiso 1 1 d RD . . H1W H -0.0401 0.3992 0.0256 0.044 Uiso 1 1 d RD . . 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 0.02118(11) 0.01715(11) 0.01672(11) 0.00984(7) 0.00599(8) 0.01252(8) Cu1 0.0528(4) 0.0395(3) 0.0421(4) 0.0308(3) 0.0087(3) 0.0248(3) S2 0.0213(5) 0.0171(5) 0.0205(5) 0.0063(4) 0.0044(4) 0.0107(4) S1 0.0274(5) 0.0272(5) 0.0223(5) 0.0083(4) 0.0085(4) 0.0156(4) O3 0.0315(17) 0.0370(18) 0.0267(16) 0.0216(14) -0.0005(13) 0.0101(14) O2 0.0434(18) 0.0220(15) 0.0302(16) 0.0141(13) 0.0120(14) 0.0163(14) O1 0.0464(19) 0.0393(18) 0.0296(16) 0.0144(14) 0.0197(14) 0.0312(16) O4 0.0300(16) 0.0273(15) 0.0240(15) 0.0079(12) 0.0064(12) 0.0196(13) O9 0.0383(18) 0.0360(17) 0.0310(16) 0.0127(13) 0.0115(14) 0.0264(15) O10 0.0330(19) 0.048(2) 0.041(2) 0.0153(16) 0.0025(15) 0.0103(16) O5 0.0326(17) 0.0290(16) 0.0340(17) 0.0105(13) 0.0021(13) 0.0229(14) O7 0.0269(15) 0.0202(14) 0.0291(15) 0.0128(12) 0.0085(12) 0.0128(12) O8 0.0302(16) 0.0294(16) 0.0234(15) 0.0016(12) -0.0003(12) 0.0115(13) N1 0.035(2) 0.0251(18) 0.0255(19) 0.0165(15) 0.0089(16) 0.0166(16) N2 0.040(2) 0.031(2) 0.031(2) 0.0191(16) 0.0097(17) 0.0222(18) C20 0.032(2) 0.048(3) 0.036(3) 0.018(2) 0.016(2) 0.029(2) C19 0.039(3) 0.041(3) 0.032(2) 0.018(2) 0.015(2) 0.030(2) C18 0.031(2) 0.032(2) 0.019(2) 0.0055(17) 0.0085(17) 0.0182(19) C22 0.029(2) 0.039(2) 0.026(2) 0.0106(19) 0.0119(18) 0.021(2) C21 0.032(2) 0.033(2) 0.022(2) 0.0076(17) 0.0101(18) 0.0212(19) C8 0.041(3) 0.047(3) 0.052(3) 0.032(2) 0.029(2) 0.033(2) C11 0.052(3) 0.052(3) 0.053(3) 0.040(3) 0.036(3) 0.034(3) C10 0.032(2) 0.044(3) 0.048(3) 0.030(2) 0.012(2) 0.024(2) C9 0.031(2) 0.039(3) 0.042(3) 0.027(2) 0.016(2) 0.023(2) C3 0.029(2) 0.0164(19) 0.028(2) 0.0113(16) 0.0138(18) 0.0116(17) C2 0.029(2) 0.0184(19) 0.028(2) 0.0098(16) 0.0122(18) 0.0150(17) C1 0.031(2) 0.027(2) 0.046(3) 0.022(2) 0.022(2) 0.0166(19) C5 0.026(2) 0.028(2) 0.043(3) 0.0170(19) 0.0175(19) 0.0181(19) C4 0.027(2) 0.0122(18) 0.024(2) 0.0054(15) 0.0048(17) 0.0091(16) C13 0.034(2) 0.032(2) 0.022(2) 0.0111(18) 0.0068(18) 0.017(2) C14 0.030(2) 0.021(2) 0.024(2) 0.0086(17) 0.0057(18) 0.0116(18) C16 0.023(2) 0.023(2) 0.026(2) 0.0154(17) 0.0110(17) 0.0134(17) C15 0.030(2) 0.029(2) 0.019(2) 0.0094(17) 0.0012(17) 0.0144(19) C12 0.034(2) 0.024(2) 0.032(2) 0.0139(19) 0.005(2) 0.0132(19) C7 0.028(2) 0.0185(19) 0.020(2) 0.0081(16) 0.0056(16) 0.0139(17) C6 0.027(2) 0.0190(19) 0.0175(19) 0.0070(15) 0.0017(16) 0.0132(17) C17 0.026(2) 0.030(2) 0.031(2) 0.0210(19) 0.0145(18) 0.0188(19) O6 0.0320(16) 0.0274(15) 0.0282(16) 0.0178(13) 0.0099(13) 0.0150(13) O1W 0.0255(16) 0.0377(17) 0.0274(16) 0.0093(13) 0.0078(13) 0.0151(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O1 2.337(3) . ? Tb1 O5 2.345(3) . ? Tb1 O7 2.354(3) 2_665 ? Tb1 O6 2.386(3) 2_665 ? Tb1 O3 2.386(3) . ? Tb1 O4 2.391(3) . ? Tb1 O1W 2.428(3) . ? Tb1 O2 2.541(3) . ? Cu1 N2 1.883(3) 2_656 ? Cu1 N1 1.885(3) . ? S2 O8 1.440(3) . ? S2 O4 1.460(3) . ? S2 O7 1.467(3) . ? S2 C4 1.775(4) . ? S1 O10 1.437(3) . ? S1 O9 1.448(3) . ? S1 O1 1.471(3) . ? S1 C18 1.784(4) . ? O3 C17 1.261(5) . ? O2 C17 1.250(5) . ? O5 C6 1.251(5) . ? O7 Tb1 2.354(3) 2_665 ? N1 C12 1.339(5) . ? N1 C13 1.341(5) . ? N2 C11 1.335(6) . ? N2 C10 1.339(6) . ? N2 Cu1 1.883(3) 2_656 ? C20 C19 1.374(6) . ? C20 C21 1.416(6) . ? C20 H20 0.9300 . ? C19 C18 1.398(6) . ? C19 H19 0.9300 . ? C18 C22 1.375(6) . ? C22 C21 1.421(6) 2_566 ? C22 H22 