# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Kou, Hui-Zhong' 'Hu, Kong-Qiu' 'Zhao, Hao-Yan' 'Tang, Jin-Kui' 'Cui, Ai-Li' _publ_contact_author_name 'Kou, Hui-Zhong' _publ_contact_author_email kouhz@mail.tsinghua.edu.cn _publ_section_title ; Multi-component synthesis of trimetallic tetranuclear clusters [Cu(L)(H2O)]2Ln(H2O)2Cr(C2O4)3.12H2O (H2L = 1,4,8,11-Tetraazacyclotradecane-2,3-dione, Ln3+ = Gd, Tb and Dy) ; # Attachment '- cc-sub.cif' #=================================================================== data_Cu2GdCr _database_code_depnum_ccdc_archive 'CCDC 778856' #TrackingRef '- cc-sub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H68 Cr Cu2 Gd N8 O32' _chemical_formula_weight 1341.21 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' Cr Cr 0.3209 0.6236 '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 18.7457(7) _cell_length_b 16.3391(7) _cell_length_c 16.9184(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.3810(10) _cell_angle_gamma 90.00 _cell_volume 5097.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4856 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 27.47 _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2728 _exptl_absorpt_coefficient_mu 2.415 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.642 _exptl_absorpt_correction_T_max 0.830 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _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 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% ? _diffrn_reflns_number 23699 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5799 _reflns_number_gt 4856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.0557P)^2^+16.0878P] 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 5799 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.1056 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 0.5000 0.780546(15) 0.2500 0.03041(9) Uani 1 2 d S . . Cu1 Cu 0.31761(3) 0.51392(3) 0.28297(3) 0.04135(14) Uani 1 1 d . . . Cr1 Cr 0.5000 1.13651(5) 0.2500 0.03189(19) Uani 1 2 d S . . C1 C 0.4055(3) 0.4985(3) 0.1462(3) 0.0522(11) Uani 1 1 d . . . H1A H 0.4547 0.5140 0.1422 0.063 Uiso 1 1 calc R . . H1B H 0.3746 0.5108 0.0952 0.063 Uiso 1 1 calc R . . C2 C 0.4034(3) 0.4078(3) 0.1613(3) 0.0562(12) Uani 1 1 d . . . H2A H 0.4400 0.3951 0.2078 0.067 Uiso 1 1 calc R . . H2B H 0.4167 0.3797 0.1156 0.067 Uiso 1 1 calc R . . C3 C 0.3319(3) 0.3735(3) 0.1752(3) 0.0528(11) Uani 1 1 d . . . H3A H 0.2931 0.3948 0.1347 0.063 Uiso 1 1 calc R . . H3B H 0.3324 0.3144 0.1697 0.063 Uiso 1 1 calc R . . C4 C 0.2532(3) 0.3570(3) 0.2773(3) 0.0589(13) Uani 1 1 d . . . H4A H 0.2617 0.2990 0.2870 0.071 Uiso 1 1 calc R . . H4B H 0.2124 0.3632 0.2335 0.071 Uiso 1 1 calc R . . C5 C 0.2367(3) 0.3972(3) 0.3511(3) 0.0600(13) Uani 1 1 d . . . H5A H 0.1899 0.3788 0.3609 0.072 Uiso 1 1 calc R . . H5B H 0.2731 0.3821 0.3971 0.072 Uiso 1 1 calc R . . C6 C 0.2314(3) 0.5344(4) 0.4124(3) 0.0662(15) Uani 1 1 d . . . H6A H 0.2733 0.5222 0.4534 0.079 Uiso 1 1 calc R . . H6B H 0.1884 0.5180 0.4329 0.079 Uiso 1 1 calc R . . C7 C 0.2284(3) 