# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Takashi Kajiwara' 'Tomonari Hiraizumi' 'Kohei Takahashi' 'Shinya Takaishi' 'Masahiro Yamashita' _publ_contact_author_name 'Takashi Kajiwara' _publ_contact_author_email KAJIWARA@AGNUS.CHEM.TOHOKU.AC.JP _publ_section_title ; Structural correlations between the crystal field and magnetic anisotropy of Ln-Cu single-molecule magnets ; # Attachment 'DyCu_complex.cif' data_DyCu_complex _database_code_depnum_ccdc_archive 'CCDC 725688' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H64 Cu2 Dy2 N14 O32' _chemical_formula_weight 1777.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.4409(15) _cell_length_b 18.0725(19) _cell_length_c 23.928(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.705(2) _cell_angle_gamma 90.00 _cell_volume 6155.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.918 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3536 _exptl_absorpt_coefficient_mu 3.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5289 _exptl_absorpt_correction_T_max 0.6707 _exptl_absorpt_process_details ; G. M. Sheldrick, SADABS. Program for Empirical Absorption Correction of Area Detector Data; University of Gottingen, Germany, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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 36451 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 30.02 _reflns_number_total 8989 _reflns_number_gt 7403 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0286P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8989 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0592 _refine_ls_wR_factor_gt 0.0577 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _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 Dy Dy 0.112168(8) 0.007116(6) 0.144867(5) 0.01174(3) Uani 1 1 d . . . Cu Cu 0.15479(2) -0.055287(15) 0.284668(12) 0.01183(6) Uani 1 1 d . . . O1 O 0.07009(12) -0.11702(9) 0.10064(7) 0.0160(4) Uani 1 1 d . . . O2 O 0.10612(12) -0.09301(9) 0.20898(7) 0.0136(3) Uani 1 1 d . . . N1 N 0.15476(14) -0.15393(11) 0.31991(8) 0.0147(4) Uani 1 1 d . . . C1 C 0.03914(19) -0.12890(15) 0.04051(10) 0.0202(5) Uani 1 1 d . . . H1 H 0.0830 -0.1624 0.0260 0.030 Uiso 1 1 calc R . . H2 H 0.0373 -0.0814 0.0205 0.030 Uiso 1 1 calc R . . H3 H -0.0238 -0.1509 0.0343 0.030 Uiso 1 1 calc R . . C2 C 0.07401(17) -0.17912(13) 0.13496(10) 0.0139(5) Uani 1 1 d . . . C3 C 0.05693(17) -0.25025(13) 0.11531(10) 0.0164(5) Uani 1 1 d . . . H4 H 0.0418 -0.2595 0.0757 0.020 Uiso 1 1 calc R . . C4 C 0.06198(18) -0.30865(14) 0.15394(11) 0.0185(5) Uani 1 1 d . . . H5 H 0.0476 -0.3576 0.1407 0.022 Uiso 1 1 calc R . . C5 C 0.08759(17) -0.29557(13) 0.21091(10) 0.0161(5) Uani 1 1 d . . . H6 H 0.0931 -0.3359 0.2367 0.019 Uiso 1 1 calc R . . C6 C 0.10594(16) -0.22284(13) 0.23169(10) 0.0133(5) Uani 1 1 d . . . C7 C 0.09588(16) -0.16340(13) 0.19345(10) 0.0124(5) Uani 1 1 d . . . C8 C 0.13306(17) -0.21415(13) 0.29205(10) 0.0152(5) Uani 1 1 d . . . H7 H 0.1352 -0.2582 0.3139 0.018 Uiso 1 1 calc R . . C9 C 0.1792(2) -0.15951(14) 0.38231(11) 0.0257(6) Uani 1 1 d . . . H8 H 0.1287 -0.1347 0.3985 0.031 Uiso 1 1 calc R . . H9 H 0.2373 -0.1303 0.3941 0.031 Uiso 1 1 calc R . . C10 C 0.1943(3) -0.23330(18) 0.40951(13) 0.0411(8) Uani 1 1 d . . . H10 H 0.1369 -0.2628 0.4002 0.062 Uiso 1 1 calc R . . H11 H 0.2101 -0.2273 0.4507 0.062 Uiso 1 1 calc R . . H12 H 0.2460 -0.2586 0.3956 0.062 Uiso 1 1 calc R . . O3 O 0.07977(12) 0.13660(9) 0.17026(7) 0.0150(3) Uani 1 1 d . . . O4 O 0.14765(12) 0.03425(9) 0.24001(7) 0.0133(3) Uani 1 1 d . . . N2 N 0.26199(14) -0.00720(10) 0.33948(8) 0.0123(4) Uani 1 1 d . . . H13 H 0.2768 -0.0389 0.3703 0.015 Uiso 1 1 calc R . . N3 N 0.08491(15) 0.02828(11) 0.38852(8) 0.0133(4) Uani 1 1 d . . . O5 O 0.02286(12) 0.02711(10) 0.42308(7) 0.0160(4) Uani 1 1 d . . . O6 O 0.05129(12) 0.00232(9) 0.33708(7) 0.0140(3) Uani 1 1 d . . . C11 C 0.03067(18) 0.19170(14) 0.13264(10) 0.0188(5) Uani 1 1 d . . . H14 H -0.0163 0.2163 0.1513 0.028 Uiso 1 1 calc R . . H15 H -0.0006 0.1677 0.0978 0.028 Uiso 1 1 calc R . . H16 H 0.0757 0.2284 0.1233 0.028 Uiso 1 1 calc R . . C12 C 0.12002(17) 0.16095(13) 0.22401(10) 0.0138(5) Uani 1 1 d . . . C13 C 0.12587(17) 0.23406(13) 0.24048(10) 0.0163(5) Uani 1 1 d . . . H17 H 0.1011 0.2719 0.2147 0.020 Uiso 1 1 calc R . . C14 C 0.16859(18) 0.25176(13) 0.29544(11) 0.0175(5) Uani 1 1 d . . . H18 H 0.1735 0.3020 0.3074 0.021 Uiso 1 1 calc R . . C15 C 0.20367(17) 0.19620(13) 0.33249(10) 0.0160(5) Uani 1 1 d . . . H19 H 0.2332 0.2087 0.3698 0.019 Uiso 1 1 calc R . . C16 C 0.19678(16) 0.12137(13) 0.31626(10) 0.0127(5) Uani 1 1 d . . . C17 C 0.15540(16) 0.10330(12) 0.26131(10) 0.0124(5) Uani 1 1 d . . . C18 C 0.23486(17) 0.06537(12) 0.36190(10) 0.0126(5) Uani 1 1 d . . . H20 H 0.2935 0.0873 0.3839 0.015 Uiso 1 1 calc R . . C19 C 0.34710(17) -0.00059(13) 0.31282(11) 0.0164(5) Uani 1 1 d . . . H21 H 0.3974 0.0245 0.3393 0.020 Uiso 1 1 calc R . . H22 H 0.3327 0.0299 0.2781 0.020 Uiso 1 1 calc R . . C20 C 0.38100(18) -0.07614(13) 0.29782(11) 0.0186(5) Uani 1 1 d . . . H23 H 0.3966 -0.1059 0.3323 0.028 Uiso 1 1 calc R . . H24 H 0.4370 -0.0706 0.2801 0.028 Uiso 1 1 calc R . . H25 H 0.3314 -0.1008 0.2714 0.028 Uiso 1 1 calc R . . C21 C 0.16838(17) 0.05438(13) 0.40319(10) 0.0139(5) Uani 1 1 d . . . H26 H 0.1844(18) 0.0703(14) 0.4379(11) 0.012(7) Uiso 1 1 d . . . O7 O 0.13934(13) 0.10796(10) 0.06765(7) 0.0211(4) Uani 1 1 d . . . O8 O 0.17774(13) -0.00557(9) 0.05666(7) 0.0193(4) Uani 1 1 d . . . N4 N 0.17512(15) 0.06127(12) 0.03893(9) 0.0177(4) Uani 1 1 d . . . O9 O 0.20744(13) 0.07814(11) -0.00353(8) 0.0262(4) Uani 1 1 d . . . O10 O 0.27401(13) 0.06553(10) 0.15870(7) 0.0214(4) Uani 1 1 d . . . O11 