# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H12 Cu N6 O16 Tb2, 2(H2 O)' _chemical_formula_sum 'C15 H16 Cu N6 O18 Tb2' _chemical_formula_weight 949.72 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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1693(3) _cell_length_b 11.2220(5) _cell_length_c 15.5135(7) _cell_angle_alpha 82.772(2) _cell_angle_beta 77.2510(10) _cell_angle_gamma 84.525(2) _cell_volume 1204.72(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9904 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 28.31 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 902 _exptl_absorpt_coefficient_mu 6.784 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3168 _exptl_absorpt_correction_T_max 0.6481 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21653 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_unetI/netI 0.0222 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 28.33 _reflns_number_total 5908 _reflns_number_gt 5543 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+1.3559P] 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 5908 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0199 _refine_ls_R_factor_gt 0.0180 _refine_ls_wR_factor_ref 0.0455 _refine_ls_wR_factor_gt 0.0447 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.003 _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 Tb2 Tb 0.516055(15) 0.661783(10) 0.349435(7) 0.00816(4) Uani 1 1 d . . . Tb1 Tb 0.476488(16) 0.769456(10) 0.756222(7) 0.00840(4) Uani 1 1 d . . . Cu1 Cu 0.19190(4) 0.81193(3) 1.042588(19) 0.01070(7) Uani 1 1 d . . . C1 C 0.3815(4) 0.4872(2) 0.80630(16) 0.0119(5) Uani 1 1 d . . . C2 C 0.3117(4) 0.5319(2) 0.89417(16) 0.0105(5) Uani 1 1 d . . . C3 C 0.2447(4) 0.4736(2) 0.97844(16) 0.0119(5) Uani 1 1 d . . . H3 H 0.2302 0.3902 0.9955 0.014 Uiso 1 1 calc R . . C4 C 0.2042(3) 0.5684(2) 1.03170(16) 0.0104(5) Uani 1 1 d . . . C5 C 0.1250(3) 0.5827(2) 1.12637(16) 0.0109(5) Uani 1 1 d . . . C6 C 0.5646(3) 1.0525(2) 0.74140(16) 0.0106(5) Uani 1 1 d . . . C7 C 0.4540(3) 1.0350(2) 0.83393(16) 0.0104(5) Uani 1 1 d . . . C8 C 0.3725(3) 1.1146(2) 0.89669(16) 0.0109(5) Uani 1 1 d . . . H8 H 0.3774 1.1996 0.8914 0.013 Uiso 1 1 calc R . . C9 C 0.2832(3) 1.0393(2) 0.96844(16) 0.0104(5) Uani 1 1 d . . . C10 C 0.1591(3) 1.0526(2) 1.05757(17) 0.0110(5) Uani 1 1 d . . . C11 C 0.5672(3) 0.7642(2) 0.54083(16) 0.0098(5) Uani 1 1 d . . . C12 C 0.7584(3) 0.7194(2) 0.55885(16) 0.0101(5) Uani 1 1 d . . . C13 C 0.9276(3) 0.6787(2) 0.50334(16) 0.0103(5) Uani 1 1 d . . . H13 H 0.9560 0.6832 0.4403 0.012 Uiso 1 1 calc R . . C14 C 1.0433(3) 0.6307(2) 0.56042(16) 0.0105(5) Uani 1 1 d . . . C15 C 1.2260(3) 0.5546(2) 0.54544(17) 0.0101(5) Uani 1 1 d . . . N1 N 0.3124(3) 0.65207(19) 0.89627(14) 0.0119(4) Uani 1 1 d . . . N2 N 0.2469(3) 0.67224(19) 0.98046(14) 0.0119(4) Uani 1 1 d . . . N3 N 0.4152(3) 0.9201(2) 0.86650(14) 0.0117(4) Uani 1 1 d . . . N4 N 0.3110(3) 0.92453(19) 0.94904(14) 0.0110(4) Uani 1 1 d . . . N5 N 0.7714(3) 0.7027(2) 0.64427(14) 0.0118(4) Uani 1 1 d . . . N6 N 0.9457(3) 0.6475(2) 0.64416(14) 0.0123(4) Uani 1 1 d . . . H6N H 0.9913 0.6250 0.6923 0.015 Uiso 1 1 calc R . . O1 O 0.4534(3) 0.56208(16) 0.74193(12) 0.0140(4) Uani 1 1 d . . . O2 O 0.3670(3) 0.37874(16) 0.79817(12) 0.0141(4) Uani 1 1 d . . . O3 O 0.0874(3) 0.49542(16) 1.18342(12) 0.0154(4) Uani 1 1 d . . . O4 O 0.1014(3) 0.69353(16) 1.14486(12) 0.0138(4) Uani 1 1 d . . . O5 O 0.6077(3) 0.95783(16) 0.70139(12) 0.0153(4) Uani 1 1 d . . . O6 O 0.6129(2) 1.15520(16) 0.70677(12) 0.0118(3) Uani 1 1 d . . . O7 O 0.1031(3) 1.15480(16) 1.08166(12) 0.0147(4) Uani 1 1 d . . . O8 O 0.1097(3) 0.95439(16) 1.10507(12) 0.0132(4) Uani 1 1 d . . . O9 O 0.4395(2) 0.79214(17) 0.60641(12) 0.0134(4) Uani 1 1 d . . . O10 O 0.5421(3) 0.76923(17) 0.46283(12) 0.0132(4) Uani 1 1 d . . . O11 O 1.3258(3) 0.56026(17) 0.46779(12) 0.0143(4) Uani 1 1 d . . . O12 O 1.2590(3) 0.48495(16) 0.61121(12) 0.0132(4) Uani 1 1 d . . . O13 O 0.1559(3) 0.84166(18) 0.75787(12) 0.0176(4) Uani 1 1 d . . . H13A H 0.1436 0.8931 0.7131 0.021 Uiso 1 1 d R . . H13B H 0.0854 0.8380 0.8111 0.021 Uiso 1 1 d R . . O14 O 0.7206(3) 0.71505(17) 0.83360(12) 0.0156(4) Uani 1 1 d . . . H14A H 0.7749 0.6429 0.8343 0.019 Uiso 1 1 d R . . H14B H 0.7431 0.7729 0.8610 0.019 Uiso 1 1 d R . . O15 O 0.2232(3) 0.63370(17) 0.30582(12) 0.0145(4) Uani 1 1 d . . . H15A H 0.2075 0.6784 0.2585 0.017 Uiso 1 1 d R . . H15B H 0.1905 0.5606 0.3227 0.017 Uiso 1 1 d R . . O16 O 0.7989(3) 0.76817(17) 0.29239(12) 0.0151(4) Uani 1 1 d . . . H16A H 0.8251 0.8279 0.3171 0.018 Uiso 1 1 d R . . H16B H 0.8580 0.7450 0.2417 0.018 Uiso 1 1 d R . . O17 O 0.2423(3) 0.9776(2) 0.48289(15) 0.0318(5) Uani 1 1 d . . . H17A H 0.2792 1.0156 0.4308 0.038 Uiso 1 1 d R . . H17B H 0.2874 0.9089 0.5040 0.038 Uiso 1 1 d R . . O18 O 0.9333(3) 0.95541(19) 0.35648(14) 0.0222(4) Uani 1 1 d . . . H18A H 0.8691 0.9635 0.4098 0.027 Uiso 1 1 d R . . H18B H 1.0555 0.9413 0.3395 0.027 Uiso 1 1 d 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 Tb2 0.00974(6) 0.00788(6) 0.00585(6) -0.00081(4) -0.00026(4) 0.00130(4) Tb1 0.01105(6) 0.00668(6) 0.00634(6) -0.00179(4) 0.00056(4) 0.00093(4) Cu1 0.01610(15) 0.00679(15) 0.00738(13) -0.00244(11) 0.00215(11) -0.00035(11) C1 0.0126(11) 0.0130(13) 0.0094(11) -0.0035(10) -0.0002(9) 0.0002(9) C2 0.0130(11) 0.0082(12) 0.0093(11) -0.0020(9) -0.0002(9) 0.0008(9) C3 0.0151(11) 0.0088(12) 0.0115(11) -0.0018(9) -0.0023(9) 0.0002(9) C4 0.0126(11) 0.0092(12) 0.0088(11) -0.0016(9) -0.0008(9) 0.0003(9) C5 0.0109(11) 0.0122(12) 0.0091(11) -0.0027(9) -0.0006(9) 0.0008(9) C6 0.0116(11) 0.0083(12) 0.0116(11) -0.0002(9) -0.0028(9) 0.0011(9) C7 0.0124(11) 0.0067(11) 0.0115(11) -0.0005(9) -0.0022(9) 0.0016(9) C8 0.0126(11) 0.0078(12) 0.0111(11) -0.0026(9) -0.0005(9) 0.0019(9) C9 0.0125(11) 0.0077(12) 0.0110(11) -0.0019(9) -0.0029(9) 0.0008(9) C10 0.0092(11) 0.0129(12) 0.0122(11) -0.0055(10) -0.0031(9) 0.0010(9) C11 0.0134(11) 0.0060(11) 0.0100(11) -0.0019(9) -0.0029(9) 0.0012(9) C12 0.0124(11) 0.0081(12) 0.0090(11) -0.0024(9) -0.0006(9) 0.0015(9) C13 0.0132(11) 0.0088(12) 0.0074(10) 0.0001(9) 0.0000(9) 0.0003(9) C14 0.0108(11) 0.0101(12) 0.0089(11) -0.0013(9) 0.0016(9) 0.0001(9) C15 0.0087(10) 0.0093(12) 0.0121(11) -0.0021(9) -0.0016(9) 0.0006(9) N1 0.0164(10) 0.0093(11) 0.0089(10) -0.0032(8) 0.0002(8) 0.0003(8) N2 0.0169(10) 0.0092(10) 0.0076(9) -0.0017(8) 0.0024(8) -0.0011(8) N3 0.0138(10) 0.0100(11) 0.0091(10) -0.0014(8) 0.0019(8) 0.0005(8) N4 0.0132(10) 0.0099(10) 0.0087(9) -0.0035(8) 0.0010(8) 0.0006(8) N5 0.0101(9) 0.0130(11) 0.0116(10) -0.0029(8) -0.0020(8) 0.0035(8) N6 0.0096(9) 0.0177(12) 0.0091(10) -0.0022(8) -0.0019(8) 0.0031(8) O1 0.0210(9) 0.0094(9) 0.0102(8) -0.0028(7) 0.0012(7) -0.0018(7) O2 0.0218(9) 0.0083(9) 0.0113(8) -0.0043(7) -0.0002(7) -0.0004(7) O3 0.0240(10) 0.0089(9) 0.0098(8) 0.0007(7) 0.0016(7) 0.0023(7) O4 0.0216(9) 0.0090(9) 0.0087(8) -0.0030(7) 0.0017(7) 0.0000(7) O5 0.0224(10) 0.0094(9) 0.0113(9) -0.0029(7) 0.0035(7) -0.0014(7) O6 0.0143(8) 0.0082(9) 0.0113(8) 0.0017(7) -0.0015(7) 0.0004(7) O7 0.0154(9) 0.0111(9) 0.0172(9) -0.0078(7) 0.0003(7) 0.0010(7) O8 0.0171(9) 0.0105(9) 0.0103(8) -0.0041(7) 0.0025(7) -0.0011(7) O9 0.0117(8) 0.0164(10) 0.0106(8) -0.0037(7) 0.0000(7) 0.0039(7) O10 0.0160(9) 0.0141(9) 0.0096(8) -0.0026(7) -0.0040(7) 0.0036(7) O11 0.0126(8) 0.0179(10) 0.0100(8) 0.0005(7) 0.0009(7) 0.0006(7) O12 0.0135(8) 0.0115(9) 0.0124(8) 0.0008(7) -0.0007(7) 0.0026(7) O13 0.0140(9) 0.0241(11) 0.0114(9) -0.0017(8) 0.0017(7) 0.0044(8) O14 0.0208(9) 0.0115(9) 0.0164(9) -0.0060(7) -0.0077(8) 0.0034(7) O15 0.0184(9) 0.0122(9) 0.0142(9) 0.0016(7) -0.0067(7) -0.0035(7) O16 0.0141(9) 0.0181(10) 0.0125(9) -0.0072(8) 0.0022(7) -0.0026(7) O17 0.0387(13) 0.0269(12) 0.0212(11) 0.0035(9) 0.0006(10) 0.0172(10) O18 0.0192(10) 0.0290(12) 0.0186(10) -0.0035(9) -0.0028(8) -0.0036(9) _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 Tb2 O11 2.2791(18) 1_455 ? Tb2 O10 2.3033(17) . ? Tb2 O12 2.3150(18) 2_766 ? Tb2 O6 2.3187(18) 2_676 ? Tb2 O2 2.3442(17) 2_666 ? Tb2 O16 2.3927(18) . ? Tb2 O15 2.4028(18) . ? Tb2 C1 3.029(2) 2_666 ? Tb1 O14 2.3269(18) . ? Tb1 O13 2.3591(18) . ? Tb1 O9 2.3763(18) . ? Tb1 O5 2.3772(19) . ? Tb1 O1 2.3899(18) . ? Tb1 N3 2.496(2) . ? Tb1 N1 2.507(2) . ? Tb1 N5 2.540(2) . ? Cu1 N4 1.905(2) . ? Cu1 N2 1.907(2) . ? Cu1 O8 1.9496(17) . ? Cu1 O4 1.9706(18) . ? C1 O2 1.256(3) . ? C1 O1 1.270(3) . ? C1 C2 1.478(3) . ? C1 Tb2 3.029(2) 2_666 ? C2 N1 1.353(3) . ? C2 C3 1.391(3) . ? C3 C4 1.398(3) . ? C3 H3 0.9500 . ? C4 N2 1.346(3) . ? C4 C5 1.476(3) . ? C5 O3 1.242(3) . ? C5 O4 1.298(3) . ? C6 O6 1.255(3) . ? C6 O5 1.276(3) . ? C6 C7 1.478(3) . ? C7 N3 1.356(3) . ? C7 C8 1.399(3) . ? C8 C9 1.384(3) . ? C8 H8 0.9500 . ? C9 N4 1.346(3) . ? C9 C10 1.486(3) . ? C10 O7 1.253(3) . ? C10 O8 1.280(3) . ? C11 O10 1.256(3) . ? C11 O9 1.259(3) . ? C11 C12 1.487(3) . ? C12 N5 1.337(3) . ? C12 C13 1.398(3) . ? C13 C14 1.372(3) . ? C13 H13 0.9500 . ? C14 N6 1.360(3) . ? C14 C15 1.483(3) . ? C15 O11 1.256(3) . ? C15 O12 1.257(3) . ? N1 N2 1.327(3) . ? N3 N4 1.337(3) . ? N5 N6 1.340(3) . ? N6 H6N 0.8800 . ? O2 Tb2 2.3442(17) 2_666 ? O6 Tb2 2.3187(18) 2_676 ? O11 Tb2 2.2791(18) 1_655 ? O12 Tb2 2.3150(18) 2_766 ? O13 H13A 0.8602 . ? O13 H13B 0.8658 . ? O14 H14A 0.8643 . ? O14 H14B 0.8650 . ? O15 H15A 0.8584 . ? O15 H15B 0.8668 . ? O16 H16A 0.8673 . ? O16 H16B 0.8652 . ? O17 H17A 0.8631 . ? O17 H17B 0.8606 . ? O18 H18A 0.8648 . ? O18 H18B 0.8622 . ? 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 O11 Tb2 O10 79.05(7) 1_455 . ? O11 Tb2 O12 80.85(6) 1_455 2_766 ? O10 Tb2 O12 90.80(6) . 2_766 ? O11 Tb2 O6 116.52(6) 1_455 2_676 ? O10 Tb2 O6 83.25(6) . 2_676 ? O12 Tb2 O6 159.89(6) 2_766 2_676 ? O11 Tb2 O2 132.50(7) 1_455 2_666 ? O10 Tb2 O2 147.40(7) . 2_666 ? O12 Tb2 O2 87.49(6) 2_766 2_666 ? O6 Tb2 O2 87.30(6) 2_676 2_666 ? O11 Tb2 O16 148.22(6) 1_455 . ? O10 Tb2 O16 75.31(6) . . ? O12 Tb2 O16 81.05(6) 2_766 . ? O6 Tb2 O16 78.86(6) 2_676 . ? O2 Tb2 O16 72.26(6) 2_666 . ? O11 Tb2 O15 72.72(6) 1_455 . ? O10 Tb2 O15 125.65(6) . . ? O12 Tb2 O15 127.76(6) 2_766 . ? O6 Tb2 O15 70.03(6) 2_676 . ? O2 Tb2 O15 79.11(6) 2_666 . ? O16 Tb2 O15 138.34(6) . . ? O11 Tb2 C1 110.44(7) 1_455 2_666 ? O10 Tb2 C1 161.77(7) . 2_666 ? O12 Tb2 C1 75.95(7) 2_766 2_666 ? O6 Tb2 C1 104.89(7) 2_676 2_666 ? O2 Tb2 C1 22.80(7) 2_666 2_666 ? O16 Tb2 C1 90.08(6) . 2_666 ? O15 Tb2 C1 72.56(6) . 2_666 ? O14 Tb1 O13 148.81(6) . . ? O14 Tb1 O9 137.88(6) . . ? O13 Tb1 O9 73.19(6) . . ? O14 Tb1 O5 90.65(7) . . ? O13 Tb1 O5 95.17(7) . . ? O9 Tb1 O5 78.18(6) . . ? O14 Tb1 O1 89.78(7) . . ? O13 Tb1 O1 99.50(7) . . ? O9 Tb1 O1 81.97(6) . . ? O5 Tb1 O1 150.69(6) . . ? O14 Tb1 N3 77.79(7) . . ? O13 Tb1 N3 76.97(7) . . ? O9 Tb1 N3 129.80(7) . . ? O5 Tb1 N3 65.31(7) . . ? O1 Tb1 N3 142.90(7) . . ? O14 Tb1 N1 76.48(7) . . ? O13 Tb1 N1 80.28(7) . . ? O9 Tb1 N1 133.98(7) . . ? O5 Tb1 N1 142.12(6) . . ? O1 Tb1 N1 65.97(6) . . ? N3 Tb1 N1 77.11(7) . . ? O14 Tb1 N5 72.94(7) . . ? O13 Tb1 N5 138.25(7) . . ? O9 Tb1 N5 65.15(6) . . ? O5 Tb1 N5 79.47(7) . . ? O1 Tb1 N5 72.66(7) . . ? N3 Tb1 N5 133.41(7) . . ? N1 Tb1 N5 127.84(7) . . ? N4 Cu1 N2 97.92(9) . . ? N4 Cu1 O8 83.77(8) . . ? N2 Cu1 O8 174.38(9) . . ? N4 Cu1 O4 172.30(9) . . ? N2 Cu1 O4 82.83(8) . . ? O8 Cu1 O4 96.22(7) . . ? O2 C1 O1 123.1(2) . . ? O2 C1 C2 119.4(2) . . ? O1 C1 C2 117.5(2) . . ? O2 C1 Tb2 46.32(12) . 2_666 ? O1 C1 Tb2 76.76(13) . 2_666 ? C2 C1 Tb2 165.69(18) . 2_666 ? N1 C2 C3 111.4(2) . . ? N1 C2 C1 116.3(2) . . ? C3 C2 C1 132.3(2) . . ? C2 C3 C4 102.8(2) . . ? C2 C3 H3 128.6 . . ? C4 C3 H3 128.6 . . ? N2 C4 C3 109.0(2) . . ? N2 C4 C5 114.2(2) . . ? C3 C4 C5 136.8(2) . . ? O3 C5 O4 123.2(2) . . ? O3 C5 C4 122.4(2) . . ? O4 C5 C4 114.4(2) . . ? O6 C6 O5 123.6(2) . . ? O6 C6 C7 120.5(2) . . ? O5 C6 C7 115.9(2) . . ? N3 C7 C8 110.9(2) . . ? N3 C7 C6 116.1(2) . . ? C8 C7 C6 133.0(2) . . ? C9 C8 C7 103.0(2) . . ? C9 C8 H8 128.5 . . ? C7 C8 H8 128.5 . . ? N4 C9 C8 109.8(2) . . ? N4 C9 C10 113.0(2) . . ? C8 C9 C10 137.1(2) . . ? O7 C10 O8 123.4(2) . . ? O7 C10 C9 120.7(2) . . ? O8 C10 C9 115.8(2) . . ? O10 C11 O9 124.5(2) . . ? O10 C11 C12 118.7(2) . . ? O9 C11 C12 116.8(2) . . ? N5 C12 C13 111.6(2) . . ? N5 C12 C11 116.3(2) . . ? C13 C12 C11 131.8(2) . . ? C14 C13 C12 104.4(2) . . ? C14 C13 H13 127.8 . . ? C12 C13 H13 127.8 . . ? N6 C14 C13 107.2(2) . . ? N6 C14 C15 120.8(2) . . ? C13 C14 C15 131.2(2) . . ? O11 C15 O12 126.4(2) . . ? O11 C15 C14 117.4(2) . . ? O12 C15 C14 116.1(2) . . ? N2 N1 C2 106.3(2) . . ? N2 N1 Tb1 136.33(17) . . ? C2 N1 Tb1 116.36(15) . . ? N1 N2 C4 110.5(2) . . ? N1 N2 Cu1 135.08(18) . . ? C4 N2 Cu1 114.41(16) . . ? N4 N3 C7 106.5(2) . . ? N4 N3 Tb1 134.96(16) . . ? C7 N3 Tb1 116.46(16) . . ? N3 N4 C9 109.8(2) . . ? N3 N4 Cu1 136.38(17) . . ? C9 N4 Cu1 113.80(16) . . ? C12 N5 N6 105.0(2) . . ? C12 N5 Tb1 116.38(15) . . ? N6 N5 Tb1 138.51(16) . . ? N5 N6 C14 111.7(2) . . ? N5 N6 H6N 124.2 . . ? C14 N6 H6N 124.2 . . ? C1 O1 Tb1 123.30(15) . . ? C1 O2 Tb2 110.89(16) . 2_666 ? C5 O4 Cu1 114.06(15) . . ? C6 O5 Tb1 124.05(16) . . ? C6 O6 Tb2 140.92(16) . 2_676 ? C10 O8 Cu1 113.34(15) . . ? C11 O9 Tb1 125.12(16) . . ? C11 O10 Tb2 146.27(17) . . ? C15 O11 Tb2 151.16(17) . 1_655 ? C15 O12 Tb2 140.93(16) . 2_766 ? Tb1 O13 H13A 113.3 . . ? Tb1 O13 H13B 112.5 . . ? H13A O13 H13B 127.7 . . ? Tb1 O14 H14A 120.3 . . ? Tb1 O14 H14B 112.4 . . ? H14A O14 H14B 127.2 . . ? Tb2 O15 H15A 113.5 . . ? Tb2 O15 H15B 110.2 . . ? H15A O15 H15B 127.8 . . ? Tb2 O16 H16A 122.4 . . ? Tb2 O16 H16B 110.3 . . ? H16A O16 H16B 126.8 . . ? H17A O17 H17B 128.0 . . ? H18A O18 H18B 127.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 N1 -173.1(2) . . . . ? O1 C1 C2 N1 6.6(3) . . . . ? Tb2 C1 C2 N1 -169.2(6) 2_666 . . . ? O2 C1 C2 C3 7.8(4) . . . . ? O1 C1 C2 C3 -172.5(3) . . . . ? Tb2 C1 C2 C3 11.6(9) 2_666 . . . ? N1 C2 C3 C4 0.3(3) . . . . ? C1 C2 C3 C4 179.5(3) . . . . ? C2 C3 C4 N2 -0.4(3) . . . . ? C2 C3 C4 C5 178.0(3) . . . . ? N2 C4 C5 O3 -176.1(2) . . . . ? C3 C4 C5 O3 5.6(5) . . . . ? N2 C4 C5 O4 2.7(3) . . . . ? C3 C4 C5 O4 -175.6(3) . . . . ? O6 C6 C7 N3 -177.5(2) . . . . ? O5 C6 C7 N3 1.6(3) . . . . ? O6 C6 C7 C8 4.9(4) . . . . ? O5 C6 C7 C8 -176.0(3) . . . . ? N3 C7 C8 C9 0.0(3) . . . . ? C6 C7 C8 C9 177.7(3) . . . . ? C7 C8 C9 N4 0.2(3) . . . . ? C7 C8 C9 C10 -176.0(3) . . . . ? N4 C9 C10 O7 -172.5(2) . . . . ? C8 C9 C10 O7 3.6(4) . . . . ? N4 C9 C10 O8 5.2(3) . . . . ? C8 C9 C10 O8 -178.7(3) . . . . ? O10 C11 C12 N5 -172.5(2) . . . . ? O9 C11 C12 N5 5.9(3) . . . . ? O10 C11 C12 C13 -0.2(4) . . . . ? O9 C11 C12 C13 178.2(3) . . . . ? N5 C12 C13 C14 2.6(3) . . . . ? C11 C12 C13 C14 -170.0(3) . . . . ? C12 C13 C14 N6 -1.9(3) . . . . ? C12 C13 C14 C15 167.9(3) . . . . ? N6 C14 C15 O11 -167.3(2) . . . . ? C13 C14 C15 O11 24.0(4) . . . . ? N6 C14 C15 O12 17.0(4) . . . . ? C13 C14 C15 O12 -151.6(3) . . . . ? C3 C2 N1 N2 -0.1(3) . . . . ? C1 C2 N1 N2 -179.4(2) . . . . ? C3 C2 N1 Tb1 170.54(16) . . . . ? C1 C2 N1 Tb1 -8.8(3) . . . . ? O14 Tb1 N1 N2 77.1(2) . . . . ? O13 Tb1 N1 N2 -82.0(2) . . . . ? O9 Tb1 N1 N2 -137.0(2) . . . . ? O5 Tb1 N1 N2 3.9(3) . . . . ? O1 Tb1 N1 N2 173.0(3) . . . . ? N3 Tb1 N1 N2 -3.3(2) . . . . ? N5 Tb1 N1 N2 132.4(2) . . . . ? O14 Tb1 N1 C2 -89.84(18) . . . . ? O13 Tb1 N1 C2 111.11(18) . . . . ? O9 Tb1 N1 C2 56.1(2) . . . . ? O5 Tb1 N1 C2 -162.97(16) . . . . ? O1 Tb1 N1 C2 6.06(17) . . . . ? N3 Tb1 N1 C2 -170.16(19) . . . . ? N5 Tb1 N1 C2 -34.5(2) . . . . ? C2 N1 N2 C4 -0.2(3) . . . . ? Tb1 N1 N2 C4 -167.95(18) . . . . ? C2 N1 N2 Cu1 -177.3(2) . . . . ? Tb1 N1 N2 Cu1 15.0(4) . . . . ? C3 C4 N2 N1 0.3(3) . . . . ? C5 C4 N2 N1 -178.4(2) . . . . ? C3 C4 N2 Cu1 178.09(17) . . . . ? C5 C4 N2 Cu1 -0.7(3) . . . . ? N4 Cu1 N2 N1 -11.6(3) . . . . ? O4 Cu1 N2 N1 176.2(3) . . . . ? N4 Cu1 N2 C4 171.41(18) . . . . ? O4 Cu1 N2 C4 -0.86(18) . . . . ? C8 C7 N3 N4 -0.2(3) . . . . ? C6 C7 N3 N4 -178.3(2) . . . . ? C8 C7 N3 Tb1 165.82(16) . . . . ? C6 C7 N3 Tb1 -12.3(3) . . . . ? O14 Tb1 N3 N4 -90.2(2) . . . . ? O13 Tb1 N3 N4 71.3(2) . . . . ? O9 Tb1 N3 N4 125.9(2) . . . . ? O5 Tb1 N3 N4 173.3(3) . . . . ? O1 Tb1 N3 N4 -17.2(3) . . . . ? N1 Tb1 N3 N4 -11.5(2) . . . . ? N5 Tb1 N3 N4 -142.0(2) . . . . ? O14 Tb1 N3 C7 108.88(18) . . . . ? O13 Tb1 N3 C7 -89.58(18) . . . . ? O9 Tb1 N3 C7 -35.0(2) . . . . ? O5 Tb1 N3 C7 12.44(16) . . . . ? O1 Tb1 N3 C7 -178.14(15) . . . . ? N1 Tb1 N3 C7 -172.41(19) . . . . ? N5 Tb1 N3 C7 57.1(2) . . . . ? C7 N3 N4 C9 0.3(3) . . . . ? Tb1 N3 N4 C9 -161.88(18) . . . . ? C7 N3 N4 Cu1 179.0(2) . . . . ? Tb1 N3 N4 Cu1 16.8(4) . . . . ? C8 C9 N4 N3 -0.3(3) . . . . ? C10 C9 N4 N3 176.8(2) . . . . ? C8 C9 N4 Cu1 -179.35(17) . . . . ? C10 C9 N4 Cu1 -2.2(3) . . . . ? N2 Cu1 N4 N3 -4.5(3) . . . . ? O8 Cu1 N4 N3 -179.1(3) . . . . ? N2 Cu1 N4 C9 174.15(18) . . . . ? O8 Cu1 N4 C9 -0.45(17) . . . . ? C13 C12 N5 N6 -2.1(3) . . . . ? C11 C12 N5 N6 171.8(2) . . . . ? C13 C12 N5 Tb1 -179.45(16) . . . . ? C11 C12 N5 Tb1 -5.6(3) . . . . ? O14 Tb1 N5 C12 -172.7(2) . . . . ? O13 Tb1 N5 C12 7.2(2) . . . . ? O9 Tb1 N5 C12 3.00(17) . . . . ? O5 Tb1 N5 C12 -78.75(18) . . . . ? O1 Tb1 N5 C12 92.04(19) . . . . ? N3 Tb1 N5 C12 -119.22(18) . . . . ? N1 Tb1 N5 C12 130.54(18) . . . . ? O14 Tb1 N5 N6 11.2(2) . . . . ? O13 Tb1 N5 N6 -168.9(2) . . . . ? O9 Tb1 N5 N6 -173.1(3) . . . . ? O5 Tb1 N5 N6 105.1(3) . . . . ? O1 Tb1 N5 N6 -84.1(3) . . . . ? N3 Tb1 N5 N6 64.6(3) . . . . ? N1 Tb1 N5 N6 -45.6(3) . . . . ? C12 N5 N6 C14 0.8(3) . . . . ? Tb1 N5 N6 C14 177.22(19) . . . . ? C13 C14 N6 N5 0.8(3) . . . . ? C15 C14 N6 N5 -170.3(2) . . . . ? O2 C1 O1 Tb1 178.90(18) . . . . ? C2 C1 O1 Tb1 -0.8(3) . . . . ? Tb2 C1 O1 Tb1 178.16(14) 2_666 . . . ? O14 Tb1 O1 C1 72.59(19) . . . . ? O13 Tb1 O1 C1 -77.5(2) . . . . ? O9 Tb1 O1 C1 -148.9(2) . . . . ? O5 Tb1 O1 C1 163.50(17) . . . . ? N3 Tb1 O1 C1 3.4(2) . . . . ? N1 Tb1 O1 C1 -2.68(18) . . . . ? N5 Tb1 O1 C1 144.8(2) . . . . ? O1 C1 O2 Tb2 -1.0(3) . . . 