0.6262(4) 0.3970(4) 0.0724(16) Uani 1 1 d . . . H7A H 0.1923 0.6367 0.3494 0.087 Uiso 1 1 calc R . . H7B H 0.2122 0.6529 0.4418 0.087 Uiso 1 1 calc R . . C8 C 0.2983(3) 0.6649(3) 0.3856(3) 0.0525(11) Uani 1 1 d . . . H8A H 0.2908 0.7230 0.3758 0.063 Uiso 1 1 calc R . . H8B H 0.3340 0.6585 0.4344 0.063 Uiso 1 1 calc R . . C9 C 0.3737(2) 0.6686(2) 0.2855(2) 0.0337(8) Uani 1 1 d . . . C10 C 0.40203(19) 0.6226(2) 0.2185(2) 0.0317(7) Uani 1 1 d . . . C11 C 0.53841(19) 0.9744(2) 0.2399(2) 0.0321(8) Uani 1 1 d . . . C12 C 0.4841(3) 1.2026(3) 0.0993(2) 0.0443(10) Uani 1 1 d . . . C13 C 0.5493(2) 1.2469(3) 0.1509(2) 0.0418(9) Uani 1 1 d . . . N1 N 0.2358(2) 0.4868(3) 0.3409(3) 0.0571(10) Uani 1 1 d . . . H1C H 0.1944 0.4981 0.3056 0.069 Uiso 1 1 calc R . . N2 N 0.3178(2) 0.3950(2) 0.2557(2) 0.0493(9) Uani 1 1 d . . . H2C H 0.3558 0.3735 0.2907 0.059 Uiso 1 1 calc R . . N3 N 0.38193(19) 0.5471(2) 0.2091(2) 0.0392(7) Uani 1 1 d . . . N4 N 0.32630(18) 0.6277(2) 0.3176(2) 0.0395(7) Uani 1 1 d . . . O1 O 0.44313(15) 0.66344(16) 0.18019(15) 0.0375(6) Uani 1 1 d . . . O2 O 0.39864(15) 0.73991(16) 0.30276(17) 0.0383(6) Uani 1 1 d . . . O3 O 0.56749(14) 0.90798(16) 0.23160(17) 0.0393(6) Uani 1 1 d . . . O4 O 0.56632(15) 1.04465(16) 0.23371(17) 0.0373(6) Uani 1 1 d . . . O5 O 0.45925(16) 1.14216(18) 0.13489(16) 0.0420(6) Uani 1 1 d . . . O6 O 0.56595(16) 1.22025(16) 0.22296(17) 0.0412(6) Uani 1 1 d . . . O7 O 0.5802(2) 1.3017(2) 0.12199(19) 0.0621(10) Uani 1 1 d . . . O8 O 0.4605(2) 1.2248(2) 0.0306(2) 0.0754(13) Uani 1 1 d . . . O1W O 0.40790(19) 0.4830(2) 0.4167(2) 0.0624(9) Uani 1 1 d . . . O2W O 0.45007(18) 0.82467(19) 0.11774(17) 0.0508(7) Uani 1 1 d . . . O3W O 0.49757(18) 1.37674(19) -0.04020(18) 0.0504(7) Uani 1 1 d . . . O4W O 0.3655(2) 1.1334(3) -0.0801(2) 0.0812(13) Uani 1 1 d . . . O5W O 0.4503(3) 0.9817(3) 0.0547(3) 0.0957(15) Uani 1 1 d . . . O6W O 0.2500(3) 0.6603(4) 0.0783(4) 0.127(2) Uani 1 1 d . . . O7W O 0.3276(4) 0.9745(3) -0.1270(5) 0.159(3) Uani 1 1 d . . . O8W O 0.3549(2) 0.7384(2) 0.0107(2) 0.0632(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.03256(14) 0.02319(14) 0.03809(15) 0.000 0.01339(10) 0.000 Cu1 0.0387(3) 0.0332(3) 0.0556(3) 0.0080(2) 0.0175(2) -0.0059(2) Cr1 0.0379(4) 0.0236(4) 0.0357(4) 0.000 0.0106(3) 0.000 C1 0.071(3) 0.036(2) 0.056(3) -0.0079(19) 0.029(2) -0.009(2) C2 0.062(3) 0.037(2) 0.072(3) -0.008(2) 0.018(2) -0.007(2) C3 0.060(3) 0.037(2) 0.058(3) 0.000(2) 0.001(2) -0.010(2) C4 0.049(3) 0.049(3) 0.075(3) 0.017(2) 0.001(2) -0.019(2) C5 0.045(3) 0.060(3) 0.076(3) 0.023(3) 0.013(2) -0.018(2) C6 0.060(3) 0.076(4) 0.073(3) 0.014(3) 0.040(3) -0.012(3) C7 0.061(3) 0.072(4) 0.098(4) 0.000(3) 0.051(3) 0.000(3) C8 0.051(3) 0.050(3) 0.065(3) 0.000(2) 0.033(2) 0.000(2) C9 0.0309(18) 0.0306(19) 0.0404(19) 0.0083(15) 0.0090(15) 0.0019(15) C10 0.0301(18) 0.0317(19) 0.0335(17) 0.0022(14) 0.0061(14) -0.0019(15) C11 0.0311(19) 0.0259(18) 0.0412(19) 0.0008(14) 0.0118(15) -0.0003(14) C12 0.057(3) 0.038(2) 0.039(2) -0.0023(17) 0.0112(18) -0.008(2) C13 0.055(3) 0.031(2) 0.041(2) -0.0025(16) 