O 0.26786(12) -0.05362(10) 0.16536(7) 0.0202(4) Uani 1 1 d . . . N5 N 0.31772(16) 0.00450(13) 0.16410(9) 0.0221(5) Uani 1 1 d . . . O12 O 0.40335(14) 0.00076(12) 0.16731(10) 0.0364(6) Uani 1 1 d . . . O13 O 0.38980(18) 0.02225(14) 0.48882(14) 0.0594(8) Uani 1 1 d . . . O14 O 0.39151(17) -0.07782(16) 0.44287(9) 0.0501(7) Uani 1 1 d . . . N6 N 0.39829(17) -0.04470(16) 0.48653(12) 0.0335(6) Uani 1 1 d . . . C22 C 0.4203(2) -0.0861(2) 0.54016(13) 0.0443(9) Uani 1 1 d . . . H27 H 0.3696 -0.1212 0.5429 0.066 Uiso 1 1 calc R . . H28 H 0.4266 -0.0515 0.5721 0.066 Uiso 1 1 calc R . . H29 H 0.4794 -0.1132 0.5411 0.066 Uiso 1 1 calc R . . O15 O 0.29864(18) 0.18402(14) 0.47691(9) 0.0469(6) Uani 1 1 d . . . O16 O 0.43374(17) 0.20480(13) 0.52866(10) 0.0445(6) Uani 1 1 d . . . N7 N 0.35355(19) 0.17965(14) 0.52172(10) 0.0303(6) Uani 1 1 d . . . C23 C 0.3211(2) 0.14465(17) 0.57005(12) 0.0342(7) Uani 1 1 d . . . H30 H 0.3750 0.1346 0.5998 0.051 Uiso 1 1 calc R . . H31 H 0.2892 0.0981 0.5579 0.051 Uiso 1 1 calc R . . H32 H 0.2773 0.1778 0.5848 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy 0.01359(6) 0.01230(6) 0.00944(5) 0.00042(4) 0.00223(4) 0.00039(4) Cu 0.01533(14) 0.00993(14) 0.00978(14) 0.00017(10) 0.00078(11) -0.00069(11) O1 0.0251(10) 0.0136(8) 0.0088(8) 0.0002(6) 0.0011(7) 0.0003(7) O2 0.0199(9) 0.0092(8) 0.0110(8) -0.0006(6) 0.0008(7) -0.0003(6) N1 0.0185(11) 0.0145(10) 0.0108(10) 0.0008(8) 0.0014(8) -0.0006(8) C1 0.0263(14) 0.0247(14) 0.0085(11) -0.0014(10) -0.0005(10) -0.0022(11) C2 0.0141(12) 0.0141(12) 0.0135(12) 0.0011(9) 0.0026(9) 0.0015(9) C3 0.0189(13) 0.0166(12) 0.0129(12) -0.0038(9) 0.0001(10) 0.0015(10) C4 0.0221(14) 0.0113(12) 0.0218(13) -0.0031(10) 0.0024(11) 0.0012(10) C5 0.0179(13) 0.0121(11) 0.0186(13) 0.0000(9) 0.0039(10) 0.0002(9) C6 0.0125(12) 0.0142(12) 0.0134(12) 0.0005(9) 0.0028(9) -0.0008(9) C7 0.0103(11) 0.0118(11) 0.0153(12) -0.0005(9) 0.0029(9) 0.0001(9) C8 0.0176(12) 0.0137(12) 0.0149(12) 0.0032(9) 0.0042(10) -0.0001(9) C9 0.0453(18) 0.0175(13) 0.0125(13) 0.0014(10) -0.0002(12) -0.0054(12) C10 0.055(2) 0.0366(19) 0.0283(17) 0.0051(14) -0.0027(16) 0.0019(16) O3 0.0206(9) 0.0120(8) 0.0114(8) 0.0016(6) 0.0001(7) 0.0024(7) O4 0.0171(9) 0.0090(8) 0.0136(8) -0.0004(6) 0.0019(7) 0.0001(6) N2 0.0139(10) 0.0113(9) 0.0118(9) 0.0003(7) 0.0024(8) 0.0009(7) N3 0.0169(10) 0.0126(10) 0.0104(10) -0.0001(7) 0.0019(8) 0.0023(8) O5 0.0156(9) 0.0231(9) 0.0105(8) -0.0020(7) 0.0060(7) -0.0019(7) O6 0.0154(8) 0.0175(9) 0.0088(8) -0.0031(6) 0.0011(6) -0.0007(7) C11 0.0232(14) 0.0166(12) 0.0154(12) 0.0038(10) -0.0005(10) 0.0032(10) C12 0.0139(12) 0.0153(12) 0.0122(11) -0.0011(9) 0.0019(9) -0.0003(9) C13 0.0191(13) 0.0111(11) 0.0191(13) 0.0031(9) 0.0040(10) 0.0011(9) C14 0.0210(13) 0.0114(11) 0.0208(13) -0.0016(9) 0.0050(10) -0.0003(10) C15 0.0169(12) 0.0160(12) 0.0155(12) -0.0029(9) 0.0035(10) -0.0015(9) C16 0.0134(11) 0.0126(11) 0.0128(11) 0.0007(9) 0.0038(9) -0.0001(9) C17 0.0137(12) 0.0111(11) 0.0132(11) -0.0022(9) 0.0048(9) -0.0002(9) C18 0.0137(11) 0.0115(11) 0.0122(11) -0.0019(9) 0.0011(9) -0.0013(9) C19 0.0149(12) 0.0147(12) 0.0201(13) -0.0025(9) 0.0043(10) -0.0014(9) C20 0.0193(13) 0.0165(12) 0.0200(13) -0.0022(10) 0.0035(10) 0.0030(10) C21 0.0169(12) 0.0145(12) 0.0102(11) -0.0008(9) 0.0014(9) -0.0001(9) O7 0.0227(10) 0.0219(10) 0.0193(9) -0.0005(7) 0.0053(8) 0.0027(8) O8 0.0247(10) 0.0191(9) 0.0148(9) 0.0029(7) 0.0047(7) 0.0001(7) N4 0.0165(11) 0.0228(11) 0.0131(10) 0.0029(8) 0.0006(8) -0.0001(9) O9 0.0305(11) 0.0344(11) 0.0162(9) 0.0078(8) 0.0111(8) 0.0003(9) O10 0.0204(10) 0.0230(10) 0.0207(10) 0.0023(8) 0.0036(8) -0.0014(8) O11 0.0207(10) 0.0239(10) 0.0162(9) 0.0035(7) 0.0041(7) 0.0041(8) N5 0.0174(11) 0.0357(14) 0.0131(10) 0.0046(9) 0.0019(9) 0.0016(10) O12 0.0145(10) 0.0588(16) 0.0359(13) 0.0128(11) 0.0044(9) 0.0054(10) O13 0.0389(15) 0.0381(15) 0.101(2) 0.0090(15) 0.0112(15) 0.0030(12) O14 0.0394(14) 0.089(2) 0.0208(12) -0.0052(13) 0.0007(10) 0.0167(13) N6 0.0228(13) 0.0414(16) 0.0358(15) 0.0073(13) 0.0036(11) 0.0036(11) C22 0.039(2) 0.069(3) 0.0242(16) 0.0163(16) 0.0019(14) 0.0170(18) O15 0.0641(17) 0.0494(15) 0.0216(12) 0.0045(10) -0.0091(11) -0.0157(12) O16 0.0463(15) 0.0492(15) 0.0380(14) 0.0066(11) 0.0068(11) -0.0195(12) N7 0.0451(17) 0.0266(13) 0.0196(12) 0.0010(10) 0.0066(12) -0.0096(11) C23 0.055(2) 0.0305(17) 0.0198(15) -0.0006(12) 0.0134(14) -0.0104(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy O4 2.3005(16) . ? Dy O5 2.3467(17) 2 ? Dy O2 2.3834(16) . ? Dy O8 2.4654(18) . ? Dy O6 2.4718(17) 2 ? Dy O11 2.4756(18) . ? Dy O3 2.4819(16) . ? Dy O1 2.5111(16) . ? Dy O10 2.5348(18) . ? Dy O7 2.6709(18) . ? Dy N3 2.849(2) 2 ? Dy N5 2.927(2) . ? Cu O4 1.9323(16) . ? Cu O2 1.9517(16) . ? Cu N1 1.972(2) . ? Cu N2 2.046(2) . ? Cu O6 2.3501(17) . ? O1 C2 1.386(3) . ? O1 C1 1.449(3) . ? O2 C7 1.327(3) . ? N1 C8 1.287(3) . ? N1 C9 1.479(3) . ? C2 C3 1.377(3) . ? C2 C7 1.411(3) . ? C3 C4 1.397(3) . ? C4 C5 1.371(3) . ? C5 C6 1.415(3) . ? C6 C7 1.403(3) . ? C6 C8 1.440(3) . ? C9 C10 1.484(4) . ? O3 C12 1.391(3) . ? O3 C11 1.446(3) . ? O4 C17 1.345(3) . ? N2 C19 1.482(3) . ? N2 C18 1.494(3) . ? N3 C21 1.287(3) . ? N3 O5 1.318(3) . ? N3 O6 1.330(2) . ? N3 Dy 2.849(2) 2 ? O5 Dy 2.3467(17) 2 ? O6 Dy 2.4718(17) 2 ? C12 C13 1.377(3) . ? C12 C17 1.411(3) . ? C13 C14 1.393(3) . ? C14 C15 1.378(3) . ? C15 C16 1.406(3) . ? C16 C17 1.388(3) . ? C16 C18 1.522(3) . ? C18 C21 1.502(3) . ? C19 C20 1.514(3) . ? O7 N4 1.253(3) . ? O8 N4 1.279(3) . ? N4 O9 1.226(3) . ? O10 N5 1.267(3) . ? O11 N5 1.277(3) . ? N5 O12 1.228(3) . ? O13 N6 1.218(4) . ? O14 N6 1.194(3) . ? N6 C22 1.473(4) . ? O15 N7 1.224(3) . ? O16 N7 1.229(3) . ? N7 C23 1.463(3) . ? 