0.9300 . ? C21 C21 1.420(8) 2_566 ? C21 C22 1.421(6) 2_566 ? C8 C11 1.379(6) . ? C8 C7 1.376(6) . ? C8 H8 0.9300 . ? C11 H11 0.9300 . ? C10 C9 1.379(6) . ? C10 H10 0.9300 . ? C9 C7 1.374(6) . ? C9 H9 0.9300 . ? C3 C4 1.365(6) . ? C3 C2 1.411(6) . ? C3 H3 0.9300 . ? C2 C1 1.412(6) . ? C2 C2 1.433(8) 2_655 ? C1 C5 1.359(6) 2_655 ? C1 H1 0.9300 . ? C5 C1 1.359(6) 2_655 ? C5 C4 1.414(6) . ? C5 H5 0.9300 . ? C13 C14 1.376(6) . ? C13 H13 0.9300 . ? C14 C16 1.388(6) . ? C14 H14 0.9300 . ? C16 C15 1.385(6) . ? C16 C17 1.512(5) . ? C15 C12 1.378(6) . ? C15 H15 0.9300 . ? C12 H12 0.9300 . ? C7 C6 1.514(5) . ? C6 O6 1.266(5) . ? O6 Tb1 2.386(3) 2_665 ? O1W H2W 0.8204 . ? O1W H1W 0.8114 . ? 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 O5 142.52(11) . . ? O1 Tb1 O7 78.32(10) . 2_665 ? O5 Tb1 O7 74.25(10) . 2_665 ? O1 Tb1 O6 81.22(10) . 2_665 ? O5 Tb1 O6 117.95(10) . 2_665 ? O7 Tb1 O6 80.28(10) 2_665 2_665 ? O1 Tb1 O3 96.39(11) . . ? O5 Tb1 O3 85.80(11) . . ? O7 Tb1 O3 135.25(9) 2_665 . ? O6 Tb1 O3 143.50(10) 2_665 . ? O1 Tb1 O4 144.01(11) . . ? O5 Tb1 O4 73.44(10) . . ? O7 Tb1 O4 126.73(9) 2_665 . ? O6 Tb1 O4 78.98(10) 2_665 . ? O3 Tb1 O4 82.51(10) . . ? O1 Tb1 O1W 73.51(11) . . ? O5 Tb1 O1W 141.35(10) . . ? O7 Tb1 O1W 142.01(10) 2_665 . ? O6 Tb1 O1W 70.76(10) 2_665 . ? O3 Tb1 O1W 73.65(10) . . ? O4 Tb1 O1W 71.71(10) . . ? O1 Tb1 O2 75.89(10) . . ? O5 Tb1 O2 75.89(10) . . ? O7 Tb1 O2 83.06(9) 2_665 . ? O6 Tb1 O2 153.96(10) 2_665 . ? O3 Tb1 O2 53.01(9) . . ? O4 Tb1 O2 127.05(9) . . ? O1W Tb1 O2 113.39(10) . . ? N2 Cu1 N1 172.02(16) 2_656 . ? O8 S2 O4 112.43(18) . . ? O8 S2 O7 112.27(17) . . ? O4 S2 O7 112.16(16) . . ? O8 S2 C4 106.98(18) . . ? O4 S2 C4 107.00(17) . . ? O7 S2 C4 105.47(17) . . ? O10 S1 O9 114.1(2) . . ? O10 S1 O1 113.1(2) . . ? O9 S1 O1 110.43(18) . . ? O10 S1 C18 107.75(19) . . ? O9 S1 C18 106.5(2) . . ? O1 S1 C18 104.31(19) . . ? C17 O3 Tb1 95.4(2) . . ? C17 O2 Tb1 88.5(2) . . ? S1 O1 Tb1 162.8(2) . . ? S2 O4 Tb1 142.97(17) . . ? C6 O5 Tb1 173.6(3) . . ? S2 O7 Tb1 150.22(17) . 2_665 ? C12 N1 C13 118.4(4) . . ? C12 N1 Cu1 121.6(3) . . ? C13 N1 Cu1 119.7(3) . . ? C11 N2 C10 117.2(4) . . ? C11 N2 Cu1 120.2(3) . 2_656 ? C10 N2 Cu1 122.5(3) . 2_656 ? C19 C20 C21 120.5(4) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C19 C18 119.5(4) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C22 C18 C19 121.7(4) . . ? C22 C18 S1 118.6(3) . . ? C19 C18 S1 119.7(3) . . ? C18 C22 C21 120.2(4) . 2_566 ? C18 C22 H22 119.9 . . ? C21 C22 H22 119.9 2_566 . ? C20 C21 C21 120.0(5) . 2_566 ? C20 C21 C22 121.9(4) . 2_566 ? C21 C21 C22 118.1(5) 2_566 2_566 ? C11 C8 C7 119.9(4) . . ? C11 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? N2 C11 C8 122.7(4) . . ? N2 C11 H11 118.7 . . ? C8 C11 H11 118.7 . . ? N2 C10 C9 123.1(4) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? C7 C9 C10 119.5(4) . . ? C7 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C4 C3 C2 120.0(4) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C1 C2 C3 122.5(4) . . ? C1 C2 C2 118.8(5) . 2_655 ? C3 C2 C2 118.6(5) . 