0.0134(18) -0.0078(19) N1 0.045(2) 0.059(3) 0.070(3) 0.015(2) 0.0167(19) -0.0104(19) N2 0.045(2) 0.037(2) 0.064(2) 0.0128(17) 0.0048(17) -0.0089(16) N3 0.0458(19) 0.0283(17) 0.0476(19) 0.0006(13) 0.0192(15) -0.0057(14) N4 0.0376(17) 0.0351(18) 0.0502(19) 0.0051(14) 0.0200(15) 0.0006(14) O1 0.0463(15) 0.0319(14) 0.0385(13) 0.0001(11) 0.0185(12) -0.0104(12) O2 0.0404(15) 0.0269(14) 0.0523(16) -0.0014(11) 0.0206(12) -0.0017(11) O3 0.0332(14) 0.0282(14) 0.0601(17) -0.0004(12) 0.0185(12) 0.0020(11) O4 0.0358(14) 0.0276(14) 0.0527(16) -0.0039(11) 0.0191(12) -0.0040(11) O5 0.0508(17) 0.0379(16) 0.0365(14) -0.0009(11) 0.0060(12) -0.0115(13) O6 0.0488(16) 0.0318(15) 0.0422(15) 0.0017(11) 0.0061(12) -0.0098(12) O7 0.077(2) 0.058(2) 0.0508(18) 0.0090(15) 0.0096(17) -0.0318(19) O8 0.101(3) 0.075(3) 0.0420(18) 0.0148(16) -0.0087(18) -0.036(2) O1W 0.054(2) 0.050(2) 0.078(2) 0.0024(17) -0.0003(17) -0.0051(17) O2W 0.066(2) 0.0398(17) 0.0449(16) 0.0058(13) 0.0045(14) -0.0005(15) O3W 0.063(2) 0.0403(17) 0.0487(17) 0.0018(13) 0.0139(14) 0.0031(15) O4W 0.080(3) 0.104(3) 0.060(2) -0.010(2) 0.0139(19) -0.034(3) O5W 0.113(4) 0.066(3) 0.107(4) 0.011(2) 0.016(3) 0.001(3) O6W 0.081(3) 0.145(5) 0.152(5) 0.080(4) 0.014(3) -0.005(3) O7W 0.200(7) 0.082(4) 0.246(8) 0.040(4) 0.177(7) 0.021(4) O8W 0.058(2) 0.072(2) 0.057(2) -0.0015(17) 0.0041(16) -0.0029(19) _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 O2 2.336(3) . ? Gd1 O2 2.336(3) 2_655 ? Gd1 O2W 2.377(3) 2_655 ? Gd1 O2W 2.377(3) . ? Gd1 O1 2.396(3) . ? Gd1 O1 2.396(3) 2_655 ? Gd1 O3 2.485(3) . ? Gd1 O3 2.485(3) 2_655 ? Cu1 N4 1.947(3) . ? Cu1 N3 1.963(3) . ? Cu1 N2 1.997(4) . ? Cu1 N1 2.012(4) . ? Cu1 O1W 2.619(4) . ? Cr1 O6 1.953(3) 2_655 ? Cr1 O6 1.953(3) . ? Cr1 O5 1.962(3) 2_655 ? Cr1 O5 1.962(3) . ? Cr1 O4 2.000(3) 2_655 ? Cr1 O4 2.000(3) . ? C1 N3 1.459(5) . ? C1 C2 1.505(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.509(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.476(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N2 1.465(6) . ? C4 C5 1.493(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.473(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N1 1.453(7) . ? C6 C7 1.523(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.498(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N4 1.478(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O2 1.270(5) . ? C9 N4 1.306(5) . ? C9 C10 1.532(5) . ? C10 O1 1.281(4) . ? C10 N3 1.291(5) . ? C11 O3 1.233(4) . ? C11 O4 1.274(4) . ? C11 C11 1.538(7) 2_655 ? C12 O8 1.221(5) . ? C12 O5 1.287(5) . ? C12 C13 1.548(6) . ? C13 O7 1.217(5) . ? C13 O6 1.279(5) . ? N1 H1C 0.9100 . ? N2 H2C 0.9100 . ? 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 O2 Gd1 O2 146.98(13) . 2_655 ? O2 Gd1 O2W 86.33(11) . 2_655 ? O2 Gd1 O2W 103.68(11) 2_655 2_655 ? O2 Gd1 O2W 103.68(11) . . ? O2 Gd1 O2W 86.33(11) 2_655 . ? O2W Gd1 O2W 144.68(15) 2_655 . ? O2 Gd1 O1 68.97(9) . . ? O2 Gd1 O1 84.55(9) 2_655 . ? O2W Gd1 O1 140.47(10) 2_655 . ? O2W Gd1 O1 73.34(10) . . ? O2 Gd1 O1 84.55(9) . 