# 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 'Guangming Li' _publ_contact_author_address ; Harbin 150080 ; _publ_contact_author_email 'gmli 2000@163.com' loop_ _publ_author_name 'Pengfei Yan' 'Ying Wang' 'Peng Chen' 'Juwen Zhang' 'Yan Wang' ; Guangming Li ; # Attachment '- 723145.CIF' data_d _database_code_depnum_ccdc_archive 'CCDC 723145' #TrackingRef '- 723145.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H22 Cu3 Gd N7 O8' _chemical_formula_weight 872.38 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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.913(2) _cell_length_b 33.876(7) _cell_length_c 7.9040(16) _cell_angle_alpha 90.00 _cell_angle_beta 104.72(3) _cell_angle_gamma 90.00 _cell_volume 2826.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.050 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1695 _exptl_absorpt_coefficient_mu 4.602 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26875 _diffrn_reflns_av_R_equivalents 0.1374 _diffrn_reflns_av_sigmaI/netI 0.1189 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6449 _reflns_number_gt 3931 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0812P)^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 SHELXL _refine_ls_extinction_coef 0.0029(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6449 _refine_ls_number_parameters 384 _refine_ls_number_restraints 518 _refine_ls_R_factor_all 0.1267 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.1746 _refine_ls_wR_factor_gt 0.1505 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 0.997 _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 Gd1 Gd 0.75153(4) 0.115154(12) 0.63721(7) 0.03034(18) Uani 1 1 d U . . Cu1 Cu 1.05745(11) 0.10410(3) 0.60973(18) 0.0373(3) Uani 1 1 d U . . Cu2 Cu 0.38608(15) 0.15787(5) 0.9592(3) 0.0758(6) Uani 1 1 d U . . Cu3 Cu 0.43243(13) 0.21091(3) 0.18076(18) 0.0451(4) Uani 1 1 d U . . C1 C 0.9609(8) 0.1831(2) 0.5772(13) 0.032(2) Uani 1 1 d U . . C2 C 0.8760(9) 0.2108(3) 0.6194(13) 0.036(2) Uani 1 1 d U . . C3 C 0.8988(10) 0.2509(3) 0.6162(15) 0.048(3) Uani 1 1 d U . . H3 H 0.8447 0.2688 0.6495 0.080 Uiso 1 1 calc R . . C4 C 1.0046(12) 0.2643(3) 0.5621(17) 0.057(3) Uani 1 1 d U . . H4 H 1.0164 0.2913 0.5502 0.080 Uiso 1 1 calc R . . C5 C 1.0891(10) 0.2387(3) 0.5272(15) 0.049(3) Uani 1 1 d U . . H5 H 1.1618 0.2484 0.5009 0.080 Uiso 1 1 calc R . . C6 C 1.0704(10) 0.1972(3) 0.5293(13) 0.038(2) Uani 1 1 d U . . C7 C 1.1680(10) 0.1718(3) 0.4948(15) 0.045(2) Uani 1 1 d U . . H7 H 1.2322 0.1836 0.4545 0.080 Uiso 1 1 calc R . . C8 C 1.2748(9) 0.1099(3) 0.4749(17) 0.048(3) Uani 