2_655 ? C5 C1 C2 121.7(4) 2_655 . ? C5 C1 H1 119.1 2_655 . ? C2 C1 H1 119.1 . . ? C1 C5 C4 118.7(4) 2_655 . ? C1 C5 H5 120.7 2_655 . ? C4 C5 H5 120.7 . . ? C3 C4 C5 122.1(4) . . ? C3 C4 S2 118.9(3) . . ? C5 C4 S2 119.0(3) . . ? N1 C13 C14 122.4(4) . . ? N1 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C13 C14 C16 119.2(4) . . ? C13 C14 H14 120.4 . . ? C16 C14 H14 120.4 . . ? C15 C16 C14 118.3(4) . . ? C15 C16 C17 121.1(4) . . ? C14 C16 C17 120.5(4) . . ? C12 C15 C16 119.1(4) . . ? C12 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? N1 C12 C15 122.5(4) . . ? N1 C12 H12 118.7 . . ? C15 C12 H12 118.7 . . ? C9 C7 C8 117.6(4) . . ? C9 C7 C6 122.5(4) . . ? C8 C7 C6 119.8(4) . . ? O5 C6 O6 124.2(4) . . ? O5 C6 C7 118.5(3) . . ? O6 C6 C7 117.3(4) . . ? O2 C17 O3 122.7(4) . . ? O2 C17 C16 120.0(4) . . ? O3 C17 C16 117.2(4) . . ? C6 O6 Tb1 123.9(3) . 2_665 ? Tb1 O1W H2W 122.8 . . ? Tb1 O1W H1W 129.7 . . ? H2W O1W H1W 104.9 . . ? 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 O1 Tb1 O3 C17 -69.9(3) . . . . ? O5 Tb1 O3 C17 72.5(3) . . . . ? O7 Tb1 O3 C17 9.9(3) 2_665 . . . ? O6 Tb1 O3 C17 -153.8(2) 2_665 . . . ? O4 Tb1 O3 C17 146.3(3) . . . . ? O1W Tb1 O3 C17 -140.6(3) . . . . ? O2 Tb1 O3 C17 -3.0(2) . . . . ? O1 Tb1 O2 C17 112.5(3) . . . . ? O5 Tb1 O2 C17 -92.4(2) . . . . ? O7 Tb1 O2 C17 -167.9(2) 2_665 . . . ? O6 Tb1 O2 C17 141.7(3) 2_665 . . . ? O3 Tb1 O2 C17 3.0(2) . . . . ? O4 Tb1 O2 C17 -36.4(3) . . . . ? O1W Tb1 O2 C17 47.8(3) . . . . ? O10 S1 O1 Tb1 3.3(7) . . . . ? O9 S1 O1 Tb1 132.5(6) . . . . ? C18 S1 O1 Tb1 -113.4(6) . . . . ? O5 Tb1 O1 S1 19.2(7) . . . . ? O7 Tb1 O1 S1 -24.4(6) 2_665 . . . ? O6 Tb1 O1 S1 -106.2(6) 2_665 . . . ? O3 Tb1 O1 S1 110.6(6) . . . . ? O4 Tb1 O1 S1 -163.4(6) . . . . ? O1W Tb1 O1 S1 -178.6(7) . . . . ? O2 Tb1 O1 S1 61.3(6) . . . . ? O8 S2 O4 Tb1 -167.3(2) . . . . ? O7 S2 O4 Tb1 -39.7(3) . . . . ? C4 S2 O4 Tb1 75.5(3) . . . . ? O1 Tb1 O4 S2 157.9(2) . . . . ? O5 Tb1 O4 S2 -23.7(3) . . . . ? O7 Tb1 O4 S2 31.2(3) 2_665 . . . ? O6 Tb1 O4 S2 100.1(3) 2_665 . . . ? O3 Tb1 O4 S2 -111.5(3) . . . . ? O1W Tb1 O4 S2 173.3(3) . . . . ? O2 Tb1 O4 S2 -80.8(3) . . . . ? O1 Tb1 O5 C6 -97(2) . . . . ? O7 Tb1 O5 C6 -52(2) 2_665 . . . ? O6 Tb1 O5 C6 17(2) 2_665 . . . ? O3 Tb1 O5 C6 168(2) . . . . ? O4 Tb1 O5 C6 85(2) . . . . ? O1W Tb1 O5 C6 111(2) . . . . ? O2 Tb1 O5 C6 -139(2) . . . . ? O8 S2 O7 Tb1 159.3(3) . . . 2_665 ? O4 S2 O7 Tb1 31.6(4) . . . 2_665 ? C4 S2 O7 Tb1 -84.6(4) . . . 2_665 ? N2 Cu1 N1 C12 56.2(13) 2_656 . . . ? N2 Cu1 N1 C13 -117.6(11) 2_656 . . . ? C21 C20 C19 C18 1.8(7) . . . . ? C20 C19 C18 C22 -1.9(7) . . . . ? C20 C19 C18 S1 176.2(3) . . . . ? O10 S1 C18 C22 -54.3(4) . . . . ? O9 S1 C18 C22 -177.1(3) . . . . ? O1 S1 C18 C22 66.0(4) . . . . ? O10 S1 C18 C19 127.5(4) . . . . ? O9 S1 C18 C19 4.7(4) . . . . ? O1 S1 C18 C19 -112.1(4) . . . . ? C19 C18 C22 C21 0.8(7) . . . 2_566 ? S1 C18 C22 C21 -177.3(3) . . . 2_566 ? C19 C20 C21 C21 -0.7(8) . . . 2_566 ? C19 C20 C21 C22 178.9(4) . . . 2_566 ? C10 N2 C11 C8 1.1(8) . . . . ? Cu1 N2 C11 C8 -175.0(4) 2_656 . . . ? C7 C8 C11 N2 -0.9(8) . . . . ? C11 N2 C10 C9 -0.3(7) . . . . ? Cu1 N2 C10 C9 175.7(4) 2_656 . . . ? N2 C10 C9 C7 -0.7(8) . . . . ? C4 C3 C2 C1 -178.8(4) . . . . ? C4 C3 C2 C2 1.0(7) . . . 2_655 ? C3 C2 C1 C5 -178.9(4) . . . 2_655 ? C2 C2 C1 C5 1.4(8) 2_655 . . 