2_666 ? C2 C1 O2 Tb2 178.69(18) . . . 2_666 ? O3 C5 O4 Cu1 175.5(2) . . . . ? C4 C5 O4 Cu1 -3.4(3) . . . . ? N2 Cu1 O4 C5 2.44(18) . . . . ? O8 Cu1 O4 C5 176.87(17) . . . . ? O6 C6 O5 Tb1 -169.62(17) . . . . ? C7 C6 O5 Tb1 11.3(3) . . . . ? O14 Tb1 O5 C6 -89.1(2) . . . . ? O13 Tb1 O5 C6 60.3(2) . . . . ? O9 Tb1 O5 C6 131.9(2) . . . . ? O1 Tb1 O5 C6 -179.76(17) . . . . ? N3 Tb1 O5 C6 -12.84(18) . . . . ? N1 Tb1 O5 C6 -20.6(3) . . . . ? N5 Tb1 O5 C6 -161.6(2) . . . . ? O5 C6 O6 Tb2 107.9(3) . . . 2_676 ? C7 C6 O6 Tb2 -73.1(3) . . . 2_676 ? O7 C10 O8 Cu1 172.08(19) . . . . ? C9 C10 O8 Cu1 -5.5(3) . . . . ? N4 Cu1 O8 C10 3.44(17) . . . . ? O4 Cu1 O8 C10 175.69(17) . . . . ? O10 C11 O9 Tb1 175.09(18) . . . . ? C12 C11 O9 Tb1 -3.2(3) . . . . ? O14 Tb1 O9 C11 6.4(2) . . . . ? O13 Tb1 O9 C11 -176.8(2) . . . . ? O5 Tb1 O9 C11 84.1(2) . . . . ? O1 Tb1 O9 C11 -74.3(2) . . . . ? N3 Tb1 O9 C11 127.17(19) . . . . ? N1 Tb1 O9 C11 -119.2(2) . . . . ? N5 Tb1 O9 C11 0.30(19) . . . . ? O9 C11 O10 Tb2 -109.4(3) . . . . ? C12 C11 O10 Tb2 68.9(4) . . . . ? O11 Tb2 O10 C11 45.2(3) 1_455 . . . ? O12 Tb2 O10 C11 -35.3(3) 2_766 . . . ? O6 Tb2 O10 C11 164.0(3) 2_676 . . . ? O2 Tb2 O10 C11 -121.9(3) 2_666 . . . ? O16 Tb2 O10 C11 -115.8(3) . . . . ? O15 Tb2 O10 C11 104.5(3) . . . . ? C1 Tb2 O10 C11 -78.1(4) 2_666 . . . ? O12 C15 O11 Tb2 -116.2(3) . . . 1_655 ? C14 C15 O11 Tb2 68.7(4) . . . 1_655 ? O11 C15 O12 Tb2 2.7(4) . . . 2_766 ? C14 C15 O12 Tb2 177.91(17) . . . 2_766 ? 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 O17 H17B O9 0.86 2.32 3.104(3) 150.8 . O17 H17B O10 0.86 2.32 3.019(3) 138.2 . O16 H16A O18 0.87 1.91 2.769(3) 168.4 . N6 H6N O3 0.88 2.21 2.915(3) 137.3 2_667 O14 H14A O3 0.86 1.78 2.630(3) 169.4 2_667 O15 H15A O4 0.86 2.05 2.807(3) 146.5 1_554 O13 H13A O18 0.86 2.00 2.819(3) 160.1 2_676 O17 H17A O5 0.86 2.03 2.850(3) 159.0 2_676 O18 H18A O17 0.86 1.85 2.696(3) 164.2 2_676 O18 H18B O6 0.86 2.51 3.349(3) 165.0 2_776 O13 H13B O7 0.87 1.90 2.760(3) 170.0 2_577 O14 H14B O7 0.86 1.86 2.651(3) 151.7 2_677 O15 H15B N6 0.87 2.57 3.424(3) 170.6 2_666 O16 H16B O4 0.87 2.12 2.930(2) 155.2 1_654 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.732 _refine_diff_density_min -0.977 _refine_diff_density_rms 0.118 _database_code_depnum_ccdc_archive 'CCDC 931526' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H12 Cu Dy2 N6 O16, 2(H2 O)' _chemical_formula_sum 'C15 H16 Cu Dy2 N6 O18' _chemical_formula_weight 956.88 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1518(3) _cell_length_b 11.2144(5) _cell_length_c 15.4635(7) _cell_angle_alpha 82.6950(10) _cell_angle_beta 77.369(2) _cell_angle_gamma 84.6290(10) _cell_volume 1197.61(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9887 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 30.60 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 906 _exptl_absorpt_coefficient_mu 7.158 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2391 _exptl_absorpt_correction_T_max 0.6342 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19770 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_unetI/netI 0.0227 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4666 _reflns_number_gt 4536 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+2.8225P] 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 4666 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0205 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0559 _refine_ls_wR_factor_gt 0.0554 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 Dy2 Dy 0.51564(2) 0.662135(13) 0.350288(10) 0.00813(6) Uani 1 1 d . . . Dy1 Dy 0.47948(2) 0.770669(13) 0.756262(10) 0.00837(6) Uani 1 1 d . . . Cu1 Cu 0.19373(6) 0.81215(3) 1.04263(3) 0.01060(9) Uani 1 1 d . . . C1 C 0.3826(5) 0.4899(3) 0.8047(2) 0.0110(7) Uani 1 1 d . . . C2 C 0.3137(5) 0.5331(3) 0.8933(2) 0.0101(6) Uani 1 1 d . . . C3 C 0.2459(5) 0.4745(3) 0.9774(2) 0.0119(7) Uani 1 1 d . . . H3 H 0.2308 0.3909 0.9942 0.014 Uiso 1 1 calc R . . C4 C 0.2053(5) 0.5684(3) 1.0313(2) 0.0107(7) Uani 1 1 d . . . C5 C 0.1257(5) 0.5823(3) 1.1258(2) 0.0114(7) Uani 1 1 d . . . C6 C 0.5665(5) 1.0529(3) 0.7409(2) 0.0103(6) Uani 1 1 d . . . C7 C 0.4553(5) 1.0360(3) 0.8334(2) 0.0104(6) Uani 1 1 d . . . C8 C 0.3726(5) 1.1155(3) 0.8955(2) 0.0114(7) Uani 1 1 d . . . H8 H 0.3759 1.2007 0.8897 0.014 Uiso 1 1 calc R . . C9 C 0.2843(4) 1.0401(3) 0.9678(2) 0.0091(6) Uani 1 1 d . . . C10 C 0.1584(5) 1.0533(3) 1.0568(2) 0.0100(6) Uani 1 1 d . . . C11 C 0.5676(5) 0.7652(3) 0.5412(2) 0.0097(6) Uani 1 1 d . . . C12 C 0.7597(5) 0.7207(3) 0.5591(2) 0.0101(6) Uani 1 1 d . . . C13 C 0.9282(5) 0.6785(3) 0.5037(2) 0.0112(7) Uani 1 1 d . . . H13 H 0.9560 0.6817 0.4405 0.013 Uiso 1 1 calc R . . C14 C 1.0434(5) 0.6318(3) 0.5610(2) 0.0108(7) Uani 1 1 d . . . C15 C 1.2274(4) 0.5544(3) 0.5456(2) 0.0091(6) Uani 1 1 d . . . N1 N 0.3158(4) 0.6530(3) 0.89586(19) 0.0117(6) Uani 1 1 d . . . N2 N 0.2500(4) 0.6731(3) 0.98006(19) 0.0124(6) Uani 1 1 d . . . N3 N 0.4181(4) 0.9201(3) 0.86645(19) 0.0114(6) Uani 1 1 d . . . N4 N 0.3129(4) 0.9247(3) 0.94860(19) 0.0114(6) Uani 1 1 d . . . N5 N 0.7739(4) 0.7052(3) 0.64437(19) 0.0116(6) Uani 1 1 d . . . N6 N 0.9474(4) 0.6494(3) 0.6445(2) 0.0122(6) Uani 1 1 d . . . H6N H 0.9934 0.6269 0.6928 0.015 Uiso 1 1 calc R . . O1 O 0.4554(3) 0.5651(2) 0.74135(16) 0.0137(5) Uani 1 1 d . . . O2 O 0.3675(3) 0.3811(2) 0.79579(16) 0.0140(5) Uani 1 1 d . . . O3 O 0.0875(4) 0.4948(2) 1.18311(17) 0.0154(5) Uani 1 1 d . . . O4 O 0.1025(4) 0.6928(2) 1.14508(16) 0.0131(5) Uani 1 1 d . . . O5 O 0.6108(4) 0.9581(2) 0.70060(17) 0.0153(5) Uani 1 1 d . . . O6 O 0.6143(3) 1.1557(2) 0.70526(16) 0.0124(5) Uani 1 1 d . . . O7 O 0.1005(3) 1.1553(2) 1.08060(17) 0.0143(5) Uani 1 1 d . . . O8 O 0.1100(3) 0.9546(2) 1.10446(16) 0.0136(5) Uani 1 1 d . . . O9 O 0.4407(3) 0.7933(2) 0.60672(16) 0.0135(5) Uani 1 1 d . . . O10 O 0.5415(3) 0.7694(2) 0.46296(16) 0.0132(5) Uani 1 1 d . . . O11 O 1.3270(3) 0.5606(2) 0.46822(16) 0.0139(5) Uani 1 1 d . . . O12 O 1.2602(3) 0.4851(2) 0.61190(16) 0.0132(5) Uani 1 1 d . . . O13 O 0.1591(3) 0.8412(2) 0.75863(17) 0.0169(5) Uani 1 1 d . . . H13A H 0.1469 0.8927 0.7139 0.020 Uiso 1 1 d R . . H13B H 0.0886 0.8376 0.8118 0.020 Uiso 1 1 d R . . O14 O 0.7230(3) 0.7164(2) 0.83370(17) 0.0150(5) Uani 1 1 d . . . H14A H 0.7773 0.6442 0.8344 0.018 Uiso 1 1 d R . . H14B H 0.7456 0.7742 0.8611 0.018 Uiso 1 1 d R . . O15 O 0.2242(3) 0.6323(2) 0.30674(17) 0.0144(5) Uani 1 1 d . . . H15A H 0.2086 0.6770 0.2594 0.017 Uiso 1 1 d R . . H15B H 0.1916 0.5592 0.3236 0.017 Uiso 1 1 d R . . O16 O 0.7978(3) 0.7673(2) 0.29266(17) 0.0153(5) Uani 1 1 d . . . H16A H 0.8240 0.8270 0.3174 0.018 Uiso 1 1 d R . . H16B H 0.8569 0.7441 0.2420 0.018 Uiso 1 1 d R . . O17 O 0.2412(4) 0.9778(3) 0.4842(2) 0.0314(7) Uani 1 1 d . . . H17A H 0.2780 1.0158 0.4322 0.038 Uiso 1 1 d R . . H17B H 0.2862 0.9091 0.5053 0.038 Uiso 1 1 d R . . O18 O 0.9327(4) 0.9549(3) 0.35522(18) 0.0219(6) Uani 1 1 d . . . H18A H 0.8684 0.9631 0.4086 0.026 Uiso 1 1 d R . . H18B H 1.0548 0.9409 0.3382 0.026 Uiso 1 1 d 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 Dy2 0.01021(9) 0.00768(9) 0.00562(9) -0.00003(6) -0.00027(6) -0.00043(6) Dy1 0.01146(9) 0.00656(9) 0.00611(9) -0.00086(6) 0.00048(6) -0.00092(6) Cu1 0.0167(2) 0.00654(19) 0.0070(2) -0.00157(15) 0.00203(16) -0.00227(15) C1 0.0116(16) 0.0134(16) 0.0076(17) -0.0023(13) -0.0010(13) -0.0002(13) C2 0.0147(16) 0.0077(15) 0.0070(16) -0.0004(13) 0.0002(13) -0.0022(12) C3 0.0152(16) 0.0085(15) 0.0114(17) -0.0008(13) -0.0021(13) -0.0001(13) C4 0.0133(16) 0.0090(15) 0.0097(17) 0.0008(13) -0.0031(13) -0.0017(12) C5 0.0105(15) 0.0132(16) 0.0103(17) -0.0015(13) -0.0019(13) -0.0010(13) C6 0.0100(15) 0.0097(15) 0.0108(17) -0.0003(13) -0.0021(13) 0.0006(12) C7 0.0117(15) 0.0090(15) 0.0101(17) -0.0002(13) -0.0017(13) -0.0006(12) C8 0.0141(16) 0.0082(15) 0.0113(17) -0.0020(13) -0.0013(13) -0.0002(12) C9 0.0100(15) 0.0065(15) 0.0106(17) -0.0008(13) -0.0019(13) -0.0002(12) C10 0.0101(15) 0.0110(16) 0.0099(17) -0.0034(13) -0.0030(13) -0.0002(12) C11 0.0127(15) 0.0055(14) 0.0097(17) 0.0005(12) -0.0004(13) -0.0009(12) C12 0.0146(16) 0.0059(14) 0.0094(16) 0.0007(12) -0.0016(13) -0.0025(12) C13 0.0136(16) 0.0099(15) 0.0089(16) -0.0007(13) 0.0002(13) -0.0009(13) C14 0.0114(16) 0.0092(15) 0.0102(17) -0.0018(13) 0.0016(13) -0.0015(13) C15 0.0094(15) 0.0074(15) 0.0100(17) -0.0012(13) -0.0003(12) -0.0015(12) N1 0.0171(14) 0.0094(13) 0.0071(14) -0.0028(11) 0.0025(11) -0.0021(11) N2 0.0179(14) 0.0109(14) 0.0072(14) -0.0017(11) 0.0014(11) -0.0026(11) N3 0.0157(14) 0.0096(14) 0.0079(14) -0.0012(11) -0.0002(11) -0.0013(11) N4 0.0154(14) 0.0102(13) 0.0077(14) -0.0031(11) 0.0007(11) -0.0010(11) N5 0.0104(13) 0.0132(14) 0.0113(15) -0.0024(11) -0.0017(11) -0.0001(11) N6 0.0100(13) 0.0160(14) 0.0097(14) -0.0005(12) -0.0019(11) 0.0025(11) O1 0.0200(12) 0.0110(12) 0.0084(12) -0.0009(10) 0.0016(10) -0.0033(10) O2 0.0215(13) 0.0093(11) 0.0109(12) -0.0037(9) -0.0009(10) -0.0021(10) O3 0.0239(13) 0.0095(12) 0.0098(13) 0.0015(10) 0.0007(10) 0.0014(10) O4 0.0226(13) 0.0072(11) 0.0082(12) -0.0022(9) 0.0006(10) -0.0024(9) O5 0.0207(13) 0.0098(12) 0.0132(13) -0.0015(10) 0.0030(10) -0.0046(10) O6 0.0153(12) 0.0091(11) 0.0111(12) 0.0015(9) -0.0003(9) -0.0016(9) O7 0.0153(12) 0.0109(12) 0.0157(13) -0.0061(10) 0.0020(10) -0.0015(10) O8 0.0173(12) 0.0115(11) 0.0104(12) -0.0032(10) 0.0021(10) -0.0022(10) O9 0.0119(11) 0.0162(12) 0.0110(12) -0.0030(10) 0.0000(9) 0.0023(9) O10 0.0166(12) 0.0140(12) 0.0091(12) -0.0020(9) -0.0036(10) 0.0021(10) O11 0.0133(12) 0.0177(12) 0.0074(12) 0.0023(10) 0.0028(9) -0.0005(10) O12 0.0137(12) 0.0122(12) 0.0111(12) 0.0026(10) -0.0002(10) 0.0009(9) O13 0.0151(12) 0.0223(13) 0.0105(13) 0.0000(10) 0.0009(10) 0.0020(10) O14 0.0202(12) 0.0089(11) 0.0178(13) -0.0044(10) -0.0078(10) 0.0014(10) O15 0.0186(12) 0.0122(11) 0.0133(13) 0.0023(10) -0.0055(10) -0.0054(10) O16 0.0148(12) 0.0173(12) 0.0127(13) -0.0043(10) 0.0025(10) -0.0053(10) O17 0.0384(17) 0.0271(15) 0.0205(16) 0.0055(13) -0.0005(13) 0.0155(13) O18 0.0194(13) 0.0294(15) 0.0166(14) -0.0023(12) -0.0017(11) -0.0057(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy2 O11 2.264(2) 1_455 ? Dy2 O10 2.288(2) . ? Dy2 O12 2.304(2) 2_766 ? Dy2 O6 2.307(2) 2_676 ? Dy2 O2 2.327(2) 2_666 ? Dy2 O16 2.377(2) . ? Dy2 O15 2.390(2) . ? Dy1 O14 2.317(2) . ? Dy1 O13 2.347(2) . ? Dy1 O5 2.366(2) . ? Dy1 O9 2.368(2) . ? Dy1 O1 2.372(2) . ? Dy1 N3 2.483(3) . ? Dy1 N1 2.496(3) . ? Dy1 N5 2.531(3) . ? Cu1 N4 1.904(3) . ? Cu1 N2 1.904(3) . ? Cu1 O8 1.945(2) . ? Cu1 O4 1.974(2) . ? C1 O1 1.261(4) . ? C1 O2 1.262(4) . ? C1 C2 1.478(5) . ? C2 N1 1.352(4) . ? C2 C3 1.388(5) . ? C3 C4 1.395(5) . ? C3 H3 0.9500 . ? C4 N2 1.354(4) . ? C4 C5 1.470(5) . ? C5 O3 1.243(4) . ? C5 O4 1.299(4) . ? C6 O6 1.257(4) . ? C6 O5 1.280(4) . ? C6 C7 1.475(5) . ? C7 N3 1.363(4) . ? C7 C8 1.392(5) . ? C8 C9 1.384(5) . ? C8 H8 0.9500 . ? C9 N4 1.351(4) . ? C9 C10 1.488(5) . ? C10 O7 1.251(4) . ? C10 O8 1.281(4) . ? C11 O9 1.255(4) . ? C11 O10 1.259(4) . ? C11 C12 1.489(5) . ? C12 N5 1.333(4) . ? C12 C13 1.398(5) . ? C13 C14 1.363(5) . ? C13 H13 0.9500 . ? C14 N6 1.353(4) . ? C14 C15 1.498(5) . ? C15 O11 1.249(4) . ? C15 O12 1.256(4) . ? N1 N2 1.325(4) . ? N3 N4 1.332(4) . ? N5 N6 1.337(4) . ? N6 H6N 0.8800 . ? O2 Dy2 2.327(2) 2_666 ? O6 Dy2 2.307(2) 2_676 ? O11 Dy2 2.264(2) 1_655 ? O12 Dy2 2.304(2) 2_766 ? O13 H13A 0.8576 . ? O13 H13B 0.8640 . ? O14 H14A 0.8641 . ? O14 H14B 0.8636 . ? O15 H15A 0.8556 . ? O15 H15B 0.8654 . ? O16 H16A 0.8660 . ? O16 H16B 0.8641 . ? O17 H17A 0.8605 . ? O17 H17B 0.8594 . ? O18 H18A 0.8632 . ? O18 H18B 0.8610 . ? 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 O11 Dy2 O10 79.19(9) 1_455 . ? O11 Dy2 O12 80.95(8) 1_455 2_766 ? O10 Dy2 O12 91.75(9) . 2_766 ? O11 Dy2 O6 116.34(8) 1_455 2_676 ? O10 Dy2 O6 82.90(9) . 2_676 ? O12 Dy2 O6 160.27(8) 2_766 2_676 ? O11 Dy2 O2 131.75(9) 1_455 2_666 ? O10 Dy2 O2 147.81(9) . 2_666 ? O12 Dy2 O2 86.04(9) 2_766 2_666 ? O6 Dy2 O2 88.46(8) 2_676 2_666 ? O11 Dy2 O16 148.43(9) 1_455 . ? O10 Dy2 O16 75.68(9) . . ? O12 Dy2 O16 81.04(9) 2_766 . ? O6 Dy2 O16 79.24(8) 2_676 . ? O2 Dy2 O16 72.26(8) 2_666 . ? O11 Dy2 O15 72.60(9) 1_455 . ? O10 Dy2 O15 125.84(9) . . ? O12 Dy2 O15 126.78(8) 2_766 . ? O6 Dy2 O15 70.38(8) 2_676 . ? O2 Dy2 O15 79.07(9) 2_666 . ? O16 Dy2 O15 138.41(9) . . ? O14 Dy1 O13 148.53(9) . . ? O14 Dy1 O5 90.85(9) . . ? O13 Dy1 O5 95.57(9) . . ? O14 Dy1 O9 138.14(8) . . ? O13 Dy1 O9 73.25(8) . . ? O5 Dy1 O9 78.02(9) . . ? O14 Dy1 O1 90.05(8) . . ? O13 Dy1 O1 99.06(9) . . ? O5 Dy1 O1 150.23(8) . . ? O9 Dy1 O1 81.57(8) . . ? O14 Dy1 N3 77.85(9) . . ? O13 Dy1 N3 76.86(9) . . ? O5 Dy1 N3 65.78(9) . . ? O9 Dy1 N3 129.82(9) . . ? O1 Dy1 N3 143.01(9) . . ? O14 Dy1 N1 76.51(9) . . ? O13 Dy1 N1 79.84(9) . . ? O5 Dy1 N1 142.62(9) . . ? O9 Dy1 N1 133.61(9) . . ? O1 Dy1 N1 66.04(9) . . ? N3 Dy1 N1 77.13(9) . . ? O14 Dy1 N5 72.97(9) . . ? O13 Dy1 N5 138.50(9) . . ? O5 Dy1 N5 79.04(9) . . ? O9 Dy1 N5 65.35(8) . . ? O1 Dy1 N5 72.81(9) . . ? N3 Dy1 N5 133.41(9) . . ? N1 Dy1 N5 127.94(9) . . ? N4 Cu1 N2 97.46(12) . . ? N4 Cu1 O8 83.80(11) . . ? N2 Cu1 O8 174.21(12) . . ? N4 Cu1 O4 172.53(11) . . ? N2 Cu1 O4 82.91(11) . . ? O8 Cu1 O4 96.58(10) . . ? O1 C1 O2 123.3(3) . . ? O1 C1 C2 117.4(3) . . ? O2 C1 C2 119.3(3) . . ? N1 C2 C3 111.3(3) . . ? N1 C2 C1 115.9(3) . . ? C3 C2 C1 132.7(3) . . ? C2 C3 C4 103.0(3) . . ? C2 C3 H3 128.5 . . ? C4 C3 H3 128.5 . . ? N2 C4 C3 108.8(3) . . ? N2 C4 C5 114.1(3) . . ? C3 C4 C5 137.1(3) . . ? O3 C5 O4 122.6(3) . . ? O3 C5 C4 122.6(3) . . ? O4 C5 C4 114.8(3) . . ? O6 C6 O5 122.9(3) . . ? O6 C6 C7 120.6(3) . . ? O5 C6 C7 116.4(3) . . ? N3 C7 C8 111.2(3) . . ? N3 C7 C6 115.6(3) . . ? C8 C7 C6 133.2(3) . . ? C9 C8 C7 103.0(3) . . ? C9 C8 H8 128.5 . . ? C7 C8 H8 128.5 . . ? N4 C9 C8 109.8(3) . . ? N4 C9 C10 113.0(3) . . ? C8 C9 C10 137.0(3) . . ? O7 C10 O8 123.5(3) . . ? O7 C10 C9 120.9(3) . . ? O8 C10 C9 115.5(3) . . ? O9 C11 O10 124.5(3) . . ? O9 C11 C12 116.9(3) . . ? O10 C11 C12 118.6(3) . . ? N5 C12 C13 111.5(3) . . ? N5 C12 C11 116.2(3) . . ? C13 C12 C11 131.9(3) . . ? C14 C13 C12 104.2(3) . . ? C14 C13 H13 127.9 . . ? C12 C13 H13 127.9 . . ? N6 C14 C13 107.7(3) . . ? N6 C14 C15 121.0(3) . . ? C13 C14 C15 130.5(3) . . ? O11 C15 O12 126.7(3) . . ? O11 C15 C14 117.4(3) . . ? O12 C15 C14 115.8(3) . . ? N2 N1 C2 106.6(3) . . ? N2 N1 Dy1 136.2(2) . . ? C2 N1 Dy1 116.3(2) . . ? N1 N2 C4 110.2(3) . . ? N1 N2 Cu1 135.4(2) . . ? C4 N2 Cu1 114.4(2) . . ? N4 N3 C7 106.2(3) . . ? N4 N3 Dy1 135.0(2) . . ? C7 N3 Dy1 116.3(2) . . ? N3 N4 C9 109.8(3) . . ? N3 N4 Cu1 136.4(2) . . ? C9 N4 Cu1 113.7(2) . . ? C12 N5 N6 105.1(3) . . ? C12 N5 Dy1 116.4(2) . . ? N6 N5 Dy1 138.4(2) . . ? N5 N6 C14 111.5(3) . . ? N5 N6 H6N 124.2 . . ? C14 N6 H6N 124.2 . . ? C1 O1 Dy1 123.7(2) . . ? C1 O2 Dy2 112.2(2) . 2_666 ? C5 O4 Cu1 113.8(2) . . ? C6 O5 Dy1 123.5(2) . . ? C6 O6 Dy2 141.1(2) . 2_676 ? C10 O8 Cu1 113.7(2) . . ? C11 O9 Dy1 124.9(2) . . ? C11 O10 Dy2 146.5(2) . . ? C15 O11 Dy2 151.3(2) . 1_655 ? C15 O12 Dy2 140.1(2) . 2_766 ? Dy1 O13 H13A 112.8 . . ? Dy1 O13 H13B 113.0 . . ? H13A O13 H13B 127.6 . . ? Dy1 O14 H14A 120.3 . . ? Dy1 O14 H14B 112.3 . . ? H14A O14 H14B 127.4 . . ? Dy2 O15 H15A 113.1 . . ? Dy2 O15 H15B 110.6 . . ? H15A O15 H15B 127.8 . . ? Dy2 O16 H16A 121.9 . . ? Dy2 O16 H16B 110.7 . . ? H16A O16 H16B 126.8 . . ? H17A O17 H17B 127.9 . . ? H18A O18 H18B 127.