2_655 ? O2 Gd1 O1 68.97(9) 2_655 2_655 ? O2W Gd1 O1 73.34(10) 2_655 2_655 ? O2W Gd1 O1 140.47(10) . 2_655 ? O1 Gd1 O1 73.99(14) . 2_655 ? O2 Gd1 O3 138.89(9) . . ? O2 Gd1 O3 73.91(9) 2_655 . ? O2W Gd1 O3 74.97(10) 2_655 . ? O2W Gd1 O3 75.58(10) . . ? O1 Gd1 O3 143.02(9) . . ? O1 Gd1 O3 122.66(9) 2_655 . ? O2 Gd1 O3 73.91(9) . 2_655 ? O2 Gd1 O3 138.89(9) 2_655 2_655 ? O2W Gd1 O3 75.58(10) 2_655 2_655 ? O2W Gd1 O3 74.97(10) . 2_655 ? O1 Gd1 O3 122.66(9) . 2_655 ? O1 Gd1 O3 143.02(9) 2_655 2_655 ? O3 Gd1 O3 66.16(12) . 2_655 ? N4 Cu1 N3 84.29(13) . . ? N4 Cu1 N2 174.15(16) . . ? N3 Cu1 N2 95.41(14) . . ? N4 Cu1 N1 95.37(16) . . ? N3 Cu1 N1 168.63(17) . . ? N2 Cu1 N1 86.08(17) . . ? O6 Cr1 O6 91.05(18) 2_655 . ? O6 Cr1 O5 83.35(12) 2_655 2_655 ? O6 Cr1 O5 92.86(12) . 2_655 ? O6 Cr1 O5 92.86(12) 2_655 . ? O6 Cr1 O5 83.35(12) . . ? O5 Cr1 O5 174.61(18) 2_655 . ? O6 Cr1 O4 93.33(11) 2_655 2_655 ? O6 Cr1 O4 173.63(12) . 2_655 ? O5 Cr1 O4 92.24(12) 2_655 2_655 ? O5 Cr1 O4 91.81(12) . 2_655 ? O6 Cr1 O4 173.63(12) 2_655 . ? O6 Cr1 O4 93.33(11) . . ? O5 Cr1 O4 91.81(12) 2_655 . ? O5 Cr1 O4 92.24(12) . . ? O4 Cr1 O4 82.70(15) 2_655 . ? N3 C1 C2 113.0(4) . . ? N3 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? N3 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? C1 C2 C3 116.3(4) . . ? C1 C2 H2A 108.2 . . ? C3 C2 H2A 108.2 . . ? C1 C2 H2B 108.2 . . ? C3 C2 H2B 108.2 . . ? H2A C2 H2B 107.4 . . ? N2 C3 C2 111.5(4) . . ? N2 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? N2 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? N2 C4 C5 109.1(4) . . ? N2 C4 H4A 109.9 . . ? C5 C4 H4A 109.9 . . ? N2 C4 H4B 109.9 . . ? C5 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? N1 C5 C4 109.8(4) . . ? N1 C5 H5A 109.7 . . ? C4 C5 H5A 109.7 . . ? N1 C5 H5B 109.7 . . ? C4 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? N1 C6 C7 113.0(4) . . ? N1 C6 H6A 109.0 . . ? C7 C6 H6A 109.0 . . ? N1 C6 H6B 109.0 . . ? C7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C6 115.6(5) . . ? C8 C7 H7A 108.4 . . ? C6 C7 H7A 108.4 . . ? C8 C7 H7B 108.4 . . ? C6 C7 H7B 108.4 . . ? H7A C7 H7B 107.5 . . ? N4 C8 C7 111.6(4) . . ? N4 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? N4 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? O2 C9 N4 128.5(4) . . ? O2 C9 C10 117.3(3) . . ? N4 C9 C10 114.2(3) . . ? O1 C10 N3 128.6(3) . . ? O1 C10 C9 116.0(3) . . ? N3 C10 C9 115.3(3) . . ? O3 C11 O4 125.9(3) . . ? O3 C11 C11 118.4(2) . 2_655 ? O4 C11 C11 115.7(2) . 2_655 ? O8 C12 O5 125.0(4) . . ? O8 C12 C13 120.8(4) . . ? O5 C12 C13 114.2(4) . . ? O7 C13 O6 125.6(4) . . ? O7 C13 C12 120.2(4) . . ? O6 C13 C12 114.3(3) . . ? C6 N1 C5 115.8(4) . . ? C6 N1 Cu1 116.8(3) . . ? C5 N1 Cu1 106.4(3) . . ? C6 N1 H1C 105.6 . . ? C5 N1 H1C 105.6 . . ? Cu1 N1 H1C 105.6 . . ? C4 N2 C3 115.0(4) . . ? C4 N2 Cu1 108.6(3) . . ? C3 N2 Cu1 116.9(3) . . ? C4 N2 H2C 105.0 . . ? C3 N2 H2C 105.0 . . ? Cu1 N2 H2C 105.0 . . ? C10 N3 C1 119.4(3) . . ? C10 N3 Cu1 112.6(3) . . ? C1 N3 Cu1 128.0(3) . . ? C9 N4 C8 118.5(4) . . ? C9 N4 Cu1 112.9(3) . . ? C8 