2_655 ? C2 C3 C4 C5 -1.1(6) . . . . ? C2 C3 C4 S2 -178.5(3) . . . . ? C1 C5 C4 C3 0.0(6) 2_655 . . . ? C1 C5 C4 S2 177.4(3) 2_655 . . . ? O8 S2 C4 C3 95.2(3) . . . . ? O4 S2 C4 C3 -144.1(3) . . . . ? O7 S2 C4 C3 -24.5(4) . . . . ? O8 S2 C4 C5 -82.3(3) . . . . ? O4 S2 C4 C5 38.4(4) . . . . ? O7 S2 C4 C5 158.0(3) . . . . ? C12 N1 C13 C14 -2.1(7) . . . . ? Cu1 N1 C13 C14 172.0(3) . . . . ? N1 C13 C14 C16 2.3(7) . . . . ? C13 C14 C16 C15 -0.8(6) . . . . ? C13 C14 C16 C17 -177.9(4) . . . . ? C14 C16 C15 C12 -0.9(6) . . . . ? C17 C16 C15 C12 176.2(4) . . . . ? C13 N1 C12 C15 0.3(7) . . . . ? Cu1 N1 C12 C15 -173.6(3) . . . . ? C16 C15 C12 N1 1.2(7) . . . . ? C10 C9 C7 C8 0.8(7) . . . . ? C10 C9 C7 C6 -176.1(4) . . . . ? C11 C8 C7 C9 -0.1(7) . . . . ? C11 C8 C7 C6 176.9(4) . . . . ? Tb1 O5 C6 O6 -12(3) . . . . ? Tb1 O5 C6 C7 170(2) . . . . ? C9 C7 C6 O5 -174.0(4) . . . . ? C8 C7 C6 O5 9.2(6) . . . . ? C9 C7 C6 O6 8.0(6) . . . . ? C8 C7 C6 O6 -168.8(4) . . . . ? Tb1 O2 C17 O3 -5.4(4) . . . . ? Tb1 O2 C17 C16 171.3(3) . . . . ? Tb1 O3 C17 O2 5.8(4) . . . . ? Tb1 O3 C17 C16 -171.0(3) . . . . ? C15 C16 C17 O2 -172.2(4) . . . . ? C14 C16 C17 O2 4.9(6) . . . . ? C15 C16 C17 O3 4.7(6) . . . . ? C14 C16 C17 O3 -178.3(4) . . . . ? O5 C6 O6 Tb1 -5.2(5) . . . 2_665 ? C7 C6 O6 Tb1 172.7(2) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.678 _refine_diff_density_min -1.114 _refine_diff_density_rms 0.133 # Attachment 'er.cif' data_er _database_code_depnum_ccdc_archive 'CCDC 772500' #TrackingRef 'er.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H16 Cu Er N2 O11 S2' _chemical_formula_sum 'C22 H16 Cu Er N2 O11 S2' _chemical_formula_weight 779.32 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.528(2) _cell_length_b 11.338(3) _cell_length_c 12.282(5) _cell_angle_alpha 99.109(3) _cell_angle_beta 100.275(3) _cell_angle_gamma 114.053(2) _cell_volume 1152.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8782 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.84 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 758 _exptl_absorpt_coefficient_mu 4.792 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.329 _exptl_absorpt_correction_T_max 0.384 _exptl_absorpt_process_details SADABS,Bruker(2002) _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 10838 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4148 _reflns_number_gt 3901 _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^)+(0.0151P)^2^+1.1587P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4148 _refine_ls_number_parameters 352 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0217 _refine_ls_R_factor_gt 0.0201 _refine_ls_wR_factor_ref 0.0487 _refine_ls_wR_factor_gt 0.0479 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.028 _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 Er1 Er 0.310490(16) 0.466922(13) 0.096046(11) 0.01720(6) Uani 1 1 d . . . Cu1 Cu 0.25376(6) -0.02429(5) 0.59636(4) 0.04212(13) Uani 1 1 d . . . S2 S 0.31030(9) 0.23563(7) -0.14585(6) 0.01923(16) Uani 1 1 d . . . S1 S 0.21916(10) 0.71232(8) 0.27233(7) 0.02323(17) Uani 1 1 d . . . O3 O 0.1825(3) 0.2823(2) 0.1673(2) 0.0348(6) Uani 1 1 d . . . O2 O 0.3760(3) 0.4545(2) 0.2994(2) 0.0305(5) Uani 1 1 d . . . O1 O 0.2235(3) 0.6035(2) 0.1920(2) 0.0327(6) Uani 1 1 d . . . O4 O 0.2425(3) 0.2982(2) -0.07127(18) 0.0248(5) Uani 1 1 d . . . O9 O 0.1294(3) 0.7700(2) 0.2118(2) 0.0310(5) Uani 1 1 d . . . O10 O 0.3737(3) 0.8082(3) 0.3434(2) 0.0436(7) Uani 1 1 d . . . O5 O 0.5156(3) 0.4079(2) 0.1120(2) 0.0297(5) Uani 1 1 d . . . O7 O 0.4565(3) 0.3334(2) -0.16314(19) 0.0243(5) Uani 1 1 d . . . O8 O 0.1954(3) 0.1506(2) -0.25236(19) 0.0294(5) Uani 1 1 d . . . N1 N 0.2441(3) 0.0852(3) 0.4983(2) 0.0264(6) Uani 1 1 d . . . N2 N 0.7244(4) 0.1451(3) 0.3217(2) 0.0308(7) Uani 1 1 d . . . C20 C -0.1343(4) 