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 N1 7.1(5) . . . . ? O2 C1 C2 N1 -173.2(3) . . . . ? O1 C1 C2 C3 -172.5(4) . . . . ? O2 C1 C2 C3 7.1(6) . . . . ? N1 C2 C3 C4 0.5(4) . . . . ? C1 C2 C3 C4 -179.9(4) . . . . ? C2 C3 C4 N2 -0.6(4) . . . . ? C2 C3 C4 C5 178.0(4) . . . . ? N2 C4 C5 O3 -175.6(3) . . . . ? C3 C4 C5 O3 5.8(6) . . . . ? N2 C4 C5 O4 2.9(4) . . . . ? C3 C4 C5 O4 -175.6(4) . . . . ? O6 C6 C7 N3 -177.5(3) . . . . ? O5 C6 C7 N3 2.2(4) . . . . ? O6 C6 C7 C8 4.9(6) . . . . ? O5 C6 C7 C8 -175.5(3) . . . . ? N3 C7 C8 C9 0.2(4) . . . . ? C6 C7 C8 C9 178.0(3) . . . . ? C7 C8 C9 N4 -0.4(4) . . . . ? C7 C8 C9 C10 -175.5(4) . . . . ? N4 C9 C10 O7 -172.0(3) . . . . ? C8 C9 C10 O7 3.0(6) . . . . ? N4 C9 C10 O8 5.6(4) . . . . ? C8 C9 C10 O8 -179.4(4) . . . . ? O9 C11 C12 N5 5.5(4) . . . . ? O10 C11 C12 N5 -172.7(3) . . . . ? O9 C11 C12 C13 177.4(3) . . . . ? O10 C11 C12 C13 -0.8(5) . . . . ? N5 C12 C13 C14 2.4(4) . . . . ? C11 C12 C13 C14 -169.9(3) . . . . ? C12 C13 C14 N6 -1.5(4) . . . . ? C12 C13 C14 C15 167.9(3) . . . . ? N6 C14 C15 O11 -166.4(3) . . . . ? C13 C14 C15 O11 25.4(5) . . . . ? N6 C14 C15 O12 17.0(4) . . . . ? C13 C14 C15 O12 -151.2(4) . . . . ? C3 C2 N1 N2 -0.2(4) . . . . ? C1 C2 N1 N2 -179.9(3) . . . . ? C3 C2 N1 Dy1 170.9(2) . . . . ? C1 C2 N1 Dy1 -8.8(4) . . . . ? O14 Dy1 N1 N2 77.3(3) . . . . ? O13 Dy1 N1 N2 -81.8(3) . . . . ? O5 Dy1 N1 N2 4.0(4) . . . . ? O9 Dy1 N1 N2 -136.7(3) . . . . ? O1 Dy1 N1 N2 173.4(3) . . . . ? N3 Dy1 N1 N2 -3.1(3) . . . . ? N5 Dy1 N1 N2 132.6(3) . . . . ? O14 Dy1 N1 C2 -90.4(2) . . . . ? O13 Dy1 N1 C2 110.6(2) . . . . ? O5 Dy1 N1 C2 -163.6(2) . . . . ? O9 Dy1 N1 C2 55.7(3) . . . . ? O1 Dy1 N1 C2 5.8(2) . . . . ? N3 Dy1 N1 C2 -170.7(3) . . . . ? N5 Dy1 N1 C2 -35.0(3) . . . . ? C2 N1 N2 C4 -0.2(4) . . . . ? Dy1 N1 N2 C4 -168.7(2) . . . . ? C2 N1 N2 Cu1 -176.5(3) . . . . ? Dy1 N1 N2 Cu1 15.1(5) . . . . ? C3 C4 N2 N1 0.5(4) . . . . ? C5 C4 N2 N1 -178.4(3) . . . . ? C3 C4 N2 Cu1 177.7(2) . . . . ? C5 C4 N2 Cu1 -1.3(4) . . . . ? N4 Cu1 N2 N1 -11.6(3) . . . . ? O4 Cu1 N2 N1 175.9(3) . . . . ? N4 Cu1 N2 C4 172.2(2) . . . . ? O4 Cu1 N2 C4 -0.3(2) . . . . ? C8 C7 N3 N4 0.0(4) . . . . ? C6 C7 N3 N4 -178.2(3) . . . . ? C8 C7 N3 Dy1 165.1(2) . . . . ? C6 C7 N3 Dy1 -13.0(4) . . . . ? O14 Dy1 N3 N4 -90.9(3) . . . . ? O13 Dy1 N3 N4 70.3(3) . . . . ? O5 Dy1 N3 N4 172.6(3) . . . . ? O9 Dy1 N3 N4 124.8(3) . . . . ? O1 Dy1 N3 N4 -17.4(4) . . . . ? N1 Dy1 N3 N4 -12.1(3) . . . . ? N5 Dy1 N3 N4 -142.8(3) . . . . ? O14 Dy1 N3 C7 109.5(2) . . . . ? O13 Dy1 N3 C7 -89.4(2) . . . . ? O5 Dy1 N3 C7 13.0(2) . . . . ? O9 Dy1 N3 C7 -34.8(3) . . . . ? O1 Dy1 N3 C7 -177.0(2) . . . . ? N1 Dy1 N3 C7 -171.8(3) . . . . ? N5 Dy1 N3 C7 57.5(3) . . . . ? C7 N3 N4 C9 -0.2(4) . . . . ? Dy1 N3 N4 C9 -161.3(2) . . . . ? C7 N3 N4 Cu1 178.9(3) . . . . ? Dy1 N3 N4 Cu1 17.9(5) . . . . ? C8 C9 N4 N3 0.4(4) . . . . ? C10 C9 N4 N3 176.8(3) . . . . ? C8 C9 N4 Cu1 -178.9(2) . . . . ? C10 C9 N4 Cu1 -2.6(3) . . . . ? N2 Cu1 N4 N3 -5.1(3) . . . . ? O8 Cu1 N4 N3 -179.4(3) . . . . ? N2 Cu1 N4 C9 174.0(2) . . . . ? O8 Cu1 N4 C9 -0.3(2) . . . . ? C13 C12 N5 N6 -2.2(4) . . . . ? C11 C12 N5 N6 171.3(3) . . . . ? C13 C12 N5 Dy1 -178.4(2) . . . . ? C11 C12 N5 Dy1 -4.8(4) . . . . ? O14 Dy1 N5 C12 -173.7(2) . . . . ? O13 Dy1 N5 C12 6.6(3) . . . . ? O5 Dy1 N5 C12 -79.4(2) . . . . ? O9 Dy1 N5 C12 2.3(2) . . . . ? O1 Dy1 N5 C12 90.8(2) . . . . ? N3 Dy1 N5 C12 -120.1(2) . . . . ? N1 Dy1 N5 C12 129.5(2) . . . . ? O14 Dy1 N5 N6 11.9(3) . . . . ? O13 Dy1 N5 N6 -167.8(3) . . . . ? O5 Dy1 N5 N6 106.2(3) . . . . ? O9 Dy1 N5 N6 -172.0(3) . . . . ? O1 Dy1 N5 N6 -83.6(3) . . . . ? N3 Dy1 N5 N6 65.6(4) . . . . ? N1 Dy1 N5 N6 -44.8(4) . . . . ? C12 N5 N6 C14 1.2(4) . . . . ? Dy1 N5 N6 C14 176.0(2) . . . . ? C13 C14 N6 N5 0.2(4) . . . . ? C15 C14 N6 N5 -170.4(3) . . . . ? O2 C1 O1 Dy1 178.8(2) . . . . ? C2 C1 O1 Dy1 -1.6(4) . . . . ? O14 Dy1 O1 C1 73.1(3) . . . . ? O13 Dy1 O1 C1 -76.6(3) . . . . ? O5 Dy1 O1 C1 164.9(2) . . . . ? O9 Dy1 O1 C1 -148.1(3) . . . . ? N3 Dy1 O1 C1 3.5(3) . . . . ? N1 Dy1 O1 C1 -2.1(2) . . . . ? N5 Dy1 O1 C1 145.2(3) . . . . ? O1 C1 O2 Dy2 -0.9(4) . . . 2_666 ? C2 C1 O2 Dy2 179.5(2) . . . 2_666 ? O3 C5 O4 Cu1 175.5(3) . . . . ? C4 C5 O4 Cu1 -3.1(4) . . . . ? N2 Cu1 O4 C5 1.9(2) . . . . ? O8 Cu1 O4 C5 176.1(2) . . . . ? O6 C6 O5 Dy1 -169.2(2) . . . . ? C7 C6 O5 Dy1 11.2(4) . . . . ? O14 Dy1 O5 C6 -89.3(3) . . . . ? O13 Dy1 O5 C6 59.9(3) . . . . ? O9 Dy1 O5 C6 131.4(3) . . . . ? O1 Dy1 O5 C6 179.2(2) . . . . ? N3 Dy1 O5 C6 -13.0(2) . . . . ? N1 Dy1 O5 C6 -20.7(3) . . . . ? N5 Dy1 O5 C6 -161.7(3) . . . . ? O5 C6 O6 Dy2 109.0(4) . . . 2_676 ? C7 C6 O6 Dy2 -71.4(5) . . . 2_676 ? O7 C10 O8 Cu1 171.8(3) . . . . ? C9 C10 O8 Cu1 -5.8(4) . . . . ? N4 Cu1 O8 C10 3.5(2) . . . . ? O4 Cu1 O8 C10 176.0(2) . . . . ? O10 C11 O9 Dy1 174.6(2) . . . . ? C12 C11 O9 Dy1 -3.5(4) . . . . ? O14 Dy1 O9 C11 6.5(3) . . . . ? O13 Dy1 O9 C11 -176.3(3) . . . . ? O5 Dy1 O9 C11 84.1(3) . . . . ? O1 Dy1 O9 C11 -74.1(3) . . . . ? N3 Dy1 O9 C11 127.8(2) . . . . ? N1 Dy1 O9 C11 -119.0(3) . . . . ? N5 Dy1 O9 C11 0.8(2) . . . . ? O9 C11 O10 Dy2 -109.8(4) . . . . ? C12 C11 O10 Dy2 68.3(5) . . . . ? O11 Dy2 O10 C11 45.6(4) 1_455 . . . ? O12 Dy2 O10 C11 -34.8(4) 2_766 . . . ? O6 Dy2 O10 C11 164.2(4) 2_676 . . . ? O2 Dy2 O10 C11 -120.2(4) 2_666 . . . ? O16 Dy2 O10 C11 -115.1(4) . . . . ? O15 Dy2 O10 C11 104.7(4) . . . . ? O12 C15 O11 Dy2 -116.0(4) . . . 1_655 ? C14 C15 O11 Dy2 67.8(6) . . . 1_655 ? O11 C15 O12 Dy2 1.2(6) . . . 2_766 ? C14 C15 O12 Dy2 177.4(2) . . . 2_766 ? 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 O17 H17B O9 0.86 2.31 3.088(4) 150.7 . O17 H17B O10 0.86 2.33 3.021(4) 137.9 . O16 H16A O18 0.87 1.90 2.757(4) 168.0 . N6 H6N O3 0.88 2.21 2.911(4) 136.6 2_667 O14 H14A O3 0.86 1.77 2.630(3) 169.8 2_667 O15 H15A O4 0.86 2.05 2.807(3) 146.6 1_554 O13 H13A O18 0.86 2.00 2.821(4) 159.6 2_676 O17 H17A O5 0.86 2.03 2.847(4) 158.8 2_676 O18 H18A O17 0.86 1.85 2.689(4) 164.0 2_676 O18 H18B O6 0.86 2.50 3.336(4) 165.0 2_776 O13 H13B O7 0.86 1.91 2.761(4) 170.0 2_577 O14 H14B O7 0.86 1.85 2.641(3) 151.3 2_677 O15 H15B N6 0.87 2.58 3.431(4) 170.0 2_666 O16 H16B O4 0.86 2.13 2.936(3) 154.9 1_654 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.359 _refine_diff_density_min -0.912 _refine_diff_density_rms 0.127 _database_code_depnum_ccdc_archive 'CCDC 931527' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H12 Cu Er2 N6 O16, 2(H2 O)' _chemical_formula_sum 'C15 H16 Cu Er2 N6 O18' _chemical_formula_weight 966.40 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1245(3) _cell_length_b 11.2018(5) _cell_length_c 15.4103(7) _cell_angle_alpha 82.608(2) _cell_angle_beta 77.4360(10) _cell_angle_gamma 84.553(2) _cell_volume 1187.58(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9842 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 30.49 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 914 _exptl_absorpt_coefficient_mu 7.994 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4230 _exptl_absorpt_correction_T_max 0.7955 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38846 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_unetI/netI 0.0233 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 30.54 _reflns_number_total 7193 _reflns_number_gt 6420 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0132P)^2^+1.5088P] 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 7193 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0221 _refine_ls_R_factor_gt 0.0173 _refine_ls_wR_factor_ref 0.0359 _refine_ls_wR_factor_gt 0.0346 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.002 _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 Er2 Er 0.514491(13) 0.663461(8) 0.351548(6) 0.00780(3) Uani 1 1 d . . . Er1 Er 0.483425(13) 0.771923(8) 0.756482(6) 0.00828(3) Uani 1 1 d . . . Cu1 Cu 0.19621(4) 0.81254(2) 1.042772(18) 0.01034(6) Uani 1 1 d . . . C1 C 0.3859(3) 0.4927(2) 0.80292(15) 0.0108(4) Uani 1 1 d . . . C2 C 0.3164(3) 0.5342(2) 0.89204(15) 0.0107(4) Uani 1 1 d . . . C3 C 0.2470(3) 0.4752(2) 0.97632(15) 0.0115(4) Uani 1 1 d . . . H3 H 0.2303 0.3917 0.9929 0.014 Uiso 1 1 calc R . . C4 C 0.2082(3) 0.5685(2) 1.03035(15) 0.0102(4) Uani 1 1 d . . . C5 C 0.1273(3) 0.5815(2) 1.12583(15) 0.0107(4) Uani 1 1 d . . . C6 C 0.5689(3) 1.0533(2) 0.73950(15) 0.0101(4) Uani 1 1 d . . . C7 C 0.4573(3) 1.03644(19) 0.83235(15) 0.0098(4) Uani 1 1 d . . . C8 C 0.3722(3) 1.1168(2) 0.89438(15) 0.0104(4) Uani 1 1 d . . . H8 H 0.3743 1.2021 0.8882 0.012 Uiso 1 1 calc R . . C9 C 0.2841(3) 1.04094(19) 0.96704(15) 0.0096(4) Uani 1 1 d . . . C10 C 0.1570(3) 1.0541(2) 1.05644(15) 0.0102(4) Uani 1 1 d . . . C11 C 0.5672(3) 0.76577(19) 0.54187(15) 0.0100(4) Uani 1 1 d . . . C12 C 0.7603(3) 0.72153(19) 0.55944(15) 0.0094(4) Uani 1 1 d . . . C13 C 0.9291(3) 0.6784(2) 0.50362(15) 0.0105(4) Uani 1 1 d . . . H13 H 0.9560 0.6807 0.4403 0.013 Uiso 1 1 calc R . . C14 C 1.0470(3) 0.6321(2) 0.56140(15) 0.0102(4) Uani 1 1 d . . . C15 C 1.2297(3) 0.5544(2) 0.54600(15) 0.0097(4) Uani 1 1 d . . . N1 N 0.3202(3) 0.65454(17) 0.89494(13) 0.0112(4) Uani 1 1 d . . . N2 N 0.2542(3) 0.67333(17) 0.97991(12) 0.0112(4) Uani 1 1 d . . . N3 N 0.4218(3) 0.92103(17) 0.86557(13) 0.0105(4) Uani 1 1 d . . . N4 N 0.3162(3) 0.92575(17) 0.94838(13) 0.0103(4) Uani 1 1 d . . . N5 N 0.7761(3) 0.70739(17) 0.64507(13) 0.0111(4) Uani 1 1 d . . . N6 N 0.9508(3) 0.65164(18) 0.64510(13) 0.0124(4) Uani 1 1 d . . . H6N H 0.9976 0.6302 0.6936 0.015 Uiso 1 1 calc R . . O1 O 0.4597(2) 0.56982(14) 0.73990(11) 0.0133(3) Uani 1 1 d . . . O2 O 0.3712(2) 0.38469(14) 0.79227(11) 0.0131(3) Uani 1 1 d . . . O3 O 0.0874(2) 0.49433(14) 1.18252(11) 0.0146(3) Uani 1 1 d . . . O4 O 0.1039(2) 0.69295(14) 1.14518(11) 0.0128(3) Uani 1 1 d . . . O5 O 0.6129(2) 0.95809(14) 0.70014(11) 0.0141(3) Uani 1 1 d . . . O6 O 0.6159(2) 1.15598(14) 0.70325(11) 0.0112(3) Uani 1 1 d . . . O7 O 0.0977(2) 1.15649(14) 1.07923(11) 0.0136(3) Uani 1 1 d . . . O8 O 0.1101(2) 0.95553(14) 1.10461(11) 0.0131(3) Uani 1 1 d . . . O9 O 0.4406(2) 0.79462(15) 0.60804(11) 0.0126(3) Uani 1 1 d . . . O10 O 0.5386(2) 0.76931(15) 0.46386(11) 0.0128(3) Uani 1 1 d . . . O11 O 1.3290(2) 0.55978(15) 0.46820(11) 0.0134(3) Uani 1 1 d . . . O12 O 1.2622(2) 0.48371(15) 0.61228(11) 0.0131(3) Uani 1 1 d . . . O13 O 0.1644(2) 0.84012(16) 0.75956(11) 0.0166(4) Uani 1 1 d . . . H13A H 0.1522 0.8916 0.7148 0.020 Uiso 1 1 d R . . H13B H 0.0939 0.8365 0.8128 0.020 Uiso 1 1 d R . . O14 O 0.7254(2) 0.71756(15) 0.83313(11) 0.0148(3) Uani 1 1 d . . . H14A H 0.7797 0.6454 0.8338 0.018 Uiso 1 1 d R . . H14B H 0.7480 0.7754 0.8605 0.018 Uiso 1 1 d R . . O15 O 0.2264(2) 0.63164(15) 0.30772(11) 0.0138(3) Uani 1 1 d . . . H15A H 0.2107 0.6763 0.2604 0.017 Uiso 1 1 d R . . H15B H 0.1937 0.5586 0.3246 0.017 Uiso 1 1 d R . . O16 O 0.7953(2) 0.76548(15) 0.29366(11) 0.0141(3) Uani 1 1 d . . . H16A H 0.8215 0.8252 0.3184 0.017 Uiso 1 1 d R . . H16B H 0.8544 0.7424 0.2430 0.017 Uiso 1 1 d R . . O17 O 0.2394(3) 0.97791(19) 0.48538(13) 0.0312(5) Uani 1 1 d . . . H17A H 0.2762 1.0160 0.4333 0.037 Uiso 1 1 d R . . H17B H 0.2845 0.9093 0.5065 0.037 Uiso 1 1 d R . . O18 O 0.9304(3) 0.95494(17) 0.35378(12) 0.0213(4) Uani 1 1 d . . . H18A H 0.8661 0.9631 0.4071 0.026 Uiso 1 1 d R . . H18B H 1.0525 0.9409 0.3368 0.026 Uiso 1 1 d 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 Er2 0.00947(4) 0.00817(4) 0.00495(5) -0.00042(3) -0.00040(3) 0.00061(3) Er1 0.01092(5) 0.00740(4) 0.00560(5) -0.00125(4) 0.00025(3) 0.00019(3) Cu1 0.01588(13) 0.00730(12) 0.00624(13) -0.00163(10) 0.00166(10) -0.00075(10) C1 0.0132(10) 0.0105(10) 0.0085(10) -0.0029(8) -0.0010(8) 0.0000(8) C2 0.0130(10) 0.0091(10) 0.0096(11) -0.0028(8) -0.0001(8) -0.0013(8) C3 0.0148(10) 0.0089(10) 0.0098(11) -0.0003(8) -0.0008(8) -0.0007(8) C4 0.0117(10) 0.0101(10) 0.0080(10) 0.0002(8) -0.0017(8) 0.0004(8) C5 0.0131(10) 0.0118(10) 0.0070(10) -0.0018(8) -0.0025(8) 0.0020(8) C6 0.0103(9) 0.0101(10) 0.0094(10) 0.0004(8) -0.0027(8) 0.0015(8) C7 0.0115(10) 0.0089(9) 0.0081(10) 0.0007(8) -0.0018(8) 0.0003(8) C8 0.0138(10) 0.0073(9) 0.0103(11) -0.0014(8) -0.0030(8) -0.0002(8) C9 0.0108(10) 0.0086(9) 0.0092(10) -0.0022(8) -0.0017(8) 0.0010(8) C10 0.0091(9) 0.0118(10) 0.0104(11) -0.0041(8) -0.0024(8) 0.0000(8) C11 0.0128(10) 0.0080(9) 0.0086(10) -0.0011(8) -0.0012(8) 0.0004(8) C12 0.0114(10) 0.0088(9) 0.0069(10) 0.0001(8) -0.0006(8) -0.0003(8) C13 0.0123(10) 0.0112(10) 0.0065(10) 0.0000(8) 0.0001(8) 0.0010(8) C14 0.0119(10) 0.0100(10) 0.0075(10) 0.0000(8) -0.0004(8) 0.0000(8) C15 0.0096(9) 0.0098(9) 0.0096(10) 0.0001(8) -0.0025(8) -0.0010(8) N1 0.0161(9) 0.0098(8) 0.0070(9) -0.0029(7) 0.0008(7) -0.0012(7) N2 0.0184(9) 0.0081(8) 0.0055(9) 0.0000(7) 0.0009(7) -0.0014(7) N3 0.0135(9) 0.0093(8) 0.0070(9) -0.0005(7) 0.0011(7) -0.0003(7) N4 0.0139(9) 0.0093(8) 0.0073(9) -0.0027(7) -0.0003(7) 0.0002(7) N5 0.0091(8) 0.0153(9) 0.0087(9) -0.0027(8) -0.0020(7) 0.0028(7) N6 0.0117(9) 0.0190(10) 0.0056(9) 0.0003(8) -0.0020(7) 0.0025(7) O1 0.0208(8) 0.0103(7) 0.0075(8) -0.0014(6) 0.0010(6) -0.0026(6) O2 0.0198(8) 0.0097(7) 0.0088(8) -0.0029(6) 0.0004(6) -0.0011(6) O3 0.0224(8) 0.0105(7) 0.0076(8) 0.0020(6) 0.0016(7) 0.0009(6) O4 0.0203(8) 0.0091(7) 0.0073(8) -0.0023(6) 0.0010(6) -0.0006(6) O5 0.0206(8) 0.0092(7) 0.0098(8) -0.0015(6) 0.0033(6) -0.0015(6) O6 0.0129(7) 0.0088(7) 0.0104(8) 0.0014(6) -0.0007(6) -0.0007(6) O7 0.0137(7) 0.0096(7) 0.0167(9) -0.0060(7) 0.0005(6) 0.0007(6) O8 0.0170(8) 0.0110(7) 0.0099(8) -0.0031(6) 0.0012(6) -0.0006(6) O9 0.0117(7) 0.0168(8) 0.0078(8) -0.0026(6) -0.0002(6) 0.0036(6) O10 0.0160(8) 0.0148(8) 0.0086(8) -0.0037(6) -0.0044(6) 0.0023(6) O11 0.0119(7) 0.0169(8) 0.0083(8) 0.0017(6) 0.0019(6) 0.0019(6) O12 0.0130(7) 0.0144(8) 0.0097(8) 0.0022(6) -0.0004(6) 0.0013(6) O13 0.0150(8) 0.0230(9) 0.0086(8) -0.0002(7) 0.0020(6) 0.0029(7) O14 0.0208(8) 0.0098(7) 0.0161(9) -0.0061(7) -0.0081(7) 0.0030(6) O15 0.0171(8) 0.0134(8) 0.0118(8) 0.0013(7) -0.0051(7) -0.0040(6) O16 0.0141(8) 0.0168(8) 0.0112(8) -0.0050(7) 0.0013(6) -0.0038(6) O17 0.0383(12) 0.0274(11) 0.0194(10) 0.0040(9) 0.0011(9) 0.0154(9) O18 0.0174(8) 0.0298(10) 0.0166(9) -0.0036(8) -0.0017(7) -0.0040(7) _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 Er2 O11 2.2465(16) 1_455 ? Er2 O10 2.2643(16) . ? Er2 O12 2.2830(16) 2_766 ? Er2 O6 2.2831(16) 2_676 ? Er2 O2 2.3032(16) 2_666 ? Er2 O16 2.3452(16) . ? Er2 O15 2.3667(16) . ? Er1 O14 2.2889(16) . ? Er1 O13 2.3207(16) . ? Er1 O1 2.3365(16) . ? Er1 O5 2.3463(16) . ? Er1 O9 2.3515(16) . ? Er1 N3 2.4638(18) . ? Er1 N1 2.4745(19) . ? Er1 N5 2.5087(18) . ? Cu1 N2 1.9061(18) . ? Cu1 N4 1.9092(19) . ? Cu1 O8 1.9498(16) . ? Cu1 O4 1.9722(16) . ? C1 O2 1.258(3) . ? C1 O1 1.271(3) . ? C1 C2 1.474(3) . ? C2 N1 1.357(3) . ? C2 C3 1.389(3) . ? C3 C4 1.389(3) . ? C3 H3 0.9500 . ? C4 N2 1.348(3) . ? C4 C5 1.480(3) . ? C5 O3 1.234(3) . ? C5 O4 1.307(3) . ? C6 O6 1.254(3) . ? C6 O5 1.274(3) . ? C6 C7 1.476(3) . ? C7 N3 1.354(3) . ? C7 C8 1.399(3) . ? C8 C9 1.386(3) . ? C8 H8 0.9500 . ? C9 N4 1.346(3) . ? C9 C10 1.491(3) . ? C10 O7 1.251(3) . ? C10 O8 1.277(3) . ? C11 O10 1.257(3) . ? C11 O9 1.260(3) . ? C11 C12 1.486(3) . ? C12 N5 1.337(3) . ? C12 C13 1.402(3) . ? C13 C14 1.375(3) . ? C13 H13 0.9500 . ? C14 N6 1.357(3) . ? C14 C15 1.487(3) . ? C15 O11 1.250(3) . ? C15 O12 1.259(3) . ? N1 N2 1.328(3) . ? N3 N4 1.338(3) . ? N5 N6 1.338(3) . ? N6 H6N 0.8800 . ? O2 Er2 2.3032(16) 2_666 ? O6 Er2 2.2831(16) 2_676 ? O11 Er2 2.2465(16) 1_655 ? O12 Er2 2.2830(16) 2_766 ? O13 H13A 0.8546 . ? O13 H13B 0.8615 . ? O14 H14A 0.8622 . ? O14 H14B 0.8624 . ? O15 H15A 0.8523 . ? O15 H15B 0.8642 . ? O16 H16A 0.8648 . ? O16 H16B 0.8619 . ? O17 H17A 0.8578 . ? O17 H17B 0.8569 . ? O18 H18A 0.8608 . ? O18 H18B 0.8580 . ? 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 O11 Er2 O10 79.53(6) 1_455 . ? O11 Er2 O12 80.54(6) 1_455 2_766 ? O10 Er2 O12 92.51(6) . 2_766 ? O11 Er2 O6 116.86(6) 1_455 2_676 ? O10 Er2 O6 82.83(6) . 2_676 ? O12 Er2 O6 160.51(6) 2_766 2_676 ? O11 Er2 O2 129.53(6) 1_455 2_666 ? O10 Er2 O2 149.36(6) . 2_666 ? O12 Er2 O2 84.51(6) 2_766 2_666 ? O6 Er2 O2 89.91(6) 2_676 2_666 ? O11 Er2 O16 148.71(6) 1_455 . ? O10 Er2 O16 76.53(6) . . ? O12 Er2 O16 80.69(6) 2_766 . ? O6 Er2 O16 79.82(6) 2_676 . ? O2 Er2 O16 72.89(6) 2_666 . ? O11 Er2 O15 72.56(6) 1_455 . ? O10 Er2 O15 126.16(6) . . ? O12 Er2 O15 125.70(6) 2_766 . ? O6 Er2 O15 70.87(6) 2_676 . ? O2 Er2 O15 78.21(6) 2_666 . ? O16 Er2 O15 138.49(6) . . ? O14 Er1 O13 148.42(6) . . ? O14 Er1 O1 90.41(6) . . ? O13 Er1 O1 98.44(6) . . ? O14 Er1 O5 91.29(6) . . ? O13 Er1 O5 95.93(6) . . ? O1 Er1 O5 149.47(6) . . ? O14 Er1 O9 138.66(6) . . ? O13 Er1 O9 72.88(6) . . ? O1 Er1 O9 80.78(6) . . ? O5 Er1 O9 77.93(6) . . ? O14 Er1 N3 78.23(6) . . ? O13 Er1 N3 76.85(6) . . ? O1 Er1 N3 143.89(6) . . ? O5 Er1 N3 65.88(6) . . ? O9 Er1 N3 129.38(6) . . ? O14 Er1 N1 76.71(6) . . ? O13 Er1 N1 79.22(6) . . ? O1 Er1 N1 66.48(6) . . ? O5 Er1 N1 143.15(6) . . ? O9 Er1 N1 132.84(6) . . ? N3 Er1 N1 77.53(6) . . ? O14 Er1 N5 72.94(6) . . ? O13 Er1 N5 138.63(6) . . ? O1 Er1 N5 72.55(6) . . ? O5 Er1 N5 78.85(6) . . ? O9 Er1 N5 65.87(6) . . ? N3 Er1 N5 133.40(6) . . ? N1 Er1 N5 128.03(6) . . ? N2 Cu1 N4 97.41(8) . . ? N2 Cu1 O8 174.06(8) . . ? N4 Cu1 O8 83.77(7) . . ? N2 Cu1 O4 82.91(7) . . ? N4 Cu1 O4 172.70(8) . . ? O8 Cu1 O4 96.67(7) . . ? O2 C1 O1 123.1(2) . . ? O2 C1 C2 119.8(2) . . ? O1 C1 C2 117.07(19) . . ? N1 C2 C3 111.37(19) . . ? N1 C2 C1 115.4(2) . . ? C3 C2 C1 133.2(2) . . ? C4 C3 C2 102.93(19) . . ? C4 C3 H3 128.5 . . ? C2 C3 H3 128.5 . . ? N2 C4 C3 109.3(2) . . ? N2 C4 C5 113.98(19) . . ? C3 C4 C5 136.7(2) . . ? O3 C5 O4 122.9(2) . . ? O3 C5 C4 122.7(2) . . ? O4 C5 C4 114.35(19) . . ? O6 C6 O5 123.3(2) . . ? O6 C6 C7 120.8(2) . . ? O5 C6 C7 115.86(19) . . ? N3 C7 C8 111.29(19) . . ? N3 C7 C6 115.55(19) . . ? C8 C7 C6 133.1(2) . . ? C9 C8 C7 102.80(19) . . ? C9 C8 H8 128.6 . . ? C7 C8 H8 128.6 . . ? N4 C9 C8 109.72(19) . . ? N4 C9 C10 113.12(19) . . ? C8 C9 C10 137.1(2) . . ? O7 C10 O8 123.9(2) . . ? O7 C10 C9 120.4(2) . . ? O8 C10 C9 115.66(19) . . ? O10 C11 O9 124.3(2) . . ? O10 C11 C12 118.94(19) . . ? O9 C11 C12 116.7(2) . . ? N5 C12 C13 111.49(19) . . ? N5 C12 C11 116.19(19) . . ? C13 C12 C11 131.9(2) . . ? C14 C13 C12 104.26(19) . . ? C14 C13 H13 127.9 . . ? C12 C13 H13 127.9 . . ? N6 C14 C13 107.21(19) . . ? N6 C14 C15 121.5(2) . . ? C13 C14 C15 130.4(2) . . ? O11 C15 O12 126.4(2) . . ? O11 C15 C14 117.5(2) . . ? O12 C15 C14 115.92(19) . . ? N2 N1 C2 106.14(18) . . ? N2 N1 Er1 136.55(14) . . ? C2 N1 Er1 116.47(14) . . ? N1 N2 C4 110.28(18) . . ? N1 N2 Cu1 134.84(15) . . ? C4 N2 Cu1 114.72(15) . . ? N4 N3 C7 106.14(17) . . ? N4 N3 Er1 135.01(14) . . ? C7 N3 Er1 116.44(14) . . ? N3 N4 C9 110.06(18) . . ? N3 N4 Cu1 136.25(14) . . ? C9 N4 Cu1 113.65(15) . . ? C12 N5 N6 105.09(17) . . ? C12 N5 Er1 116.31(14) . . ? N6 N5 Er1 138.37(14) . . ? N5 N6 C14 111.90(18) . . ? N5 N6 H6N 124.1 . . ? C14 N6 H6N 124.1 . . ? C1 O1 Er1 124.08(14) . . ? C1 O2 Er2 114.91(14) . 2_666 ? C5 O4 Cu1 113.95(14) . . ? C6 O5 Er1 123.81(14) . . ? C6 O6 Er2 141.16(14) . 2_676 ? C10 O8 Cu1 113.49(14) . . ? C11 O9 Er1 124.72(14) . . ? C11 O10 Er2 146.97(15) . . ? C15 O11 Er2 149.97(15) . 1_655 ? C15 O12 Er2 139.83(14) . 