N4 Cu1 127.2(3) . . ? C10 O1 Gd1 115.0(2) . . ? C9 O2 Gd1 117.6(2) . . ? C11 O3 Gd1 118.5(2) . . ? C11 O4 Cr1 113.0(2) . . ? C12 O5 Cr1 113.1(3) . . ? C13 O6 Cr1 113.9(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.820 _refine_diff_density_min -0.890 _refine_diff_density_rms 0.114 #===End data_Cu2TbCr _database_code_depnum_ccdc_archive 'CCDC 778857' #TrackingRef '- cc-sub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H68 Cr Cu2 N8 O32 Tb' _chemical_formula_weight 1342.88 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' Cr Cr 0.3209 0.6236 '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 18.7089(18) _cell_length_b 16.3018(16) _cell_length_c 16.9124(14) _cell_angle_alpha 90.00 _cell_angle_beta 100.505(3) _cell_angle_gamma 90.00 _cell_volume 5071.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3526 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 27.48 _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2732 _exptl_absorpt_coefficient_mu 2.514 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.642 _exptl_absorpt_correction_T_max 0.830 _exptl_absorpt_process_details 'ABSCOR; Higashi, 1995' _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 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% ? _diffrn_reflns_number 24048 _diffrn_reflns_av_R_equivalents 0.0991 _diffrn_reflns_av_sigmaI/netI 0.0829 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5784 _reflns_number_gt 3526 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.0675P)^2^+41.1644P] 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 SHELXL _refine_ls_extinction_coef 0.00075(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5784 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1197 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1901 _refine_ls_wR_factor_gt 0.1341 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 Tb1 Tb 0.5000 0.78108(3) 0.2500 0.0458(2) Uani 1 2 d S . . Cu1 Cu 0.31780(6) 0.51461(7) 0.28316(7) 0.0557(3) Uani 1 1 d . . . Cr1 Cr 0.5000 1.13664(11) 0.2500 0.0455(5) Uani 1 2 d S . . C1 C 0.4059(6) 0.4991(6) 0.1466(6) 0.065(3) Uani 1 1 d . . . H1A H 0.4554 0.5143 0.1438 0.078 Uiso 1 1 calc R . . H1B H 0.3757 0.5123 0.0952 0.078 Uiso 1 1 calc R . . C2 C 0.4027(6) 0.4081(6) 0.1603(7) 0.071(3) Uani 1 1 d . . . H2A H 0.4396 0.3942 0.2065 0.085 Uiso 1 1 calc R . . H2B H 0.4154 0.3804 0.1140 0.085 Uiso 1 1 calc R . . C3 C 0.3309(6) 0.3747(6) 0.1742(6) 0.069(3) Uani 1 1 d . . . H3A H 0.2920 0.3973 0.1343 0.083 Uiso 1 1 calc R . . H3B H 0.3304 0.3156 0.1678 0.083 Uiso 1 1 calc R . . C4 C 0.2526(6) 0.3587(6) 0.2773(7) 0.071(3) Uani 1 1 d . . . H4A H 0.2601 0.3002 0.2862 0.086 Uiso 1 1 calc R . . H4B H 0.2116 0.3662 0.2338 0.086 Uiso 1 1 calc R . . C5 C 0.2373(6) 0.3979(7) 0.3512(6) 0.073(3) Uani 1 1 d . . . H5A H 0.1908 0.3791 0.3617 0.088 Uiso 1 1 calc R . . H5B H 0.2745 0.3827 0.3966 0.088 Uiso 1 1 calc R . . C6 C 0.2312(6) 0.5358(7) 0.4128(7) 0.080(3) Uani 1 1 d . . . H6A H 0.2729 0.5236 0.4544 0.096 Uiso 1 1 calc R . . H6B H 0.1878 0.5200 0.4328 0.096 Uiso 1 1 