0.5595(4) 0.4226(3) 0.0314(8) Uani 1 1 d . . . H20 H -0.2349 0.5550 0.4181 0.038 Uiso 1 1 calc R . . C19 C -0.0448(4) 0.6269(4) 0.3570(3) 0.0302(8) Uani 1 1 d . . . H19 H -0.0834 0.6693 0.3093 0.036 Uiso 1 1 calc R . . C18 C 0.1062(4) 0.6317(3) 0.3624(3) 0.0240(7) Uani 1 1 d . . . C22 C 0.1662(4) 0.5721(4) 0.4338(3) 0.0278(7) Uani 1 1 d . . . H22 H 0.2666 0.5770 0.4365 0.033 Uiso 1 1 calc R . . C21 C -0.0769(4) 0.4966(3) 0.4969(3) 0.0239(7) Uani 1 1 d . . . C8 C 0.5645(5) 0.2434(4) 0.2453(3) 0.0358(9) Uani 1 1 d . . . H8 H 0.4717 0.2538 0.2396 0.043 Uiso 1 1 calc R . . C11 C 0.5933(5) 0.1643(4) 0.3107(4) 0.0423(10) Uani 1 1 d . . . H11 H 0.5190 0.1223 0.3490 0.051 Uiso 1 1 calc R . . C10 C 0.8287(4) 0.2084(4) 0.2668(3) 0.0355(9) Uani 1 1 d . . . H10 H 0.9210 0.1971 0.2738 0.043 Uiso 1 1 calc R . . C9 C 0.8071(4) 0.2897(4) 0.2003(3) 0.0312(8) Uani 1 1 d . . . H9 H 0.8839 0.3324 0.1640 0.037 Uiso 1 1 calc R . . C3 C 0.5013(4) 0.1204(3) -0.0864(3) 0.0236(7) Uani 1 1 d . . . H3 H 0.5616 0.1679 -0.1305 0.028 Uiso 1 1 calc R . . C2 C 0.5487(4) 0.0368(3) -0.0323(3) 0.0226(7) Uani 1 1 d . . . C1 C 0.6873(4) 0.0229(3) -0.0413(3) 0.0294(8) Uani 1 1 d . . . H1 H 0.7507 0.0707 -0.0838 0.035 Uiso 1 1 calc R . . C5 C 0.2705(4) 0.0593(3) -0.0111(3) 0.0275(7) Uani 1 1 d . . . H5 H 0.1786 0.0673 -0.0051 0.033 Uiso 1 1 calc R . . C4 C 0.3669(4) 0.1321(3) -0.0745(3) 0.0212(7) Uani 1 1 d . . . C13 C 0.3390(4) 0.2175(3) 0.5337(3) 0.0289(8) Uani 1 1 d . . . H13 H 0.3992 0.2543 0.6097 0.035 Uiso 1 1 calc R . . C14 C 0.3504(4) 0.3001(3) 0.4624(3) 0.0256(7) Uani 1 1 d . . . H14 H 0.4196 0.3909 0.4894 0.031 Uiso 1 1 calc R . . C16 C 0.2588(4) 0.2482(3) 0.3499(3) 0.0213(7) Uani 1 1 d . . . C15 C 0.1586(4) 0.1121(3) 0.3131(3) 0.0279(7) Uani 1 1 d . . . H15 H 0.0947 0.0738 0.2381 0.033 Uiso 1 1 calc R . . C12 C 0.1550(4) 0.0346(3) 0.3888(3) 0.0281(7) Uani 1 1 d . . . H12 H 0.0881 -0.0568 0.3633 0.034 Uiso 1 1 calc R . . C7 C 0.6718(4) 0.3073(3) 0.1881(3) 0.0216(7) Uani 1 1 d . . . C6 C 0.6357(4) 0.3884(3) 0.1111(3) 0.0221(7) Uani 1 1 d . . . C17 C 0.2731(4) 0.3352(3) 0.2683(3) 0.0253(7) Uani 1 1 d . . . O6 O 0.7257(3) 0.4280(2) 0.04781(19) 0.0281(5) Uani 1 1 d . . . O1W O 0.0303(3) 0.3772(2) 0.0093(2) 0.0314(6) Uani 1 1 d D . . H2W H -0.0131 0.3294 -0.0558 0.047 Uiso 1 1 d RD . . H1W H -0.0340 0.4019 0.0258 0.047 Uiso 1 1 d RD . . 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 Er1 0.02597(9) 0.01675(8) 0.01422(8) 0.01010(6) 0.00638(6) 0.01208(6) Cu1 0.0567(3) 0.0387(3) 0.0398(3) 0.0314(2) 0.0078(2) 0.0242(2) S2 0.0254(4) 0.0162(4) 0.0172(4) 0.0064(3) 0.0045(3) 0.0101(3) S1 0.0293(4) 0.0249(4) 0.0193(4) 0.0089(3) 0.0087(3) 0.0138(3) O3 0.0372(14) 0.0332(14) 0.0251(13) 0.0190(11) 0.0007(11) 0.0062(11) O2 0.0464(15) 0.0234(13) 0.0265(13) 0.0149(10) 0.0129(11) 0.0158(11) O1 0.0515(15) 0.0347(14) 0.0282(13) 0.0137(11) 0.0217(12) 0.0283(12) O4 0.0321(12) 0.0254(12) 0.0227(12) 0.0078(10) 0.0079(10) 0.0176(10) O9 0.0431(14) 0.0347(14) 0.0289(13) 0.0168(11) 0.0154(11) 0.0252(12) O10 0.0358(14) 0.0450(16) 0.0354(15) 0.0125(13) 0.0023(12) 0.0064(12) O5 0.0361(13) 0.0266(13) 0.0315(13) 0.0103(10) 0.0027(11) 0.0205(11) O7 0.0309(12) 0.0194(11) 0.0257(12) 0.0134(9) 0.0097(10) 0.0107(10) O8 0.0323(13) 0.0275(13) 0.0217(12) 0.0029(10) 0.0009(10) 0.0108(10) N1 0.0343(16) 0.0251(15) 0.0250(15) 0.0155(12) 0.0079(12) 0.0151(13) N2 0.0442(18) 0.0302(16) 0.0271(15) 0.0188(13) 