2_766 ? Er1 O13 H13A 112.2 . . ? Er1 O13 H13B 113.3 . . ? H13A O13 H13B 127.5 . . ? Er1 O14 H14A 120.4 . . ? Er1 O14 H14B 112.1 . . ? H14A O14 H14B 127.5 . . ? Er2 O15 H15A 112.8 . . ? Er2 O15 H15B 111.2 . . ? H15A O15 H15B 127.8 . . ? Er2 O16 H16A 121.3 . . ? Er2 O16 H16B 111.3 . . ? H16A O16 H16B 126.9 . . ? H17A O17 H17B 127.9 . . ? H18A O18 H18B 127.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 N1 -173.5(2) . . . . ? O1 C1 C2 N1 6.8(3) . . . . ? O2 C1 C2 C3 7.1(4) . . . . ? O1 C1 C2 C3 -172.6(2) . . . . ? N1 C2 C3 C4 0.3(3) . . . . ? C1 C2 C3 C4 179.7(2) . . . . ? C2 C3 C4 N2 -0.5(2) . . . . ? C2 C3 C4 C5 177.7(3) . . . . ? N2 C4 C5 O3 -175.8(2) . . . . ? C3 C4 C5 O3 6.0(4) . . . . ? N2 C4 C5 O4 3.4(3) . . . . ? C3 C4 C5 O4 -174.7(2) . . . . ? O6 C6 C7 N3 -177.4(2) . . . . ? O5 C6 C7 N3 2.5(3) . . . . ? O6 C6 C7 C8 5.2(4) . . . . ? O5 C6 C7 C8 -174.9(2) . . . . ? N3 C7 C8 C9 0.2(3) . . . . ? C6 C7 C8 C9 177.7(2) . . . . ? C7 C8 C9 N4 0.1(2) . . . . ? C7 C8 C9 C10 -175.7(3) . . . . ? N4 C9 C10 O7 -172.4(2) . . . . ? C8 C9 C10 O7 3.3(4) . . . . ? N4 C9 C10 O8 5.3(3) . . . . ? C8 C9 C10 O8 -179.0(2) . . . . ? O10 C11 C12 N5 -173.0(2) . . . . ? O9 C11 C12 N5 5.3(3) . . . . ? O10 C11 C12 C13 -0.9(4) . . . . ? O9 C11 C12 C13 177.3(2) . . . . ? N5 C12 C13 C14 2.5(3) . . . . ? C11 C12 C13 C14 -169.9(2) . . . . ? C12 C13 C14 N6 -1.7(2) . . . . ? C12 C13 C14 C15 167.6(2) . . . . ? N6 C14 C15 O11 -166.1(2) . . . . ? C13 C14 C15 O11 25.9(3) . . . . ? N6 C14 C15 O12 18.4(3) . . . . ? C13 C14 C15 O12 -149.6(2) . . . . ? C3 C2 N1 N2 0.0(3) . . . . ? C1 C2 N1 N2 -179.57(19) . . . . ? C3 C2 N1 Er1 171.25(15) . . . . ? C1 C2 N1 Er1 -8.3(2) . . . . ? O14 Er1 N1 N2 76.9(2) . . . . ? O13 Er1 N1 N2 -82.5(2) . . . . ? O1 Er1 N1 N2 173.3(2) . . . . ? O5 Er1 N1 N2 3.0(3) . . . . ? O9 Er1 N1 N2 -136.7(2) . . . . ? N3 Er1 N1 N2 -3.8(2) . . . . ? N5 Er1 N1 N2 132.3(2) . . . . ? O14 Er1 N1 C2 -90.87(16) . . . . ? O13 Er1 N1 C2 109.72(16) . . . . ? O1 Er1 N1 C2 5.49(15) . . . . ? O5 Er1 N1 C2 -164.80(14) . . . . ? O9 Er1 N1 C2 55.55(18) . . . . ? N3 Er1 N1 C2 -171.53(17) . . . . ? N5 Er1 N1 C2 -35.44(19) . . . . ? C2 N1 N2 C4 -0.3(2) . . . . ? Er1 N1 N2 C4 -168.89(16) . . . . ? C2 N1 N2 Cu1 -175.43(17) . . . . ? Er1 N1 N2 Cu1 16.0(3) . . . . ? C3 C4 N2 N1 0.5(3) . . . . ? C5 C4 N2 N1 -178.15(18) . . . . ? C3 C4 N2 Cu1 176.69(15) . . . . ? C5 C4 N2 Cu1 -1.9(2) . . . . ? N4 Cu1 N2 N1 -12.1(2) . . . . ? O4 Cu1 N2 N1 175.2(2) . . . . ? N4 Cu1 N2 C4 172.90(16) . . . . ? O4 Cu1 N2 C4 0.25(16) . . . . ? C8 C7 N3 N4 -0.5(2) . . . . ? C6 C7 N3 N4 -178.41(18) . . . . ? C8 C7 N3 Er1 164.59(14) . . . . ? C6 C7 N3 Er1 -13.4(2) . . . . ? O14 Er1 N3 N4 -90.5(2) . . . . ? O13 Er1 N3 N4 70.0(2) . . . . ? O1 Er1 N3 N4 -16.3(3) . . . . ? O5 Er1 N3 N4 172.7(2) . . . . ? O9 Er1 N3 N4 124.30(19) . . . . ? N1 Er1 N3 N4 -11.7(2) . . . . ? N5 Er1 N3 N4 -142.94(18) . . . . ? O14 Er1 N3 C7 110.03(16) . . . . ? O13 Er1 N3 C7 -89.53(16) . . . . ? O1 Er1 N3 C7 -175.83(14) . . . . ? O5 Er1 N3 C7 13.23(14) . . . . ? O9 Er1 N3 C7 -35.18(18) . . . . ? N1 Er1 N3 C7 -171.19(16) . . . . ? N5 Er1 N3 C7 57.58(18) . . . . ? C7 N3 N4 C9 0.5(2) . . . . ? Er1 N3 N4 C9 -160.43(16) . . . . ? C7 N3 N4 Cu1 178.12(17) . . . . ? Er1 N3 N4 Cu1 17.2(3) . . . . ? C8 C9 N4 N3 -0.4(3) . . . . ? C10 C9 N4 N3 176.52(18) . . . . ? C8 C9 N4 Cu1 -178.57(15) . . . . ? C10 C9 N4 Cu1 -1.7(2) . . . . ? N2 Cu1 N4 N3 -4.5(2) . . . . ? O8 Cu1 N4 N3 -178.7(2) . . . . ? N2 Cu1 N4 C9 173.02(16) . . . . ? O8 Cu1 N4 C9 -1.12(16) . . . . ? C13 C12 N5 N6 -2.2(2) . . . . ? C11 C12 N5 N6 171.47(19) . . . . ? C13 C12 N5 Er1 -177.72(14) . . . . ? C11 C12 N5 Er1 -4.1(2) . . . . ? O14 Er1 N5 C12 -174.83(17) . . . . ? O13 Er1 N5 C12 6.3(2) . . . . ? O1 Er1 N5 C12 89.19(16) . . . . ? O5 Er1 N5 C12 -79.99(16) . . . . ? O9 Er1 N5 C12 1.67(15) . . . . ? N3 Er1 N5 C12 -120.55(16) . . . . ? N1 Er1 N5 C12 128.22(15) . . . . ? O14 Er1 N5 N6 11.7(2) . . . . ? O13 Er1 N5 N6 -167.18(19) . . . . ? O1 Er1 N5 N6 -84.3(2) . . . . ? O5 Er1 N5 N6 106.5(2) . . . . ? O9 Er1 N5 N6 -171.8(2) . . . . ? N3 Er1 N5 N6 66.0(2) . . . . ? N1 Er1 N5 N6 -45.3(2) . . . . ? C12 N5 N6 C14 1.0(2) . . . . ? Er1 N5 N6 C14 175.01(16) . . . . ? C13 C14 N6 N5 0.5(3) . . . . ? C15 C14 N6 N5 -170.00(19) . . . . ? O2 C1 O1 Er1 178.64(16) . . . . ? C2 C1 O1 Er1 -1.7(3) . . . . ? O14 Er1 O1 C1 73.38(18) . . . . ? O13 Er1 O1 C1 -76.20(18) . . . . ? O5 Er1 O1 C1 166.61(16) . . . . ? O9 Er1 O1 C1 -147.19(18) . . . . ? N3 Er1 O1 C1 3.0(2) . . . . ? N1 Er1 O1 C1 -1.91(17) . . . . ? N5 Er1 O1 C1 145.33(19) . . . . ? O1 C1 O2 Er2 -0.7(3) . . . 2_666 ? C2 C1 O2 Er2 179.59(16) . . . 2_666 ? O3 C5 O4 Cu1 176.09(18) . . . . ? C4 C5 O4 Cu1 -3.1(2) . . . . ? N2 Cu1 O4 C5 1.70(15) . . . . ? O8 Cu1 O4 C5 175.74(15) . . . . ? O6 C6 O5 Er1 -169.07(16) . . . . ? C7 C6 O5 Er1 11.1(3) . . . . ? O14 Er1 O5 C6 -89.61(17) . . . . ? O13 Er1 O5 C6 59.60(18) . . . . ? O1 Er1 O5 C6 177.41(15) . . . . ? O9 Er1 O5 C6 130.64(18) . . . . ? N3 Er1 O5 C6 -13.12(16) . . . . ? N1 Er1 O5 C6 -20.3(2) . . . . ? N5 Er1 O5 C6 -161.94(18) . . . . ? O5 C6 O6 Er2 109.7(2) . . . 2_676 ? C7 C6 O6 Er2 -70.4(3) . . . 2_676 ? O7 C10 O8 Cu1 171.51(17) . . . . ? C9 C10 O8 Cu1 -6.2(2) . . . . ? N4 Cu1 O8 C10 4.19(16) . . . . ? O4 Cu1 O8 C10 176.86(15) . . . . ? O10 C11 O9 Er1 174.16(16) . . . . ? C12 C11 O9 Er1 -4.0(3) . . . . ? O14 Er1 O9 C11 6.5(2) . . . . ? O13 Er1 O9 C11 -175.39(18) . . . . ? O1 Er1 O9 C11 -73.52(17) . . . . ? O5 Er1 O9 C11 84.46(17) . . . . ? N3 Er1 O9 C11 128.73(16) . . . . ? N1 Er1 O9 C11 -118.94(17) . . . . ? N5 Er1 O9 C11 1.40(16) . . . . ? O9 C11 O10 Er2 -111.7(3) . . . . ? C12 C11 O10 Er2 66.4(3) . . . . ? O11 Er2 O10 C11 46.9(3) 1_455 . . . ? O12 Er2 O10 C11 -33.0(3) 2_766 . . . ? O6 Er2 O10 C11 166.0(3) 2_676 . . . ? O2 Er2 O10 C11 -116.5(3) 2_666 . . . ? O16 Er2 O10 C11 -112.8(3) . . . . ? O15 Er2 O10 C11 106.0(3) . . . . ? O12 C15 O11 Er2 -117.9(3) . . . 1_655 ? C14 C15 O11 Er2 67.1(4) . . . 1_655 ? O11 C15 O12 Er2 2.5(4) . . . 2_766 ? C14 C15 O12 Er2 177.59(15) . . . 2_766 ? 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 O17 H17B O9 0.86 2.30 3.077(3) 150.2 . O17 H17B O10 0.86 2.32 3.010(2) 137.9 . O16 H16A O18 0.86 1.90 2.751(2) 167.4 . N6 H6N O3 0.88 2.22 2.908(3) 134.8 2_667 O14 H14A O3 0.86 1.77 2.623(2) 170.5 2_667 O15 H15A O4 0.85 2.06 2.811(2) 146.7 1_554 O13 H13A O18 0.85 2.01 2.822(3) 159.1 2_676 O17 H17A O5 0.86 2.03 2.846(3) 158.7 2_676 O18 H18A O17 0.86 1.84 2.679(3) 163.6 2_676 O18 H18B O6 0.86 2.49 3.324(2) 164.9 2_776 O13 H13B O7 0.86 1.91 2.766(2) 169.7 2_577 O14 H14B O7 0.86 1.85 2.640(2) 150.7 2_677 O15 H15B N6 0.86 2.61 3.458(3) 169.0 2_666 O16 H16B O4 0.86 2.14 2.946(2) 154.5 1_654 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.659 _refine_diff_density_min -0.680 _refine_diff_density_rms 0.124 _database_code_depnum_ccdc_archive 'CCDC 931528' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H12 Cu N6 O16 Y2, 2(H2 O)' _chemical_formula_sum 'C15 H16 Cu N6 O18 Y2' _chemical_formula_weight 809.70 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1476(4) _cell_length_b 11.2218(6) _cell_length_c 15.4597(8) _cell_angle_alpha 82.665(3) _cell_angle_beta 77.383(2) _cell_angle_gamma 84.547(3) _cell_volume 1197.27(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6581 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 798 _exptl_absorpt_coefficient_mu 5.791 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4221 _exptl_absorpt_correction_T_max 0.6544 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18639 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_unetI/netI 0.0390 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4609 _reflns_number_gt 3979 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+0.2919P] 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 4609 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0850 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 Y2 Y 0.51592(4) 0.66326(3) 0.35091(2) 0.00797(10) Uani 1 1 d . . . Y1 Y 0.48124(4) 0.77147(3) 0.75631(2) 0.00829(10) Uani 1 1 d . . . Cu1 Cu 0.19494(6) 0.81213(4) 1.04293(3) 0.01042(12) Uani 1 1 d . . . C1 C 0.3836(5) 0.4919(3) 0.8041(2) 0.0104(7) Uani 1 1 d . . . C2 C 0.3141(5) 0.5340(3) 0.8928(2) 0.0102(7) Uani 1 1 d . . . C3 C 0.2462(5) 0.4745(3) 0.9768(2) 0.0106(7) Uani 1 1 d . . . H3 H 0.2308 0.3910 0.9931 0.013 Uiso 1 1 calc R . . C4 C 0.2059(5) 0.5685(3) 1.0314(2) 0.0097(7) Uani 1 1 d . . . C5 C 0.1260(5) 0.5819(3) 1.1261(2) 0.0092(7) Uani 1 1 d . . . C6 C 0.5665(4) 1.0532(3) 0.7401(2) 0.0100(7) Uani 1 1 d . . . C7 C 0.4555(5) 1.0355(3) 0.8333(2) 0.0092(7) Uani 1 1 d . . . C8 C 0.3723(5) 1.1162(3) 0.8954(2) 0.0113(7) Uani 1 1 d . . . H8 H 0.3761 1.2013 0.8894 0.014 Uiso 1 1 calc R . . C9 C 0.2833(5) 1.0408(3) 0.9677(2) 0.0097(7) Uani 1 1 d . . . C10 C 0.1578(5) 1.0534(3) 1.0569(2) 0.0095(7) Uani 1 1 d . . . C11 C 0.5683(5) 0.7651(3) 0.5411(2) 0.0093(7) Uani 1 1 d . . . C12 C 0.7604(5) 0.7209(3) 0.5587(2) 0.0102(7) Uani 1 1 d . . . C13 C 0.9293(5) 0.6784(3) 0.5035(2) 0.0104(7) Uani 1 1 d . . . H13 H 0.9570 0.6812 0.4403 0.013 Uiso 1 1 calc R . . C14 C 1.0456(5) 0.6316(3) 0.5610(2) 0.0103(7) Uani 1 1 d . . . C15 C 1.2287(5) 0.5543(3) 0.5454(2) 0.0098(7) Uani 1 1 d . . . N1 N 0.3169(4) 0.6539(3) 0.89542(18) 0.0110(6) Uani 1 1 d . . . N2 N 0.2515(4) 0.6731(3) 0.98058(18) 0.0112(6) Uani 1 1 d . . . N3 N 0.4201(4) 0.9209(3) 0.86610(18) 0.0092(6) Uani 1 1 d . . . N4 N 0.3148(4) 0.9258(3) 0.94913(18) 0.0109(6) Uani 1 1 d . . . N5 N 0.7748(4) 0.7052(3) 0.64491(19) 0.0121(6) Uani 1 1 d . . . N6 N 0.9491(4) 0.6497(3) 0.64448(19) 0.0126(6) Uani 1 1 d . . . H6N H 0.9955 0.6275 0.6928 0.015 Uiso 1 1 calc R . . O1 O 0.4565(3) 0.5685(2) 0.74054(15) 0.0132(5) Uani 1 1 d . . . O2 O 0.3690(3) 0.3836(2) 0.79358(15) 0.0126(5) Uani 1 1 d . . . O3 O 0.0873(3) 0.4939(2) 1.18301(16) 0.0151(5) Uani 1 1 d . . . O4 O 0.1035(3) 0.6923(2) 1.14554(15) 0.0127(5) Uani 1 1 d . . . O5 O 0.6109(3) 0.9584(2) 0.70079(16) 0.0146(5) Uani 1 1 d . . . O6 O 0.6132(3) 1.1561(2) 0.70448(15) 0.0109(5) Uani 1 1 d . . . O7 O 0.0986(3) 1.1553(2) 1.08030(16) 0.0128(5) Uani 1 1 d . . . O8 O 0.1099(3) 0.9549(2) 1.10504(15) 0.0126(5) Uani 1 1 d . . . O9 O 0.4416(3) 0.7942(2) 0.60739(15) 0.0118(5) Uani 1 1 d . . . O10 O 0.5404(3) 0.7693(2) 0.46346(16) 0.0132(5) Uani 1 1 d . . . O11 O 1.3275(3) 0.5609(2) 0.46818(15) 0.0130(5) Uani 1 1 d . . . O12 O 1.2616(3) 0.4836(2) 0.61162(15) 0.0118(5) Uani 1 1 d . . . O13 O 0.1626(3) 0.8410(2) 0.75895(16) 0.0177(6) Uani 1 1 d . . . H13A H 0.1504 0.8925 0.7142 0.021 Uiso 1 1 d R . . H13B H 0.0921 0.8374 0.8121 0.021 Uiso 1 1 d R . . O14 O 0.7235(3) 0.7172(2) 0.83320(16) 0.0146(5) Uani 1 1 d . . . H14A H 0.7778 0.6450 0.8339 0.017 Uiso 1 1 d R . . H14B H 0.7460 0.7750 0.8606 0.017 Uiso 1 1 d R . . O15 O 0.2266(3) 0.6318(2) 0.30726(16) 0.0145(5) Uani 1 1 d . . . H15A H 0.2109 0.6765 0.2599 0.017 Uiso 1 1 d R . . H15B H 0.1939 0.5587 0.3241 0.017 Uiso 1 1 d R . . O16 O 0.7972(3) 0.7658(2) 0.29319(15) 0.0146(5) Uani 1 1 d . . . H16A H 0.8234 0.8255 0.3179 0.018 Uiso 1 1 d R . . H16B H 0.8563 0.7427 0.2425 0.018 Uiso 1 1 d R . . O17 O 0.2401(4) 0.9776(3) 0.48470(19) 0.0305(7) Uani 1 1 d . . . H17A H 0.2769 1.0156 0.4326 0.037 Uiso 1 1 d R . . H17B H 0.2852 0.9089 0.5058 0.037 Uiso 1 1 d R . . O18 O 0.9315(4) 0.9551(2) 0.35520(17) 0.0211(6) Uani 1 1 d . . . H18A H 0.8672 0.9632 0.4085 0.025 Uiso 1 1 d R . . H18B H 1.0536 0.9410 0.3382 0.025 Uiso 1 1 d 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 Y2 0.01046(17) 0.00761(19) 0.00484(17) -0.00014(12) -0.00019(12) 0.00040(13) Y1 0.01162(18) 0.00665(19) 0.00544(17) -0.00098(13) 0.00056(13) 0.00016(13) Cu1 0.0169(2) 0.0066(2) 0.0060(2) -0.00110(16) 0.00178(17) -0.00086(17) C1 0.0100(16) 0.012(2) 0.0084(17) -0.0010(14) -0.0010(13) 0.0015(14) C2 0.0133(17) 0.0086(19) 0.0078(17) -0.0006(14) -0.0009(14) 0.0001(14) C3 0.0180(18) 0.0052(18) 0.0082(17) -0.0006(13) -0.0019(14) -0.0002(14) C4 0.0129(17) 0.0094(19) 0.0062(16) 0.0001(13) -0.0018(13) 0.0003(14) C5 0.0110(16) 0.0085(19) 0.0084(17) -0.0007(14) -0.0034(13) 0.0009(13) C6 0.0077(16) 0.011(2) 0.0116(17) -0.0023(14) -0.0031(14) 0.0019(14) C7 0.0092(16) 0.0075(19) 0.0110(17) -0.0002(13) -0.0028(13) 0.0005(13) C8 0.0140(17) 0.0083(19) 0.0117(18) -0.0026(14) -0.0021(14) -0.0005(14) C9 0.0116(17) 0.0083(19) 0.0098(17) -0.0012(13) -0.0044(14) 0.0023(14) C10 0.0086(16) 0.012(2) 0.0101(17) -0.0049(14) -0.0041(13) -0.0004(14) C11 0.0147(17) 0.0044(18) 0.0091(17) 0.0003(13) -0.0036(14) -0.0006(13) C12 0.0129(17) 0.0055(18) 0.0115(17) -0.0011(13) -0.0013(14) 0.0002(13) C13 0.0140(17) 0.0078(19) 0.0092(17) -0.0017(13) -0.0013(14) -0.0010(14) C14 0.0136(17) 0.0084(19) 0.0082(17) 0.0007(14) -0.0007(14) -0.0030(14) C15 0.0091(16) 0.0081(19) 0.0126(18) -0.0022(14) -0.0029(14) 0.0000(13) N1 0.0172(15) 0.0086(16) 0.0060(14) -0.0028(11) 0.0009(12) 0.0004(12) N2 0.0174(15) 0.0078(16) 0.0069(14) -0.0008(11) 0.0010(12) -0.0016(12) N3 0.0133(14) 0.0080(16) 0.0040(14) 0.0001(11) 0.0022(11) 0.0001(12) N4 0.0157(15) 0.0098(16) 0.0066(14) -0.0016(11) -0.0007(12) -0.0004(12) N5 0.0105(14) 0.0152(17) 0.0103(15) -0.0018(12) -0.0025(12) 0.0023(12) N6 0.0111(14) 0.0177(17) 0.0080(14) 0.0002(12) -0.0028(12) 0.0041(12) O1 0.0219(13) 0.0095(14) 0.0066(12) -0.0007(10) 0.0012(10) -0.0026(10) O2 0.0209(13) 0.0074(13) 0.0083(12) -0.0024(9) -0.0001(10) 0.0000(10) O3 0.0232(14) 0.0110(14) 0.0076(12) 0.0023(10) 0.0011(10) 0.0017(11) O4 0.0209(13) 0.0098(14) 0.0056(12) -0.0009(10) 0.0010(10) -0.0011(10) O5 0.0218(13) 0.0109(14) 0.0092(12) -0.0025(10) 0.0020(10) -0.0011(11) O6 0.0147(12) 0.0062(13) 0.0101(12) 0.0015(10) -0.0005(10) -0.0003(10) O7 0.0149(12) 0.0084(13) 0.0143(13) -0.0063(10) 0.0014(10) -0.0001(10) O8 0.0174(13) 0.0103(14) 0.0084(12) -0.0027(10) 0.0021(10) -0.0018(10) O9 0.0121(12) 0.0141(14) 0.0075(12) -0.0020(10) -0.0002(10) 0.0033(10) O10 0.0164(12) 0.0135(14) 0.0104(12) -0.0028(10) -0.0049(10) 0.0029(10) O11 0.0121(12) 0.0163(14) 0.0078(12) 0.0026(10) 0.0014(10) 0.0000(10) O12 0.0141(12) 0.0107(13) 0.0089(12) 0.0016(10) -0.0011(10) 0.0016(10) O13 0.0164(13) 0.0265(16) 0.0067(12) 0.0010(11) 0.0017(10) 0.0027(11) O14 0.0219(13) 0.0059(13) 0.0179(14) -0.0035(10) -0.0085(11) 0.0023(10) O15 0.0202(13) 0.0103(14) 0.0127(13) 0.0050(10) -0.0054(10) -0.0039(10) O16 0.0171(13) 0.0155(14) 0.0111(13) -0.0065(10) 0.0015(10) -0.0044(10) O17 0.0373(17) 0.0257(17) 0.0193(15) 0.0072(12) 0.0010(13) 0.0151(13) O18 0.0178(13) 0.0290(17) 0.0159(14) -0.0038(12) -0.0010(11) -0.0034(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y2 O11 2.262(2) 1_455 ? Y2 O10 2.275(2) . ? Y2 O12 2.289(2) 2_766 ? Y2 O6 2.289(2) 2_676 ? Y2 O2 2.315(2) 2_666 ? Y2 O16 2.357(2) . ? Y2 O15 2.381(2) . ? Y1 O14 2.301(2) . ? Y1 O13 2.330(2) . ? Y1 O1 2.348(2) . ? Y1 O5 2.358(2) . ? Y1 O9 2.360(2) . ? Y1 N3 2.480(3) . ? Y1 N1 2.493(3) . ? Y1 N5 2.524(3) . ? Cu1 N2 1.903(3) . ? Cu1 N4 1.912(3) . ? Cu1 O8 1.953(2) . ? Cu1 O4 1.980(2) . ? C1 O2 1.263(4) . ? C1 O1 1.274(4) . ? C1 C2 1.475(5) . ? C2 N1 1.353(4) . ? C2 C3 1.389(5) . ? C3 C4 1.404(5) . ? C3 H3 0.9500 . ? C4 N2 1.352(4) . ? C4 C5 1.472(5) . ? C5 O3 1.245(4) . ? C5 O4 1.299(4) . ? C6 O6 1.256(4) . ? C6 O5 1.273(4) . ? C6 C7 1.483(5) . ? C7 N3 1.346(4) . ? C7 C8 1.402(5) . ? C8 C9 1.386(5) . ? C8 H8 0.9500 . ? C9 N4 1.346(4) . ? C9 C10 1.487(5) . ? C10 O7 1.251(4) . ? C10 O8 1.281(4) . ? C11 O10 1.253(4) . ? C11 O9 1.265(4) . ? C11 C12 1.485(5) . ? C12 N5 1.347(4) . ? C12 C13 1.399(5) . ? C13 C14 1.370(5) . ? C13 H13 0.9500 . ? C14 N6 1.355(4) . ? C14 C15 1.491(5) . ? C15 O11 1.245(4) . ? C15 O12 1.263(4) . ? N1 N2 1.335(4) . ? N3 N4 1.343(4) . ? N5 N6 1.338(4) . ? N6 H6N 0.8800 . ? O2 Y2 2.315(2) 2_666 ? O6 Y2 2.289(2) 2_676 ? O11 Y2 2.262(2) 1_655 ? O12 Y2 2.289(2) 2_766 ? O13 H13A 0.8574 . ? O13 H13B 0.8639 . ? O14 H14A 0.8639 . ? O14 H14B 0.8642 . ? O15 H15A 0.8552 . ? O15 H15B 0.8661 . ? O16 H16A 0.8666 . ? O16 H16B 0.8640 . ? O17 H17A 0.8605 . ? O17 H17B 0.8591 . ? O18 H18A 0.8630 . ? O18 H18B 0.8604 . ? 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 O11 Y2 O10 79.27(9) 1_455 . ? O11 Y2 O12 80.76(8) 1_455 2_766 ? O10 Y2 O12 91.92(8) . 2_766 ? O11 Y2 O6 116.56(8) 1_455 2_676 ? O10 Y2 O6 83.08(8) . 2_676 ? O12 Y2 O6 160.41(9) 2_766 2_676 ? O11 Y2 O2 130.32(9) 1_455 2_666 ? O10 Y2 O2 148.99(9) . 