calc R . . C7 C 0.2289(6) 0.6268(7) 0.3965(7) 0.081(3) Uani 1 1 d . . . H7A H 0.1931 0.6369 0.3483 0.097 Uiso 1 1 calc R . . H7B H 0.2122 0.6541 0.4407 0.097 Uiso 1 1 calc R . . C8 C 0.2991(5) 0.6656(6) 0.3857(6) 0.063(3) Uani 1 1 d . . . H8A H 0.2916 0.7239 0.3761 0.076 Uiso 1 1 calc R . . H8B H 0.3347 0.6589 0.4346 0.076 Uiso 1 1 calc R . . C9 C 0.3746(4) 0.6698(5) 0.2859(5) 0.0469(19) Uani 1 1 d . . . C10 C 0.4031(5) 0.6229(5) 0.2191(5) 0.0456(19) Uani 1 1 d . . . C11 C 0.5383(4) 0.9746(5) 0.2411(5) 0.0446(19) Uani 1 1 d . . . C12 C 0.4842(5) 1.2019(6) 0.0996(6) 0.059(2) Uani 1 1 d . . . C13 C 0.5507(5) 1.2458(6) 0.1512(5) 0.054(2) Uani 1 1 d . . . N1 N 0.2360(5) 0.4879(5) 0.3412(5) 0.069(2) Uani 1 1 d . . . H1C H 0.1945 0.4990 0.3057 0.083 Uiso 1 1 calc R . . N2 N 0.3176(4) 0.3953(5) 0.2558(5) 0.065(2) Uani 1 1 d . . . H2C H 0.3556 0.3733 0.2905 0.078 Uiso 1 1 calc R . . N3 N 0.3818(4) 0.5474(4) 0.2089(4) 0.0550(18) Uani 1 1 d . . . N4 N 0.3271(4) 0.6288(4) 0.3180(4) 0.0535(18) Uani 1 1 d . . . O1 O 0.4437(3) 0.6633(3) 0.1804(3) 0.0504(14) Uani 1 1 d . . . O2 O 0.3992(3) 0.7404(3) 0.3029(4) 0.0502(14) Uani 1 1 d . . . O3 O 0.5670(3) 0.9077(3) 0.2322(4) 0.0513(14) Uani 1 1 d . . . O4 O 0.5668(3) 1.0447(3) 0.2343(3) 0.0491(14) Uani 1 1 d . . . O5 O 0.4595(3) 1.1420(3) 0.1348(3) 0.0529(15) Uani 1 1 d . . . O6 O 0.5660(3) 1.2203(3) 0.2232(3) 0.0540(15) Uani 1 1 d . . . O7 O 0.5808(4) 1.3013(4) 0.1220(4) 0.076(2) Uani 1 1 d . . . O8 O 0.4614(5) 1.2243(5) 0.0307(4) 0.091(3) Uani 1 1 d . . . O1W O 0.4085(4) 0.4835(4) 0.4173(4) 0.077(2) Uani 1 1 d . . . O2W O 0.4497(4) 0.8251(4) 0.1172(4) 0.0676(18) Uani 1 1 d . . . O3W O 0.4983(4) 1.3761(4) -0.0404(4) 0.0652(17) Uani 1 1 d . . . O4W O 0.3673(5) 1.1304(6) -0.0796(5) 0.102(3) Uani 1 1 d . . . O5W O 0.4509(6) 0.9818(5) 0.0543(6) 0.117(3) Uani 1 1 d . . . O6W O 0.2498(6) 0.6608(7) 0.0776(7) 0.141(4) Uani 1 1 d . . . O7W O 0.3267(8) 0.9736(6) -0.1280(9) 0.176(6) Uani 1 1 d . . . O8W O 0.3553(4) 0.7382(5) 0.0104(4) 0.083(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.0479(4) 0.0366(3) 0.0562(4) 0.000 0.0180(3) 0.000 Cu1 0.0531(7) 0.0469(7) 0.0706(7) 0.0083(5) 0.0207(6) -0.0056(5) Cr1 0.0494(11) 0.0365(10) 0.0527(11) 0.000 0.0153(9) 0.000 C1 0.081(7) 0.044(5) 0.077(6) -0.017(5) 0.029(5) -0.009(5) C2 0.074(7) 0.055(6) 0.089(7) -0.012(5) 0.030(6) -0.011(5) C3 0.069(7) 0.057(6) 0.076(7) -0.006(5) 0.000(5) -0.018(5) C4 0.062(7) 0.058(6) 0.094(8) 0.009(5) 0.014(6) -0.016(5) C5 0.057(6) 0.081(8) 0.082(7) 0.016(6) 0.016(5) -0.015(5) C6 0.072(7) 0.088(8) 0.090(8) 0.018(6) 0.045(6) 0.004(6) C7 0.073(8) 0.083(8) 0.098(8) 0.001(6) 0.043(6) 0.008(6) C8 0.058(6) 0.062(6) 0.080(6) -0.003(5) 0.041(5) -0.005(5) C9 0.042(5) 0.044(5) 0.055(5) 0.010(4) 0.009(4) 0.003(4) C10 0.046(5) 0.045(5) 0.050(5) 0.005(4) 0.021(4) 0.000(4) C11 0.048(5) 0.039(4) 0.051(5) 0.003(3) 0.019(4) 0.004(4) C12 0.066(6) 0.058(6) 0.054(5) -0.008(4) 0.013(5) -0.005(5) C13 0.069(6) 0.046(5) 0.055(5) 0.001(4) 0.027(5) -0.008(4) N1 0.055(5) 0.070(6) 0.085(6) 0.017(5) 0.020(4) -0.007(4) N2 