1 1 d U . . H8A H 1.3521 0.1252 0.4917 0.080 Uiso 1 1 calc R . . H8B H 1.2497 0.1013 0.3539 0.080 Uiso 1 1 calc R . . C9 C 1.2972(9) 0.0745(3) 0.5949(16) 0.047(3) Uani 1 1 d U . . H9A H 1.3335 0.0532 0.5417 0.080 Uiso 1 1 calc R . . H9B H 1.3565 0.0813 0.7049 0.080 Uiso 1 1 calc R . . C10 C 1.1576(9) 0.0256(3) 0.6663(14) 0.037(2) Uani 1 1 d U . . H10 H 1.2206 0.0073 0.6637 0.080 Uiso 1 1 calc R . . C11 C 1.0444(9) 0.0117(2) 0.7144(13) 0.032(2) Uani 1 1 d U . . C12 C 1.0397(10) -0.0284(3) 0.7639(14) 0.041(2) Uani 1 1 d U . . H12 H 1.1065 -0.0450 0.7587 0.080 Uiso 1 1 calc R . . C13 C 0.9427(10) -0.0431(3) 0.8179(15) 0.047(3) Uani 1 1 d U . . H13 H 0.9426 -0.0696 0.8487 0.080 Uiso 1 1 calc R . . C14 C 0.8440(10) -0.0195(3) 0.8280(13) 0.037(2) Uani 1 1 d U . . H14 H 0.7777 -0.0298 0.8685 0.080 Uiso 1 1 calc R . . C15 C 0.8412(9) 0.0195(2) 0.7789(14) 0.035(2) Uani 1 1 d U . . C16 C 0.9421(8) 0.0358(2) 0.7206(12) 0.0275(18) Uani 1 1 d U . . C17 C 0.6432(11) 0.0327(3) 0.8549(18) 0.058(3) Uani 1 1 d U . . H17A H 0.5843 0.0539 0.8524 0.080 Uiso 1 1 calc R . . H17B H 0.6763 0.0241 0.9734 0.080 Uiso 1 1 calc R . . H17C H 0.6007 0.0112 0.7853 0.080 Uiso 1 1 calc R . . C18 C 0.6785(10) 0.2199(3) 0.6899(17) 0.055(3) Uani 1 1 d U . . H18A H 0.6139 0.2052 0.7250 0.080 Uiso 1 1 calc R . . H18B H 0.6423 0.2329 0.5807 0.080 Uiso 1 1 calc R . . H18C H 0.7136 0.2392 0.7776 0.080 Uiso 1 1 calc R . . C19 C 0.8423(12) 0.1356(4) 1.0960(16) 0.058(3) Uani 1 1 d U . . H19A H 0.9199 0.1385 1.1854 0.080 Uiso 1 1 calc R . . H19B H 0.7936 0.1144 1.1265 0.080 Uiso 1 1 calc R . . H19C H 0.7946 0.1597 1.0859 0.080 Uiso 1 1 calc R . . C20 C 0.5153(9) 0.1397(3) 0.8554(16) 0.055(3) Uani 0.50 1 d PU . . N4' N 0.5153(9) 0.1397(3) 0.8554(16) 0.055(3) Uani 0.50 1 d PU . . C21 C 0.2226(10) 0.1420(3) 0.9778(17) 0.051(3) Uani 1 1 d U . . C22 C 0.5422(12) 0.1699(3) 0.2979(15) 0.065(3) Uani 0.50 1 d PU . . N6' N 0.5422(12) 0.1699(3) 0.2979(15) 0.065(3) Uani 0.50 1 d PU . . C23 C 0.3922(9) 0.2267(3) -0.0666(15) 0.051(2) Uani 0.50 1 d PU . . N7' N 0.3922(9) 0.2267(3) -0.0666(15) 0.051(2) Uani 0.50 1 d PU . . O1 O 0.9322(6) 0.14510(16) 0.5802(9) 0.0337(14) Uani 1 1 d U . . O2 O 0.7772(6) 0.19335(18) 0.6695(9) 0.0406(16) Uani 1 1 d U . . O3 O 0.9319(6) 0.07379(17) 0.6778(9) 0.0359(14) Uani 1 1 d U . . O4 O 0.7471(6) 0.04651(18) 0.7845(11) 0.0452(16) Uani 1 1 d U . . O5 O 0.7230(6) 0.0705(2) 0.3856(10) 0.0485(17) Uani 1 1 d U . . O6 O 0.5513(10) 0.0404(3) 0.2514(16) 0.104(4) Uani 1 1 d U . . O7 O 0.5594(7) 0.0747(2) 0.4885(11) 0.0497(16) Uani 1 1 d U . . O8 O 0.8701(7) 0.1271(2) 0.9337(10) 