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 O4 Dy O5 132.32(6) . 2 ? O4 Dy O2 63.32(5) . . ? O5 Dy O2 116.52(6) 2 . ? O4 Dy O8 144.43(6) . . ? O5 Dy O8 79.36(6) 2 . ? O2 Dy O8 122.79(6) . . ? O4 Dy O6 83.94(6) . 2 ? O5 Dy O6 54.55(5) 2 2 ? O2 Dy O6 73.81(5) . 2 ? O8 Dy O6 131.47(6) . 2 ? O4 Dy O11 81.67(6) . . ? O5 Dy O11 145.72(6) 2 . ? O2 Dy O11 70.52(6) . . ? O8 Dy O11 70.20(6) . . ? O6 Dy O11 144.29(6) 2 . ? O4 Dy O3 64.94(5) . . ? O5 Dy O3 81.69(6) 2 . ? O2 Dy O3 121.96(5) . . ? O8 Dy O3 114.38(5) . . ? O6 Dy O3 76.42(5) 2 . ? O11 Dy O3 124.89(6) . . ? O4 Dy O1 127.24(5) . . ? O5 Dy O1 74.44(6) 2 . ? O2 Dy O1 63.93(5) . . ? O8 Dy O1 69.92(6) . . ? O6 Dy O1 82.64(5) 2 . ? O11 Dy O1 80.47(6) . . ? O3 Dy O1 154.60(6) . . ? O4 Dy O10 74.65(6) . . ? O5 Dy O10 131.79(6) 2 . ? O2 Dy O10 111.42(6) . . ? O8 Dy O10 70.84(6) . . ? O6 Dy O10 151.45(6) 2 . ? O11 Dy O10 51.11(6) . . ? O3 Dy O10 77.47(6) . . ? O1 Dy O10 125.41(6) . . ? O4 Dy O7 120.33(6) . . ? O5 Dy O7 67.51(6) 2 . ? O2 Dy O7 171.46(5) . . ? O8 Dy O7 49.37(5) . . ? O6 Dy O7 113.63(5) 2 . ? O11 Dy O7 101.84(6) . . ? O3 Dy O7 65.28(5) . . ? O1 Dy O7 111.80(5) . . ? O10 Dy O7 64.30(5) . . ? O4 Dy N3 107.11(6) . 2 ? O5 Dy N3 27.25(5) 2 2 ? O2 Dy N3 98.00(6) . 2 ? O8 Dy N3 106.38(6) . 2 ? O6 Dy N3 27.81(5) 2 2 ? O11 Dy N3 161.08(6) . 2 ? O3 Dy N3 73.83(6) . 2 ? O1 Dy N3 80.93(6) . 2 ? O10 Dy N3 146.73(6) . 2 ? O7 Dy N3 88.32(6) . 2 ? O4 Dy N5 78.29(6) . . ? O5 Dy N5 144.46(6) 2 . ? O2 Dy N5 91.88(6) . . ? O8 Dy N5 66.88(6) . . ? O6 Dy N5 160.93(6) 2 . ? O11 Dy N5 25.64(6) . . ? O3 Dy N5 101.82(6) . . ? O1 Dy N5 102.64(6) . . ? O10 Dy N5 25.55(6) . . ? O7 Dy N5 81.75(6) . . ? N3 Dy N5 170.07(6) 2 . ? O4 Cu O2 78.58(7) . . ? O4 Cu N1 171.74(8) . . ? O2 Cu N1 93.16(7) . . ? O4 Cu N2 87.87(7) . . ? O2 Cu N2 149.12(8) . . ? N1 Cu N2 99.47(8) . . ? O4 Cu O6 86.83(6) . . ? O2 Cu O6 119.20(6) . . ? N1 Cu O6 97.25(7) . . ? N2 Cu O6 87.15(7) . . ? O4 Cu Dy 38.18(5) . . ? O2 Cu Dy 40.95(5) . . ? N1 Cu Dy 133.65(6) . . ? N2 Cu Dy 118.03(6) . . ? O6 Cu Dy 110.09(4) . . ? C2 O1 C1 116.32(18) . . ? C2 O1 Dy 119.39(13) . . ? C1 O1 Dy 124.27(14) . . ? C7 O2 Cu 126.91(15) . . ? C7 O2 Dy 124.20(14) . . ? Cu O2 Dy 106.59(7) . . ? C8 N1 C9 117.5(2) . . ? C8 N1 Cu 124.08(17) . . ? C9 N1 Cu 118.44(15) . . ? C3 C2 O1 124.5(2) . . ? C3 C2 C7 121.6(2) . . ? O1 C2 C7 113.9(2) . . ? C2 C3 C4 119.5(2) . . ? C5 C4 C3 120.2(2) . . ? C4 C5 C6 120.8(2) . . ? C7 C6 C5 119.3(2) . . ? C7 C6 C8 123.5(2) . . ? C5 C6 C8 117.2(2) . . ? O2 C7 C6 123.9(2) . . ? O2 C7 C2 117.8(2) . . ? C6 C7 C2 118.3(2) . . ? N1 C8 C6 127.8(2) . . ? N1 C9 C10 119.8(2) . . ? C12 O3 C11 116.27(18) . . ? C12 O3 Dy 117.27(13) . . ? C11 O3 Dy 126.15(14) . . ? C17 O4 Cu 125.02(14) . . ? C17 O4 Dy 124.27(14) . . ? Cu O4 Dy 110.55(7) . . ? C19 N2 C18 111.75(18) . . ? C19 N2 Cu 110.54(15) . . ? C18 N2 Cu 112.78(14) . . ? C21 N3 O5 122.7(2) . . ? C21 N3 O6 124.1(2) . . ? O5 N3 O6 113.21(18) . . ? C21 N3 Dy 166.20(17) . 2 ? O5 N3 Dy 54.62(11) . 2 ? O6 N3 Dy 60.11(11) . 2 ? N3 O5 Dy 98.12(13) . 2 ? N3 O6 Cu 118.96(13) . . ? N3 O6 Dy 92.08(12) . 2 ? Cu O6 Dy 145.17(7) . 2 ? C13 C12 O3 124.3(2) . . ? C13 C12 C17 122.0(2) . . ? O3 C12 C17 113.7(2) . . ? C12 C13 C14 119.1(2) . . ? C15 C14 C13 119.8(2) . . ? C14 C15 C16 121.5(2) . . ? C17 C16 C15 119.2(2) . . ? C17 C16 C18 124.7(2) . . ? C15 C16 C18 116.2(2) . . ? O4 C17 C16 124.9(2) . . ? O4 C17 C12 116.6(2) . . ? C16 C17 C12 118.5(2) . . ? N2 C18 C21 110.81(19) . . ? N2 C18 C16 114.26(19) . . ? C21 C18 C16 111.5(2) . . ? N2 C19 C20 110.74(19) . . ? N3 C21 C18 122.8(2) . . ? N4 O7 Dy 92.41(13) . . ? N4 O8 Dy 101.66(14) . . ? O9 N4 O7 122.5(2) . . ? O9 N4 O8 121.1(2) . . ? O7 N4 O8 116.5(2) . . ? N5 O10 Dy 94.78(14) . . ? N5 O11 Dy 97.33(14) . . ? O12 N5 O10 122.2(2) . . ? O12 N5 O11 121.3(2) . . ? O10 N5 O11 116.5(2) . . ? O12 N5 Dy 174.18(19) . . ? O10 N5 Dy 59.67(12) . . ? O11 N5 Dy 57.03(12) . . ? O14 N6 O13 122.9(3) . . ? O14 N6 C22 118.8(3) . . ? O13 N6 C22 118.3(3) . . ? O15 N7 O16 123.4(3) . . ? O15 N7 C23 118.3(3) . . ? O16 N7 C23 118.3(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.836 _refine_diff_density_min -1.026 _refine_diff_density_rms 0.116 # Attachment 'GdCu_complex.cif' data_GdCu_compelx _database_code_depnum_ccdc_archive 'CCDC 725689' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H64 Cu2 Gd2 N14 O32' _chemical_formula_weight 1766.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.4662(14) _cell_length_b 18.0741(18) _cell_length_c 23.962(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.811(2) _cell_angle_gamma 90.00 _cell_volume 6173.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 2.906 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.4267 _exptl_absorpt_correction_T_max 0.5638 _exptl_absorpt_process_details ; G. M. Sheldrick, SADABS. Program for Empirical Absorption Correction of Area Detector Data; University of Gottingen, Germany, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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 31364 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.00 _reflns_number_total 7368 _reflns_number_gt 6571 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0440P)^2^+1.9445P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7368 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0720 _refine_ls_wR_factor_gt 0.0709 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.005 _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 Gd Gd 0.112188(9) 0.006819(7) 0.144186(5) 0.01244(5) Uani 1 1 d . . . Cu Cu 0.15503(2) -0.056014(17) 0.284816(12) 0.01295(8) Uani 1 1 d . . . O1 O 0.07110(13) -0.11872(10) 0.10076(7) 0.0177(4) Uani 1 1 d . . . O2 O 0.10719(12) -0.09409(10) 