0.062(5) 0.049(5) 0.082(6) 0.008(4) 0.009(4) -0.019(4) N3 0.059(5) 0.040(4) 0.069(5) 0.005(3) 0.020(4) -0.005(3) N4 0.053(4) 0.051(4) 0.062(4) 0.007(3) 0.024(4) 0.007(4) O1 0.059(4) 0.043(3) 0.053(3) 0.000(3) 0.019(3) -0.010(3) O2 0.043(3) 0.041(3) 0.073(4) -0.002(3) 0.025(3) -0.012(3) O3 0.035(3) 0.045(3) 0.080(4) 0.002(3) 0.024(3) 0.001(3) O4 0.042(3) 0.039(3) 0.073(4) -0.004(3) 0.027(3) -0.003(3) O5 0.058(4) 0.042(3) 0.059(4) 0.000(3) 0.014(3) -0.013(3) O6 0.068(4) 0.044(3) 0.048(3) 0.003(3) 0.007(3) -0.010(3) O7 0.091(5) 0.072(5) 0.066(4) 0.012(3) 0.015(4) -0.032(4) O8 0.114(7) 0.092(6) 0.057(4) 0.013(4) -0.010(4) -0.041(5) O1W 0.071(5) 0.068(5) 0.085(5) 0.003(4) -0.003(4) -0.006(4) O2W 0.077(5) 0.062(4) 0.061(4) 0.007(3) 0.006(3) 0.003(4) O3W 0.078(5) 0.056(4) 0.063(4) 0.000(3) 0.018(3) 0.004(3) O4W 0.094(6) 0.131(8) 0.083(5) -0.007(5) 0.025(5) -0.036(6) O5W 0.142(9) 0.080(6) 0.127(8) 0.006(5) 0.015(6) -0.001(6) O6W 0.101(8) 0.153(10) 0.168(10) 0.070(8) 0.020(7) 0.001(7) O7W 0.220(14) 0.092(8) 0.267(15) 0.052(8) 0.179(13) 0.021(8) O8W 0.080(5) 0.089(6) 0.075(5) 0.003(4) 0.000(4) -0.002(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 Tb1 O2 2.325(5) 2_655 ? Tb1 O2 2.325(5) . ? Tb1 O2W 2.382(6) 2_655 ? Tb1 O2W 2.382(6) . ? Tb1 O1 2.394(6) . ? Tb1 O1 2.394(6) 2_655 ? Tb1 O3 2.462(6) . ? Tb1 O3 2.462(6) 2_655 ? Cu1 N4 1.950(7) . ? Cu1 N3 1.962(7) . ? Cu1 N2 1.999(8) . ? Cu1 N1 2.010(8) . ? Cr1 O6 1.948(6) . ? Cr1 O6 1.948(6) 2_655 ? Cr1 O5 1.959(6) . ? Cr1 O5 1.959(6) 2_655 ? Cr1 O4 2.000(6) 2_655 ? Cr1 O4 2.000(6) . ? C1 N3 1.450(11) . ? C1 C2 1.504(13) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.509(13) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.484(12) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N2 1.458(12) . ? C4 C5 1.477(14) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.476(13) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N1 1.458(14) . ? C6 C7 1.507(15) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.498(13) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N4 1.471(11) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O2 1.254(10) . ? C9 N4 1.307(10) . ? C9 C10 1.537(11) . ? C10 O1 1.274(9) . ? C10 N3 1.295(10) . ? C11 O3 1.236(9) . ? C11 O4 1.277(9) . ? C11 C11 1.516(16) 2_655 ? C12 O8 1.221(11) . ? C12 O5 1.274(11) . ? C12 C13 1.557(13) . ? C13 O7 1.217(10) . ? C13 O6 1.269(10) . ? N1 H1C 0.9100 . ? N2 H2C 0.9100 . ? 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 O2 Tb1 O2 146.9(3) 2_655 . ? O2 Tb1 O2W 103.9(2) 2_655 2_655 ? O2 Tb1 O2W 86.1(2) . 2_655 ? O2 Tb1 O2W 86.1(2) 2_655 . ? O2 Tb1 O2W 103.9(2) . . ? O2W Tb1 O2W 144.9(3) 2_655 . ? O2 Tb1 O1 84.1(2) 2_655 . ? O2 Tb1 O1 69.26(19) . . ? O2W Tb1 O1 140.2(2) 2_655 . ? O2W Tb1 O1 73.5(2) . . ? O2 Tb1 O1 69.26(19) 2_655 2_655 ? O2 Tb1 O1 84.1(2) . 2_655 ? O2W Tb1 O1 73.5(2) 2_655 2_655 ? O2W Tb1 O1 140.2(2) . 2_655 ? O1 Tb1 O1 73.3(3) . 2_655 ? O2 Tb1 O3 74.06(19) 2_655 . ? O2 Tb1 O3 138.81(19) . . ? O2W Tb1 O3 75.0(2) 2_655 . ? O2W Tb1 O3 75.8(2) . . ? O1 Tb1 O3 143.18(19) . . ? O1 Tb1 O3 123.0(2) 2_655 . ? O2 Tb1 O3 138.81(19) 2_655 2_655 ? O2 Tb1 O3 74.06(19) . 