0.0447(15) Uani 1 1 d DU . . H8 H 0.88(2) 0.151(3) 0.89(3) 0.20(10) Uiso 1 1 d D . . N1 N 1.1727(8) 0.1348(2) 0.5150(12) 0.044(2) Uani 1 1 d U . . N2 N 1.1756(7) 0.0616(2) 0.6274(12) 0.0386(19) Uani 1 1 d U . . N3 N 0.6102(9) 0.0614(3) 0.3725(14) 0.054(2) Uani 1 1 d U . . N4 N 0.5895(8) 0.1304(3) 0.7874(13) 0.0424(18) Uani 0.50 1 d PU . . C20' C 0.5895(8) 0.1304(3) 0.7874(13) 0.0424(18) Uani 0.50 1 d PU . . N5 N 0.1255(9) 0.1331(3) 0.9789(16) 0.064(3) Uani 1 1 d U . . N6 N 0.6233(9) 0.1511(3) 0.3889(14) 0.0456(18) Uani 0.50 1 d PU . . C22' C 0.6233(9) 0.1511(3) 0.3889(14) 0.0456(18) Uani 0.50 1 d PU . . N7 N 0.3916(9) 0.2487(3) -0.1739(14) 0.045(2) Uani 0.50 1 d PU . . C23' C 0.3916(9) 0.2487(3) -0.1739(14) 0.045(2) Uani 0.50 1 d PU . . 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 0.0222(3) 0.0325(3) 0.0394(3) -0.0012(2) 0.0135(2) 0.00228(17) Cu1 0.0253(6) 0.0375(6) 0.0536(9) 0.0061(5) 0.0183(6) 0.0029(4) Cu2 0.0538(10) 0.0848(11) 0.1085(16) -0.0505(10) 0.0570(11) -0.0252(8) Cu3 0.0528(8) 0.0394(7) 0.0427(9) -0.0016(6) 0.0115(7) 0.0038(6) C1 0.027(4) 0.028(3) 0.040(6) 0.013(4) 0.004(4) 0.005(3) C2 0.030(5) 0.036(4) 0.039(6) 0.004(4) 0.001(4) -0.002(3) C3 0.043(6) 0.035(4) 0.061(8) -0.003(5) 0.004(5) 0.005(4) C4 0.064(7) 0.041(5) 0.065(9) 0.007(5) 0.013(6) -0.012(4) C5 0.045(6) 0.051(5) 0.050(7) 0.009(5) 0.012(5) -0.015(4) C6 0.037(5) 0.047(4) 0.030(6) 0.010(4) 0.009(4) -0.008(3) C7 0.036(5) 0.052(4) 0.050(7) 0.003(5) 0.016(5) -0.012(4) C8 0.023(5) 0.063(6) 0.064(8) -0.011(5) 0.022(5) -0.010(4) C9 0.022(5) 0.063(6) 0.060(8) -0.006(5) 0.014(5) 0.002(4) C10 0.029(5) 0.042(4) 0.043(6) -0.008(4) 0.012(5) 0.007(3) C11 0.034(5) 0.025(4) 0.038(6) -0.002(4) 0.010(4) 0.008(3) C12 0.051(6) 0.028(4) 0.042(6) 0.001(4) 0.007(5) 0.011(4) C13 0.050(6) 0.031(5) 0.055(8) 0.008(5) 0.004(5) 0.001(4) C14 0.048(6) 0.037(4) 0.026(6) 0.004(4) 0.007(5) -0.004(4) C15 0.030(5) 0.035(4) 0.041(6) 0.000(4) 0.014(4) 0.002(3) C16 0.030(4) 0.030(4) 0.021(5) 0.000(3) 0.005(4) 0.004(3) C17 0.047(7) 0.052(6) 0.087(10) 0.008(6) 0.039(7) 0.004(5) C18 0.051(7) 0.045(5) 0.074(9) -0.011(6) 0.024(7) 0.005(5) C19 0.059(8) 0.073(7) 0.042(6) -0.015(6) 0.013(6) -0.003(6) C20 0.033(5) 0.067(6) 0.074(8) -0.015(5) 0.028(5) -0.005(4) N4' 0.033(5) 0.067(6) 0.074(8) -0.015(5) 0.028(5) -0.005(4) C21 0.037(6) 0.064(7) 0.060(8) -0.015(6) 0.025(6) -0.004(5) C22 0.080(7) 0.064(6) 0.045(6) 0.006(5) 0.004(5) 0.019(5) N6' 0.080(7) 0.064(6) 0.045(6) 0.006(5) 0.004(5) 0.019(5) C23 0.036(5) 0.067(6) 0.050(5) 0.014(4) 0.011(4) 0.001(4) N7' 0.036(5) 0.067(6) 0.050(5) 0.014(4) 0.011(4) 0.001(4) O1 