0.20918(7) 0.0145(4) Uani 1 1 d . . . N1 N 0.15471(16) -0.15468(12) 0.32008(9) 0.0159(4) Uani 1 1 d . . . C1 C 0.0399(2) -0.13063(16) 0.04069(11) 0.0207(6) Uani 1 1 d . . . H1 H 0.0824 -0.1655 0.0265 0.031 Uiso 1 1 calc R . . H2 H 0.0401 -0.0835 0.0206 0.031 Uiso 1 1 calc R . . H3 H -0.0237 -0.1510 0.0344 0.031 Uiso 1 1 calc R . . C2 C 0.07435(18) -0.18067(14) 0.13518(11) 0.0154(5) Uani 1 1 d . . . C3 C 0.05667(19) -0.25147(15) 0.11571(11) 0.0180(5) Uani 1 1 d . . . H4 H 0.0416 -0.2609 0.0762 0.022 Uiso 1 1 calc R . . C4 C 0.06102(19) -0.30976(15) 0.15463(11) 0.0196(6) Uani 1 1 d . . . H5 H 0.0457 -0.3586 0.1416 0.024 Uiso 1 1 calc R . . C5 C 0.08721(19) -0.29659(14) 0.21134(11) 0.0183(5) Uani 1 1 d . . . H6 H 0.0929 -0.3369 0.2372 0.022 Uiso 1 1 calc R . . C6 C 0.10593(18) -0.22396(14) 0.23201(11) 0.0145(5) Uani 1 1 d . . . C7 C 0.09626(17) -0.16464(14) 0.19358(11) 0.0135(5) Uani 1 1 d . . . C8 C 0.13299(19) -0.21506(14) 0.29228(11) 0.0168(5) Uani 1 1 d . . . H7 H 0.1351 -0.2590 0.3142 0.020 Uiso 1 1 calc R . . C9 C 0.1781(2) -0.16023(16) 0.38234(12) 0.0272(7) Uani 1 1 d . . . H8 H 0.1266 -0.1364 0.3981 0.033 Uiso 1 1 calc R . . H9 H 0.2352 -0.1301 0.3946 0.033 Uiso 1 1 calc R . . C10 C 0.1948(3) -0.2342(2) 0.40976(15) 0.0471(10) Uani 1 1 d . . . H10 H 0.1376 -0.2641 0.4011 0.071 Uiso 1 1 calc R . . H11 H 0.2116 -0.2280 0.4509 0.071 Uiso 1 1 calc R . . H12 H 0.2460 -0.2592 0.3954 0.071 Uiso 1 1 calc R . . O3 O 0.07994(13) 0.13671(10) 0.17110(7) 0.0167(4) Uani 1 1 d . . . O4 O 0.14743(13) 0.03380(10) 0.24056(7) 0.0146(4) Uani 1 1 d . . . N2 N 0.26291(16) -0.00816(11) 0.33970(10) 0.0136(4) Uani 1 1 d . . . H13 H 0.2779 -0.0400 0.3704 0.016 Uiso 1 1 calc R . . N3 N 0.08717(16) 0.02690(12) 0.38929(9) 0.0148(4) Uani 1 1 d . . . O5 O 0.02604(13) 0.02561(11) 0.42419(8) 0.0178(4) Uani 1 1 d . . . O6 O 0.05301(14) 0.00164(9) 0.33785(8) 0.0155(4) Uani 1 1 d . . . C11 C 0.0302(2) 0.19163(15) 0.13367(11) 0.0197(6) Uani 1 1 d . . . H14 H -0.0167 0.2159 0.1525 0.030 Uiso 1 1 calc R . . H15 H -0.0012 0.1676 0.0989 0.030 Uiso 1 1 calc R . . H16 H 0.0747 0.2286 0.1243 0.030 Uiso 1 1 calc R . . C12 C 0.12024(18) 0.16060(15) 0.22493(11) 0.0154(5) Uani 1 1 d . . . C13 C 0.12682(19) 0.23370(15) 0.24127(11) 0.0183(5) Uani 1 1 d . . . H17 H 0.1024 0.2716 0.2155 0.022 Uiso 1 1 calc R . . C14 C 0.16979(19) 0.25124(15) 0.29622(12) 0.0193(6) Uani 1 1 d . . . H18 H 0.1750 0.3014 0.3082 0.023 Uiso 1 1 calc R . . C15 C 0.20479(18) 0.19531(15) 0.33318(11) 0.0167(5) Uani 1 1 d . . . H19 H 0.2342 0.2076 0.3705 0.020 Uiso 1 1 calc R . . C16 C 0.19782(18) 0.12065(14) 0.31672(11) 0.0142(5) Uani 1 1 d . . . C17 C 0.15583(17) 0.10266(14) 0.26199(10) 0.0127(5) Uani 1 1 d . . . C18 C 0.23618(18) 0.06416(14) 0.36230(11) 0.0141(5) Uani 1 1 d . . . H20 H 0.2950 0.0859 0.3841 0.017 Uiso 1 1 calc R . . C19 C 0.3476(2) -0.00141(14) 0.31275(13) 0.0184(6) Uani 1 1 d . . . H21 H 0.3982 0.0234 0.3392 0.022 Uiso 1 1 calc R . . H22 H 0.3329 0.0294 0.2782 0.022 Uiso 1 1 calc R . . C20 C 0.3809(2) -0.07678(15) 0.29731(12) 0.0202(6) Uani 1 1 d . . . H23 H 0.3989 -0.1062 0.3318 0.030 Uiso 1 1 calc R . . H24 H 0.4351 -0.0711 0.2781 0.030 Uiso 1 1 calc R . . H25 H 0.3301 -0.1019 0.2720 0.030 Uiso 1 1 calc R . . C21 C 0.17064(19) 0.05333(15) 0.40373(11) 0.0158(5) Uani 1 1 d . . . H26 H 0.187(2) 0.0677(16) 0.4369(12) 0.011(7) Uiso 1 1 d . . . O7 O 0.13745(13) 0.10650(11) 0.06776(8) 0.0209(4) Uani 1 1 d . . . O8 O 0.17965(15) -0.00599(10) 0.05529(9) 0.0204(4) Uani 1 1 d . . . N4 N 0.17531(16) 0.06157(13) 0.03873(10) 0.0194(5) Uani 1 1 d . . . O9 O 0.20781(15) 0.08045(12) -0.00328(8) 0.0268(5) Uani 1 1 d . . . O10 O 0.27592(14) 0.06544(11) 0.15862(8) 0.0229(4) Uani 1 1 d . . . O11 O 0.27013(14) -0.05394(11) 0.16505(8) 0.0217(4) Uani 1 1 d . . . N5 N 0.31965(18) 0.00442(14) 0.16378(11) 0.0229(6) Uani 1 1 d . . . O12 O 0.40488(17) 0.00097(13) 0.16697(12) 0.0380(6) Uani 1 1 d . . . O13 O 0.3901(2) 0.02194(17) 0.48896(16) 0.0624(9) Uani 1 1 d . . . O14 O 0.39244(18) -0.07738(18) 0.44290(10) 0.0524(8) Uani 1 1 d . . . N6 N 0.3989(2) -0.04499(18) 0.48666(13) 0.0370(7) Uani 1 1 d . . . C22 C 0.4208(3) -0.0852(2) 0.54026(14) 0.0457(10) Uani 1 1 d . . . H27 H 0.3694 -0.1192 0.5438 0.069 Uiso 1 1 calc R . . H28 H 0.4289 -0.0500 0.5718 0.069 Uiso 1 1 calc R . . H29 H 0.4789 -0.1134 0.5411 0.069 Uiso 1 1 calc R . . O15 O 0.3003(2) 0.18451(16) 0.47696(10) 0.0522(7) Uani 1 1 d . . . O16 O 0.43587(19) 0.20476(15) 0.52902(11) 0.0479(7) Uani 1 1 d . . . N7 N 0.3548(2) 0.17929(15) 0.52166(11) 0.0337(6) Uani 1 1 d . . . C23 C 0.3230(3) 0.14516(19) 0.57044(13) 0.0377(8) Uani 1 1 d . . . H30 H 0.3772 0.1350 0.6000 0.057 Uiso 1 1 calc R . . H31 H 0.2904 0.0987 0.5587 0.057 Uiso 1 1 calc R . . H32 H 0.2800 0.1789 0.5853 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd 0.01440(8) 0.01266(7) 0.01047(8) 0.00064(4) 0.00274(5) 0.00019(5) Cu 0.01691(16) 0.01093(15) 0.01068(15) 0.00030(11) 0.00141(12) -0.00082(12) O1 0.0274(10) 0.0149(9) 0.0101(9) -0.0003(7) 0.0015(8) -0.0011(8) O2 0.0200(9) 0.0116(9) 0.0114(9) -0.0010(7) 0.0013(7) 0.0003(7) N1 0.0193(11) 0.0157(11) 0.0128(11) 0.0010(8) 0.0026(9) -0.0019(9) C1 0.0269(15) 0.0249(15) 0.0096(12) -0.0017(10) 0.0008(11) -0.0027(12) C2 0.0152(12) 0.0158(13) 0.0150(13) 0.0013(10) 0.0019(10) 0.0001(10) C3 0.0216(14) 0.0175(13) 0.0143(13) -0.0027(10) 0.0011(11) 0.0035(11) C4 0.0243(14) 0.0124(13) 0.0221(14) -0.0025(10) 0.0033(11) -0.0012(11) C5 0.0211(14) 0.0122(12) 0.0223(14) 0.0005(10) 0.0052(11) 0.0002(10) C6 0.0152(12) 0.0138(12) 0.0145(13) 0.0004(10) 0.0023(10) 0.0008(10) C7 0.0128(12) 0.0117(12) 0.0165(13) -0.0015(10) 0.0036(10) 0.0001(9) C8 0.0205(13) 0.0129(12) 0.0172(13) 0.0029(10) 