2_655 ? O2W Tb1 O3 75.8(2) 2_655 2_655 ? O2W Tb1 O3 75.0(2) . 2_655 ? O1 Tb1 O3 123.02(19) . 2_655 ? O1 Tb1 O3 143.18(19) 2_655 2_655 ? O3 Tb1 O3 66.0(2) . 2_655 ? N4 Cu1 N3 84.4(3) . . ? N4 Cu1 N2 174.1(3) . . ? N3 Cu1 N2 95.3(3) . . ? N4 Cu1 N1 95.3(3) . . ? N3 Cu1 N1 168.4(3) . . ? N2 Cu1 N1 86.1(3) . . ? O6 Cr1 O6 91.1(4) . 2_655 ? O6 Cr1 O5 83.3(2) . . ? O6 Cr1 O5 93.1(2) 2_655 . ? O6 Cr1 O5 93.1(2) . 2_655 ? O6 Cr1 O5 83.3(2) 2_655 2_655 ? O5 Cr1 O5 174.9(3) . 2_655 ? O6 Cr1 O4 173.5(2) . 2_655 ? O6 Cr1 O4 93.2(2) 2_655 2_655 ? O5 Cr1 O4 91.6(2) . 2_655 ? O5 Cr1 O4 92.2(2) 2_655 2_655 ? O6 Cr1 O4 93.2(2) . . ? O6 Cr1 O4 173.5(2) 2_655 . ? O5 Cr1 O4 92.2(2) . . ? O5 Cr1 O4 91.6(2) 2_655 . ? O4 Cr1 O4 83.0(3) 2_655 . ? N3 C1 C2 113.5(8) . . ? N3 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? N3 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C1 C2 C3 116.1(9) . . ? C1 C2 H2A 108.3 . . ? C3 C2 H2A 108.3 . . ? C1 C2 H2B 108.3 . . ? C3 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? N2 C3 C2 111.6(8) . . ? N2 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? N2 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? N2 C4 C5 109.4(8) . . ? N2 C4 H4A 109.8 . . ? C5 C4 H4A 109.8 . . ? N2 C4 H4B 109.8 . . ? C5 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? N1 C5 C4 109.6(8) . . ? N1 C5 H5A 109.7 . . ? C4 C5 H5A 109.7 . . ? N1 C5 H5B 109.7 . . ? C4 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? N1 C6 C7 112.3(9) . . ? N1 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? N1 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C8 C7 C6 116.2(9) . . ? C8 C7 H7A 108.2 . . ? C6 C7 H7A 108.2 . . ? C8 C7 H7B 108.2 . . ? C6 C7 H7B 108.2 . . ? H7A C7 H7B 107.4 . . ? N4 C8 C7 111.5(8) . . ? N4 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? N4 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? O2 C9 N4 128.7(8) . . ? O2 C9 C10 117.5(7) . . ? N4 C9 C10 113.8(8) . . ? O1 C10 N3 128.3(8) . . ? O1 C10 C9 116.2(7) . . ? N3 C10 C9 115.6(7) . . ? O3 C11 O4 125.5(7) . . ? O3 C11 C11 118.1(5) . 2_655 ? O4 C11 C11 116.3(4) . 2_655 ? O8 C12 O5 125.5(9) . . ? O8 C12 C13 120.2(9) . . ? O5 C12 C13 114.3(8) . . ? O7 C13 O6 126.4(9) . . ? O7 C13 C12 119.7(8) . . ? O6 C13 C12 113.9(8) . . ? C6 N1 C5 116.1(8) . . ? C6 N1 Cu1 117.2(7) . . ? C5 N1 Cu1 105.8(6) . . ? C6 N1 H1C 105.5 . . ? C5 N1 H1C 105.5 . . ? Cu1 N1 H1C 105.5 . . ? C4 N2 C3 115.3(8) . . ? C4 N2 Cu1 107.9(6) . . ? C3 N2 Cu1 116.2(6) . . ? C4 N2 H2C 105.5 . . ? C3 N2 H2C 105.5 . . ? Cu1 N2 H2C 105.5 . . ? C10 N3 C1 119.0(7) . . ? C10 N3 Cu1 112.4(6) . . ? C1 N3 Cu1 128.5(6) . . ? C9 N4 C8 118.7(8) . . ? C9 N4 Cu1 113.1(6) . . ? C8 N4 Cu1 126.8(6) . . ? C10 O1 Tb1 114.3(5) . . ? C9 O2 Tb1 117.6(5) . . ? C11 O3 Tb1 118.8(5) . . ? C11 O4 Cr1 112.2(5) . . ? C12 O5 Cr1 113.1(6) . . ? C13 O6 Cr1 114.3(6) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.345 _refine_diff_density_min -2.156 _refine_diff_density_rms 0.180