0.028(3) 0.034(3) 0.042(4) 0.002(3) 0.014(3) 0.002(2) O2 0.034(4) 0.039(3) 0.052(5) -0.002(3) 0.018(3) 0.003(2) O3 0.028(3) 0.034(3) 0.052(4) 0.012(3) 0.023(3) 0.007(2) O4 0.042(4) 0.036(3) 0.068(4) 0.006(3) 0.032(3) 0.003(2) O5 0.037(3) 0.056(4) 0.057(4) -0.022(3) 0.021(3) 0.000(3) O6 0.098(8) 0.103(7) 0.117(9) -0.074(7) 0.039(7) -0.043(6) O7 0.035(3) 0.063(4) 0.055(5) -0.006(3) 0.019(3) -0.011(3) O8 0.034(4) 0.060(4) 0.040(4) -0.001(3) 0.009(3) 0.003(3) N1 0.033(5) 0.052(4) 0.053(6) -0.002(4) 0.024(4) -0.005(3) N2 0.026(4) 0.043(4) 0.046(6) -0.007(4) 0.007(4) 0.001(3) N3 0.050(4) 0.049(4) 0.069(5) -0.023(4) 0.024(4) -0.018(4) N4 0.026(4) 0.054(4) 0.051(5) -0.009(4) 0.016(4) 0.003(3) C20' 0.026(4) 0.054(4) 0.051(5) -0.009(4) 0.016(4) 0.003(3) N5 0.039(5) 0.070(6) 0.086(9) 0.015(6) 0.021(6) -0.012(5) N6 0.042(4) 0.045(4) 0.046(4) 0.001(3) 0.004(3) 0.005(3) C22' 0.042(4) 0.045(4) 0.046(4) 0.001(3) 0.004(3) 0.005(3) N7 0.043(6) 0.046(5) 0.044(5) 0.004(4) 0.007(5) -0.008(4) C23' 0.043(6) 0.046(5) 0.044(5) 0.004(4) 0.007(5) -0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O1 2.361(6) . ? Gd1 O3 2.371(6) . ? Gd1 O8 2.406(8) . ? Gd1 N4 2.423(8) . ? Gd1 N6 2.429(10) . ? Gd1 O5 2.455(7) . ? Gd1 O7 2.531(7) . ? Gd1 O4 2.606(6) . ? Gd1 O2 2.669(6) . ? Gd1 N3 2.904(9) . ? Gd1 H8 2.4(2) . ? Cu1 O3 1.896(6) . ? Cu1 N2 1.913(8) . ? Cu1 O1 1.921(6) . ? Cu1 N1 1.925(8) . ? Cu2 C20 1.905(10) . ? Cu2 C21 1.904(11) . ? Cu2 N7' 2.342(10) 1_556 ? Cu2 C23 2.342(10) 1_556 ? Cu2 Cu3 2.470(2) 1_556 ? Cu3 C23' 1.911(9) 4_566 ? Cu3 N7 1.911(9) 4_566 ? Cu3 C22 1.913(11) . ? Cu3 C23 1.965(11) . ? Cu3 Cu2 2.470(2) 1_554 ? C1 O1 1.326(10) . ? C1 C2 1.417(13) . ? C1 C6 1.425(13) . ? C2 O2 1.373(11) . ? C2 C3 1.383(13) . ? C3 C4 1.404(15) . ? C3 H3 0.9300 . ? C4 C5 1.345(15) . ? C4 H4 0.9300 . ? C5 C6 1.421(13) . ? C5 H5 0.9300 . ? C6 C7 1.449(14) . ? C7 N1 1.261(12) . ? C7 H7 0.9300 . ? C8 N1 1.494(12) . ? C8 C9 1.511(15) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N2 1.481(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.285(12) . ? C10 C11 1.460(12) . ? C10 H10 0.9300 . ? C11 C16 1.396(11) . ? C11 C12 1.418(12) . ? C12 C13 1.334(14) . ? C12 H12 0.9300 . ? C13 C14 1.361(14) . ? C13 H13 0.9300 . ? C14 C15 1.374(12) . ? C14 H14 0.9300 . ? C15 O4 1.385(10) . ? C15 C16 1.410(12) . ? C16 O3 1.327(10) . ? C17 O4 1.461(11) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 O2 1.444(11) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O8 1.422(13) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N4 1.124(12) . ? C21 N5 1.104(13) . ? C22 N6 1.175(14) . ? C23 N7 1.129(13) . ? C23 Cu2 2.342(10) 1_554 ? O5 N3 1.247(10) . ? O6 N3 1.234(12) . ? O7 N3 1.269(11) . ? O8 H8 0.90(5) . ? N7 Cu3 1.911(9) 4_565 ? 