0.0042(10) 0.0003(10) C9 0.0443(19) 0.0212(15) 0.0144(14) 0.0018(11) 0.0001(13) -0.0043(14) C10 0.066(3) 0.039(2) 0.033(2) 0.0052(16) -0.0015(18) 0.0026(19) O3 0.0225(10) 0.0140(9) 0.0127(9) 0.0019(7) 0.0009(7) 0.0024(8) O4 0.0200(9) 0.0092(8) 0.0149(9) -0.0010(7) 0.0039(7) 0.0011(7) N2 0.0169(11) 0.0120(10) 0.0118(11) 0.0010(8) 0.0021(9) 0.0005(8) N3 0.0193(11) 0.0128(10) 0.0122(11) -0.0003(8) 0.0026(9) 0.0019(9) O5 0.0173(10) 0.0244(10) 0.0130(9) -0.0012(8) 0.0057(7) -0.0018(8) O6 0.0160(10) 0.0187(10) 0.0116(9) -0.0026(7) 0.0016(8) -0.0011(7) C11 0.0241(14) 0.0163(13) 0.0173(13) 0.0047(10) -0.0004(11) 0.0048(11) C12 0.0153(12) 0.0165(13) 0.0144(13) 0.0001(10) 0.0030(10) -0.0017(10) C13 0.0204(13) 0.0147(13) 0.0204(14) 0.0041(10) 0.0053(11) 0.0014(11) C14 0.0232(14) 0.0123(12) 0.0234(14) -0.0017(10) 0.0069(11) -0.0012(11) C15 0.0180(13) 0.0167(13) 0.0155(13) -0.0029(10) 0.0034(10) -0.0017(10) C16 0.0130(12) 0.0131(12) 0.0173(13) 0.0006(10) 0.0053(10) -0.0001(10) C17 0.0139(12) 0.0122(12) 0.0126(12) -0.0019(9) 0.0043(9) -0.0011(10) C18 0.0146(12) 0.0138(12) 0.0138(12) -0.0020(9) 0.0018(10) -0.0010(10) C19 0.0161(14) 0.0176(14) 0.0218(15) -0.0020(10) 0.0039(11) -0.0007(10) C20 0.0200(14) 0.0194(14) 0.0218(14) -0.0019(11) 0.0054(11) 0.0017(11) C21 0.0205(13) 0.0157(13) 0.0109(13) -0.0025(10) 0.0017(10) -0.0004(10) O7 0.0225(10) 0.0216(10) 0.0192(10) 0.0013(8) 0.0058(8) 0.0027(8) O8 0.0258(11) 0.0193(10) 0.0170(10) 0.0029(7) 0.0060(9) 0.0009(8) N4 0.0174(11) 0.0242(12) 0.0160(11) 0.0023(9) 0.0007(9) -0.0010(10) O9 0.0321(12) 0.0338(12) 0.0170(10) 0.0076(9) 0.0116(9) -0.0001(10) O10 0.0210(10) 0.0259(11) 0.0221(10) 0.0019(8) 0.0043(8) -0.0022(9) O11 0.0212(10) 0.0264(11) 0.0180(10) 0.0037(8) 0.0050(8) 0.0056(8) N5 0.0175(13) 0.0365(15) 0.0147(12) 0.0047(10) 0.0028(10) 0.0022(10) O12 0.0151(11) 0.0596(18) 0.0396(15) 0.0141(11) 0.0058(10) 0.0053(10) O13 0.0439(17) 0.0436(17) 0.099(3) 0.0116(17) 0.0102(17) 0.0016(14) O14 0.0411(15) 0.093(2) 0.0215(13) -0.0016(14) 0.0013(11) 0.0204(15) N6 0.0265(15) 0.0461(19) 0.0382(17) 0.0073(14) 0.0049(13) 0.0041(13) C22 0.035(2) 0.073(3) 0.0285(18) 0.0144(18) 0.0048(15) 0.0148(19) O15 0.070(2) 0.0565(18) 0.0243(13) 0.0041(12) -0.0074(13) -0.0172(15) O16 0.0523(17) 0.0501(17) 0.0413(15) 0.0066(12) 0.0083(13) -0.0167(14) N7 0.0469(18) 0.0305(15) 0.0241(14) 0.0015(11) 0.0076(13) -0.0107(13) C23 0.060(2) 0.0327(18) 0.0224(16) 0.0006(13) 0.0140(16) -0.0084(17) _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 Gd O4 2.3301(17) . ? Gd O5 2.3836(19) 2 ? Gd O2 2.4073(17) . ? Gd O3 2.4995(18) . ? Gd O8 2.500(2) . ? Gd O6 2.501(2) 2 ? Gd O11 2.5074(19) . ? Gd O1 2.5246(18) . ? Gd O10 2.564(2) . ? Gd O7 2.6384(19) . ? Gd N3 2.882(2) 2 ? Gd N5 2.958(3) . ? Cu O4 1.9319(18) . ? Cu O2 1.9519(17) . ? Cu N1 1.974(2) . ? Cu N2 2.053(2) . ? Cu O6 2.3490(19) . ? O1 C2 1.387(3) . ? O1 C1 1.449(3) . ? O2 C7 1.331(3) . ? N1 C8 1.289(3) . ? N1 C9 1.476(3) . ? C2 C3 1.371(4) . ? C2 C7 1.411(4) . ? C3 C4 1.401(4) . ? C4 C5 1.368(4) . ? C5 C6 1.413(4) . ? C6 C7 1.405(4) . ? C6 C8 1.439(4) . ? C9 C10 1.492(4) . ? O3 C12 1.391(3) . ? O3 C11 1.445(3) . ? O4 C17 1.344(3) . ? N2 C19 1.484(4) . ? N2 C18 1.491(3) . ? N3 C21 1.290(4) . ? N3 O5 1.317(3) . ? N3 O6 1.328(3) . ? N3 Gd 2.882(2) 2 ? O5 Gd 2.3836(19) 2 ? O6 Gd 2.501(2) 2 ? C12 C13 1.377(4) . ? C12 C17 1.412(4) . ? C13 C14 1.393(4) . ? C14 C15 1.382(4) . ? C15 C16 1.405(4) . ? C16 C17 1.387(4) . ? C16 C18 1.529(4) . ? C18 C21 1.498(4) . ? C19 C20 1.511(4) . ? O7 N4 1.254(3) . ? O8 N4 1.282(3) . ? N4 O9 1.230(3) . ? O10 N5 1.267(3) . ? O11 N5 1.278(3) . ? N5 O12 1.224(4) . ? O13 N6 1.219(4) . ? O14 N6 1.191(4) . ? N6 C22 1.463(4) . ? O15 N7 1.221(4) . ? O16 N7 1.244(4) . ? N7 C23 1.464(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Gd O5 131.88(6) . 2 ? O4 Gd O2 62.81(6) . . ? O5 Gd O2 116.00(6) 2 . ? O4 Gd O3 64.32(6) . . ? O5 Gd O3 82.64(6) 2 . ? O2 Gd O3 121.15(6) . . ? O4 Gd O8 144.34(7) . . ? O5 Gd O8 80.28(7) 2 . ? O2 Gd O8 122.69(6) . . ? O3 Gd O8 115.08(6) . . ? O4 Gd O6 83.76(6) . 2 ? O5 Gd O6 53.80(6) 2 2 ? O2 Gd O6 74.06(6) . 2 ? O3 Gd O6 76.41(6) . 2 ? O8 Gd O6 131.77(7) . 2 ? O4 Gd O11 81.72(6) . . ? O5 Gd O11 145.96(6) 2 . ? O2 Gd O11 70.49(6) . . ? O3 Gd O11 124.31(6) . . ? O8 Gd O11 69.80(6) . . ? O6 Gd O11 144.51(6) 2 . ? O4 Gd O1 126.37(6) . . ? O5 Gd O1 74.56(6) 2 . ? O2 Gd O1 63.56(6) . . ? O3 Gd O1 155.41(6) . . ? O8 Gd O1 70.39(6) . . ? O6 Gd O1 82.68(6) 2 . ? O11 Gd O1 80.28(6) . . ? O4 Gd O10 74.85(6) . . ? O5 Gd O10 132.95(6) 2 . ? O2 Gd O10 110.78(6) . . ? O3 Gd O10 77.63(6) . . ? O8 Gd O10 70.58(7) . . ? O6 Gd O10 151.66(6) 2 . ? O11 Gd O10 50.55(7) . . ? O1 Gd O10 125.05(6) . . ? O4 Gd O7 120.81(6) . . ? O5 Gd O7 67.96(6) 2 . ? O2 Gd O7 171.63(6) . . ? O3 Gd O7 65.90(6) . . ? O8 Gd O7 49.58(6) . . ? O6 Gd O7 113.23(6) 2 . ? O11 Gd O7 102.02(6) . . ? O1 Gd O7 112.23(6) . . ? O10 Gd O7 65.00(6) . . ? O4 Gd N3 106.80(6) . 2 ? O5 Gd N3 26.89(6) 2 2 ? O2 Gd N3 97.85(6) . 2 ? O3 Gd N3 74.43(6) . 2 ? O8 Gd N3 106.97(7) . 2 ? O6 Gd N3 27.42(6) 2 2 ? O11 Gd N3 160.98(7) . 2 ? O1 Gd N3 81.04(6) . 2 ? O10 Gd N3 147.49(6) . 2 ? O7 Gd N3 88.35(6) . 