2_666 ? O12 Y2 O2 85.33(8) 2_766 2_666 ? O6 Y2 O2 89.26(8) 2_676 2_666 ? O11 Y2 O16 148.76(8) 1_455 . ? O10 Y2 O16 76.36(8) . . ? O12 Y2 O16 80.82(8) 2_766 . ? O6 Y2 O16 79.59(8) 2_676 . ? O2 Y2 O16 72.71(8) 2_666 . ? O11 Y2 O15 72.32(8) 1_455 . ? O10 Y2 O15 126.07(8) . . ? O12 Y2 O15 126.06(9) 2_766 . ? O6 Y2 O15 70.83(8) 2_676 . ? O2 Y2 O15 78.46(8) 2_666 . ? O16 Y2 O15 138.58(8) . . ? O14 Y1 O13 148.49(9) . . ? O14 Y1 O1 90.39(8) . . ? O13 Y1 O1 98.65(9) . . ? O14 Y1 O5 91.08(9) . . ? O13 Y1 O5 95.56(9) . . ? O1 Y1 O5 150.11(8) . . ? O14 Y1 O9 138.25(8) . . ? O13 Y1 O9 73.20(8) . . ? O1 Y1 O9 81.14(8) . . ? O5 Y1 O9 78.00(8) . . ? O14 Y1 N3 77.95(9) . . ? O13 Y1 N3 76.91(9) . . ? O1 Y1 N3 143.45(9) . . ? O5 Y1 N3 65.62(9) . . ? O9 Y1 N3 129.68(9) . . ? O14 Y1 N1 76.70(9) . . ? O13 Y1 N1 79.51(9) . . ? O1 Y1 N1 66.22(9) . . ? O5 Y1 N1 142.74(9) . . ? O9 Y1 N1 133.28(9) . . ? N3 Y1 N1 77.37(9) . . ? O14 Y1 N5 72.89(9) . . ? O13 Y1 N5 138.61(9) . . ? O1 Y1 N5 72.53(9) . . ? O5 Y1 N5 79.41(9) . . ? O9 Y1 N5 65.55(8) . . ? N3 Y1 N5 133.51(9) . . ? N1 Y1 N5 127.76(9) . . ? N2 Cu1 N4 97.89(12) . . ? N2 Cu1 O8 174.11(11) . . ? N4 Cu1 O8 83.55(11) . . ? N2 Cu1 O4 82.74(11) . . ? N4 Cu1 O4 172.36(11) . . ? O8 Cu1 O4 96.60(10) . . ? O2 C1 O1 122.7(3) . . ? O2 C1 C2 119.9(3) . . ? O1 C1 C2 117.4(3) . . ? N1 C2 C3 111.8(3) . . ? N1 C2 C1 115.5(3) . . ? C3 C2 C1 132.7(3) . . ? C2 C3 C4 102.8(3) . . ? C2 C3 H3 128.6 . . ? C4 C3 H3 128.6 . . ? N2 C4 C3 108.8(3) . . ? N2 C4 C5 114.1(3) . . ? C3 C4 C5 137.1(3) . . ? O3 C5 O4 122.9(3) . . ? O3 C5 C4 122.4(3) . . ? O4 C5 C4 114.7(3) . . ? O6 C6 O5 123.5(3) . . ? O6 C6 C7 120.9(3) . . ? O5 C6 C7 115.6(3) . . ? N3 C7 C8 111.6(3) . . ? N3 C7 C6 115.9(3) . . ? C8 C7 C6 132.5(3) . . ? C9 C8 C7 102.6(3) . . ? C9 C8 H8 128.7 . . ? C7 C8 H8 128.7 . . ? N4 C9 C8 109.7(3) . . ? N4 C9 C10 112.8(3) . . ? C8 C9 C10 137.5(3) . . ? O7 C10 O8 123.3(3) . . ? O7 C10 C9 120.5(3) . . ? O8 C10 C9 116.1(3) . . ? O10 C11 O9 124.3(3) . . ? O10 C11 C12 119.0(3) . . ? O9 C11 C12 116.6(3) . . ? N5 C12 C13 111.3(3) . . ? N5 C12 C11 116.1(3) . . ? C13 C12 C11 132.2(3) . . ? C14 C13 C12 104.5(3) . . ? C14 C13 H13 127.8 . . ? C12 C13 H13 127.8 . . ? N6 C14 C13 107.4(3) . . ? N6 C14 C15 121.3(3) . . ? C13 C14 C15 130.4(3) . . ? O11 C15 O12 126.7(3) . . ? O11 C15 C14 117.2(3) . . ? O12 C15 C14 116.0(3) . . ? N2 N1 C2 106.2(3) . . ? N2 N1 Y1 136.4(2) . . ? C2 N1 Y1 116.5(2) . . ? N1 N2 C4 110.4(3) . . ? N1 N2 Cu1 134.8(2) . . ? C4 N2 Cu1 114.6(2) . . ? N4 N3 C7 106.1(3) . . ? N4 N3 Y1 135.1(2) . . ? C7 N3 Y1 116.4(2) . . ? N3 N4 C9 110.0(3) . . ? N3 N4 Cu1 135.9(2) . . ? C9 N4 Cu1 114.0(2) . . ? N6 N5 C12 104.7(3) . . ? N6 N5 Y1 138.8(2) . . ? C12 N5 Y1 116.3(2) . . ? N5 N6 C14 112.0(3) . . ? N5 N6 H6N 124.0 . . ? C14 N6 H6N 124.0 . . ? C1 O1 Y1 123.9(2) . . ? C1 O2 Y2 114.4(2) . 2_666 ? C5 O4 Cu1 113.8(2) . . ? C6 O5 Y1 124.0(2) . . ? C6 O6 Y2 141.4(2) . 2_676 ? C10 O8 Cu1 113.3(2) . . ? C11 O9 Y1 125.2(2) . . ? C11 O10 Y2 146.6(2) . . ? C15 O11 Y2 151.1(2) . 1_655 ? C15 O12 Y2 140.5(2) . 2_766 ? Y1 O13 H13A 112.6 . . ? Y1 O13 H13B 113.1 . . ? H13A O13 H13B 127.6 . . ? Y1 O14 H14A 120.3 . . ? Y1 O14 H14B 112.2 . . ? H14A O14 H14B 127.4 . . ? Y2 O15 H15A 112.9 . . ? Y2 O15 H15B 111.1 . . ? H15A O15 H15B 127.8 . . ? Y2 O16 H16A 121.5 . . ? Y2 O16 H16B 111.1 . . ? H16A O16 H16B 126.8 . . ? H17A O17 H17B 127.9 . . ? H18A O18 H18B 127.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 N1 -173.2(3) . . . . ? O1 C1 C2 N1 6.7(4) . . . . ? O2 C1 C2 C3 7.6(6) . . . . ? O1 C1 C2 C3 -172.6(4) . . . . ? N1 C2 C3 C4 0.4(4) . . . . ? C1 C2 C3 C4 179.7(3) . . . . ? C2 C3 C4 N2 -0.8(4) . . . . ? C2 C3 C4 C5 177.7(4) . . . . ? N2 C4 C5 O3 -175.5(3) . . . . ? C3 C4 C5 O3 6.0(6) . . . . ? N2 C4 C5 O4 2.9(4) . . . . ? C3 C4 C5 O4 -175.5(4) . . . . ? O6 C6 C7 N3 -177.3(3) . . . . ? O5 C6 C7 N3 2.1(4) . . . . ? O6 C6 C7 C8 4.9(5) . . . . ? O5 C6 C7 C8 -175.7(3) . . . . ? N3 C7 C8 C9 -0.4(4) . . . . ? C6 C7 C8 C9 177.5(3) . . . . ? C7 C8 C9 N4 0.7(4) . . . . ? C7 C8 C9 C10 -175.9(4) . . . . ? N4 C9 C10 O7 -172.5(3) . . . . ? C8 C9 C10 O7 4.0(6) . . . . ? N4 C9 C10 O8 4.8(4) . . . . ? C8 C9 C10 O8 -178.7(4) . . . . ? O10 C11 C12 N5 -172.5(3) . . . . ? O9 C11 C12 N5 6.2(5) . . . . ? O10 C11 C12 C13 -1.0(6) . . . . ? O9 C11 C12 C13 177.8(4) . . . . ? N5 C12 C13 C14 2.1(4) . . . . ? C11 C12 C13 C14 -169.7(4) . . . . ? C12 C13 C14 N6 -1.5(4) . . . . ? C12 C13 C14 C15 167.8(3) . . . . ? N6 C14 C15 O11 -166.2(3) . . . . ? C13 C14 C15 O11 25.8(5) . . . . ? N6 C14 C15 O12 17.7(5) . . . . ? C13 C14 C15 O12 -150.3(4) . . . . ? C3 C2 N1 N2 0.1(4) . . . . ? C1 C2 N1 N2 -179.3(3) . . . . ? C3 C2 N1 Y1 170.8(2) . . . . ? C1 C2 N1 Y1 -8.6(4) . . . . ? O14 Y1 N1 N2 76.5(3) . . . . ? O13 Y1 N1 N2 -82.7(3) . . . . ? O1 Y1 N1 N2 172.9(3) . . . . ? O5 Y1 N1 N2 2.7(4) . . . . ? O9 Y1 N1 N2 -137.4(3) . . . . ? N3 Y1 N1 N2 -3.9(3) . . . . ? N5 Y1 N1 N2 132.1(3) . . . . ? O14 Y1 N1 C2 -90.5(2) . . . . ? O13 Y1 N1 C2 110.3(2) . . . . ? O1 Y1 N1 C2 5.9(2) . . . . ? O5 Y1 N1 C2 -164.3(2) . . . . ? O9 Y1 N1 C2 55.6(3) . . . . ? N3 Y1 N1 C2 -170.9(2) . . . . ? N5 Y1 N1 C2 -35.0(3) . . . . ? C2 N1 N2 C4 -0.6(4) . . . . ? Y1 N1 N2 C4 -168.5(2) . . . . ? C2 N1 N2 Cu1 -175.9(2) . . . . ? Y1 N1 N2 Cu1 16.2(5) . . . . ? C3 C4 N2 N1 0.9(4) . . . . ? C5 C4 N2 N1 -178.0(3) . . . . ? C3 C4 N2 Cu1 177.2(2) . . . . ? C5 C4 N2 Cu1 -1.7(4) . . . . ? N4 Cu1 N2 N1 -12.3(3) . . . . ? O4 Cu1 N2 N1 175.3(3) . . . . ? N4 Cu1 N2 C4 172.5(2) . . . . ? O4 Cu1 N2 C4 0.2(2) . . . . ? C8 C7 N3 N4 -0.1(4) . . . . ? C6 C7 N3 N4 -178.3(3) . . . . ? C8 C7 N3 Y1 165.0(2) . . . . ? C6 C7 N3 Y1 -13.2(3) . . . . ? O14 Y1 N3 N4 -90.5(3) . . . . ? O13 Y1 N3 N4 70.4(3) . . . . ? O1 Y1 N3 N4 -16.5(4) . . . . ? O5 Y1 N3 N4 172.8(3) . . . . ? O9 Y1 N3 N4 125.0(3) . . . . ? N1 Y1 N3 N4 -11.6(3) . . . . ? N5 Y1 N3 N4 -142.3(3) . . . . ? O14 Y1 N3 C7 110.0(2) . . . . ? O13 Y1 N3 C7 -89.1(2) . . . . ? O1 Y1 N3 C7 -176.0(2) . . . . ? O5 Y1 N3 C7 13.3(2) . . . . ? O9 Y1 N3 C7 -34.5(3) . . . . ? N1 Y1 N3 C7 -171.1(2) . . . . ? N5 Y1 N3 C7 58.2(3) . . . . ? C7 N3 N4 C9 0.5(3) . . . . ? Y1 N3 N4 C9 -160.4(2) . . . . ? C7 N3 N4 Cu1 177.9(3) . . . . ? Y1 N3 N4 Cu1 17.0(5) . . . . ? C8 C9 N4 N3 -0.8(4) . . . . ? C10 C9 N4 N3 176.7(3) . . . . ? C8 C9 N4 Cu1 -178.8(2) . . . . ? C10 C9 N4 Cu1 -1.3(3) . . . . ? N2 Cu1 N4 N3 -4.3(3) . . . . ? O8 Cu1 N4 N3 -178.6(3) . . . . ? N2 Cu1 N4 C9 173.0(2) . . . . ? O8 Cu1 N4 C9 -1.3(2) . . . . ? C13 C12 N5 N6 -1.9(4) . . . . ? C11 C12 N5 N6 171.4(3) . . . . ? C13 C12 N5 Y1 -178.5(2) . . . . ? C11 C12 N5 Y1 -5.2(4) . . . . ? O14 Y1 N5 N6 11.4(3) . . . . ? O13 Y1 N5 N6 -167.7(3) . . . . ? O1 Y1 N5 N6 -84.6(3) . . . . ? O5 Y1 N5 N6 105.9(3) . . . . ? O9 Y1 N5 N6 -172.6(4) . . . . ? N3 Y1 N5 N6 65.0(4) . . . . ? N1 Y1 N5 N6 -45.7(4) . . . . ? O14 Y1 N5 C12 -173.6(3) . . . . ? O13 Y1 N5 C12 7.3(3) . . . . ? O1 Y1 N5 C12 90.4(2) . . . . ? O5 Y1 N5 C12 -79.1(2) . . . . ? O9 Y1 N5 C12 2.4(2) . . . . ? N3 Y1 N5 C12 -120.0(2) . . . . ? N1 Y1 N5 C12 129.3(2) . . . . ? C12 N5 N6 C14 0.9(4) . . . . ? Y1 N5 N6 C14 176.3(3) . . . . ? C13 C14 N6 N5 0.4(4) . . . . ? C15 C14 N6 N5 -170.0(3) . . . . ? O2 C1 O1 Y1 178.8(2) . . . . ? C2 C1 O1 Y1 -1.1(4) . . . . ? O14 Y1 O1 C1 72.8(3) . . . . ? O13 Y1 O1 C1 -76.9(3) . . . . ? O5 Y1 O1 C1 165.7(2) . . . . ? O9 Y1 O1 C1 -148.2(3) . . . . ? N3 Y1 O1 C1 2.8(3) . . . . ? N1 Y1 O1 C1 -2.4(2) . . . . ? N5 Y1 O1 C1 144.7(3) . . . . ? O1 C1 O2 Y2 -0.4(4) . . . 2_666 ? C2 C1 O2 Y2 179.5(2) . . . 2_666 ? O3 C5 O4 Cu1 175.7(3) . . . . ? C4 C5 O4 Cu1 -2.7(3) . . . . ? N2 Cu1 O4 C5 1.5(2) . . . . ? O8 Cu1 O4 C5 175.6(2) . . . . ? O6 C6 O5 Y1 -169.0(2) . . . . ? C7 C6 O5 Y1 11.7(4) . . . . ? O14 Y1 O5 C6 -89.7(2) . . . . ? O13 Y1 O5 C6 59.5(2) . . . . ? O1 Y1 O5 C6 177.6(2) . . . . ? O9 Y1 O5 C6 130.9(3) . . . . ? N3 Y1 O5 C6 -13.5(2) . . . . ? N1 Y1 O5 C6 -20.5(3) . . . . ? N5 Y1 O5 C6 -162.1(3) . . . . ? O5 C6 O6 Y2 109.0(4) . . . 2_676 ? C7 C6 O6 Y2 -71.6(4) . . . 2_676 ? O7 C10 O8 Cu1 171.4(2) . . . . ? C9 C10 O8 Cu1 -5.8(4) . . . . ? N4 Cu1 O8 C10 4.0(2) . . . . ? O4 Cu1 O8 C10 176.4(2) . . . . ? O10 C11 O9 Y1 174.4(2) . . . . ? C12 C11 O9 Y1 -4.3(4) . . . . ? O14 Y1 O9 C11 6.9(3) . . . . ? O13 Y1 O9 C11 -175.5(3) . . . . ? O1 Y1 O9 C11 -73.6(3) . . . . ? O5 Y1 O9 C11 84.9(3) . . . . ? N3 Y1 O9 C11 128.4(3) . . . . ? N1 Y1 O9 C11 -118.6(3) . . . . ? N5 Y1 O9 C11 1.2(3) . . . . ? O9 C11 O10 Y2 -111.7(4) . . . . ? C12 C11 O10 Y2 67.0(5) . . . . ? O11 Y2 O10 C11 47.0(4) 1_455 . . . ? O12 Y2 O10 C11 -33.2(4) 2_766 . . . ? O6 Y2 O10 C11 165.8(4) 2_676 . . . ? O2 Y2 O10 C11 -117.3(4) 2_666 . . . ? O16 Y2 O10 C11 -113.3(4) . . . . ? O15 Y2 O10 C11 105.7(4) . . . . ? O12 C15 O11 Y2 -116.3(4) . . . 1_655 ? C14 C15 O11 Y2 68.0(5) . . . 1_655 ? O11 C15 O12 Y2 2.1(6) . . . 2_766 ? C14 C15 O12 Y2 177.8(2) . . . 2_766 ? 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 O17 H17B O9 0.86 2.31 3.089(4) 150.3 . O17 H17B O10 0.86 2.33 3.018(4) 137.9 . O16 H16A O18 0.87 1.91 2.768(3) 168.0 . N6 H6N O3 0.88 2.21 2.908(4) 136.0 2_667 O14 H14A O3 0.86 1.77 2.626(3) 170.1 2_667 O15 H15A O4 0.86 2.06 2.810(3) 146.5 1_554 O13 H13A O18 0.86 2.01 2.827(4) 159.6 2_676 O17 H17A O5 0.86 2.04 2.856(4) 158.7 2_676 O18 H18A O17 0.86 1.84 2.679(4) 163.7 2_676 O18 H18B O6 0.86 2.51 3.348(3) 165.0 2_776 O13 H13B O7 0.86 1.91 2.765(3) 169.7 2_577 O14 H14B O7 0.86 1.86 2.652(3) 150.9 2_677 O15 H15B N6 0.87 2.59 3.443(4) 169.4 2_666 O16 H16B O4 0.86 2.14 2.939(3) 154.6 1_654 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.029 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.118 _database_code_depnum_ccdc_archive 'CCDC 931529' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 Cu3 Eu4 N12 O32' _chemical_formula_sum 'C30 H22 Cu3 Eu4 N12 O32' _chemical_formula_weight 1861.06 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9914(5) _cell_length_b 17.1874(10) _cell_length_c 19.9307(13) _cell_angle_alpha 66.266(3) _cell_angle_beta 84.632(4) _cell_angle_gamma 81.115(4) _cell_volume 2164.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2528 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 25.77 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.855 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1762 _exptl_absorpt_coefficient_mu 7.278 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7595 _exptl_absorpt_correction_T_max 0.8681 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46814 _diffrn_reflns_av_R_equivalents 0.1350 _diffrn_reflns_av_unetI/netI 0.1609 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 30.03 _reflns_number_total 12551 _reflns_number_gt 7367 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. 252 Least-Squares Restraints were used to achieve the better atomic ellipsoid shape and good refinement effect as follows: ISOR 0.001 N1 N5 N11 N4 C18 C17 C16 C26 C27 C23 O23 O9 C28 C7 C6 N12 ISOR 0.005 C12 C11 C21 O16 N6 N12 N9 N2 O24 O29 O17 ISOR 0.007 C14 C10 O10 O3 C25 C1 O12 N8 C30 ISOR 0.01 O13 O14 O16 N3 O31 O32 ; _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^)+(0.0081P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12551 _refine_ls_number_parameters 730 _refine_ls_number_restraints 252 _refine_ls_R_factor_all 0.1249 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.965 _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 Eu1 Eu 0.75835(8) 0.10226(3) 0.29890(2) 0.00653(11) Uani 1 1 d . . . Eu2 Eu 0.18735(8) 0.44625(3) 0.11088(2) 0.00577(11) Uani 1 1 d . . . Eu3 Eu 0.41476(8) 0.21301(3) 0.09135(2) 0.00653(11) Uani 1 1 d . . . Eu4 Eu 0.40617(8) 0.27175(3) -0.39791(3) 0.00848(11) Uani 1 1 d . . . Cu1 Cu 0.75335(19) 0.15589(7) 0.50785(6) 0.0092(3) Uani 1 1 d . . . Cu2 Cu 0.15790(19) 0.54582(7) 0.29130(6) 0.0088(3) Uani 1 1 d . . . Cu3 Cu 0.55330(19) 0.12638(7) -0.09579(6) 0.0093(3) Uani 1 1 d . . . C1 C 0.8439(14) -0.0032(5) 0.6185(5) 0.0049(18) Uani 1 1 d U . . C2 C 0.7894(14) -0.0197(5) 0.5556(5) 0.007(2) Uani 1 1 d . . . C3 C 0.7640(15) -0.0902(6) 0.5401(5) 0.011(2) Uani 1 1 d . . . H3 H 0.7789 -0.1492 0.5718 0.013 Uiso 1 1 calc R . . C4 C 0.7125(15) -0.0530(6) 0.4682(5) 0.012(2) Uani 1 1 d . . . C5 C 0.6500(14) -0.0866(6) 0.4168(5) 0.008(2) Uani 1 1 d . . . C6 C 0.7671(14) 0.3288(6) 0.4622(5) 0.0088(19) Uani 1 1 d U . . C7 C 0.7943(14) 0.3109(5) 0.3956(5) 0.0053(18) Uani 1 1 d U . . C8 C 0.8347(13) 0.3555(5) 0.3209(4) 0.0044(18) Uani 1 1 d . . . H8 H 0.8527 0.4142 0.2959 0.005 Uiso 1 1 calc R . . C9 C 0.8423(15) 0.2940(5) 0.2917(5) 0.009(2) Uani 1 1 d . . . C10 C 0.8892(15) 0.2976(6) 0.2170(5) 0.011(2) Uani 1 1 d U . . C11 C 0.2959(15) 0.4085(6) 0.4157(5) 0.010(2) Uani 1 1 d U . . C12 C 0.2975(15) 0.3748(6) 0.3589(5) 0.011(2) Uani 1 1 d U . . C13 C 0.3571(15) 0.2964(6) 0.3552(5) 0.012(2) Uani 1 1 d . . . H13 H 0.4065 0.2443 0.3932 0.014 Uiso 1 1 calc R . . C14 C 0.3284(14) 0.3113(5) 0.2834(5) 0.009(2) Uani 1 1 d U . . C15 C 0.3738(14) 0.2540(6) 0.2447(5) 0.009(2) Uani 1 1 d . . . C16 C 0.0982(14) 0.7234(5) 0.2227(5) 0.0072(19) Uani 1 1 d U . . C17 C 0.1342(14) 0.6926(6) 0.1627(5) 0.0089(19) Uani 1 1 d U . . C18 C 0.1671(13) 0.7258(5) 0.0869(5) 0.0042(17) Uani 1 1 d U . . H18 H 0.1636 0.7843 0.0544 0.005 Uiso 1 1 calc R . . C19 C 0.2061(14) 0.6540(5) 0.0695(5) 0.008(2) Uani 1 1 d . . . C20 C 0.2729(15) 0.6446(6) 0.0017(5) 0.011(2) Uani 1 1 d . . . C21 C 0.7657(14) 0.0585(6) 0.1752(5) 0.0068(19) Uani 1 1 d U . . C22 C 0.7400(15) 0.0390(6) 0.1115(5) 0.008(2) Uani 1 1 d . . . C23 C 0.8189(14) -0.0269(5) 0.0892(5) 0.0065(18) Uani 1 1 d U . . H23 H 0.9007 -0.0779 0.1157 0.008 Uiso 1 1 calc R . . C24 C 0.7504(14) -0.0006(5) 0.0200(5) 0.007(2) Uani 1 1 d . . . C25 C 0.7715(14) -0.0339(6) -0.0390(5) 0.0072(19) Uani 1 1 d U . . C26 C 0.2156(14) 0.4008(5) -0.0371(5) 0.0036(17) Uani 1 1 d U . . C27 C 0.2883(14) 0.3484(6) -0.0804(5) 0.0078(19) Uani 1 1 d U . . C28 C 0.2819(14) 0.3680(6) -0.1555(5) 0.0084(19) Uani 1 1 d U . . H28 H 0.2339 0.4206 -0.1933 0.010 Uiso 1 1 calc R . . C29 C 0.3638(14) 0.2911(6) -0.1610(5) 0.009(2) Uani 1 1 d . . . C30 C 0.4095(14) 0.2604(5) -0.2206(5) 0.009(2) Uani 1 1 d U . . N1 N 0.7632(11) 0.0511(4) 0.4942(4) 0.0045(15) Uani 1 1 d U . . N2 N 0.7177(12) 0.0326(4) 0.4391(4) 0.0086(17) Uani 1 1 d U . . N3 N 0.7794(12) 0.2288(5) 0.4075(4) 0.0108(18) Uani 1 1 d U . . N4 N 0.8055(11) 0.2164(4) 0.3453(4) 0.0041(15) Uani 1 1 d U . . N5 N 0.2403(12) 0.4327(5) 0.2927(4) 0.0079(16) Uani 1 1 d U . . N6 N 0.2593(12) 0.3949(4) 0.2448(4) 0.0073(17) Uani 1 1 d U . . N7 N 0.1574(12) 0.6045(5) 0.1876(4) 0.0091(17) Uani 1 1 d . . . N8 N 0.2008(12) 0.5813(4) 0.1304(4) 0.0080(17) Uani 1 1 d U . . N9 N 0.6306(12) 0.1013(4) 0.0574(4) 0.0093(17) Uani 1 1 d U . . N10 N 0.6392(12) 0.0754(5) 0.0017(4) 0.0107(18) Uani 1 1 d . . . N11 N 0.3672(11) 0.2661(4) -0.0441(4) 0.0041(15) Uani 1 1 d U . . N12 N 0.4149(12) 0.2320(4) -0.0942(4) 0.0078(16) Uani 1 1 d U . . O1 O 0.8274(10) 0.0758(4) 0.6084(3) 0.0112(15) Uani 1 1 d . . . O2 O 0.9120(10) -0.0629(4) 0.6748(3) 0.0079(14) Uani 1 1 d . . . O3 O 0.6381(10) -0.0365(4) 0.3506(3) 0.0093(15) Uani 1 1 d U . . O4 O 0.6003(10) -0.1620(4) 0.4435(3) 0.0125(16) Uani 1 1 d . . . O5 O 0.7188(10) 0.2659(4) 0.5216(3) 0.0102(15) Uani 1 1 d . . . O6 O 0.7802(12) 0.4014(4) 0.4601(4) 0.024(2) Uani 1 1 d . . . O7 O 0.8816(10) 0.2284(4) 0.2087(3) 0.0083(14) Uani 1 1 d . . . O8 O 0.9336(10) 0.3649(4) 0.1681(3) 0.0080(14) Uani 1 1 d . . . O9 O 0.2385(10) 0.4897(4) 0.3962(3) 0.0112(14) Uani 1 1 d U . . O10 O 0.3417(10) 0.3599(4) 0.4796(3) 0.0125(15) Uani 1 1 d U . . O11 O 0.3319(10) 0.2819(4) 0.1767(3) 0.0069(14) Uani 1 1 d . . . O12 O 0.4502(10) 0.1782(4) 0.2818(3) 0.0110(15) Uani 1 1 d U . . O13 O 0.1212(10) 0.6641(4) 0.2880(3) 0.0097(15) Uani 1 1 d U . . O14 O 0.0480(11) 0.7997(4) 0.2097(3) 0.0158(17) Uani 1 1 d U . . O15 O 0.2738(10) 0.5684(4) 0.0021(3) 0.0106(15) Uani 1 1 d . . . O16 O 0.3342(9) 0.7047(4) -0.0517(3) 0.0068(14) Uani 1 1 d U . . O17 O 0.6660(10) 0.1278(4) 0.1760(3) 0.0090(14) Uani 1 1 d U . . O18 O 0.8778(11) 0.0133(4) 0.2253(3) 0.0125(16) Uani 1 1 d . . . O19 O 0.6998(10) 0.0216(4) -0.1015(3) 0.0096(14) Uani 1 1 d . . . O20 O 0.8571(11) -0.1051(4) -0.0303(3) 0.0151(16) Uani 1 1 d . . . O21 O 0.2695(10) 0.3727(4) 0.0288(3) 0.0102(15) Uani 1 1 d . . . O22 O 0.1089(9) 0.4693(4) -0.0671(3) 0.0068(14) Uani 1 1 d . . . O23 O 0.4956(10) 0.1827(4) -0.1999(3) 0.0109(14) Uani 1 1 d U . . O24 O 0.3713(10) 0.3047(4) -0.2860(3) 0.0085(14) Uani 1 1 d U . . O25 O -0.1558(10) 0.5333(4) 0.3248(3) 0.0130(16) Uani 1 1 d . . . H25A H -0.1553 0.4959 0.3683 0.016 Uiso 1 1 d R . . H25B H -0.2021 0.5840 0.3174 0.016 Uiso 1 1 d R . . O26 O 0.5286(10) 0.4416(4) 0.1146(3) 0.0147(16) Uani 1 1 d . . . H26A H 0.5580 0.4923 0.0944 0.018 Uiso 1 1 d R . . H26C H 0.5862 0.4120 0.0915 0.018 Uiso 1 1 d R . . O27 O 0.3084(10) 0.0766(4) 0.1817(3) 0.0161(17) Uani 1 1 d . . . H27A H 0.2375 0.0690 0.2161 0.019 Uiso 1 1 d R . . H27B H 0.2697 0.0463 0.1579 0.019 Uiso 1 1 d R . . O28 O 0.0724(10) 0.2278(4) 0.0826(3) 0.0132(16) Uani 1 1 d . . . H28C H 0.0155 0.2250 0.1230 0.016 Uiso 1 1 d R . . H28A H 0.0519 0.1862 0.0726 0.016 Uiso 1 1 d R . . O29 O 0.6602(11) 0.1781(4) -0.3238(4) 0.0204(17) Uani 1 1 d U . . H29A H 0.6446 0.1652 -0.2785 0.025 Uiso 1 1 d R . . H29B H 0.7386 0.1415 -0.3341 0.025 Uiso 1 1 d R . . O30 O 0.2069(11) 0.1720(4) -0.3120(3) 0.0168(17) Uani 1 1 d . . . H30A H 0.2148 0.1204 -0.3066 0.020 Uiso 1 1 d R . . H30B H 0.1424 0.1870 -0.2813 0.020 Uiso 1 1 d R . . O31 O 0.0857(11) 0.3423(4) -0.4072(4) 0.0235(18) Uani 1 1 d U . . H31A H 0.0311 0.3796 -0.4447 0.028 Uiso 1 1 d R . . H31B H 0.0106 0.3391 -0.3709 0.028 Uiso 1 1 d R . . O32 O 0.5433(11) 0.4003(4) -0.4226(4) 0.0229(19) Uani 1 1 d U . . H32A H 0.6108 0.4149 -0.4623 0.028 Uiso 1 1 d R . . H32B H 0.5991 0.4259 -0.4029 0.028 Uiso 1 1 d 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 Eu1 0.0083(3) 0.0051(2) 0.0059(2) -0.00184(18) -0.0007(2) -0.00072(19) Eu2 0.0068(3) 0.0047(2) 0.0054(2) -0.00179(18) 0.00046(19) -0.00061(19) Eu3 0.0079(3) 0.0054(2) 0.0055(2) -0.00173(18) -0.00016(19) 0.00039(19) Eu4 0.0132(3) 0.0066(2) 0.0054(2) -0.00245(19) -0.0005(2) -0.0006(2) Cu1 0.0155(8) 0.0060(5) 0.0054(6) -0.0013(5) -0.0007(5) -0.0016(5) Cu2 0.0131(7) 0.0062(5) 0.0066(6) -0.0024(5) -0.0009(5) 0.0004(5) Cu3 0.0131(7) 0.0081(6) 0.0068(6) -0.0038(5) -0.0009(5) 0.0005(5) C1 0.002(4) 0.009(4) 0.003(4) -0.003(3) 0.001(3) -0.002(3) C2 0.010(6) 0.004(4) 0.005(4) -0.001(4) 0.001(4) -0.002(4) C3 0.016(6) 0.008(5) 0.005(5) 0.000(4) 0.000(4) -0.002(4) C4 0.008(6) 0.016(5) 0.012(5) -0.006(4) 0.005(4) -0.005(4) C5 0.004(5) 0.008(5) 0.010(5) -0.003(4) 0.004(4) -0.002(4) C6 0.009(2) 0.009(2) 0.009(2) -0.0036(12) -0.0005(10) -0.0005(10) C7 0.005(2) 0.005(2) 0.005(2) -0.0023(11) 0.0002(10) -0.0006(10) C8 0.006(5) 0.004(4) 0.003(4) 0.000(3) 0.000(4) -0.001(4) C9 0.013(6) 0.007(4) 0.006(4) -0.002(4) 0.004(4) -0.006(4) C10 0.004(4) 0.014(4) 0.013(4) -0.003(3) -0.002(3) 0.001(3) C11 0.006(4) 0.008(3) 0.014(4) -0.003(3) 