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 O3 64.8(2) . . ? O1 Gd1 O8 81.1(2) . . ? O3 Gd1 O8 75.2(2) . . ? O1 Gd1 N4 138.7(3) . . ? O3 Gd1 N4 138.1(3) . . ? O8 Gd1 N4 76.5(3) . . ? O1 Gd1 N6 88.2(3) . . ? O3 Gd1 N6 134.0(3) . . ? O8 Gd1 N6 139.4(3) . . ? N4 Gd1 N6 86.9(3) . . ? O1 Gd1 O5 92.9(2) . . ? O3 Gd1 O5 71.1(2) . . ? O8 Gd1 O5 144.9(2) . . ? N4 Gd1 O5 124.7(3) . . ? N6 Gd1 O5 74.1(3) . . ? O1 Gd1 O7 141.1(2) . . ? O3 Gd1 O7 107.7(2) . . ? O8 Gd1 O7 136.1(3) . . ? N4 Gd1 O7 73.8(3) . . ? N6 Gd1 O7 70.0(3) . . ? O5 Gd1 O7 51.0(2) . . ? O1 Gd1 O4 125.4(2) . . ? O3 Gd1 O4 61.39(19) . . ? O8 Gd1 O4 77.4(3) . . ? N4 Gd1 O4 82.7(3) . . ? N6 Gd1 O4 137.4(3) . . ? O5 Gd1 O4 78.4(2) . . ? O7 Gd1 O4 67.5(2) . . ? O1 Gd1 O2 61.26(19) . . ? O3 Gd1 O2 120.7(2) . . ? O8 Gd1 O2 73.9(2) . . ? N4 Gd1 O2 79.3(3) . . ? N6 Gd1 O2 66.7(3) . . ? O5 Gd1 O2 132.7(2) . . ? O7 Gd1 O2 129.6(2) . . ? O4 Gd1 O2 148.9(2) . . ? O1 Gd1 N3 116.6(2) . . ? O3 Gd1 N3 89.8(3) . . ? O8 Gd1 N3 149.6(3) . . ? N4 Gd1 N3 99.6(3) . . ? N6 Gd1 N3 69.0(3) . . ? O5 Gd1 N3 25.2(2) . . ? O7 Gd1 N3 25.8(2) . . ? O4 Gd1 N3 72.3(3) . . ? O2 Gd1 N3 135.7(3) . . ? O1 Gd1 H8 68(4) . . ? O3 Gd1 H8 85(4) . . ? O8 Gd1 H8 21.5(16) . . ? N4 Gd1 H8 80(5) . . ? N6 Gd1 H8 120(2) . . ? O5 Gd1 H8 154(5) . . ? O7 Gd1 H8 151(4) . . ? O4 Gd1 H8 98.8(17) . . ? O2 Gd1 H8 53(2) . . ? N3 Gd1 H8 171.1(17) . . ? O3 Cu1 N2 95.4(3) . . ? O3 Cu1 O1 83.3(2) . . ? N2 Cu1 O1 176.5(3) . . ? O3 Cu1 N1 173.7(4) . . ? N2 Cu1 N1 86.6(3) . . ? O1 Cu1 N1 94.4(3) . . ? O3 Cu1 Gd1 41.77(17) . . ? N2 Cu1 Gd1 136.7(2) . . ? O1 Cu1 Gd1 41.65(18) . . ? N1 Cu1 Gd1 135.2(3) . . ? C20 Cu2 C21 138.8(5) . . ? C20 Cu2 N7' 104.1(4) . 1_556 ? C21 Cu2 N7' 109.6(4) . 1_556 ? C20 Cu2 C23 104.1(4) . 1_556 ? C21 Cu2 C23 109.6(4) . 1_556 ? N7' Cu2 C23 0.00(5) 1_556 1_556 ? C20 Cu2 Cu3 120.0(3) . 1_556 ? C21 Cu2 Cu3 100.2(3) . 1_556 ? N7' Cu2 Cu3 48.1(3) 1_556 1_556 ? C23 Cu2 Cu3 48.1(3) 1_556 1_556 ? C23' Cu3 N7 0.0(7) 4_566 4_566 ? C23' Cu3 C22 116.2(5) 4_566 . ? N7 Cu3 C22 116.2(5) 4_566 . ? C23' Cu3 C23 112.1(4) 4_566 . ? N7 Cu3 C23 112.1(4) 4_566 . ? C22 Cu3 C23 129.3(5) . . ? C23' Cu3 Cu2 155.5(3) 4_566 1_554 ? N7 Cu3 Cu2 155.5(3) 4_566 1_554 ? C22 Cu3 Cu2 78.7(4) . 1_554 ? C23 Cu3 Cu2 62.5(3) . 