2 ? O4 Gd N5 78.52(7) . . ? O5 Gd N5 145.17(7) 2 . ? O2 Gd N5 91.59(6) . . ? O3 Gd N5 101.64(6) . . ? O8 Gd N5 66.49(7) . . ? O6 Gd N5 161.00(7) 2 . ? O11 Gd N5 25.38(6) . . ? O1 Gd N5 102.33(7) . . ? O10 Gd N5 25.25(6) . . ? O7 Gd N5 82.15(6) . . ? N3 Gd N5 170.49(7) 2 . ? O4 Cu O2 78.96(7) . . ? O4 Cu N1 171.96(8) . . ? O2 Cu N1 93.02(8) . . ? O4 Cu N2 87.91(8) . . ? O2 Cu N2 148.64(8) . . ? N1 Cu N2 99.41(9) . . ? O4 Cu O6 86.67(7) . . ? O2 Cu O6 120.18(7) . . ? N1 Cu O6 96.99(8) . . ? N2 Cu O6 86.89(8) . . ? O4 Cu Gd 38.45(5) . . ? O2 Cu Gd 41.05(5) . . ? N1 Cu Gd 133.67(6) . . ? N2 Cu Gd 117.99(6) . . ? O6 Cu Gd 110.58(5) . . ? C2 O1 C1 116.4(2) . . ? C2 O1 Gd 119.92(15) . . ? C1 O1 Gd 123.67(15) . . ? C7 O2 Cu 127.23(16) . . ? C7 O2 Gd 124.03(15) . . ? Cu O2 Gd 106.77(7) . . ? C8 N1 C9 117.3(2) . . ? C8 N1 Cu 124.18(18) . . ? C9 N1 Cu 118.51(17) . . ? C3 C2 O1 124.5(2) . . ? C3 C2 C7 121.8(2) . . ? O1 C2 C7 113.8(2) . . ? C2 C3 C4 119.4(2) . . ? C5 C4 C3 120.3(2) . . ? C4 C5 C6 120.9(2) . . ? C7 C6 C5 119.2(2) . . ? C7 C6 C8 123.5(2) . . ? C5 C6 C8 117.3(2) . . ? O2 C7 C6 123.6(2) . . ? O2 C7 C2 118.1(2) . . ? C6 C7 C2 118.3(2) . . ? N1 C8 C6 127.9(2) . . ? N1 C9 C10 119.9(3) . . ? C12 O3 C11 116.6(2) . . ? C12 O3 Gd 117.63(15) . . ? C11 O3 Gd 125.47(15) . . ? C17 O4 Cu 125.13(15) . . ? C17 O4 Gd 124.25(15) . . ? Cu O4 Gd 110.52(8) . . ? C19 N2 C18 111.74(19) . . ? C19 N2 Cu 110.48(17) . . ? C18 N2 Cu 112.72(16) . . ? C21 N3 O5 122.4(2) . . ? C21 N3 O6 124.0(2) . . ? O5 N3 O6 113.5(2) . . ? C21 N3 Gd 165.49(19) . 2 ? O5 N3 Gd 54.97(12) . 2 ? O6 N3 Gd 60.13(12) . 2 ? N3 O5 Gd 98.14(14) . 2 ? N3 O6 Cu 119.07(15) . . ? N3 O6 Gd 92.45(14) . 2 ? Cu O6 Gd 144.73(8) . 2 ? C13 C12 O3 124.0(2) . . ? C13 C12 C17 122.2(2) . . ? O3 C12 C17 113.8(2) . . ? C12 C13 C14 119.0(2) . . ? C15 C14 C13 119.7(2) . . ? C14 C15 C16 121.5(2) . . ? C17 C16 C15 119.3(2) . . ? C17 C16 C18 124.5(2) . . ? C15 C16 C18 116.2(2) . . ? O4 C17 C16 125.1(2) . . ? O4 C17 C12 116.6(2) . . ? C16 C17 C12 118.3(2) . . ? N2 C18 C21 111.0(2) . . ? N2 C18 C16 114.3(2) . . ? C21 C18 C16 111.5(2) . . ? N2 C19 C20 110.7(2) . . ? N3 C21 C18 122.7(2) . . ? N4 O7 Gd 93.90(14) . . ? N4 O8 Gd 99.78(15) . . ? O9 N4 O7 122.6(2) . . ? O9 N4 O8 120.8(2) . . ? O7 N4 O8 116.6(2) . . ? N5 O10 Gd 95.05(16) . . ? N5 O11 Gd 97.42(15) . . ? O12 N5 O10 122.1(3) . . ? O12 N5 O11 121.3(2) . . ? O10 N5 O11 116.6(2) . . ? O12 N5 Gd 174.2(2) . . ? O10 N5 Gd 59.70(14) . . ? O11 N5 Gd 57.20(13) . . ? O14 N6 O13 122.3(3) . . ? O14 N6 C22 120.1(3) . . ? O13 N6 C22 117.5(3) . . ? O15 N7 O16 123.3(3) . . ? O15 N7 C23 119.2(3) . . ? O16 N7 C23 117.4(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.081 _refine_diff_density_min -0.805 _refine_diff_density_rms 0.113 # Attachment 'TbCu_complex.cif' data_TbCu_complex _database_code_depnum_ccdc_archive 'CCDC 725690' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H64 Cu2 N14 O32 Tb2' _chemical_formula_weight 1770.03 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.459(3) _cell_length_b 18.079(4) _cell_length_c 23.943(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.718(4) _cell_angle_gamma 90.00 _cell_volume 6169(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3528 _exptl_absorpt_coefficient_mu 3.050 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4023 _exptl_absorpt_correction_T_max 0.5709 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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 35944 _diffrn_reflns_av_R_equivalents 0.1243 _diffrn_reflns_av_sigmaI/netI 0.1032 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 30.07 _reflns_number_total 9000 _reflns_number_gt 6380 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9000 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0692 _refine_ls_goodness_of_fit_ref 0.831 _refine_ls_restrained_S_all 0.831 _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 Tb Tb 0.112339(12) 0.006891(8) 0.144546(6) 0.01401(5) Uani 1 1 d . . . Cu Cu 0.15492(3) -0.05576(2) 0.284685(16) 0.01435(9) Uani 1 1 d . . . O1 O 0.07038(18) -0.11792(12) 0.10051(9) 0.0190(5) Uani 1 1 d . . . O2 O 0.10706(17) -0.09344(12) 0.20891(9) 0.0162(5) Uani 1 1 d . . . N1 N 0.1553(2) -0.15445(15) 0.31988(11) 0.0164(6) Uani 1 1 d . . . C1 C 0.0392(3) -0.1300(2) 0.04035(13) 0.0226(8) Uani 1 1 d . . . H1 H 0.0841 -0.1621 0.0256 0.034 Uiso 1 1 calc R . . H2 H 0.0352 -0.0824 0.0205 0.034 Uiso 1 1 calc R . . H3 H -0.0227 -0.1536 0.0344 0.034 Uiso 1 1 calc R . . C2 C 0.0742(3) -0.17986(18) 0.13495(14) 0.0169(7) Uani 1 1 d . . . C3 C 0.0566(3) -0.25081(19) 0.11559(15) 0.0198(7) Uani 1 1 d . . . H4 H 0.0414 -0.2602 0.0761 0.024 Uiso 1 1 calc R . . C4 C 0.0611(3) -0.30941(18) 0.15430(14) 0.0206(8) Uani 1 1 d . . . H5 H 0.0462 -0.3582 0.1411 0.025 Uiso 1 1 calc R . . C5 C 0.0870(3) -0.29641(18) 0.21134(15) 0.0198(7) Uani 1 1 d . . . H6 H 0.0922 -0.3365 0.2373 0.024 Uiso 1 1 calc R . . C6 C 0.1060(2) -0.22349(17) 0.23146(13) 0.0150(7) Uani 1 1 d . . . C7 C 0.0963(2) -0.16415(17) 0.19337(13) 0.0132(7) Uani 1 1 d . . . C8 C 0.1334(3) -0.21459(18) 0.29236(14) 0.0175(7) Uani 1 1 d . . . H7 H 0.1353 -0.2585 0.3144 0.021 Uiso 1 1 calc R . . C9 C 0.1796(3) -0.1600(2) 0.38207(14) 0.0271(9) Uani 1 1 d . . . H8 H 0.1288 -0.1356 0.3982 0.033 Uiso 1 1 calc R . . H9 H 0.2372 -0.1305 0.3939 0.033 Uiso 1 1 calc R . . C10 C 0.1954(4) -0.2339(3) 0.40924(18) 0.0474(13) Uani 1 1 d . . . H10 H 0.1375 -0.2630 0.4013 0.071 Uiso 1 1 calc R . . H11 H 0.2138 -0.2278 0.4503 0.071 Uiso 1 1 calc R . . H12 H 0.2454 -0.2597 0.3941 0.071 Uiso 1 1 calc R . . O3 O 0.07962(17) 0.13664(12) 0.17056(9) 0.0174(5) Uani 1 1 d . . . O4 O 0.14751(17) 0.03400(12) 0.24016(9) 0.0160(5) Uani 1 1 d . . . N2 N 0.2623(2) -0.00759(14) 0.33946(11) 0.0153(6) Uani 1 1 d . . . H13 H 0.2771 -0.0393 0.3703 0.018 Uiso 1 1 calc R . . N3 N 0.0860(2) 0.02723(15) 0.38876(11) 0.0154(6) Uani 1 1 d . . . O5 O 0.02378(17) 0.02631(13) 0.42342(9) 0.0188(5) Uani 1 1 d . . . O6 O 0.05212(16) 0.00158(12) 0.33725(8) 0.0158(5) Uani 1 1 d . . . C11 C 0.0297(3) 0.19182(18) 0.13321(14) 0.0206(8) Uani 1 1 d . . . H14 H -0.0165 0.2166 0.1524 0.031 Uiso 1 1 calc R . . H15 H -0.0025 0.1678 0.0986 0.031 Uiso 1 1 calc R . . H16 H 0.0744 0.2284 0.1234 0.031 Uiso 1 1 calc R . . C12 C 0.1200(2) 0.16087(18) 0.22420(14) 0.0169(7) Uani 1 1 d . . . C13 C 0.1263(3) 0.23405(18) 0.24113(15) 0.0193(7) Uani 1 1 d . . . H17 H 0.1014 0.2721 0.2156 0.023 Uiso 1 1 calc R . . C14 C 0.1692(3) 0.25134(18) 0.29576(14) 0.0197(7) Uani 1 1 d . . . H18 H 0.1746 0.3015 0.3077 0.024 Uiso 1 1 calc R . . C15 C 0.2041(3) 0.19594(18) 0.33261(14) 0.0186(7) Uani 1 1 d . . . H19 H 0.2336 0.2086 0.3699 0.022 Uiso 1 1 calc R . . C16 C 0.1973(2) 0.12115(17) 0.31675(13) 0.0147(7) Uani 1 1 d . . . C17 C 0.1555(2) 0.10315(18) 0.26158(13) 0.0154(7) Uani 1 1 d . . . C18 C 0.2355(2) 0.06443(17) 0.36187(13) 0.0154(7) Uani 1 1 d . . . H20 H 0.2941 0.0861 0.3839 0.019 Uiso 1 1 calc R . . C19 C 0.3477(2) -0.00100(18) 0.31272(14) 0.0194(7) Uani 1 1 d . . . H21 H 0.3981 0.0240 0.3392 0.023 Uiso 1 1 calc R . . H22 H 0.3334 0.0295 0.2780 0.023 Uiso 1 1 calc R . . C20 C 0.3809(3) -0.07631(18) 0.29792(14) 0.0213(8) Uani 1 1 d . . . H23 H 0.3984 -0.1054 0.3326 0.032 Uiso 1 1 calc R . . H24 H 0.4355 -0.0709 0.2790 0.032 Uiso 1 1 calc R . . H25 H 0.3304 -0.1015 0.2726 0.032 Uiso 1 1 calc R . . C21 C 0.1689(3) 0.05349(18) 0.40306(14) 0.0162(7) Uani 1 1 d . . . H26 H 0.186(3) 0.069(2) 0.4362(17) 0.035(12) Uiso 1 1 d . . . O7 O 0.13832(18) 0.10674(13) 0.06774(10) 0.0229(6) Uani 1 1 d . . . O8 O 0.17866(19) -0.00594(12) 0.05603(10) 0.0217(5) Uani 1 1 d . . . N4 N 0.1756(2) 0.06144(16) 0.03896(12) 0.0204(6) Uani 1 1 d . . . O9 O 0.20769(19) 0.07948(15) -0.00315(10) 0.0285(6) Uani 1 1 d . . . O10 O 0.27484(18) 0.06555(14) 0.15871(10) 0.0250(6) Uani 1 1 d . . . O11 O 0.26937(18) -0.05360(14) 0.16549(10) 0.0228(6) Uani 1 1 d . . . N5 N 0.3187(2) 0.00446(18) 0.16405(12) 0.0253(7) Uani 1 1 d . . . O12 O 0.4041(2) 0.00138(17) 0.16700(12) 0.0405(8) Uani 1 1 d . . . O13 O 0.3895(3) 0.0226(2) 0.48904(18) 0.0675(11) Uani 1 1 d . . . O14 O 0.3924(2) -0.0770(2) 0.44271(13) 0.0554(10) Uani 1 1 d . . . N6 N 0.3985(3) -0.0444(2) 0.48607(17) 0.0415(9) Uani 1 1 d . . . C22 C 0.4206(4) -0.0852(3) 0.54037(17) 0.0528(14) Uani 1 1 d . . . H27 H 0.3705 -0.1209 0.5431 0.079 Uiso 1 1 calc R . . H28 H 0.4256 -0.0502 0.5720 0.079 Uiso 1 1 calc R . . H29 H 0.4802 -0.1115 0.5420 0.079 Uiso 1 1 calc R . . O15 O 0.2988(3) 0.1842(2) 0.47715(13) 0.0558(10) Uani 1 1 d . . . O16 O 0.4348(3) 0.20459(19) 0.52894(13) 0.0513(9) Uani 1 1 d . . . N7 N 0.3538(3) 0.1791(2) 0.52142(14) 0.0379(9) Uani 1 1 d . . . C23 C 0.3223(4) 0.1450(2) 0.57058(16) 0.0421(12) Uani 1 1 d . . . H30 H 0.3768 0.1338 0.5996 0.063 Uiso 1 1 calc R . . H31 H 0.2884 0.0991 0.5588 0.063 Uiso 1 1 calc R . . H32 H 0.2805 0.1792 0.5861 0.063 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb 0.01645(8) 0.01415(8) 0.01179(7) 0.00070(6) 0.00346(6) 0.00038(7) Cu 0.0189(2) 0.01164(19) 0.01238(19) 0.00031(15) 0.00235(16) -0.00074(16) O1 0.0294(15) 0.0177(12) 0.0095(11) 0.0005(9) 0.0019(10) 0.0000(10) O2 0.0247(14) 0.0132(11) 0.0115(11) -0.0005(9) 0.0055(10) -0.0020(9) N1 0.0212(16) 0.0169(14) 0.0116(13) 0.0008(11) 0.0045(12) 0.0002(12) C1 0.030(2) 0.0244(19) 0.0124(16) 0.0001(14) 0.0012(15) -0.0026(16) C2 0.0144(17) 0.0186(17) 0.0184(17) 0.0000(14) 0.0050(14) 0.0017(13) C3 0.0203(19) 0.0210(17) 0.0179(17) -0.0038(14) 0.0027(15) 0.0031(14) C4 0.026(2) 0.0128(16) 0.0238(18) -0.0021(14) 0.0047(16) -0.0002(14) C5 0.0211(19) 0.0146(16) 0.0238(18) 0.0005(14) 0.0041(15) 0.0000(14) C6 0.0154(17) 0.0154(16) 0.0138(16) -0.0008(13) 0.0019(13) -0.0004(13) C7 0.0154(17) 0.0127(15) 0.0129(16) -0.0008(12) 0.0061(13) 0.0013(12) C8 0.0215(19) 0.0157(16) 0.0152(16) 0.0054(13) 0.0030(14) -0.0009(14) C9 0.046(3) 0.0213(18) 0.0128(17) 0.0046(14) 0.0015(17) -0.0056(17) C10 0.063(4) 0.047(3) 0.030(2) 0.001(2) -0.001(2) 0.008(2) O3 0.0250(14) 0.0160(11) 0.0104(11) 0.0013(9) 0.0006(10) 0.0007(10) O4 0.0227(13) 0.0127(11) 0.0117(11) -0.0007(9) -0.0001(10) -0.0007(9) N2 0.0155(14) 0.0135(13) 0.0171(13) 0.0013(11) 0.0034(11) -0.0015(11) N3 0.0210(16) 0.0127(13) 0.0135(13) 0.0011(10) 0.0052(12) 0.0016(11) O5 0.0173(13) 0.0267(13) 0.0143(11) -0.0016(10) 0.0081(10) 0.0005(10) O6 0.0180(12) 0.0192(12) 0.0100(10) -0.0029(9) 0.0017(9) -0.0009(10) C11 0.024(2) 0.0187(17) 0.0182(17) 0.0041(14) 0.0013(15) 0.0028(15) C12 0.0175(18) 0.0173(16) 0.0164(17) -0.0022(13) 0.0044(14) -0.0006(13) C13 0.023(2) 0.0152(16) 0.0211(18) 0.0032(14) 0.0070(15) 0.0028(14) C14 0.024(2) 0.0125(16) 0.0232(18) -0.0039(14) 0.0060(15) -0.0020(14) C15 0.0216(19) 0.0167(16) 0.0178(17) -0.0026(14) 0.0041(14) -0.0019(14) C16 0.0161(17) 0.0122(15) 0.0160(16) -0.0001(13) 0.0032(13) -0.0010(13) C17 0.0159(17) 0.0164(16) 0.0148(16) -0.0043(13) 0.0052(13) -0.0017(13) C18 0.0155(17) 0.0143(16) 0.0165(16) -0.0019(13) 0.0028(13) -0.0018(13) C19 0.0184(17) 0.0184(17) 0.0213(16) 0.0002(14) 0.0033(14) -0.0028(15) C20 0.024(2) 0.0202(17) 0.0206(18) -0.0024(14) 0.0060(15) 0.0011(15) C21 0.0217(19) 0.0171(17) 0.0099(16) -0.0030(13) 0.0033(14) -0.0019(14) O7 0.0259(15) 0.0230(13) 0.0209(13) 0.0015(11) 0.0069(11) 0.0021(11) O8 0.0285(14) 0.0178(12) 0.0189(11) 0.0031(10) 0.0042(10) 0.0017(11) N4 0.0194(16) 0.0248(16) 0.0165(15) 0.0030(13) 0.0020(12) -0.0007(13) O9 0.0325(17) 0.0365(15) 0.0187(13) 0.0076(12) 0.0111(12) 0.0011(12) O10 0.0258(15) 0.0254(14) 0.0230(13) 0.0022(11) 0.0022(11) -0.0024(11) O11 0.0242(15) 0.0260(14) 0.0188(12) 0.0045(11) 0.0051(11) 0.0052(11) N5 0.0221(16) 0.0386(19) 0.0148(13) 0.0028(14) 0.0020(12) 0.0030(15) O12 0.0190(14) 0.060(2) 0.0418(16) 0.0139(15) 0.0044(13) 0.0035(15) O13 0.048(2) 0.046(2) 0.111(3) 0.009(2) 0.019(2) 0.0034(17) O14 0.049(2) 0.093(3) 0.0235(16) -0.0034(18) 0.0047(15) 0.018(2) N6 0.028(2) 0.052(3) 0.044(2) 0.008(2) 0.0059(18) 0.0003(18) C22 0.045(3) 0.084(4) 0.030(2) 0.022(3) 0.007(2) 0.018(3) O15 