0.0089(14) 0.0215(14) C20 0.0316(18) 0.046(2) 0.0315(19) 0.0185(17) 0.0163(16) 0.0251(17) C19 0.040(2) 0.037(2) 0.0269(18) 0.0145(16) 0.0132(16) 0.0257(17) C18 0.0301(17) 0.0266(17) 0.0170(15) 0.0059(13) 0.0089(14) 0.0131(14) C22 0.0319(18) 0.039(2) 0.0209(17) 0.0113(15) 0.0117(14) 0.0210(16) C21 0.0323(17) 0.0282(18) 0.0178(15) 0.0067(13) 0.0099(13) 0.0182(14) C8 0.046(2) 0.044(2) 0.046(2) 0.0310(19) 0.0290(19) 0.0331(19) C11 0.056(3) 0.051(2) 0.051(2) 0.040(2) 0.036(2) 0.035(2) C10 0.0334(19) 0.040(2) 0.045(2) 0.0257(18) 0.0106(17) 0.0223(17) C9 0.0301(18) 0.040(2) 0.038(2) 0.0276(17) 0.0164(16) 0.0201(16) C3 0.0315(17) 0.0170(16) 0.0265(17) 0.0116(13) 0.0136(14) 0.0103(14) C2 0.0296(17) 0.0151(15) 0.0275(17) 0.0095(13) 0.0121(14) 0.0109(13) C1 0.0358(19) 0.0265(18) 0.037(2) 0.0201(16) 0.0218(16) 0.0156(15) C5 0.0297(18) 0.0277(18) 0.037(2) 0.0177(15) 0.0172(16) 0.0178(15) C4 0.0283(17) 0.0137(15) 0.0214(16) 0.0067(13) 0.0032(13) 0.0096(13) C13 0.0378(19) 0.0307(19) 0.0192(17) 0.0120(14) 0.0045(15) 0.0157(16) C14 0.0317(18) 0.0215(17) 0.0234(17) 0.0095(14) 0.0072(14) 0.0107(14) C16 0.0251(16) 0.0255(17) 0.0225(17) 0.0144(14) 0.0110(13) 0.0153(14) C15 0.0343(18) 0.0281(18) 0.0195(17) 0.0105(14) 0.0024(14) 0.0127(15) C12 0.0343(18) 0.0215(17) 0.0281(18) 0.0140(14) 0.0063(15) 0.0104(15) C7 0.0325(17) 0.0208(16) 0.0165(15) 0.0090(13) 0.0065(13) 0.0151(14) C6 0.0321(18) 0.0149(15) 0.0174(16) 0.0049(13) 0.0008(14) 0.0110(13) C17 0.0304(18) 0.0313(19) 0.0275(18) 0.0179(15) 0.0153(15) 0.0195(16) O6 0.0399(14) 0.0263(12) 0.0219(12) 0.0178(10) 0.0091(11) 0.0140(11) O1W 0.0313(13) 0.0411(15) 0.0254(12) 0.0104(11) 0.0072(10) 0.0190(11) _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 Er1 O5 2.297(2) . ? Er1 O1 2.299(2) . ? Er1 O7 2.322(2) 2_665 ? Er1 O6 2.334(2) 2_665 ? Er1 O3 2.348(2) . ? Er1 O4 2.361(2) . ? Er1 O1W 2.393(2) . ? Er1 O2 2.505(3) . ? Cu1 N2 1.878(3) 2_656 ? Cu1 N1 1.878(3) . ? S2 O8 1.438(2) . ? S2 O7 1.461(2) . ? S2 O4 1.462(2) . ? S2 C4 1.763(3) . ? S1 O10 1.431(3) . ? S1 O9 1.448(2) . ? S1 O1 1.473(2) . ? S1 C18 1.778(3) . ? O3 C17 1.266(4) . ? O2 C17 1.249(4) . ? O5 C6 1.252(4) . ? O7 Er1 2.322(2) 2_665 ? N1 C13 1.343(4) . ? N1 C12 1.346(4) . ? N2 C10 1.329(5) . ? N2 C11 1.341(5) . ? N2 Cu1 1.878(3) 2_656 ? C20 C19 1.367(5) . ? C20 C21 1.409(5) . ? C20 H20 0.9300 . ? C19 C18 1.407(5) . ? C19 H19 0.9300 . ? C18 C22 1.369(5) . ? C22 C21 1.409(5) 2_566 ? C22 H22 0.9300 . ? C21 C22 1.409(5) 2_566 ? C21 C21 1.422(6) 2_566 ? C8 C11 1.369(5) . ? C8 C7 1.370(5) . ? C8 H8 0.9300 . ? C11 H11 0.9300 . ? C10 C9 1.376(5) . ? C10 H10 0.9300 . ? C9 C7 1.369(5) . ? C9 H9 0.9300 . ? C3 C4 1.371(5) . ? C3 C2 1.409(5) . ? C3 H3 0.9300 . ? C2 C1 1.413(5) . ? C2 C2 1.424(6) 2_655 ? C1 C5 1.360(5) 2_655 ? C1 H1 0.9300 . ? C5 C1 1.360(5) 2_655 ? C5 C4 1.404(5) . ? C5 H5 0.9300 . ? C13 C14 1.367(5) . ? C13 H13 0.9300 . ? C14 C16 1.382(5) . ? C14 H14 0.9300 . ? C16 C15 1.386(5) . ? C16 C17 1.500(4) . ? C15 C12 1.372(5) . ? C15 H15 0.9300 . ? C12 H12 0.9300 . ? C7 C6 1.508(4) . ? C6 O6 1.256(4) . ? O6 Er1 2.334(2) 2_665 ? O1W H2W 0.8167 . ? O1W H1W 0.8127 . ? 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 O5 Er1 O1 142.45(9) . . ? O5 Er1 O7 74.36(8) . 2_665 ? O1 Er1 O7 78.86(9) . 2_665 ? O5 Er1 O6 117.29(9) . 2_665 ? O1 Er1 O6 82.61(9) . 