1_554 ? O1 C1 C2 117.9(8) . . ? O1 C1 C6 123.3(8) . . ? C2 C1 C6 118.8(8) . . ? O2 C2 C3 125.9(9) . . ? O2 C2 C1 113.0(7) . . ? C3 C2 C1 121.0(9) . . ? C2 C3 C4 119.2(10) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 121.0(10) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 121.8(10) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 117.9(9) . . ? C5 C6 C7 118.1(9) . . ? C1 C6 C7 123.8(8) . . ? N1 C7 C6 125.1(9) . . ? N1 C7 H7 117.5 . . ? C6 C7 H7 117.5 . . ? N1 C8 C9 109.0(8) . . ? N1 C8 H8A 109.9 . . ? C9 C8 H8A 109.9 . . ? N1 C8 H8B 109.9 . . ? C9 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? N2 C9 C8 109.5(8) . . ? N2 C9 H9A 109.8 . . ? C8 C9 H9A 109.8 . . ? N2 C9 H9B 109.8 . . ? C8 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? N2 C10 C11 124.1(8) . . ? N2 C10 H10 118.0 . . ? C11 C10 H10 118.0 . . ? C16 C11 C12 117.8(8) . . ? C16 C11 C10 123.8(8) . . ? C12 C11 C10 118.3(8) . . ? C13 C12 C11 122.2(9) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C12 C13 C14 120.2(9) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C15 120.7(9) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C14 C15 O4 126.2(8) . . ? C14 C15 C16 120.5(8) . . ? O4 C15 C16 113.3(7) . . ? O3 C16 C11 125.1(8) . . ? O3 C16 C15 116.3(7) . . ? C11 C16 C15 118.6(8) . . ? O4 C17 H17A 109.5 . . ? O4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O2 C18 H18A 109.5 . . ? O2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O8 C19 H19A 109.5 . . ? O8 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O8 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C20 Cu2 176.3(11) . . ? N5 C21 Cu2 176.1(13) . . ? N6 C22 Cu3 166.0(11) . . ? N7 C23 Cu3 152.2(10) . . ? N7 C23 Cu2 136.8(10) . 1_554 ? Cu3 C23 Cu2 69.3(3) . 1_554 ? C1 O1 Cu1 122.7(5) . . ? C1 O1 Gd1 129.3(5) . . ? Cu1 O1 Gd1 105.6(2) . . ? C2 O2 C18 115.3(7) . . ? C2 O2 Gd1 118.1(5) . . ? C18 O2 Gd1 124.4(6) . . ? C16 O3 Cu1 125.3(5) . . ? C16 O3 Gd1 128.3(5) . . ? Cu1 O3 Gd1 106.0(2) . . ? C15 O4 C17 117.0(7) . . ? C15 O4 Gd1 118.6(5) . . ? C17 O4 Gd1 124.0(5) . . ? N3 O5 Gd1 98.0(6) . . ? N3 O7 Gd1 93.7(5) . . ? C19 O8 Gd1 136.7(7) . . ? C19 O8 H8 103(10) . . ? Gd1 O8 H8 81(10) . . ? C7 N1 C8 122.8(8) . . ? C7 N1 Cu1 125.2(7) . . ? C8 N1 Cu1 111.9(6) . . ? C10 N2 C9 121.3(8) . . ? C10 N2 Cu1 126.2(6) . . ? C9 N2 Cu1 112.5(6) . . ? O6 N3 O5 121.1(10) . . ? O6 N3 O7 121.8(10) . . ? O5 N3 O7 117.1(9) . . ? O6 N3 Gd1 175.6(9) . . ? O5 N3 Gd1 56.8(5) . . ? O7 N3 Gd1 60.4(5) . . ? C20 N4 Gd1 176.0(9) . . ? C22 N6 Gd1 162.9(10) . . ? C23 N7 Cu3 165.4(10) . 4_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H8 O2 0.90(5) 2.29(14) 3.058(10) 142(18) . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.891 _refine_diff_density_min -2.249 _refine_diff_density_rms 0.202