0.070(3) 0.065(2) 0.0273(17) 0.0074(16) -0.0069(17) -0.0214(19) O16 0.055(2) 0.059(2) 0.0415(18) 0.0043(16) 0.0126(16) -0.0219(18) N7 0.056(3) 0.035(2) 0.0240(19) 0.0004(16) 0.0107(18) -0.0120(18) C23 0.071(4) 0.035(2) 0.025(2) -0.0010(19) 0.020(2) -0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb O4 2.312(2) . ? Tb O5 2.359(2) 2 ? Tb O2 2.390(2) . ? Tb O8 2.480(3) . ? Tb O6 2.491(2) 2 ? Tb O3 2.493(2) . ? Tb O11 2.494(3) . ? Tb O1 2.521(2) . ? Tb O10 2.548(3) . ? Tb O7 2.649(2) . ? Tb N3 2.868(3) 2 ? Tb N5 2.942(3) . ? Cu O4 1.935(2) . ? Cu O2 1.952(2) . ? Cu N1 1.973(3) . ? Cu N2 2.050(3) . ? Cu O6 2.345(2) . ? O1 C2 1.386(4) . ? O1 C1 1.451(4) . ? O2 C7 1.333(4) . ? N1 C8 1.283(4) . ? N1 C9 1.474(4) . ? C2 C3 1.373(5) . ? C2 C7 1.410(4) . ? C3 C4 1.402(5) . ? C4 C5 1.374(5) . ? C5 C6 1.415(5) . ? C6 C7 1.400(4) . ? C6 C8 1.454(4) . ? C9 C10 1.486(5) . ? O3 C12 1.389(4) . ? O3 C11 1.448(4) . ? O4 C17 1.349(4) . ? N2 C18 1.485(4) . ? N2 C19 1.489(5) . ? N3 C21 1.281(4) . ? N3 O5 1.323(4) . ? N3 O6 1.331(3) . ? N3 Tb 2.868(3) 2 ? O5 Tb 2.359(2) 2 ? O6 Tb 2.491(2) 2 ? C12 C13 1.382(5) . ? C12 C17 1.414(4) . ? C13 C14 1.386(5) . ? C14 C15 1.373(5) . ? C15 C16 1.403(4) . ? C16 C17 1.395(4) . ? C16 C18 1.524(4) . ? C18 C21 1.503(5) . ? C19 C20 1.506(5) . ? O7 N4 1.250(4) . ? O8 N4 1.283(4) . ? N4 O9 1.223(4) . ? O10 N5 1.269(4) . ? O11 N5 1.273(4) . ? N5 O12 1.227(4) . ? O13 N6 1.223(5) . ? O14 N6 1.184(5) . ? N6 C22 1.481(5) . ? O15 N7 1.217(4) . ? O16 N7 1.243(5) . ? N7 C23 1.468(5) . ? 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 O4 Tb O5 132.06(8) . 2 ? O4 Tb O2 63.13(7) . . ? O5 Tb O2 116.37(8) 2 . ? O4 Tb O8 144.46(8) . . ? O5 Tb O8 79.77(8) 2 . ? O2 Tb O8 122.62(8) . . ? O4 Tb O6 83.79(8) . 2 ? O5 Tb O6 54.29(7) 2 2 ? O2 Tb O6 73.89(8) . 2 ? O8 Tb O6 131.62(7) . 2 ? O4 Tb O3 64.69(7) . . ? O5 Tb O3 82.00(8) 2 . ? O2 Tb O3 121.67(8) . . ? O8 Tb O3 114.75(7) . . ? O6 Tb O3 76.44(8) 2 . ? O4 Tb O11 81.56(8) . . ? O5 Tb O11 146.04(8) 2 . ? O2 Tb O11 70.40(8) . . ? O8 Tb O11 70.15(8) . . ? O6 Tb O11 144.26(8) 2 . ? O3 Tb O11 124.56(8) . . ? O4 Tb O1 126.94(7) . . ? O5 Tb O1 74.38(8) 2 . ? O2 Tb O1 63.81(7) . . ? O8 Tb O1 70.08(8) . . ? O6 Tb O1 82.48(8) 2 . ? O3 Tb O1 154.74(8) . . ? O11 Tb O1 80.69(8) . . ? O4 Tb O10 74.71(8) . . ? O5 Tb O10 132.31(8) 2 . ? O2 Tb O10 111.05(8) . . ? O8 Tb O10 70.84(8) . . ? O6 Tb O10 151.52(8) 2 . ? O3 Tb O10 77.57(8) . . ? O11 Tb O10 50.79(8) . . ? O1 Tb O10 125.43(8) . . ? O4 Tb O7 120.64(8) . . ? O5 Tb O7 67.62(8) 2 . ? O2 Tb O7 171.42(8) . . ? O8 Tb O7 49.45(8) . . ? O6 Tb O7 113.53(7) 2 . ? O3 Tb O7 65.63(8) . . ? O11 Tb O7 101.97(8) . . ? O1 Tb O7 111.84(7) . . ? O10 Tb O7 64.72(7) . . ? O4 Tb N3 106.90(8) . 2 ? O5 Tb N3 27.15(8) 2 2 ? O2 Tb N3 97.90(8) . 2 ? O8 Tb N3 106.69(8) . 2 ? O6 Tb N3 27.64(7) 2 2 ? O3 Tb N3 74.08(8) . 2 ? O11 Tb N3 161.09(8) . 2 ? O1 Tb N3 80.77(8) . 2 ? O10 Tb N3 147.15(8) . 2 ? O7 Tb N3 88.39(8) . 2 ? O4 Tb N5 78.36(8) . . ? O5 Tb N5 144.85(8) 2 . ? O2 Tb N5 91.62(8) . . ? O8 Tb N5 66.80(8) . . ? O6 Tb N5 160.82(7) 2 . ? O3 Tb N5 101.81(9) . . ? O11 Tb N5 25.41(8) . . ? O1 Tb N5 102.65(9) . . ? O10 Tb N5 25.46(8) . . ? O7 Tb N5 82.04(8) . . ? N3 Tb N5 170.43(8) 2 . ? O4 Cu O2 78.61(9) . . ? O4 Cu N1 171.84(10) . . ? O2 Cu N1 93.23(10) . . ? O4 Cu N2 87.81(10) . . ? O2 Cu N2 148.68(11) . . ? N1 Cu N2 99.42(11) . . ? O4 Cu O6 86.78(9) . . ? O2 Cu O6 119.71(9) . . ? N1 Cu O6 97.29(10) . . ? N2 Cu O6 87.09(10) . . ? O4 Cu Tb 38.28(6) . . ? O2 Cu Tb 40.86(6) . . ? N1 Cu Tb 133.65(8) . . ? N2 Cu Tb 117.91(8) . . ? O6 Cu Tb 110.30(5) . . ? C2 O1 C1 116.3(3) . . ? C2 O1 Tb 119.45(18) . . ? C1 O1 Tb 124.19(19) . . ? C7 O2 Cu 126.9(2) . . ? C7 O2 Tb 124.24(19) . . ? Cu O2 Tb 106.84(9) . . ? C8 N1 C9 117.2(3) . . ? C8 N1 Cu 124.4(2) . . ? C9 N1 Cu 118.4(2) . . ? C3 C2 O1 124.6(3) . . ? C3 C2 C7 121.4(3) . . ? O1 C2 C7 114.0(3) . . ? C2 C3 C4 119.8(3) . . ? C5 C4 C3 120.2(3) . . ? C4 C5 C6 120.2(3) . . ? C7 C6 C5 120.0(3) . . ? C7 C6 C8 123.3(3) . . ? C5 C6 C8 116.7(3) . . ? O2 C7 C6 124.0(3) . . ? O2 C7 C2 117.8(3) . . ? C6 C7 C2 118.2(3) . . ? N1 C8 C6 127.6(3) . . ? N1 C9 C10 119.8(3) . . ? C12 O3 C11 116.2(2) . . ? C12 O3 Tb 117.39(18) . . ? C11 O3 Tb 126.13(18) . . ? C17 O4 Cu 125.07(19) . . ? C17 O4 Tb 124.29(19) . . ? Cu O4 Tb 110.51(10) . . ? C18 N2 C19 111.8(3) . . ? C18 N2 Cu 112.8(2) . . ? C19 N2 Cu 110.7(2) . . ? C21 N3 O5 122.8(3) . . ? C21 N3 O6 123.9(3) . . ? O5 N3 O6 113.2(3) . . ? C21 N3 Tb 165.6(2) . 2 ? O5 N3 Tb 54.47(15) . 2 ? O6 N3 Tb 60.22(15) . 2 ? N3 O5 Tb 98.37(17) . 2 ? N3 O6 Cu 118.94(19) . . ? N3 O6 Tb 92.14(18) . 2 ? Cu O6 Tb 145.22(9) . 2 ? C13 C12 O3 124.7(3) . . ? C13 C12 C17 121.5(3) . . ? O3 C12 C17 113.8(3) . . ? C12 C13 C14 119.3(3) . . ? C15 C14 C13 120.0(3) . . ? C14 C15 C16 121.8(3) . . ? C17 C16 C15 118.7(3) . . ? C17 C16 C18 124.2(3) . . ? C15 C16 C18 117.1(3) . . ? O4 C17 C16 124.9(3) . . ? O4 C17 C12 116.4(3) . . ? C16 C17 C12 118.7(3) . . ? N2 C18 C21 110.9(3) . . ? N2 C18 C16 114.8(3) . . ? C21 C18 C16 111.0(3) . . ? N2 C19 C20 110.4(3) . . ? N3 C21 C18 123.2(3) . . ? N4 O7 Tb 93.51(18) . . ? N4 O8 Tb 100.71(19) . . ? O9 N4 O7 122.6(3) . . ? O9 N4 O8 121.2(3) . . ? O7 N4 O8 116.2(3) . . ? N5 O10 Tb 94.9(2) . . ? N5 O11 Tb 97.38(19) . . ? O12 N5 O10 121.8(3) . . ? O12 N5 O11 121.7(3) . . ? O10 N5 O11 116.6(3) . . ? O12 N5 Tb 174.0(2) . . ? O10 N5 Tb 59.65(18) . . ? O11 N5 Tb 57.21(17) . . ? O14 N6 O13 123.5(4) . . ? O14 N6 C22 119.7(4) . . ? O13 N6 C22 116.8(4) . . ? O15 N7 O16 124.0(4) . . ? O15 N7 C23 119.0(4) . . ? O16 N7 C23 116.9(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.541 _refine_diff_density_min -1.044 _refine_diff_density_rms 0.157