2_665 ? O7 Er1 O6 79.95(8) 2_665 2_665 ? O5 Er1 O3 85.53(9) . . ? O1 Er1 O3 96.10(9) . . ? O7 Er1 O3 135.85(8) 2_665 . ? O6 Er1 O3 143.49(8) 2_665 . ? O5 Er1 O4 73.50(8) . . ? O1 Er1 O4 144.00(8) . . ? O7 Er1 O4 126.22(8) 2_665 . ? O6 Er1 O4 78.05(8) 2_665 . ? O3 Er1 O4 82.43(9) . . ? O5 Er1 O1W 141.14(8) . . ? O1 Er1 O1W 73.34(9) . . ? O7 Er1 O1W 142.27(8) 2_665 . ? O6 Er1 O1W 71.69(8) 2_665 . ? O3 Er1 O1W 73.02(8) . . ? O4 Er1 O1W 71.86(8) . . ? O5 Er1 O2 75.28(8) . . ? O1 Er1 O2 75.72(8) . . ? O7 Er1 O2 82.90(8) 2_665 . ? O6 Er1 O2 154.56(8) 2_665 . ? O3 Er1 O2 53.78(8) . . ? O4 Er1 O2 127.38(8) . . ? O1W Er1 O2 113.52(8) . . ? N2 Cu1 N1 171.28(13) 2_656 . ? O8 S2 O7 112.17(14) . . ? O8 S2 O4 112.29(14) . . ? O7 S2 O4 112.23(13) . . ? O8 S2 C4 106.72(14) . . ? O7 S2 C4 105.84(14) . . ? O4 S2 C4 107.07(14) . . ? O10 S1 O9 114.06(16) . . ? O10 S1 O1 113.09(16) . . ? O9 S1 O1 110.29(15) . . ? O10 S1 C18 107.70(16) . . ? O9 S1 C18 106.44(15) . . ? O1 S1 C18 104.54(15) . . ? C17 O3 Er1 95.3(2) . . ? C17 O2 Er1 88.48(19) . . ? S1 O1 Er1 162.68(17) . . ? S2 O4 Er1 143.09(14) . . ? C6 O5 Er1 170.8(2) . . ? S2 O7 Er1 150.36(14) . 2_665 ? C13 N1 C12 117.8(3) . . ? C13 N1 Cu1 119.8(2) . . ? C12 N1 Cu1 122.1(2) . . ? C10 N2 C11 116.8(3) . . ? C10 N2 Cu1 123.4(2) . 2_656 ? C11 N2 Cu1 119.7(3) . 2_656 ? C19 C20 C21 121.2(3) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C19 C18 119.3(3) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C22 C18 C19 121.1(3) . . ? C22 C18 S1 119.3(3) . . ? C19 C18 S1 119.6(3) . . ? C18 C22 C21 120.5(3) . 2_566 ? C18 C22 H22 119.7 . . ? C21 C22 H22 119.7 2_566 . ? C20 C21 C22 122.2(3) . 2_566 ? C20 C21 C21 119.1(4) . 2_566 ? C22 C21 C21 118.7(4) 2_566 2_566 ? C11 C8 C7 120.2(3) . . ? C11 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? N2 C11 C8 122.6(3) . . ? N2 C11 H11 118.7 . . ? C8 C11 H11 118.7 . . ? N2 C10 C9 123.3(3) . . ? N2 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? C7 C9 C10 119.5(3) . . ? C7 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C2 C1 122.3(3) . . ? C3 C2 C2 118.1(4) . 2_655 ? C1 C2 C2 119.6(4) . 2_655 ? C5 C1 C2 121.0(3) 2_655 . ? C5 C1 H1 119.5 2_655 . ? C2 C1 H1 119.5 . . ? C1 C5 C4 119.4(3) 2_655 . ? C1 C5 H5 120.3 2_655 . ? C4 C5 H5 120.3 . . ? C3 C4 C5 121.4(3) . . ? C3 C4 S2 118.8(3) . . ? C5 C4 S2 119.7(2) . . ? N1 C13 C14 122.5(3) . . ? N1 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C13 C14 C16 119.7(3) . . ? C13 C14 H14 120.1 . . ? C16 C14 H14 120.1 . . ? C14 C16 C15 118.1(3) . . ? C14 C16 C17 121.0(3) . . ? C15 C16 C17 120.8(3) . . ? C12 C15 C16 119.1(3) . . ? C12 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? N1 C12 C15 122.7(3) . . ? N1 C12 H12 118.6 . . ? C15 C12 H12 118.6 . . ? C9 C7 C8 117.5(3) . . ? C9 C7 C6 122.4(3) . . ? C8 C7 C6 120.1(3) . . ? O5 C6 O6 124.6(3) . . ? O5 C6 C7 118.0(3) . . ? O6 C6 C7 117.4(3) . . ? O2 C17 O3 122.0(3) . . ? O2 C17 C16 120.0(3) . . ? O3 C17 C16 117.9(3) . . ? C6 O6 Er1 126.8(2) . 2_665 ? Er1 O1W H2W 123.1 . . ? Er1 O1W H1W 129.8 . . ? H2W O1W H1W 104.7 . . ? 