0.000(3) -0.001(3) C12 0.013(4) 0.015(4) 0.011(4) -0.010(3) -0.004(3) -0.002(3) C13 0.012(6) 0.016(5) 0.008(5) -0.004(4) -0.002(4) -0.004(4) C14 0.010(5) 0.007(4) 0.011(4) -0.003(3) -0.001(3) -0.006(3) C15 0.008(6) 0.007(5) 0.010(5) -0.003(4) 0.003(4) 0.000(4) C16 0.007(2) 0.007(2) 0.007(2) -0.0024(12) -0.0006(10) -0.0011(10) C17 0.009(2) 0.008(2) 0.009(2) -0.0037(12) 0.0001(10) -0.0015(10) C18 0.004(2) 0.0039(19) 0.004(2) -0.0012(11) -0.0002(10) -0.0003(10) C19 0.007(5) 0.008(4) 0.008(5) -0.003(4) 0.003(4) -0.004(4) C20 0.012(6) 0.011(5) 0.008(5) 0.000(4) -0.005(4) -0.003(4) C21 0.006(4) 0.008(3) 0.005(3) 0.000(3) 0.002(3) -0.004(3) C22 0.009(6) 0.009(5) 0.006(5) -0.001(4) 0.003(4) -0.004(4) C23 0.007(2) 0.006(2) 0.006(2) -0.0028(12) 0.0004(10) -0.0002(10) C24 0.007(6) 0.004(4) 0.009(5) -0.001(4) 0.003(4) -0.003(4) C25 0.007(4) 0.011(4) 0.007(4) -0.007(3) 0.002(3) -0.003(3) C26 0.003(2) 0.0040(19) 0.0035(19) -0.0011(11) -0.0007(10) -0.0004(10) C27 0.007(2) 0.008(2) 0.008(2) -0.0029(12) 0.0001(10) -0.0007(10) C28 0.008(2) 0.008(2) 0.009(2) -0.0027(12) -0.0002(10) -0.0017(10) C29 0.004(5) 0.008(5) 0.014(5) -0.005(4) 0.002(4) 0.000(4) C30 0.005(4) 0.004(4) 0.012(4) 0.002(3) 0.000(3) 0.000(3) N1 0.0042(18) 0.0047(17) 0.0046(17) -0.0019(11) -0.0004(10) -0.0005(10) N2 0.011(4) 0.007(3) 0.007(3) -0.002(3) 0.005(3) -0.006(3) N3 0.012(5) 0.014(4) 0.012(4) -0.008(3) -0.002(3) -0.006(3) N4 0.0033(18) 0.0045(17) 0.0041(17) -0.0009(11) -0.0004(10) -0.0013(10) N5 0.0078(19) 0.0079(18) 0.0080(18) -0.0033(11) -0.0005(10) 0.0000(10) N6 0.010(4) 0.004(3) 0.009(3) -0.004(3) -0.004(3) 0.003(3) N7 0.010(5) 0.008(4) 0.009(4) -0.005(3) 0.004(3) 0.001(3) N8 0.013(4) 0.003(3) 0.006(3) 0.001(3) 0.001(3) -0.002(3) N9 0.016(4) 0.005(3) 0.006(3) 0.000(3) 0.001(3) -0.003(3) N10 0.015(5) 0.012(4) 0.006(4) -0.005(3) 0.000(4) -0.002(4) N11 0.0040(18) 0.0041(17) 0.0038(17) -0.0012(11) -0.0003(10) -0.0005(10) N12 0.0078(19) 0.0078(18) 0.0074(18) -0.0030(11) 0.0001(9) -0.0002(10) O1 0.015(4) 0.006(3) 0.013(3) -0.004(3) 0.002(3) -0.003(3) O2 0.006(4) 0.009(3) 0.007(3) -0.001(3) -0.002(3) -0.001(3) O3 0.013(4) 0.009(3) 0.004(3) 0.001(2) 0.001(3) -0.007(3) O4 0.014(4) 0.010(3) 0.016(4) -0.007(3) 0.003(3) -0.006(3) O5 0.016(4) 0.008(3) 0.007(3) -0.003(3) -0.004(3) -0.001(3) O6 0.038(6) 0.016(4) 0.024(4) -0.016(3) 0.013(4) -0.012(4) O7 0.009(4) 0.010(3) 0.007(3) -0.004(3) 0.003(3) -0.004(3) O8 0.011(4) 0.003(3) 0.008(3) 0.000(3) 0.000(3) -0.003(3) O9 0.0118(17) 0.0112(16) 0.0107(17) -0.0044(10) -0.0014(10) -0.0009(10) O10 0.015(4) 0.018(3) 0.006(3) -0.007(3) -0.003(3) -0.001(3) O11 0.008(4) 0.010(3) 0.004(3) -0.004(3) 0.001(3) 0.000(3) O12 0.018(4) 0.004(3) 0.011(3) -0.003(2) -0.006(3) 0.003(3) O13 0.019(4) 0.004(3) 0.004(3) -0.001(2) 0.003(3) 0.002(3) O14 0.029(5) 0.006(3) 0.014(3) -0.006(3) 0.004(3) -0.002(3) O15 0.008(4) 0.013(3) 0.008(3) -0.001(3) -0.001(3) -0.004(3) O16 0.007(3) 0.002(2) 0.008(3) 0.000(2) 0.004(2) 0.001(2) O17 0.012(3) 0.007(3) 0.011(3) -0.006(2) 0.003(2) -0.002(2) O18 0.022(5) 0.009(3) 0.006(3) -0.004(3) -0.006(3) 0.003(3) O19 0.007(4) 0.012(3) 0.013(3) -0.009(3) -0.001(3) 0.002(3) O20 0.028(5) 0.010(3) 0.006(3) -0.004(3) -0.002(3) 0.008(3) O21 0.014(4) 0.011(3) 0.006(3) -0.003(3) -0.002(3) -0.003(3) O22 0.003(4) 0.005(3) 0.009(3) 0.000(3) 0.000(3) -0.001(3) O23 0.0112(17) 0.0111(16) 0.0108(17) -0.0051(10) -0.0004(10) 0.0001(10) O24 0.009(3) 0.011(3) 0.004(3) -0.002(2) -0.003(2) 0.002(2) O25 0.021(5) 0.006(3) 0.013(3) -0.004(3) 0.001(3) -0.002(3) O26 0.015(4) 0.013(4) 0.017(4) -0.008(3) 0.007(3) -0.004(3) O27 0.019(5) 0.020(4) 0.013(4) -0.008(3) 0.005(3) -0.012(3) O28 0.014(4) 0.016(4) 0.012(4) -0.008(3) 0.001(3) -0.004(3) O29 0.025(4) 0.023(3) 0.011(3) -0.009(3) -0.005(3) 0.011(3) O30 0.025(5) 0.012(3) 0.016(4) -0.011(3) 0.007(3) -0.001(3) O31 0.026(5) 0.024(4) 0.011(3) -0.001(3) -0.001(3) 0.006(3) O32 0.027(5) 0.026(4) 0.024(4) -0.014(3) 0.008(3) -0.019(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 Eu1 O12 2.317(7) . ? Eu1 O2 2.346(7) 2_756 ? Eu1 O7 2.414(6) . ? Eu1 O3 2.436(5) . ? Eu1 O17 2.439(6) . ? Eu1 O18 2.524(6) . ? Eu1 N4 2.555(6) . ? Eu1 N2 2.566(7) . ? Eu1 C1 3.238(10) 2_756 ? Eu2 O8 2.347(6) 1_455 ? Eu2 O22 2.356(7) 2_565 ? Eu2 O26 2.382(7) . ? Eu2 O21 2.423(6) . ? Eu2 O15 2.440(6) . ? Eu2 N8 2.520(7) . ? Eu2 N6 2.524(7) . ? Eu2 O11 2.666(6) . ? Eu2 H26A 2.7777 . ? Eu2 H26C 2.7830 . ? Eu3 O16 2.304(6) 2_665 ? Eu3 O28 2.383(7) . ? Eu3 O17 2.419(7) . ? Eu3 O11 2.420(6) . ? Eu3 O27 2.486(6) . ? Eu3 N11 2.514(7) . ? Eu3 N9 2.527(8) . ? Eu3 O21 2.596(6) . ? Eu3 H28C 2.7981 . ? Eu3 H28A 2.7320 . ? Eu4 O10 2.341(6) 1_554 ? Eu4 O31 2.363(8) . ? Eu4 O29 2.370(7) . ? Eu4 O32 2.394(6) . ? Eu4 O30 2.396(6) . ? Eu4 O4 2.408(6) 2_655 ? Eu4 O24 2.495(6) . ? Eu4 O5 2.601(7) 1_554 ? Eu4 Cu1 3.7482(13) 1_554 ? Eu4 H32A 2.8196 . ? Cu1 N3 1.894(8) . ? Cu1 N1 1.916(7) . ? Cu1 O1 1.983(6) . ? Cu1 O5 1.992(6) . ? Cu1 Eu4 3.7482(13) 1_556 ? Cu2 N7 1.899(7) . ? Cu2 N5 1.930(7) . ? Cu2 O13 1.985(6) . ? Cu2 O9 2.011(6) . ? Cu2 O25 2.249(7) . ? Cu3 N10 1.895(8) . ? Cu3 N12 1.932(8) . ? Cu3 O23 1.956(6) . ? Cu3 O19 1.969(6) . ? C1 O2 1.250(10) . ? C1 O1 1.278(10) . ? C1 C2 1.484(11) . ? C1 Eu1 3.238(10) 2_756 ? C2 N1 1.336(10) . ? C2 C3 1.404(11) . ? C3 C4 1.371(13) . ? C3 H3 0.9500 . ? C4 N2 1.353(11) . ? C4 C5 1.488(12) . ? C5 O3 1.254(10) . ? C5 O4 1.277(9) . ? C6 O6 1.250(10) . ? C6 O5 1.300(10) . ? C6 C7 1.468(11) . ? C7 N3 1.353(10) . ? C7 C8 1.399(11) . ? C8 C9 1.389(11) . ? C8 H8 0.9500 . ? C9 N4 1.377(10) . ? C9 C10 1.474(12) . ? C10 O8 1.237(10) . ? C10 O7 1.274(10) . ? C11 O10 1.248(11) . ? C11 O9 1.296(10) . ? C11 C12 1.462(12) . ? C12 N5 1.346(11) . ? C12 C13 1.378(12) . ? C13 C14 1.377(12) . ? C13 H13 0.9500 . ? C14 N6 1.362(11) . ? C14 C15 1.461(12) . ? C15 O12 1.271(10) . ? C15 O11 1.289(10) . ? C16 O14 1.229(10) . ? C16 O13 1.294(10) . ? C16 C17 1.480(12) . ? C17 N7 1.378(11) . ? C17 C18 1.393(12) . ? C18 C19 1.393(11) . ? C18 H18 0.9500 . ? C19 N8 1.351(11) . ? C19 C20 1.451(12) . ? C20 O16 1.244(10) . ? C20 O15 1.306(10) . ? C21 O18 1.244(11) . ? C21 O17 1.289(10) . ? C21 C22 1.470(12) . ? C22 N9 1.366(12) . ? C22 C23 1.397(12) . ? C23 C24 1.376(12) . ? C23 H23 0.9500 . ? C24 N10 1.342(12) . ? C24 C25 1.488(11) . ? C25 O20 1.228(11) . ? C25 O19 1.313(11) . ? C26 O22 1.243(10) . ? C26 O21 1.276(10) . ? C26 C27 1.488(12) . ? C27 N11 1.356(11) . ? C27 C28 1.399(12) . ? C28 C29 1.400(12) . ? C28 H28 0.9500 . ? C29 N12 1.350(11) . ? C29 C30 1.475(12) . ? C30 O24 1.246(10) . ? C30 O23 1.292(10) . ? N1 N2 1.337(9) . ? N3 N4 1.332(9) . ? N5 N6 1.341(9) . ? N7 N8 1.347(9) . ? N9 N10 1.345(9) . ? N11 N12 1.342(9) . ? O2 Eu1 2.346(7) 2_756 ? O4 Eu4 2.408(6) 2_655 ? O5 Eu4 2.601(7) 1_556 ? O8 Eu2 2.347(6) 1_655 ? O10 Eu4 2.341(6) 1_556 ? O16 Eu3 2.304(6) 2_665 ? O22 Eu2 2.356(7) 2_565 ? O25 H25A 0.8468 . ? O25 H25B 0.8389 . ? O26 H26A 0.8502 . ? O26 H26C 0.8509 . ? O27 H27A 0.7868 . ? O27 H27B 0.9143 . ? O28 H28C 0.8514 . ? O28 H28A 0.8494 . ? O29 H29A 0.8385 . ? O29 H29B 0.8466 . ? O30 H30A 0.8426 . ? O30 H30B 0.8267 . ? O31 H31A 0.8401 . ? O31 H31B 0.8419 . ? O32 H32A 0.8482 . ? O32 H32B 0.8493 . ? 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 O12 Eu1 O2 161.2(2) . 2_756 ? O12 Eu1 O7 88.7(2) . . ? O2 Eu1 O7 81.3(2) 2_756 . ? O12 Eu1 O3 93.4(2) . . ? O2 Eu1 O3 101.6(2) 2_756 . ? O7 Eu1 O3 159.20(19) . . ? O12 Eu1 O17 72.6(2) . . ? O2 Eu1 O17 117.5(2) 2_756 . ? O7 Eu1 O17 69.14(19) . . ? O3 Eu1 O17 91.74(19) . . ? O12 Eu1 O18 119.8(2) . . ? O2 Eu1 O18 76.7(2) 2_756 . ? O7 Eu1 O18 93.0(2) . . ? O3 Eu1 O18 68.1(2) . . ? O17 Eu1 O18 52.6(2) . . ? O12 Eu1 N4 80.6(2) . . ? O2 Eu1 N4 80.8(2) 2_756 . ? O7 Eu1 N4 64.5(2) . . ? O3 Eu1 N4 136.2(2) . . ? O17 Eu1 N4 126.3(2) . . ? O18 Eu1 N4 150.4(2) . . ? O12 Eu1 N2 94.7(2) . . ? O2 Eu1 N2 82.4(2) 2_756 . ? O7 Eu1 N2 137.1(2) . . ? O3 Eu1 N2 63.3(2) . . ? O17 Eu1 N2 151.8(2) . . ? O18 Eu1 N2 121.1(2) . . ? N4 Eu1 N2 73.9(2) . . ? O12 Eu1 C1 158.3(2) . 2_756 ? O2 Eu1 C1 18.3(2) 2_756 2_756 ? O7 Eu1 C1 99.0(2) . 2_756 ? O3 Eu1 C1 86.6(2) . 2_756 ? O17 Eu1 C1 129.1(2) . 2_756 ? O18 Eu1 C1 80.3(2) . 2_756 ? N4 Eu1 C1 84.3(2) . 2_756 ? N2 Eu1 C1 66.0(2) . 2_756 ? O8 Eu2 O22 71.2(2) 1_455 2_565 ? O8 Eu2 O26 141.3(2) 1_455 . ? O22 Eu2 O26 146.9(2) 2_565 . ? O8 Eu2 O21 92.2(2) 1_455 . ? O22 Eu2 O21 103.2(2) 2_565 . ? O26 Eu2 O21 84.7(2) . . ? O8 Eu2 O15 143.1(2) 1_455 . ? O22 Eu2 O15 74.7(2) 2_565 . ? O26 Eu2 O15 74.7(2) . . ? O21 Eu2 O15 82.0(2) . . ? O8 Eu2 N8 118.6(2) 1_455 . ? O22 Eu2 N8 75.9(2) 2_565 . ? O26 Eu2 N8 79.8(2) . . ? O21 Eu2 N8 145.8(2) . . ? O15 Eu2 N8 64.6(2) . . ? O8 Eu2 N6 78.1(2) 1_455 . ? O22 Eu2 N6 119.7(2) 2_565 . ? O26 Eu2 N6 74.3(2) . . ? O21 Eu2 N6 129.0(2) . . ? O15 Eu2 N6 132.7(2) . . ? N8 Eu2 N6 75.4(2) . . ? O8 Eu2 O11 70.7(2) 1_455 . ? O22 Eu2 O11 139.67(19) 2_565 . ? O26 Eu2 O11 73.0(2) . . ? O21 Eu2 O11 65.61(19) . . ? O15 Eu2 O11 135.7(2) . . ? N8 Eu2 O11 135.6(2) . . ? N6 Eu2 O11 63.9(2) . . ? O8 Eu2 H26A 156.5 1_455 . ? O22 Eu2 H26A 130.2 2_565 . ? O26 Eu2 H26A 16.8 . . ? O21 Eu2 H26A 91.5 . . ? O15 Eu2 H26A 60.5 . . ? N8 Eu2 H26A 66.4 . . ? N6 Eu2 H26A 81.5 . . ? O11 Eu2 H26A 89.8 . . ? O8 Eu2 H26C 136.0 1_455 . ? O22 Eu2 H26C 149.6 2_565 . ? O26 Eu2 H26C 16.8 . . ? O21 Eu2 H26C 68.1 . . ? O15 Eu2 H26C 75.2 . . ? N8 Eu2 H26C 95.1 . . ? N6 Eu2 H26C 84.7 . . ? O11 Eu2 H26C 65.3 . . ? H26A Eu2 H26C 28.9 . . ? O16 Eu3 O28 139.7(2) 2_665 . ? O16 Eu3 O17 77.2(2) 2_665 . ? O28 Eu3 O17 139.6(2) . . ? O16 Eu3 O11 85.7(2) 2_665 . ? O28 Eu3 O11 83.5(2) . . ? O17 Eu3 O11 84.5(2) . . ? O16 Eu3 O27 145.5(2) 2_665 . ? O28 Eu3 O27 73.7(2) . . ? O17 Eu3 O27 68.3(2) . . ? O11 Eu3 O27 91.6(2) . . ? O16 Eu3 N11 82.3(2) 2_665 . ? O28 Eu3 N11 76.3(2) . . ? O17 Eu3 N11 136.9(2) . . ? O11 Eu3 N11 131.5(2) . . ? O27 Eu3 N11 122.9(2) . . ? O16 Eu3 N9 87.2(2) 2_665 . ? O28 Eu3 N9 120.1(2) . . ? O17 Eu3 N9 64.0(2) . . ? O11 Eu3 N9 148.5(2) . . ? O27 Eu3 N9 77.3(2) . . ? N11 Eu3 N9 77.6(2) . . ? O16 Eu3 O21 71.6(2) 2_665 . ? O28 Eu3 O21 68.5(2) . . ? O17 Eu3 O21 138.48(18) . . ? O11 Eu3 O21 66.80(19) . . ? O27 Eu3 O21 137.9(2) . . ? N11 Eu3 O21 64.8(2) . . ? N9 Eu3 O21 138.5(2) . . ? O16 Eu3 H28C 141.7 2_665 . ? O28 Eu3 H28C 16.6 . . ? O17 Eu3 H28C 126.4 . . ? O11 Eu3 H28C 69.5 . . ? O27 Eu3 H28C 66.7 . . ? N11 Eu3 H28C 92.4 . . ? N9 Eu3 H28C 128.9 . . ? O21 Eu3 H28C 71.9 . . ? O16 Eu3 H28A 149.5 2_665 . ? O28 Eu3 H28A 17.5 . . ? O17 Eu3 H28A 133.1 . . ? O11 Eu3 H28A 98.8 . . ? O27 Eu3 H28A 64.9 . . ? N11 Eu3 H28A 72.1 . . ? N9 Eu3 H28A 102.8 . . ? O21 Eu3 H28A 82.5 . . ? H28C Eu3 H28A 29.3 . . ? O10 Eu4 O31 69.8(2) 1_554 . ? O10 Eu4 O29 140.9(2) 1_554 . ? O31 Eu4 O29 149.3(2) . . ? O10 Eu4 O32 74.3(2) 1_554 . ? O31 Eu4 O32 92.9(2) . . ? O29 Eu4 O32 95.3(2) . . ? O10 Eu4 O30 127.1(2) 1_554 . ? O31 Eu4 O30 72.7(2) . . ? O29 Eu4 O30 83.4(2) . . ? O32 Eu4 O30 143.6(2) . . ? O10 Eu4 O4 81.3(2) 1_554 2_655 ? O31 Eu4 O4 105.1(2) . 2_655 ? O29 Eu4 O4 85.8(2) . 2_655 ? O32 Eu4 O4 142.5(2) . 2_655 ? O30 Eu4 O4 73.9(2) . 2_655 ? O10 Eu4 O24 130.7(2) 1_554 . ? O31 Eu4 O24 78.7(2) . . ? O29 Eu4 O24 76.4(2) . . ? O32 Eu4 O24 70.4(2) . . ? O30 Eu4 O24 74.0(2) . . ? O4 Eu4 O24 144.7(2) 2_655 . ? O10 Eu4 O5 71.0(2) 1_554 1_554 ? O31 Eu4 O5 140.7(2) . 1_554 ? O29 Eu4 O5 69.9(2) . 1_554 ? O32 Eu4 O5 73.8(2) . 1_554 ? O30 Eu4 O5 137.3(2) . 1_554 ? O4 Eu4 O5 71.5(2) 2_655 1_554 ? O24 Eu4 O5 127.3(2) . 1_554 ? O10 Eu4 Cu1 80.04(17) 1_554 1_554 ? O31 Eu4 Cu1 139.93(16) . 1_554 ? O29 Eu4 Cu1 65.77(16) . 1_554 ? O32 Eu4 Cu1 103.99(18) . 1_554 ? O30 Eu4 Cu1 108.43(15) . 1_554 ? O4 Eu4 Cu1 42.87(16) 2_655 1_554 ? O24 Eu4 Cu1 141.18(16) . 1_554 ? O5 Eu4 Cu1 30.25(12) 1_554 1_554 ? O10 Eu4 H32A 63.9 1_554 . ? O31 Eu4 H32A 99.8 . . ? O29 Eu4 H32A 96.1 . . ? O32 Eu4 H32A 16.2 . . ? O30 Eu4 H32A 159.8 . . ? O4 Eu4 H32A 126.2 2_655 . ? O24 Eu4 H32A 86.3 . . ? O5 Eu4 H32A 59.4 1_554 . ? Cu1 Eu4 H32A 89.5 1_554 . ? N3 Cu1 N1 97.0(3) . . ? N3 Cu1 O1 159.6(3) . . ? N1 Cu1 O1 82.3(3) . . ? N3 Cu1 O5 83.2(3) . . ? N1 Cu1 O5 175.1(3) . . ? O1 Cu1 O5 99.2(2) . . ? N3 Cu1 Eu4 108.8(2) . 1_556 ? N1 Cu1 Eu4 134.9(2) . 1_556 ? O1 Cu1 Eu4 85.05(19) . 1_556 ? O5 Cu1 Eu4 41.12(19) . 1_556 ? N7 Cu2 N5 96.4(3) . . ? N7 Cu2 O13 82.7(3) . . ? N5 Cu2 O13 170.2(3) . . ? N7 Cu2 O9 163.5(3) . . ? N5 Cu2 O9 83.1(3) . . ? O13 Cu2 O9 95.0(2) . . ? N7 Cu2 O25 104.3(3) . . ? N5 Cu2 O25 99.0(3) . . ? O13 Cu2 O25 90.6(3) . . ? O9 Cu2 O25 92.0(3) . . ? N10 Cu3 N12 99.0(3) . . ? N10 Cu3 O23 173.2(3) . . ? N12 Cu3 O23 82.3(3) . . ? N10 Cu3 O19 82.6(3) . . ? N12 Cu3 O19 177.6(3) . . ? O23 Cu3 O19 95.8(3) . . ? O2 C1 O1 123.4(8) . . ? O2 C1 C2 121.3(8) . . ? O1 C1 C2 115.1(8) . . ? O1 C1 Eu1 109.5(6) . 2_756 ? C2 C1 Eu1 119.6(6) . 2_756 ? N1 C2 C3 108.5(8) . . ? N1 C2 C1 113.3(7) . . ? C3 C2 C1 138.2(8) . . ? C4 C3 C2 103.1(8) . . ? C4 C3 H3 128.5 . . ? C2 C3 H3 128.5 . . ? N2 C4 C3 112.0(8) . . ? N2 C4 C5 114.2(8) . . ? C3 C4 C5 133.7(9) . . ? O3 C5 O4 124.5(8) . . ? O3 C5 C4 117.2(8) . . ? O4 C5 C4 118.1(8) . . ? O6 C6 O5 123.0(8) . . ? O6 C6 C7 121.3(8) . . ? O5 C6 C7 115.6(7) . . ? N3 C7 C8 108.4(7) . . ? N3 C7 C6 113.9(7) . . ? C8 C7 C6 137.7(7) . . ? C9 C8 C7 103.8(7) . . ? C9 C8 H8 128.1 . . ? C7 C8 H8 128.1 . . ? N4 C9 C8 110.9(7) . . ? N4 C9 C10 117.4(7) . . ? C8 C9 C10 131.6(8) . . ? O8 C10 O7 125.2(9) . . ? O8 C10 C9 119.4(8) . . ? O7 C10 C9 115.4(8) . . ? O10 C11 O9 123.1(8) . . ? O10 C11 C12 120.8(8) . . ? O9 C11 C12 116.1(8) . . ? N5 C12 C13 109.7(8) . . ? N5 C12 C11 115.5(8) . . ? C13 C12 C11 134.6(9) . . ? C14 C13 C12 103.7(9) . . ? C14 C13 H13 128.2 . . ? C12 C13 H13 128.2 . . ? N6 C14 C13 111.1(8) . . ? N6 C14 C15 118.8(8) . . ? C13 C14 C15 129.9(9) . . ? O12 C15 O11 124.1(8) . . ? O12 C15 C14 116.7(8) . . ? O11 C15 C14 119.2(8) . . ? O14 C16 O13 124.3(8) . . ? O14 C16 C17 121.0(8) . . ? O13 C16 C17 114.7(7) . . ? N7 C17 C18 108.1(8) . . ? N7 C17 C16 112.9(7) . . ? C18 C17 C16 138.8(8) . . ? C17 C18 C19 104.5(8) . . ? C17 C18 H18 127.7 . . ? C19 C18 H18 127.7 . . ? N8 C19 C18 110.8(8) . . ? N8 C19 C20 116.9(8) . . ? C18 C19 C20 131.7(8) . . ? O16 C20 O15 122.9(9) . . ? O16 C20 C19 121.3(8) . . ? O15 C20 C19 115.7(8) . . ? O18 C21 O17 120.7(8) . . ? O18 C21 C22 123.7(9) . . ? O17 C21 C22 115.6(8) . . ? N9 C22 C23 110.0(8) . . ? N9 C22 C21 115.5(8) . . ? C23 C22 C21 134.1(9) . . ? C24 C23 C22 103.7(9) . . ? C24 C23 H23 128.1 . . ? C22 C23 H23 128.1 . . ? N10 C24 C23 110.2(8) . . ? N10 C24 C25 113.3(8) . . ? C23 C24 C25 136.4(9) . . ? O20 C25 O19 123.9(8) . . ? O20 C25 C24 122.4(9) . . ? O19 C25 C24 113.6(8) . . ? O22 C26 O21 123.9(8) . . ? O22 C26 C27 118.7(8) . . ? O21 C26 C27 117.3(8) . . ? N11 C27 C28 110.9(8) . . ? N11 C27 C26 118.5(8) . . ? C28 C27 C26 130.6(9) . . ? C27 C28 C29 102.8(8) . . ? C27 C28 H28 128.6 . . ? C29 C28 H28 128.6 . . ? N12 C29 C28 109.9(8) . . ? N12 C29 C30 114.0(8) . . ? C28 C29 C30 136.1(9) . . ? O24 C30 O23 121.7(9) . . ? O24 C30 C29 123.9(8) . . ? O23 C30 C29 114.4(8) . . ? C2 N1 N2 110.9(6) . . ? C2 N1 Cu1 114.4(6) . . ? N2 N1 Cu1 133.6(6) . . ? N1 N2 C4 105.4(7) . . ? N1 N2 Eu1 134.6(5) . . ? C4 N2 Eu1 115.7(6) . . ? N4 N3 C7 111.2(7) . . ? N4 N3 Cu1 134.4(5) . . ? C7 N3 Cu1 114.0(6) . . ? N3 N4 C9 105.7(6) . . ? N3 N4 Eu1 138.3(5) . . ? C9 N4 Eu1 115.3(5) . . ? N6 N5 C12 109.5(7) . . ? N6 N5 Cu2 137.4(6) . . ? C12 N5 Cu2 113.1(6) . . ? N5 N6 C14 106.0(7) . . ? N5 N6 Eu2 133.9(6) . . ? C14 N6 Eu2 120.1(5) . . ? N8 N7 C17 109.4(7) . . ? N8 N7 Cu2 135.1(6) . . ? C17 N7 Cu2 114.8(6) . . ? N7 N8 C19 107.2(7) . . ? N7 N8 Eu2 134.1(5) . . ? C19 N8 Eu2 116.4(5) . . ? N10 N9 C22 106.6(7) . . ? N10 N9 Eu3 134.7(6) . . ? C22 N9 Eu3 117.0(6) . . ? C24 N10 N9 109.4(8) . . ? C24 N10 Cu3 115.7(6) . . ? N9 N10 Cu3 134.6(6) . . ? N12 N11 C27 107.2(7) . . ? N12 N11 Eu3 134.0(5) . . ? C27 N11 Eu3 118.7(5) . . ? N11 N12 C29 109.2(7) . . ? N11 N12 Cu3 136.7(6) . . ? C29 N12 Cu3 113.8(6) . . ? C1 O1 Cu1 113.8(5) . . ? C1 O2 Eu1 125.6(6) . 2_756 ? C5 O3 Eu1 123.9(5) . . ? C5 O4 Eu4 135.2(6) . 2_655 ? C6 O5 Cu1 111.5(5) . . ? C6 O5 Eu4 125.1(6) . 1_556 ? Cu1 O5 Eu4 108.6(2) . 1_556 ? C10 O7 Eu1 125.6(6) . . ? C10 O8 Eu2 145.4(7) . 1_655 ? C11 O9 Cu2 112.1(6) . . ? C11 O10 Eu4 176.1(7) . 1_556 ? C15 O11 Eu3 128.9(6) . . ? C15 O11 Eu2 117.6(5) . . ? Eu3 O11 Eu2 112.6(2) . . ? C15 O12 Eu1 137.2(6) . . ? C16 O13 Cu2 114.1(5) . . ? C20 O15 Eu2 123.0(6) . . ? C20 O16 Eu3 142.9(6) . 2_665 ? C21 O17 Eu3 124.6(6) . . ? C21 O17 Eu1 94.5(5) . . ? Eu3 O17 Eu1 138.3(3) . . ? C21 O18 Eu1 91.7(6) . . ? C25 O19 Cu3 114.1(5) . . ? C26 O21 Eu2 125.0(6) . . ? C26 O21 Eu3 118.7(5) . . ? Eu2 O21 Eu3 115.0(2) . . ? C26 O22 Eu2 154.6(6) . 2_565 ? C30 O23 Cu3 115.2(6) . . ? C30 O24 Eu4 132.5(6) . . ? Cu2 O25 H25A 105.3 . . ? Cu2 O25 H25B 102.1 . . ? H25A O25 H25B 118.6 . . ? Eu2 O26 H26A 109.0 . . ? Eu2 O26 H26C 109.4 . . ? H26A O26 H26C 109.4 . . ? Eu3 O27 H27A 129.1 . . ? Eu3 O27 H27B 110.3 . . ? H27A O27 H27B 105.4 . . ? Eu3 O28 H28C 110.5 . . ? Eu3 O28 H28A 105.2 . . ? H28C O28 H28A 110.6 . . ? Eu4 O29 H29A 116.3 . . ? Eu4 O29 H29B 125.8 . . ? H29A O29 H29B 112.8 . . ? Eu4 O30 H30A 123.5 . . ? Eu4 O30 H30B 117.1 . . ? H30A O30 H30B 118.5 . . ? Eu4 O31 H31A 128.2 . . ? Eu4 O31 H31B 124.0 . . ? H31A O31 H31B 107.2 . . ? Eu4 O32 H32A 111.7 . . ? Eu4 O32 H32B 143.3 . . ? H32A O32 H32B 96.