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 O5 Er1 O3 C17 71.5(2) . . . . ? O1 Er1 O3 C17 -70.8(2) . . . . ? O7 Er1 O3 C17 9.5(3) 2_665 . . . ? O6 Er1 O3 C17 -156.62(18) 2_665 . . . ? O4 Er1 O3 C17 145.4(2) . . . . ? O1W Er1 O3 C17 -141.3(2) . . . . ? O2 Er1 O3 C17 -3.50(18) . . . . ? O5 Er1 O2 C17 -91.8(2) . . . . ? O1 Er1 O2 C17 112.3(2) . . . . ? O7 Er1 O2 C17 -167.4(2) 2_665 . . . ? O6 Er1 O2 C17 144.8(2) 2_665 . . . ? O3 Er1 O2 C17 3.53(19) . . . . ? O4 Er1 O2 C17 -36.6(2) . . . . ? O1W Er1 O2 C17 48.0(2) . . . . ? O10 S1 O1 Er1 3.9(6) . . . . ? O9 S1 O1 Er1 133.0(5) . . . . ? C18 S1 O1 Er1 -112.9(5) . . . . ? O5 Er1 O1 S1 20.2(6) . . . . ? O7 Er1 O1 S1 -24.8(5) 2_665 . . . ? O6 Er1 O1 S1 -106.0(5) 2_665 . . . ? O3 Er1 O1 S1 110.8(5) . . . . ? O4 Er1 O1 S1 -163.7(5) . . . . ? O1W Er1 O1 S1 -179.0(5) . . . . ? O2 Er1 O1 S1 60.6(5) . . . . ? O8 S2 O4 Er1 -167.5(2) . . . . ? O7 S2 O4 Er1 -40.0(3) . . . . ? C4 S2 O4 Er1 75.7(2) . . . . ? O5 Er1 O4 S2 -24.7(2) . . . . ? O1 Er1 O4 S2 157.77(19) . . . . ? O7 Er1 O4 S2 30.9(3) 2_665 . . . ? O6 Er1 O4 S2 98.8(2) 2_665 . . . ? O3 Er1 O4 S2 -112.3(2) . . . . ? O1W Er1 O4 S2 173.2(2) . . . . ? O2 Er1 O4 S2 -80.7(2) . . . . ? O1 Er1 O5 C6 -99.0(13) . . . . ? O7 Er1 O5 C6 -52.9(13) 2_665 . . . ? O6 Er1 O5 C6 16.7(14) 2_665 . . . ? O3 Er1 O5 C6 166.8(14) . . . . ? O4 Er1 O5 C6 83.4(13) . . . . ? O1W Er1 O5 C6 111.1(13) . . . . ? O2 Er1 O5 C6 -139.5(14) . . . . ? O8 S2 O7 Er1 160.2(2) . . . 2_665 ? O4 S2 O7 Er1 32.7(3) . . . 2_665 ? C4 S2 O7 Er1 -83.8(3) . . . 2_665 ? N2 Cu1 N1 C13 -113.7(8) 2_656 . . . ? N2 Cu1 N1 C12 60.2(10) 2_656 . . . ? C21 C20 C19 C18 1.1(5) . . . . ? C20 C19 C18 C22 -1.3(5) . . . . ? C20 C19 C18 S1 177.0(3) . . . . ? O10 S1 C18 C22 -54.8(3) . . . . ? O9 S1 C18 C22 -177.5(3) . . . . ? O1 S1 C18 C22 65.8(3) . . . . ? O10 S1 C18 C19 126.9(3) . . . . ? O9 S1 C18 C19 4.2(3) . . . . ? O1 S1 C18 C19 -112.5(3) . . . . ? C19 C18 C22 C21 0.5(5) . . . 2_566 ? S1 C18 C22 C21 -177.8(3) . . . 2_566 ? C19 C20 C21 C22 179.2(3) . . . 2_566 ? C19 C20 C21 C21 -0.2(6) . . . 2_566 ? C10 N2 C11 C8 0.9(6) . . . . ? Cu1 N2 C11 C8 -175.1(3) 2_656 . . . ? C7 C8 C11 N2 -0.3(6) . . . . ? C11 N2 C10 C9 -0.5(6) . . . . ? Cu1 N2 C10 C9 175.3(3) 2_656 . . . ? N2 C10 C9 C7 -0.4(6) . . . . ? C4 C3 C2 C1 -179.3(3) . . . . ? C4 C3 C2 C2 1.5(5) . . . 2_655 ? C3 C2 C1 C5 -179.5(3) . . . 2_655 ? C2 C2 C1 C5 -0.3(6) 2_655 . . 2_655 ? C2 C3 C4 C5 -1.7(5) . . . . ? C2 C3 C4 S2 -178.9(2) . . . . ? C1 C5 C4 C3 1.2(5) 2_655 . . . ? C1 C5 C4 S2 178.3(3) 2_655 . . . ? O8 S2 C4 C3 95.0(3) . . . . ? O7 S2 C4 C3 -24.7(3) . . . . ? O4 S2 C4 C3 -144.6(2) . . . . ? O8 S2 C4 C5 -82.2(3) . . . . ? O7 S2 C4 C5 158.1(3) . . . . ? O4 S2 C4 C5 38.2(3) . . . . ? C12 N1 C13 C14 -1.6(5) . . . . ? Cu1 N1 C13 C14 172.5(3) . . . . ? N1 C13 C14 C16 1.7(5) . . . . ? C13 C14 C16 C15 -0.6(5) . . . . ? C13 C14 C16 C17 -177.7(3) . . . . ? C14 C16 C15 C12 -0.5(5) . . . . ? C17 C16 C15 C12 176.6(3) . . . . ? C13 N1 C12 C15 0.5(5) . . . . ? Cu1 N1 C12 C15 -173.5(3) . . . . ? C16 C15 C12 N1 0.5(5) . . . . ? C10 C9 C7 C8 1.0(5) . . . . ? C10 C9 C7 C6 -176.4(3) . . . . ? C11 C8 C7 C9 -0.7(6) . . . . ? C11 C8 C7 C6 176.8(3) . . . . ? Er1 O5 C6 O6 -11.2(16) . . . . ? Er1 O5 C6 C7 171.2(12) . . . . ? C9 C7 C6 O5 -174.5(3) . . . . ? C8 C7 C6 O5 8.2(5) . . . . ? C9 C7 C6 O6 7.8(5) . . . . ? C8 C7 C6 O6 -169.6(3) . . . . ? Er1 O2 C17 O3 -6.2(3) . . . . ? Er1 O2 C17 C16 171.0(3) . . . . ? Er1 O3 C17 O2 6.7(3) . . . . ? Er1 O3 C17 C16 -170.6(2) . . . . ? C14 C16 C17 O2 4.6(5) . . . . ? C15 C16 C17 O2 -172.4(3) . . . . ? C14 C16 C17 O3 -178.0(3) . . . . ? C15 C16 C17 O3 5.0(5) . . . . ? O5 C6 O6 Er1 -5.2(4) . . . 2_665 ? C7 C6 O6 Er1 172.36(19) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.795 _refine_diff_density_min -1.163 _refine_diff_density_rms 0.091