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 N1 -165.1(9) . . . . ? O1 C1 C2 N1 10.6(12) . . . . ? Eu1 C1 C2 N1 -123.0(7) 2_756 . . . ? O2 C1 C2 C3 11.6(18) . . . . ? O1 C1 C2 C3 -172.7(11) . . . . ? Eu1 C1 C2 C3 53.6(15) 2_756 . . . ? N1 C2 C3 C4 -3.1(11) . . . . ? C1 C2 C3 C4 -179.8(12) . . . . ? C2 C3 C4 N2 3.9(12) . . . . ? C2 C3 C4 C5 -174.9(11) . . . . ? N2 C4 C5 O3 10.6(13) . . . . ? C3 C4 C5 O3 -170.6(11) . . . . ? N2 C4 C5 O4 -164.9(9) . . . . ? C3 C4 C5 O4 13.9(18) . . . . ? O6 C6 C7 N3 178.7(9) . . . . ? O5 C6 C7 N3 -4.9(13) . . . . ? O6 C6 C7 C8 -0.4(19) . . . . ? O5 C6 C7 C8 176.0(11) . . . . ? N3 C7 C8 C9 -0.2(11) . . . . ? C6 C7 C8 C9 178.9(12) . . . . ? C7 C8 C9 N4 1.0(11) . . . . ? C7 C8 C9 C10 -176.2(11) . . . . ? N4 C9 C10 O8 -176.1(9) . . . . ? C8 C9 C10 O8 0.9(17) . . . . ? N4 C9 C10 O7 3.3(14) . . . . ? C8 C9 C10 O7 -179.6(10) . . . . ? O10 C11 C12 N5 178.2(9) . . . . ? O9 C11 C12 N5 0.5(13) . . . . ? O10 C11 C12 C13 -7.0(18) . . . . ? O9 C11 C12 C13 175.3(10) . . . . ? N5 C12 C13 C14 -1.0(11) . . . . ? C11 C12 C13 C14 -176.0(11) . . . . ? C12 C13 C14 N6 1.4(11) . . . . ? C12 C13 C14 C15 176.4(9) . . . . ? N6 C14 C15 O12 175.3(8) . . . . ? C13 C14 C15 O12 0.6(15) . . . . ? N6 C14 C15 O11 -6.0(13) . . . . ? C13 C14 C15 O11 179.4(9) . . . . ? O14 C16 C17 N7 -169.9(9) . . . . ? O13 C16 C17 N7 9.2(12) . . . . ? O14 C16 C17 C18 16.6(19) . . . . ? O13 C16 C17 C18 -164.3(12) . . . . ? N7 C17 C18 C19 1.0(11) . . . . ? C16 C17 C18 C19 174.8(12) . . . . ? C17 C18 C19 N8 -0.9(11) . . . . ? C17 C18 C19 C20 -172.0(10) . . . . ? N8 C19 C20 O16 -159.6(9) . . . . ? C18 C19 C20 O16 11.0(17) . . . . ? N8 C19 C20 O15 16.9(13) . . . . ? C18 C19 C20 O15 -172.5(10) . . . . ? O18 C21 C22 N9 -171.8(8) . . . . ? O17 C21 C22 N9 6.9(12) . . . . ? O18 C21 C22 C23 0.6(16) . . . . ? O17 C21 C22 C23 179.3(9) . . . . ? N9 C22 C23 C24 -0.2(10) . . . . ? C21 C22 C23 C24 -172.9(9) . . . . ? C22 C23 C24 N10 0.2(10) . . . . ? C22 C23 C24 C25 178.7(10) . . . . ? N10 C24 C25 O20 -175.0(9) . . . . ? C23 C24 C25 O20 6.6(17) . . . . ? N10 C24 C25 O19 8.5(11) . . . . ? C23 C24 C25 O19 -169.9(10) . . . . ? O22 C26 C27 N11 -165.5(8) . . . . ? O21 C26 C27 N11 15.4(12) . . . . ? O22 C26 C27 C28 10.8(15) . . . . ? O21 C26 C27 C28 -168.3(9) . . . . ? N11 C27 C28 C29 -0.2(10) . . . . ? C26 C27 C28 C29 -176.8(9) . . . . ? C27 C28 C29 N12 -0.5(10) . . . . ? C27 C28 C29 C30 -179.2(10) . . . . ? N12 C29 C30 O24 178.9(9) . . . . ? C28 C29 C30 O24 -2.4(17) . . . . ? N12 C29 C30 O23 -1.7(12) . . . . ? C28 C29 C30 O23 176.9(10) . . . . ? C3 C2 N1 N2 1.3(11) . . . . ? C1 C2 N1 N2 179.0(8) . . . . ? C3 C2 N1 Cu1 171.0(6) . . . . ? C1 C2 N1 Cu1 -11.4(10) . . . . ? N3 Cu1 N1 C2 166.6(7) . . . . ? O1 Cu1 N1 C2 7.2(7) . . . . ? Eu4 Cu1 N1 C2 -67.9(8) 1_556 . . . ? N3 Cu1 N1 N2 -26.7(9) . . . . ? O1 Cu1 N1 N2 173.8(9) . . . . ? Eu4 Cu1 N1 N2 98.8(8) 1_556 . . . ? C2 N1 N2 C4 1.1(11) . . . . ? Cu1 N1 N2 C4 -165.9(7) . . . . ? C2 N1 N2 Eu1 -153.4(7) . . . . ? Cu1 N1 N2 Eu1 39.6(13) . . . . ? C3 C4 N2 N1 -3.2(11) . . . . ? C5 C4 N2 N1 175.8(8) . . . . ? C3 C4 N2 Eu1 156.9(7) . . . . ? C5 C4 N2 Eu1 -24.1(11) . . . . ? O12 Eu1 N2 N1 -95.4(9) . . . . ? O2 Eu1 N2 N1 65.9(9) 2_756 . . . ? O7 Eu1 N2 N1 -2.4(11) . . . . ? O3 Eu1 N2 N1 173.1(10) . . . . ? O17 Eu1 N2 N1 -156.6(7) . . . . ? O18 Eu1 N2 N1 135.4(8) . . . . ? N4 Eu1 N2 N1 -16.6(8) . . . . ? C1 Eu1 N2 N1 74.3(9) 2_756 . . . ? O12 Eu1 N2 C4 112.0(7) . . . . ? O2 Eu1 N2 C4 -86.6(7) 2_756 . . . ? O7 Eu1 N2 C4 -154.9(6) . . . . ? O3 Eu1 N2 C4 20.5(7) . . . . ? O17 Eu1 N2 C4 50.9(10) . . . . ? O18 Eu1 N2 C4 -17.2(8) . . . . ? N4 Eu1 N2 C4 -169.2(7) . . . . ? C1 Eu1 N2 C4 -78.2(7) 2_756 . . . ? C8 C7 N3 N4 -0.6(11) . . . . ? C6 C7 N3 N4 -179.9(8) . . . . ? C8 C7 N3 Cu1 173.3(6) . . . . ? C6 C7 N3 Cu1 -6.0(11) . . . . ? N1 Cu1 N3 N4 -2.8(9) . . . . ? O1 Cu1 N3 N4 83.9(11) . . . . ? O5 Cu1 N3 N4 -177.9(9) . . . . ? Eu4 Cu1 N3 N4 -145.3(8) 1_556 . . . ? N1 Cu1 N3 C7 -174.9(7) . . . . ? O1 Cu1 N3 C7 -88.2(11) . . . . ? O5 Cu1 N3 C7 10.0(7) . . . . ? Eu4 Cu1 N3 C7 42.6(7) 1_556 . . . ? C7 N3 N4 C9 1.2(11) . . . . ? Cu1 N3 N4 C9 -171.1(8) . . . . ? C7 N3 N4 Eu1 -167.5(7) . . . . ? Cu1 N3 N4 Eu1 20.2(15) . . . . ? C8 C9 N4 N3 -1.3(11) . . . . ? C10 C9 N4 N3 176.3(8) . . . . ? C8 C9 N4 Eu1 170.4(6) . . . . ? C10 C9 N4 Eu1 -12.0(11) . . . . ? O12 Eu1 N4 N3 86.0(9) . . . . ? O2 Eu1 N4 N3 -96.4(9) 2_756 . . . ? O7 Eu1 N4 N3 179.0(10) . . . . ? O3 Eu1 N4 N3 0.8(11) . . . . ? O17 Eu1 N4 N3 146.1(8) . . . . ? O18 Eu1 N4 N3 -137.2(8) . . . . ? N2 Eu1 N4 N3 -11.7(9) . . . . ? C1 Eu1 N4 N3 -78.3(9) 2_756 . . . ? O12 Eu1 N4 C9 -82.0(7) . . . . ? O2 Eu1 N4 C9 95.7(7) 2_756 . . . ? O7 Eu1 N4 C9 11.1(6) . . . . ? O3 Eu1 N4 C9 -167.1(6) . . . . ? O17 Eu1 N4 C9 -21.8(8) . . . . ? O18 Eu1 N4 C9 54.8(9) . . . . ? N2 Eu1 N4 C9 -179.6(7) . . . . ? C1 Eu1 N4 C9 113.8(7) 2_756 . . . ? C13 C12 N5 N6 0.3(11) . . . . ? C11 C12 N5 N6 176.3(8) . . . . ? C13 C12 N5 Cu2 -178.9(6) . . . . ? C11 C12 N5 Cu2 -2.9(11) . . . . ? N7 Cu2 N5 N6 -12.4(10) . . . . ? O9 Cu2 N5 N6 -175.8(9) . . . . ? O25 Cu2 N5 N6 93.2(9) . . . . ? N7 Cu2 N5 C12 166.5(7) . . . . ? O9 Cu2 N5 C12 3.1(7) . . . . ? O25 Cu2 N5 C12 -87.9(7) . . . . ? C12 N5 N6 C14 0.6(10) . . . . ? Cu2 N5 N6 C14 179.5(7) . . . . ? C12 N5 N6 Eu2 178.7(7) . . . . ? Cu2 N5 N6 Eu2 -2.4(14) . . . . ? C13 C14 N6 N5 -1.3(11) . . . . ? C15 C14 N6 N5 -176.9(8) . . . . ? C13 C14 N6 Eu2 -179.7(6) . . . . ? C15 C14 N6 Eu2 4.7(11) . . . . ? O8 Eu2 N6 N5 -105.5(8) 1_455 . . . ? O22 Eu2 N6 N5 -45.4(8) 2_565 . . . ? O26 Eu2 N6 N5 101.9(8) . . . . ? O21 Eu2 N6 N5 171.3(7) . . . . ? O15 Eu2 N6 N5 51.0(9) . . . . ? N8 Eu2 N6 N5 18.6(8) . . . . ? O11 Eu2 N6 N5 -179.7(9) . . . . ? O8 Eu2 N6 C14 72.3(7) 1_455 . . . ? O22 Eu2 N6 C14 132.4(7) 2_565 . . . ? O26 Eu2 N6 C14 -80.3(7) . . . . ? O21 Eu2 N6 C14 -10.8(8) . . . . ? O15 Eu2 N6 C14 -131.1(6) . . . . ? N8 Eu2 N6 C14 -163.5(7) . . . . ? O11 Eu2 N6 C14 -1.8(6) . . . . ? C18 C17 N7 N8 -0.8(11) . . . . ? C16 C17 N7 N8 -176.4(8) . . . . ? C18 C17 N7 Cu2 170.8(6) . . . . ? C16 C17 N7 Cu2 -4.7(11) . . . . ? N5 Cu2 N7 N8 -1.3(9) . . . . ? O13 Cu2 N7 N8 168.9(9) . . . . ? O9 Cu2 N7 N8 86.0(13) . . . . ? O25 Cu2 N7 N8 -102.3(9) . . . . ? N5 Cu2 N7 C17 -170.1(7) . . . . ? O13 Cu2 N7 C17 0.1(7) . . . . ? O9 Cu2 N7 C17 -82.8(13) . . . . ? O25 Cu2 N7 C17 88.9(7) . . . . ? C17 N7 N8 C19 0.3(10) . . . . ? Cu2 N7 N8 C19 -169.0(7) . . . . ? C17 N7 N8 Eu2 -161.4(7) . . . . ? Cu2 N7 N8 Eu2 29.3(14) . . . . ? C18 C19 N8 N7 0.4(11) . . . . ? C20 C19 N8 N7 173.0(8) . . . . ? C18 C19 N8 Eu2 165.8(6) . . . . ? C20 C19 N8 Eu2 -21.6(11) . . . . ? O8 Eu2 N8 N7 35.9(9) 1_455 . . . ? O22 Eu2 N8 N7 94.9(9) 2_565 . . . ? O26 Eu2 N8 N7 -107.7(9) . . . . ? O21 Eu2 N8 N7 -172.1(7) . . . . ? O15 Eu2 N8 N7 174.4(9) . . . . ? N6 Eu2 N8 N7 -31.4(8) . . . . ? O11 Eu2 N8 N7 -55.2(10) . . . . ? O8 Eu2 N8 C19 -124.5(7) 1_455 . . . ? O22 Eu2 N8 C19 -65.5(7) 2_565 . . . ? O26 Eu2 N8 C19 91.8(7) . . . . ? O21 Eu2 N8 C19 27.4(9) . . . . ? O15 Eu2 N8 C19 14.0(6) . . . . ? N6 Eu2 N8 C19 168.1(7) . . . . ? O11 Eu2 N8 C19 144.3(6) . . . . ? C23 C22 N9 N10 0.1(10) . . . . ? C21 C22 N9 N10 174.3(7) . . . . ? C23 C22 N9 Eu3 167.7(6) . . . . ? C21 C22 N9 Eu3 -18.1(10) . . . . ? O16 Eu3 N9 N10 -104.0(7) 2_665 . . . ? O28 Eu3 N9 N10 44.7(8) . . . . ? O17 Eu3 N9 N10 178.9(8) . . . . ? O11 Eu3 N9 N10 178.8(6) . . . . ? O27 Eu3 N9 N10 107.0(7) . . . . ? N11 Eu3 N9 N10 -21.3(7) . . . . ? O21 Eu3 N9 N10 -46.2(9) . . . . ? O16 Eu3 N9 C22 92.9(6) 2_665 . . . ? O28 Eu3 N9 C22 -118.4(6) . . . . ? O17 Eu3 N9 C22 15.8(6) . . . . ? O11 Eu3 N9 C22 15.7(9) . . . . ? O27 Eu3 N9 C22 -56.1(6) . . . . ? N11 Eu3 N9 C22 175.6(7) . . . . ? O21 Eu3 N9 C22 150.7(5) . . . . ? C23 C24 N10 N9 -0.1(10) . . . . ? C25 C24 N10 N9 -179.0(7) . . . . ? C23 C24 N10 Cu3 174.1(6) . . . . ? C25 C24 N10 Cu3 -4.8(10) . . . . ? C22 N9 N10 C24 0.0(10) . . . . ? Eu3 N9 N10 C24 -164.3(6) . . . . ? C22 N9 N10 Cu3 -172.6(7) . . . . ? Eu3 N9 N10 Cu3 23.0(13) . . . . ? N12 Cu3 N10 C24 -177.7(7) . . . . ? O19 Cu3 N10 C24 0.5(6) . . . . ? N12 Cu3 N10 N9 -5.4(9) . . . . ? O19 Cu3 N10 N9 172.8(9) . . . . ? C28 C27 N11 N12 0.8(10) . . . . ? C26 C27 N11 N12 177.9(7) . . . . ? C28 C27 N11 Eu3 177.0(6) . . . . ? C26 C27 N11 Eu3 -6.0(11) . . . . ? O16 Eu3 N11 N12 100.4(7) 2_665 . . . ? O28 Eu3 N11 N12 -114.0(7) . . . . ? O17 Eu3 N11 N12 38.5(8) . . . . ? O11 Eu3 N11 N12 177.7(6) . . . . ? O27 Eu3 N11 N12 -54.2(8) . . . . ? N9 Eu3 N11 N12 11.5(7) . . . . ? O21 Eu3 N11 N12 173.5(8) . . . . ? O16 Eu3 N11 C27 -74.5(6) 2_665 . . . ? O28 Eu3 N11 C27 71.1(7) . . . . ? O17 Eu3 N11 C27 -136.4(6) . . . . ? O11 Eu3 N11 C27 2.8(8) . . . . ? O27 Eu3 N11 C27 131.0(6) . . . . ? N9 Eu3 N11 C27 -163.3(7) . . . . ? O21 Eu3 N11 C27 -1.3(6) . . . . ? C27 N11 N12 C29 -1.1(10) . . . . ? Eu3 N11 N12 C29 -176.4(6) . . . . ? C27 N11 N12 Cu3 172.4(7) . . . . ? Eu3 N11 N12 Cu3 -2.8(13) . . . . ? C28 C29 N12 N11 1.0(11) . . . . ? C30 C29 N12 N11 -179.9(7) . . . . ? C28 C29 N12 Cu3 -174.2(6) . . . . ? C30 C29 N12 Cu3 4.9(10) . . . . ? N10 Cu3 N12 N11 -4.8(9) . . . . ? O23 Cu3 N12 N11 -178.1(9) . . . . ? N10 Cu3 N12 C29 168.5(7) . . . . ? O23 Cu3 N12 C29 -4.8(6) . . . . ? O2 C1 O1 Cu1 170.9(7) . . . . ? C2 C1 O1 Cu1 -4.7(10) . . . . ? Eu1 C1 O1 Cu1 133.4(4) 2_756 . . . ? N3 Cu1 O1 C1 -90.4(10) . . . . ? N1 Cu1 O1 C1 -1.1(6) . . . . ? O5 Cu1 O1 C1 174.3(6) . . . . ? Eu4 Cu1 O1 C1 135.6(6) 1_556 . . . ? O1 C1 O2 Eu1 -76.9(11) . . . 2_756 ? C2 C1 O2 Eu1 98.5(9) . . . 2_756 ? O4 C5 O3 Eu1 -174.7(7) . . . . ? C4 C5 O3 Eu1 10.1(12) . . . . ? O12 Eu1 O3 C5 -109.7(8) . . . . ? O2 Eu1 O3 C5 59.1(8) 2_756 . . . ? O7 Eu1 O3 C5 155.1(7) . . . . ? O17 Eu1 O3 C5 177.7(8) . . . . ? O18 Eu1 O3 C5 129.5(8) . . . . ? N4 Eu1 O3 C5 -29.7(9) . . . . ? N2 Eu1 O3 C5 -16.2(7) . . . . ? C1 Eu1 O3 C5 48.6(8) 2_756 . . . ? O3 C5 O4 Eu4 30.6(16) . . . 2_655 ? C4 C5 O4 Eu4 -154.2(7) . . . 2_655 ? O6 C6 O5 Cu1 -171.0(8) . . . . ? C7 C6 O5 Cu1 12.6(10) . . . . ? O6 C6 O5 Eu4 54.8(12) . . . 1_556 ? C7 C6 O5 Eu4 -121.5(7) . . . 1_556 ? N3 Cu1 O5 C6 -12.6(7) . . . . ? O1 Cu1 O5 C6 146.9(6) . . . . ? Eu4 Cu1 O5 C6 -141.7(8) 1_556 . . . ? N3 Cu1 O5 Eu4 129.1(3) . . . 1_556 ? O1 Cu1 O5 Eu4 -71.4(3) . . . 1_556 ? O8 C10 O7 Eu1 -172.1(7) . . . . ? C9 C10 O7 Eu1 8.6(12) . . . . ? O12 Eu1 O7 C10 69.4(8) . . . . ? O2 Eu1 O7 C10 -94.7(8) 2_756 . . . ? O3 Eu1 O7 C10 165.6(7) . . . . ? O17 Eu1 O7 C10 141.3(8) . . . . ? O18 Eu1 O7 C10 -170.8(8) . . . . ? N4 Eu1 O7 C10 -10.8(7) . . . . ? N2 Eu1 O7 C10 -26.0(9) . . . . ? C1 Eu1 O7 C10 -90.1(8) 2_756 . . . ? O7 C10 O8 Eu2 -92.4(13) . . . 1_655 ? C9 C10 O8 Eu2 87.0(13) . . . 1_655 ? O10 C11 O9 Cu2 -175.6(8) . . . . ? C12 C11 O9 Cu2 2.0(10) . . . . ? N7 Cu2 O9 C11 -92.0(11) . . . . ? N5 Cu2 O9 C11 -2.8(6) . . . . ? O13 Cu2 O9 C11 -173.1(6) . . . . ? O25 Cu2 O9 C11 96.1(6) . . . . ? O12 C15 O11 Eu3 -8.8(13) . . . . ? C14 C15 O11 Eu3 172.6(6) . . . . ? O12 C15 O11 Eu2 -177.2(7) . . . . ? C14 C15 O11 Eu2 4.1(11) . . . . ? O16 Eu3 O11 C15 -97.9(7) 2_665 . . . ? O28 Eu3 O11 C15 121.0(7) . . . . ? O17 Eu3 O11 C15 -20.4(7) . . . . ? O27 Eu3 O11 C15 47.6(7) . . . . ? N11 Eu3 O11 C15 -173.7(7) . . . . ? N9 Eu3 O11 C15 -20.3(9) . . . . ? O21 Eu3 O11 C15 -169.7(8) . . . . ? O16 Eu3 O11 Eu2 71.0(3) 2_665 . . . ? O28 Eu3 O11 Eu2 -70.1(3) . . . . ? O17 Eu3 O11 Eu2 148.5(3) . . . . ? O27 Eu3 O11 Eu2 -143.5(3) . . . . ? N11 Eu3 O11 Eu2 -4.8(4) . . . . ? N9 Eu3 O11 Eu2 148.6(3) . . . . ? O21 Eu3 O11 Eu2 -0.7(2) . . . . ? O8 Eu2 O11 C15 -87.2(6) 1_455 . . . ? O22 Eu2 O11 C15 -107.3(6) 2_565 . . . ? O26 Eu2 O11 C15 79.2(6) . . . . ? O21 Eu2 O11 C15 171.1(7) . . . . ? O15 Eu2 O11 C15 124.1(6) . . . . ? N8 Eu2 O11 C15 24.4(8) . . . . ? N6 Eu2 O11 C15 -1.3(6) . . . . ? O8 Eu2 O11 Eu3 102.6(3) 1_455 . . . ? O22 Eu2 O11 Eu3 82.4(4) 2_565 . . . ? O26 Eu2 O11 Eu3 -91.1(3) . . . . ? O21 Eu2 O11 Eu3 0.8(2) . . . . ? O15 Eu2 O11 Eu3 -46.1(4) . . . . ? N8 Eu2 O11 Eu3 -145.8(3) . . . . ? N6 Eu2 O11 Eu3 -171.6(3) . . . . ? O11 C15 O12 Eu1 82.3(12) . . . . ? C14 C15 O12 Eu1 -99.0(10) . . . . ? O2 Eu1 O12 C15 54.1(12) 2_756 . . . ? O7 Eu1 O12 C15 -3.1(8) . . . . ? O3 Eu1 O12 C15 -162.4(8) . . . . ? O17 Eu1 O12 C15 -71.7(8) . . . . ? O18 Eu1 O12 C15 -95.8(8) . . . . ? N4 Eu1 O12 C15 61.3(8) . . . . ? N2 Eu1 O12 C15 134.1(8) . . . . ? C1 Eu1 O12 C15 108.1(9) 2_756 . . . ? O14 C16 O13 Cu2 169.9(8) . . . . ? C17 C16 O13 Cu2 -9.2(10) . . . . ? N7 Cu2 O13 C16 5.3(7) . . . . ? O9 Cu2 O13 C16 168.9(7) . . . . ? O25 Cu2 O13 C16 -99.0(7) . . . . ? O16 C20 O15 Eu2 173.0(7) . . . . ? C19 C20 O15 Eu2 -3.4(12) . . . . ? O8 Eu2 O15 C20 99.2(7) 1_455 . . . ? O22 Eu2 O15 C20 76.1(7) 2_565 . . . ? O26 Eu2 O15 C20 -91.1(7) . . . . ? O21 Eu2 O15 C20 -177.7(7) . . . . ? N8 Eu2 O15 C20 -5.3(7) . . . . ? N6 Eu2 O15 C20 -40.4(8) . . . . ? O11 Eu2 O15 C20 -135.5(7) . . . . ? O15 C20 O16 Eu3 -108.1(10) . . . 2_665 ? C19 C20 O16 Eu3 68.1(15) . . . 2_665 ? O18 C21 O17 Eu3 -172.2(6) . . . . ? C22 C21 O17 Eu3 9.0(10) . . . . ? O18 C21 O17 Eu1 -7.6(9) . . . . ? C22 C21 O17 Eu1 173.6(6) . . . . ? O16 Eu3 O17 C21 -106.4(7) 2_665 . . . ? O28 Eu3 O17 C21 93.4(7) . . . . ? O11 Eu3 O17 C21 166.7(7) . . . . ? O27 Eu3 O17 C21 72.8(6) . . . . ? N11 Eu3 O17 C21 -42.7(7) . . . . ? N9 Eu3 O17 C21 -13.2(6) . . . . ? O21 Eu3 O17 C21 -148.2(6) . . . . ? O16 Eu3 O17 Eu1 97.0(4) 2_665 . . . ? O28 Eu3 O17 Eu1 -63.1(5) . . . . ? O11 Eu3 O17 Eu1 10.2(4) . . . . ? O27 Eu3 O17 Eu1 -83.8(4) . . . . ? N11 Eu3 O17 Eu1 160.7(3) . . . . ? N9 Eu3 O17 Eu1 -169.8(4) . . . . ? O21 Eu3 O17 Eu1 55.3(5) . . . . ? O12 Eu1 O17 C21 -149.5(5) . . . . ? O2 Eu1 O17 C21 47.7(5) 2_756 . . . ? O7 Eu1 O17 C21 115.2(5) . . . . ? O3 Eu1 O17 C21 -56.4(5) . . . . ? O18 Eu1 O17 C21 4.1(5) . . . . ? N4 Eu1 O17 C21 146.8(5) . . . . ? N2 Eu1 O17 C21 -83.2(7) . . . . ? C1 Eu1 O17 C21 30.7(6) 2_756 . . . ? O12 Eu1 O17 Eu3 11.3(3) . . . . ? O2 Eu1 O17 Eu3 -151.5(3) 2_756 . . . ? O7 Eu1 O17 Eu3 -84.0(4) . . . . ? O3 Eu1 O17 Eu3 104.4(4) . . . . ? O18 Eu1 O17 Eu3 164.9(5) . . . . ? N4 Eu1 O17 Eu3 -52.4(5) . . . . ? N2 Eu1 O17 Eu3 77.5(6) . . . . ? C1 Eu1 O17 Eu3 -168.5(3) 2_756 . . . ? O17 C21 O18 Eu1 7.4(8) . . . . ? C22 C21 O18 Eu1 -174.0(8) . . . . ? O12 Eu1 O18 C21 25.2(6) . . . . ? O2 Eu1 O18 C21 -145.3(5) 2_756 . . . ? O7 Eu1 O18 C21 -65.0(5) . . . . ? O3 Eu1 O18 C21 106.2(5) . . . . ? O17 Eu1 O18 C21 -4.2(5) . . . . ? N4 Eu1 O18 C21 -103.7(6) . . . . ? N2 Eu1 O18 C21 142.3(5) . . . . ? C1 Eu1 O18 C21 -163.6(5) 2_756 . . . ? O20 C25 O19 Cu3 175.4(7) . . . . ? C24 C25 O19 Cu3 -8.1(9) . . . . ? N10 Cu3 O19 C25 4.5(6) . . . . ? O23 Cu3 O19 C25 177.9(6) . . . . ? O22 C26 O21 Eu2 -1.9(12) . . . . ? C27 C26 O21 Eu2 177.1(5) . . . . ? O22 C26 O21 Eu3 164.3(6) . . . . ? C27 C26 O21 Eu3 -16.7(10) . . . . ? O8 Eu2 O21 C26 98.2(7) 1_455 . . . ? O22 Eu2 O21 C26 27.0(7) 2_565 . . . ? O26 Eu2 O21 C26 -120.4(7) . . . . ? O15 Eu2 O21 C26 -45.1(7) . . . . ? N8 Eu2 O21 C26 -57.3(9) . . . . ? N6 Eu2 O21 C26 174.7(6) . . . . ? O11 Eu2 O21 C26 165.9(7) . . . . ? O8 Eu2 O21 Eu3 -68.4(3) 1_455 . . . ? O22 Eu2 O21 Eu3 -139.6(2) 2_565 . . . ? O26 Eu2 O21 Eu3 73.0(3) . . . . ? O15 Eu2 O21 Eu3 148.2(3) . . . . ? N8 Eu2 O21 Eu3 136.0(4) . . . . ? N6 Eu2 O21 Eu3 8.1(4) . . . . ? O11 Eu2 O21 Eu3 -0.8(2) . . . . ? O16 Eu3 O21 C26 100.0(7) 2_665 . . . ? O28 Eu3 O21 C26 -74.6(6) . . . . ? O17 Eu3 O21 C26 143.2(6) . . . . ? O11 Eu3 O21 C26 -166.7(7) . . . . ? O27 Eu3 O21 C26 -102.1(7) . . . . ? N11 Eu3 O21 C26 9.9(6) . . . . ? N9 Eu3 O21 C26 37.0(8) . . . . ? O16 Eu3 O21 Eu2 -92.4(3) 2_665 . . . ? O28 Eu3 O21 Eu2 93.0(3) . . . . ? O17 Eu3 O21 Eu2 -49.3(4) . . . . ? O11 Eu3 O21 Eu2 0.8(2) . . . . ? O27 Eu3 O21 Eu2 65.5(4) . . . . ? N11 Eu3 O21 Eu2 177.5(4) . . . . ? N9 Eu3 O21 Eu2 -155.4(3) . . . . ? O21 C26 O22 Eu2 -102.1(13) . . . 2_565 ? C27 C26 O22 Eu2 78.9(15) . . . 2_565 ? O24 C30 O23 Cu3 177.1(7) . . . . ? C29 C30 O23 Cu3 -2.2(10) . . . . ? N12 Cu3 O23 C30 3.9(6) . . . . ? O19 Cu3 O23 C30 -174.5(6) . . . . ? O23 C30 O24 Eu4 5.4(14) . . . . ? C29 C30 O24 Eu4 -175.3(6) . . . . ? O10 Eu4 O24 C30 -177.5(8) 1_554 . . . ? O31 Eu4 O24 C30 132.1(8) . . . . ? O29 Eu4 O24 C30 -29.9(8) . . . . ? O32 Eu4 O24 C30 -130.7(9) . . . . ? O30 Eu4 O24 C30 57.0(8) . . . . ? O4 Eu4 O24 C30 31.9(10) 2_655 . . . ? O5 Eu4 O24 C30 -80.9(8) 1_554 . . . ? Cu1 Eu4 O24 C30 -42.6(9) 1_554 . . . ? 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 O27 H27A O2 0.79 2.29 3.059(9) 165.1 2_656 O31 H31A O6 0.84 2.58 3.287(11) 142.4 1_454 O32 H32B O9 0.85 2.03 2.833(8) 158.3 2_665 O30 H30A O18 0.84 2.36 3.073(8) 142.0 2_655 O30 H30A O3 0.84 2.07 2.774(9) 140.3 2_655 O31 H31B O13 0.84 1.80 2.636(9) 171.7 2_565 O30 H30B O14 0.83 1.92 2.724(9) 165.1 2_565 O25 H25B O24 0.84 1.98 2.795(9) 163.0 2_565 O32 H32A O6 0.85 1.92 2.730(10) 158.1 1_554 O29 H29B O1 0.85 1.91 2.697(9) 153.1 1_554 O28 H28A O20 0.85 1.91 2.670(8) 148.9 2_655 O27 H27B O20 0.91 2.52 3.158(9) 127.1 2_655 O27 H27B O19 0.91 1.90 2.762(8) 156.5 2_655 O26 H26C O16 0.85 2.41 3.223(8) 159.5 2_665 O26 H26C O15 0.85 1.95 2.645(9) 137.9 2_665 O26 H26A O22 0.85 2.47 3.041(9) 125.3 2_665 O28 H28C O7 0.85 1.89 2.736(9) 175.2 1_455 O25 H25A O6 0.85 1.97 2.789(9) 163.6 1_455 O29 H29A O23 0.84 1.90 2.650(9) 148.3 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.895 _refine_diff_density_min -1.774 _refine_diff_density_rms 0.407 _database_code_depnum_ccdc_archive 'CCDC 931530' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 Cu3 Gd4 N12 O32' _chemical_formula_sum 'C30 H22 Cu3 Gd4 N12 O32' _chemical_formula_weight 1882.22 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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.99920(10) _cell_length_b 17.1837(3) _cell_length_c 19.8953(3) _cell_angle_alpha 66.2160(10) _cell_angle_beta 84.592(2) _cell_angle_gamma 81.0060(10) _cell_volume 2161.42(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9586 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 30.02 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.892 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1770 _exptl_absorpt_coefficient_mu 7.622 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6577 _exptl_absorpt_correction_T_max 0.8036 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39950 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_unetI/netI 0.0517 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.63 _diffrn_reflns_theta_max 27.88 _reflns_number_total 10103 _reflns_number_gt 7869 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10103 _refine_ls_number_parameters 730 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0661 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 0.75929(4) 0.102860(16) 0.298913(13) 0.00844(6) Uani 1 1 d . . . Gd2 Gd 0.18807(4) 0.446092(15) 0.111263(13) 0.00751(6) Uani 1 1 d . . . Gd3 Gd 0.41623(4) 0.213866(16) 0.091409(13) 0.00835(6) Uani 1 1 d . . . Gd4 Gd 0.40548(4) 0.271014(16) -0.397399(13) 0.01049(6) Uani 1 1 d . . . Cu1 Cu 0.75210(10) 0.15590(4) 0.50813(3) 0.01163(14) Uani 1 1 d . . . Cu2 Cu 0.15745(9) 0.54556(4) 0.29178(3) 0.01098(14) Uani 1 1 d . . . Cu3 Cu 0.55263(9) 0.12591(4) -0.09524(3) 0.01156(14) Uani 1 1 d . . . C1 C 0.8452(7) -0.0032(3) 0.6181(3) 0.0088(10) Uani 1 1 d . . . C2 C 0.7915(7) -0.0198(3) 0.5553(3) 0.0110(11) Uani 1 1 d . . . C3 C 0.7642(7) -0.0890(3) 0.5407(3) 0.0120(11) Uani 1 1 d . . . H3 H 0.7765 -0.1478 0.5733 0.014 Uiso 1 1 calc R . . C4 C 0.7141(7) -0.0529(3) 0.4670(3) 0.0114(11) Uani 1 1 d . . . C5 C 0.6499(8) -0.0865(3) 0.4170(3) 0.0109(11) Uani 1 1 d . . . C6 C 0.7630(8) 0.3306(3) 0.4614(3) 0.0116(11) Uani 1 1 d . . . C7 C 0.7942(7) 0.3102(3) 0.3956(3) 0.0103(11) Uani 1 1 d . . . C8 C 0.8344(8) 0.3554(3) 0.3212(3) 0.0151(12) Uani 1 1 d . . . H8 H 0.8518 0.4141 0.2962 0.018 Uiso 1 1 calc R . . C9 C 0.8427(8) 0.2935(3) 0.2922(3) 0.0102(11) Uani 1 1 d . . . C10 C 0.8919(7) 0.2963(3) 0.2176(3) 0.0112(11) Uani 1 1 d . . . C11 C 0.2923(8) 0.4087(3) 0.4170(3) 0.0124(11) Uani 1 1 d . . . C12 C 0.2975(7) 0.3747(3) 0.3593(3) 0.0104(11) Uani 1 1 d . . . C13 C 0.3580(7) 0.2958(3) 0.3563(3) 0.0108(11) Uani 1 1 d . . . H13 H 0.4068 0.2437 0.3947 0.013 Uiso 1 1 calc R . . C14 C 0.3303(7) 0.3109(3) 0.2831(3) 0.0078(10) Uani 1 1 d . . . C15 C 0.3752(7) 0.2528(3) 0.2449(3) 0.0119(11) Uani 1 1 d . . . C16 C 0.1010(8) 0.7231(3) 0.2223(3) 0.0131(11) Uani 1 1 d . . . C17 C 0.1392(7) 0.6906(3) 0.1628(3) 0.0106(11) Uani 1 1 d . . . C18 C 0.1672(7) 0.7248(3) 0.0875(3) 0.0123(11) Uani 1 1 d . . . H18 H 0.1610 0.7836 0.0553 0.015 Uiso 1 1 calc R . . C19 C 0.2066(7) 0.6539(3) 0.0697(3) 0.0108(11) Uani 1 1 d . . . C20 C 0.2735(7) 0.6431(3) 0.0015(3) 0.0094(10) Uani 1 1 d . . . C21 C 0.7667(7) 0.0595(3) 0.1747(3) 0.0101(11) Uani 1 1 d . . . C22 C 0.7398(7) 0.0400(3) 0.1110(3) 0.0109(11) Uani 1 1 d . . . C23 C 0.8188(8) -0.0271(3) 0.0908(3) 0.0128(11) Uani 1 1 d . . . H23 H 0.8998 -0.0780 0.1181 0.015 Uiso 1 1 calc R . . C24 C 0.7495(7) -0.0010(3) 0.0205(3) 0.0103(11) Uani 1 1 d . . . C25 C 0.7752(8) -0.0336(3) -0.0388(3) 0.0123(11) Uani 1 1 d . . . C26 C 0.2142(7) 0.4010(3) -0.0375(3) 0.0086(10) Uani 1 1 d . . . C27 C 0.2857(7) 0.3483(3) -0.0795(3) 0.0094(11) Uani 1 1 d . . . C28 C 0.2812(7) 0.3675(3) -0.1549(3) 0.0101(11) Uani 1 1 d . . . H28 H 0.2330 0.4200 -0.1929 0.012 Uiso 1 1 calc R . . C29 C 0.3639(7) 0.2918(3) -0.1608(3) 0.0095(11) Uani 1 1 d . . . C30 C 0.4102(7) 0.2596(3) -0.2203(3) 0.0122(11) Uani 1 1 d . . . N1 N 0.7611(6) 0.0524(3) 0.4933(2) 0.0098(9) Uani 1 1 d . . . N2 N 0.7175(6) 0.0331(3) 0.4390(2) 0.0107(9) Uani 1 1 d . . . N3 N 0.7778(6) 0.2288(3) 0.4075(2) 0.0119(9) Uani 1 1 d . . . N4 N 0.8088(6) 0.2167(3) 0.3447(2) 0.0110(9) Uani 1 1 d . . . N5 N 0.2384(6) 0.4327(3) 0.2925(2) 0.0106(9) Uani 1 1 d . . . N6 N 0.2583(6) 0.3943(3) 0.2454(2) 0.0092(9) Uani 1 1 d . . . N7 N 0.1585(6) 0.6042(3) 0.1877(2) 0.0101(9) Uani 1 1 d . . . N8 N 0.1987(6) 0.5800(3) 0.1315(2) 0.0115(9) Uani 1 1 d . . . N9 N 0.6274(6) 0.1016(3) 0.0586(2) 0.0098(9) Uani 1 1 d . . . N10 N 0.6371(6) 0.0756(3) 0.0032(2) 0.0101(9) Uani 1 1 d . . . N11 N 0.3694(6) 0.2655(3) -0.0434(2) 0.0102(9) Uani 1 1 d . . . N12 N 0.4126(6) 0.2319(3) -0.0934(2) 0.0105(9) Uani 1 1 d . . . O1 O 0.8261(5) 0.0750(2) 0.60874(19) 0.0140(8) Uani 1 1 d . . . O2 O 0.9114(5) -0.0645(2) 0.67530(18) 0.0133(8) Uani 1 1 d . . . O3 O 0.6387(5) -0.0355(2) 0.35000(18) 0.0138(8) Uani 1 1 d . . . O4 O 0.6005(5) -0.1620(2) 0.44253(19) 0.0141(8) Uani 1 1 d . . . O5 O 0.7192(5) 0.2647(2) 0.52210(19) 0.0137(8) Uani 1 1 d . . . O6 O 0.7788(6) 0.4011(2) 0.4605(2) 0.0225(9) Uani 1 1 d . . . O7 O 0.8828(5) 0.2283(2) 0.20821(18) 0.0132(8) Uani 1 1 d . . . O8 O 0.9368(5) 0.3651(2) 0.16738(18) 0.0111(8) Uani 1 1 d . . . O9 O 0.2374(6) 0.4890(2) 0.39695(19) 0.0156(8) Uani 1 1 d . . . O10 O 0.3410(5) 0.3590(2) 0.48011(19) 0.0160(8) Uani 1 1 d . . . O11 O 0.3336(5) 0.2815(2) 0.17779(18) 0.0119(8) Uani 1 1 d . . . O12 O 0.4524(5) 0.1775(2) 0.28144(18) 0.0112(8) Uani 1 1 d . . . O13 O 0.1248(5) 0.6638(2) 0.28796(19) 0.0151(8) Uani 1 1 d . . . O14 O 0.0496(6) 0.8002(2) 0.20873(19) 0.0172(9) Uani 1 1 d . . . O15 O 0.2742(5) 0.5684(2) 0.00209(18) 0.0124(8) Uani 1 1 d . . . O16 O 0.3339(5) 0.7043(2) -0.05188(18) 0.0100(8) Uani 1 1 d . . . O17 O 0.6663(5) 0.1286(2) 0.17671(18) 0.0118(8) Uani 1 1 d . . . O18 O 0.8798(5) 0.0148(2) 0.22507(19) 0.0144(8) Uani 1 1 d . . . O19 O 0.6994(5) 0.0205(2) -0.10068(19) 0.0134(8) Uani 1 1 d . . . O20 O 0.8599(6) -0.1053(2) -0.02861(19) 0.0175(9) Uani 1 1 d . . . O21 O 0.2691(5) 0.3728(2) 0.02946(18) 0.0113(8) Uani 1 1 d . . . O22 O 0.1055(5) 0.4698(2) -0.06678(19) 0.0112(8) Uani 1 1 d . . . O23 O 0.4949(5) 0.1819(2) -0.19910(18) 0.0140(8) Uani 1 1 d . . . O24 O 0.3693(5) 0.3043(2) -0.28643(18) 0.0139(8) Uani 1 1 d . . . O25 O -0.1564(5) 0.5337(2) 0.32472(18) 0.0136(8) Uani 1 1 d . . . H25A H -0.1560 0.4963 0.3683 0.016 Uiso 1 1 d R . . H25B H -0.2027 0.5844 0.3173 0.016 Uiso 1 1 d R . . O26 O 0.5280(5) 0.4419(2) 0.1149(2) 0.0150(8) Uani 1 1 d . . . H26A H 0.5574 0.4926 0.0947 0.018 Uiso 1 1 d R . . H26C H 0.5856 0.4122 0.0918 0.018 Uiso 1 1 d R . . O27 O 0.3074(5) 0.0778(2) 0.18034(19) 0.0167(8) Uani 1 1 d . . . H27A H 0.2364 0.0702 0.2148 0.020 Uiso 1 1 d R . . H27B H 0.2686 0.0474 0.1566 0.020 Uiso 1 1 d R . . O28 O 0.0752(5) 0.2278(2) 0.08178(18) 0.0137(8) Uani 1 1 d . . . H28C H 0.0184 0.2250 0.1222 0.016 Uiso 1 1 d R . . H28A H 0.0548 0.1863 0.0718 0.016 Uiso 1 1 d R . . O29 O 0.6562(6) 0.1781(2) -0.3236(2) 0.0209(9) Uani 1 1 d . . . H29A H 0.6406 0.1652 -0.2784 0.025 Uiso 1 1 d R . . H29B H 0.7346 0.1415 -0.3340 0.025 Uiso 1 1 d R . . O30 O 0.2067(6) 0.1718(2) -0.3110(2) 0.0196(9) Uani 1 1 d . . . H30A H 0.2146 0.1202 -0.3056 0.023 Uiso 1 1 d R . . H30B H 0.1422 0.1868 -0.2803 0.023 Uiso 1 1 d R . . O31 O 0.0844(6) 0.3411(3) -0.4060(2) 0.0225(9) Uani 1 1 d . . . H31A H 0.0298 0.3784 -0.4434 0.027 Uiso 1 1 d R . . H31B H 0.0093 0.3380 -0.3697 0.027 Uiso 1 1 d R . . O32 O 0.5419(6) 0.3985(2) -0.4211(2) 0.0231(10) Uani 1 1 d . . . H32A H 0.6095 0.4131 -0.4608 0.028 Uiso 1 1 d R . . H32B H 0.5978 0.4241 -0.4014 0.028 Uiso 1 1 d 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 Gd1 0.01072(13) 0.00737(12) 0.00631(12) -0.00198(9) -0.00185(9) 0.00035(10) Gd2 0.00911(13) 0.00651(12) 0.00576(12) -0.00168(9) -0.00073(9) 0.00043(10) Gd3 0.01022(13) 0.00752(12) 0.00602(12) -0.00197(9) -0.00089(9) 0.00089(10) Gd4 0.01563(14) 0.00903(12) 0.00621(12) -0.00287(10) -0.00161(10) 0.00042(11) Cu1 0.0184(4) 0.0083(3) 0.0072(3) -0.0024(2) -0.0011(3) -0.0008(3) Cu2 0.0168(3) 0.0084(3) 0.0070(3) -0.0028(2) -0.0024(3) 0.0012(3) Cu3 0.0158(3) 0.0102(3) 0.0075(3) -0.0033(2) -0.0032(3) 0.0029(3) C1 0.007(2) 0.011(3) 0.008(2) -0.004(2) 0.0026(19) 0.001(2) C2 0.009(3) 0.008(2) 0.011(3) 0.002(2) -0.003(2) 0.002(2) C3 0.012(3) 0.017(3) 0.009(3) -0.006(2) 0.000(2) -0.003(2) C4 0.011(3) 0.013(3) 0.011(3) -0.003(2) 0.001(2) -0.006(2) C5 0.016(3) 0.010(3) 0.005(2) -0.0006(19) -0.001(2) -0.002(2) C6 0.013(3) 0.008(2) 0.012(3) -0.002(2) 0.003(2) -0.002(2) C7 0.012(3) 0.007(2) 0.011(3) -0.003(2) -0.002(2) 0.002(2) C8 0.018(3) 0.013(3) 0.015(3) -0.007(2) 0.005(2) -0.008(2) C9 0.016(3) 0.005(2) 0.005(2) 0.0012(19) 0.002(2) 0.000(2) C10 0.006(3) 0.010(3) 0.018(3) -0.006(2) -0.002(2) -0.001(2) C11 0.012(3) 0.013(3) 0.010(3) -0.003(2) -0.003(2) 0.000(2) C12 0.012(3) 0.009(3) 0.010(3) -0.004(2) 0.001(2) -0.003(2) C13 0.013(3) 0.011(3) 0.008(2) -0.003(2) 0.002(2) -0.006(2) C14 0.010(3) 0.007(2) 0.005(2) -0.0007(19) -0.0024(19) -0.001(2) C15 0.010(3) 0.015(3) 0.010(3) -0.003(2) 0.001(2) -0.005(2) C16 0.016(3) 0.011(3) 0.014(3) -0.008(2) 0.000(2) 0.001(2) C17 0.012(3) 0.011(3) 0.010(3) -0.006(2) 0.000(2) -0.001(2) C18 0.014(3) 0.012(3) 0.010(3) -0.004(2) 0.004(2) -0.001(2) C19 0.011(3) 0.007(2) 0.012(3) -0.001(2) 0.001(2) -0.002(2) C20 0.005(2) 0.013(3) 0.009(2) -0.004(2) -0.0013(19) 0.003(2) C21 0.013(3) 0.009(2) 0.008(2) -0.003(2) 0.003(2) -0.004(2) C22 0.011(3) 0.014(3) 0.005(2) -0.003(2) -0.003(2) 0.003(2) C23 0.015(3) 0.009(3) 0.011(3) -0.001(2) 0.001(2) -0.002(2) C24 0.011(3) 0.007(2) 0.013(3) -0.005(2) -0.003(2) 0.002(2) C25 0.015(3) 0.009(3) 0.014(3) -0.005(2) 0.001(2) -0.001(2) C26 0.004(2) 0.010(3) 0.009(2) -0.0017(19) -0.0012(19) 0.001(2) C27 0.008(3) 0.008(2) 0.010(2) -0.0004(19) -0.004(2) -0.001(2) C28 0.012(3) 0.009(2) 0.008(2) 0.000(2) -0.004(2) -0.002(2) C29 0.008(3) 0.010(2) 0.009(2) -0.003(2) 0.001(2) 0.001(2) C30 0.010(3) 0.015(3) 0.011(3) -0.005(2) -0.003(2) 0.002(2) N1 0.011(2) 0.013(2) 0.007(2) -0.0045(17) -0.0024(17) -0.0024(19) N2 0.011(2) 0.014(2) 0.007(2) -0.0036(17) -0.0018(17) -0.0011(19) N3 0.018(2) 0.009(2) 0.009(2) -0.0040(17) -0.0030(18) -0.0012(19) N4 0.011(2) 0.012(2) 0.009(2) -0.0045(17) -0.0033(17) 0.0040(19) N5 0.015(2) 0.009(2) 0.008(2) -0.0039(17) -0.0020(18) 0.0005(19) N6 0.011(2) 0.009(2) 0.006(2) -0.0009(16) 0.0004(17) -0.0002(18) N7 0.012(2) 0.009(2) 0.010(2) -0.0051(17) -0.0039(17) 0.0037(18) N8 0.009(2) 0.014(2) 0.011(2) -0.0046(18) -0.0014(18) -0.0004(19) N9 0.013(2) 0.007(2) 0.011(2) -0.0058(17) -0.0027(18) 0.0013(18) N10 0.013(2) 0.009(2) 0.008(2) -0.0027(17) -0.0027(17) 0.0014(19) N11 0.009(2) 0.009(2) 0.013(2) -0.0064(18) -0.0013(17) 0.0039(18) N12 0.014(2) 0.009(2) 0.008(2) -0.0043(17) -0.0009(18) 0.0027(19) O1 0.018(2) 0.0136(19) 0.0113(19) -0.0057(15) -0.0051(15) 0.0000(17) O2 0.016(2) 0.0132(19) 0.0087(18) -0.0017(15) -0.0050(15) -0.0011(16) O3 0.021(2) 0.0124(19) 0.0079(18) -0.0033(15) -0.0023(15) -0.0031(17) O4 0.019(2) 0.0140(19) 0.0093(18) -0.0048(15) 0.0012(15) -0.0031(17) O5 0.020(2) 0.0109(18) 0.0099(18) -0.0048(15) 0.0017(16) -0.0010(16) O6 0.041(3) 0.015(2) 0.015(2) -0.0082(16) 0.0081(18) -0.011(2) O7 0.020(2) 0.0108(18) 0.0088(18) -0.0038(14) 0.0003(15) -0.0025(17) O8 0.0134(19) 0.0089(18) 0.0074(17) 0.0012(14) -0.0045(14) -0.0013(15) O9 0.025(2) 0.0099(19) 0.0111(19) -0.0048(15) -0.0079(16) 0.0043(17) O10 0.020(2) 0.016(2) 0.0098(19) -0.0031(15) -0.0058(16) 0.0033(17) O11 0.0133(19) 0.0114(18) 0.0099(18) -0.0035(14) -0.0017(15) 0.0005(16) O12 0.0111(19) 0.0104(18) 0.0097(18) -0.0031(14) 0.0000(14) 0.0030(15) O13 0.024(2) 0.0083(18) 0.0101(19) -0.0013(14) 0.0006(16) -0.0015(17) O14 0.025(2) 0.0106(19) 0.014(2) -0.0057(15) 0.0016(17) 0.0027(18) O15 0.017(2) 0.0101(18) 0.0077(18) -0.0007(14) 0.0007(15) -0.0017(16) O16 0.0107(18) 0.0083(17) 0.0077(17) 0.0001(14) -0.0024(14) 0.0007(15) O17 0.016(2) 0.0103(18) 0.0086(18) -0.0034(14) -0.0046(15) 0.0024(16) O18 0.014(2) 0.016(2) 0.0138(19) -0.0085(16) -0.0046(16) 0.0065(17) O19 0.015(2) 0.0139(19) 0.0126(19) -0.0085(15) -0.0035(15) 0.0036(16) O20 0.028(2) 0.0124(19) 0.0119(19) -0.0068(15) -0.0009(17) 0.0043(18) O21 0.0126(19) 0.0133(19) 0.0068(17) -0.0040(14) -0.0028(14) 0.0027(16) O22 0.0107(19) 0.0068(17) 0.0142(19) -0.0033(14) -0.0035(15) 0.0033(15) O23 0.021(2) 0.0136(19) 0.0047(17) -0.0038(14) -0.0049(15) 0.0077(17) O24 0.017(2) 0.0144(19) 0.0064(18) -0.0016(15) -0.0010(15) 0.0023(17) O25 0.019(2) 0.0058(17) 0.0109(18) 0.0007(14) -0.0001(15) 0.0021(16) O26 0.0108(19) 0.0129(19) 0.022(2) -0.0101(16) 0.0044(16) 0.0020(16) O27 0.022(2) 0.015(2) 0.0124(19) -0.0039(15) 0.0013(16) -0.0052(17) O28 0.019(2) 0.016(2) 0.0088(18) -0.0071(15) -0.0005(15) -0.0029(17) O29 0.030(2) 0.020(2) 0.0113(19) -0.0092(16) -0.0027(17) 0.0120(19) O30 0.027(2) 0.0119(19) 0.020(2) -0.0083(16) 0.0117(18) -0.0052(18) O31 0.022(2) 0.030(2) 0.012(2) -0.0086(17) -0.0001(17) 0.0082(19) O32 0.029(2) 0.028(2) 0.019(2) -0.0141(18) 0.0053(18) -0.014(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 Gd1 O12 2.302(3) . ? Gd1 O2 2.342(4) 2_756 ? Gd1 O7 2.408(3) . ? Gd1 O17 2.423(3) . ? Gd1 O3 2.433(3) . ? Gd1 O18 2.513(4) . ? Gd1 N4 2.546(4) . ? Gd1 N2 2.560(4) . ? Gd1 C21 2.849(5) . ? Gd2 O8 2.327(3) 1_455 ? Gd2 O22 2.340(3) 2_565 ? Gd2 O26 2.376(3) . ? Gd2 O21 2.411(3) . ? Gd2 O15 2.443(3) . ? Gd2 N8 2.503(4) . ? Gd2 N6 2.520(4) . ? Gd2 O11 2.669(3) . ? Gd3 O16 2.296(3) 2_665 ? Gd3 O28 2.379(4) . ? Gd3 O17 2.417(3) . ? Gd3 O11 2.419(4) . ? Gd3 O27 2.479(3) . ? Gd3 N11 2.498(4) . ? Gd3 N9 2.506(4) . ? Gd3 O21 2.585(3) . ? Gd4 O10 2.335(3) 1_554 ? Gd4 O29 2.345(4) . ? Gd4 O31 2.364(4) . ? Gd4 O32 2.381(4) . ? Gd4 O4 2.389(4) 2_655 ? Gd4 O30 2.392(3) . ? Gd4 O24 2.477(4) . ? Gd4 O5 2.608(4) 1_554 ? Cu1 N3 1.895(4) . ? Cu1 N1 1.908(4) . ? Cu1 O5 1.974(4) . ? Cu1 O1 1.983(3) . ? Cu2 N7 1.902(4) . ? Cu2 N5 1.928(4) . ? Cu2 O13 1.980(4) . ? Cu2 O9 2.011(3) . ? Cu2 O25 2.249(4) . ? Cu3 N10 1.904(4) . ? Cu3 N12 1.941(4) . ? Cu3 O23 1.947(3) . ? Cu3 O19 1.976(4) . ? C1 O2 1.265(6) . ? C1 O1 1.267(6) . ? C1 C2 1.481(7) . ? C2 N1 1.356(6) . ? C2 C3 1.376(7) . ? C3 C4 1.397(7) . ? C3 H3 0.9500 . ? C4 N2 1.356(6) . ? C4 C5 1.468(7) . ? C5 O3 1.268(6) . ? C5 O4 1.278(6) . ? C6 O6 1.226(6) . ? C6 O5 1.331(6) . ? C6 C7 1.475(7) . ? C7 N3 1.344(6) . ? C7 C8 1.392(7) . ? C8 C9 1.390(7) . ? C8 H8 0.9500 . ? C9 N4 1.352(6) . ? C9 C10 1.475(7) . ? C10 O8 1.264(6) . ? C10 O7 1.268(6) . ? C11 O10 1.244(6) . ? C11 O9 1.276(6) . ? C11 C12 1.479(7) . ? C12 N5 1.355(6) . ? C12 C13 1.379(7) . ? C13 C14 1.399(7) . ? C13 H13 0.9500 . ? C14 N6 1.360(6) . ? C14 C15 1.463(7) . ? C15 O12 1.262(6) . ? C15 O11 1.268(6) . ? C16 O14 1.241(6) . ? C16 O13 1.299(6) . ? C16 C17 1.486(7) . ? C17 N7 1.352(6) . ? C17 C18 1.378(7) . ? C18 C19 1.383(7) . ? C18 H18 0.9500 . ? C19 N8 1.371(6) . ? C19 C20 1.467(7) . ? C20 O16 1.251(6) . ? C20 O15 1.278(6) . ? C21 O18 1.249(6) . ? C21 O17 1.295(6) . ? C21 C22 1.470(7) . ? C22 N9 1.352(6) . ? C22 C23 1.389(7) . ? C23 C24 1.396(7) . ? C23 H23 0.9500 . ? C24 N10 1.354(6) . ? C24 C25 1.482(7) . ? C25 O20 1.226(6) . ? C25 O19 1.307(6) . ? C26 O22 1.250(6) . ? C26 O21 1.295(6) . ? C26 C27 1.469(7) . ? C27 N11 1.370(6) . ? C27 C28 1.402(7) . ? C28 C29 1.385(7) . ? C28 H28 0.9500 . ? C29 N12 1.355(6) . ? C29 C30 1.487(7) . ? C30 O24 1.261(6) . ? C30 O23 1.288(6) . ? N1 N2 1.324(6) . ? N3 N4 1.340(6) . ? N5 N6 1.333(6) . ? N7 N8 1.335(6) . ? N9 N10 1.337(6) . ? N11 N12 1.330(6) . ? O2 Gd1 2.342(4) 2_756 ? O4 Gd4 2.389(4) 2_655 ? O5 Gd4 2.608(4) 1_556 ? O8 Gd2 2.327(3) 1_655 ? O10 Gd4 2.335(3) 1_556 ? O16 Gd3 2.296(3) 2_665 ? O22 Gd2 2.340(3) 2_565 ? O25 H25A 0.8451 . ? O25 H25B 0.8382 . ? O26 H26A 0.8501 . ? O26 H26C 0.8500 . ? O27 H27A 0.7860 . ? O27 H27B 0.9143 . ? O28 H28C 0.8500 . ? O28 H28A 0.8495 . ? O29 H29A 0.8368 . ? O29 H29B 0.8459 . ? O30 H30A 0.8423 . ? O30 H30B 0.8257 . ? O31 H31A 0.8387 . ? O31 H31B 0.8410 . ? O32 H32A 0.8471 . ? O32 H32B 0.8496 . ? 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 O12 Gd1 O2 161.49(12) . 2_756 ? O12 Gd1 O7 89.12(12) . . ? O2 Gd1 O7 80.72(12) 2_756 . ? O12 Gd1 O17 71.98(12) . . ? O2 Gd1 O17 117.67(12) 2_756 . ? O7 Gd1 O17 68.96(12) . . ? O12 Gd1 O3 92.86(12) . . ? O2 Gd1 O3 102.25(12) 2_756 . ? O7 Gd1 O3 158.60(12) . . ? O17 Gd1 O3 91.41(11) . . ? O12 Gd1 O18 119.41(12) . . ? O2 Gd1 O18 76.71(12) 2_756 . ? O7 Gd1 O18 92.26(12) . . ? O17 Gd1 O18 52.78(12) . . ? O3 Gd1 O18 68.26(12) . . ? O12 Gd1 N4 81.55(13) . . ? O2 Gd1 N4 80.12(13) 2_756 . ? O7 Gd1 N4 64.53(12) . . ? O17 Gd1 N4 126.15(12) . . ? O3 Gd1 N4 136.83(12) . . ? O18 Gd1 N4 149.56(13) . . ? O12 Gd1 N2 94.66(13) . . ? O2 Gd1 N2 82.85(12) 2_756 . ? O7 Gd1 N2 137.63(12) . . ? O17 Gd1 N2 151.40(12) . . ? O3 Gd1 N2 63.45(12) . . ? O18 Gd1 N2 121.33(13) . . ? N4 Gd1 N2 74.33(13) . . ? O12 Gd1 C21 95.44(14) . . ? O2 Gd1 C21 98.31(14) 2_756 . ? O7 Gd1 C21 81.62(13) . . ? O17 Gd1 C21 26.92(13) . . ? O3 Gd1 C21 76.97(12) . . ? O18 Gd1 C21 25.98(13) . . ? N4 Gd1 C21 146.00(13) . . ? N2 Gd1 C21 139.53(14) . . ? O8 Gd2 O22 71.34(12) 1_455 2_565 ? O8 Gd2 O26 141.61(12) 1_455 . ? O22 Gd2 O26 146.60(12) 2_565 . ? O8 Gd2 O21 91.67(12) 1_455 . ? O22 Gd2 O21 102.72(12) 2_565 . ? O26 Gd2 O21 85.00(12) . . ? O8 Gd2 O15 142.84(12) 1_455 . ? O22 Gd2 O15 74.42(12) 2_565 . ? O26 Gd2 O15 74.59(12) . . ? O21 Gd2 O15 82.07(12) . . ? O8 Gd2 N8 118.50(13) 1_455 . ? O22 Gd2 N8 75.95(13) 2_565 . ? O26 Gd2 N8 79.95(13) . . ? O21 Gd2 N8 146.38(12) . . ? O15 Gd2 N8 65.03(13) . . ? O8 Gd2 N6 78.18(12) 1_455 . ? O22 Gd2 N6 119.97(13) 2_565 . ? O26 Gd2 N6 74.62(13) . . ? O21 Gd2 N6 129.01(13) . . ? O15 Gd2 N6 133.01(12) . . ? N8 Gd2 N6 75.31(13) . . ? O8 Gd2 O11 70.73(11) 1_455 . ? O22 Gd2 O11 139.82(11) 2_565 . ? O26 Gd2 O11 73.10(11) . . ? O21 Gd2 O11 65.84(11) . . ? O15 Gd2 O11 135.77(12) . . ? N8 Gd2 O11 135.31(12) . . ? N6 Gd2 O11 63.63(12) . . ? O16 Gd3 O28 139.99(12) 2_665 . ? O16 Gd3 O17 77.23(11) 2_665 . ? O28 Gd3 O17 139.57(12) . . ? O16 Gd3 O11 85.94(12) 2_665 . ? O28 Gd3 O11 84.26(12) . . ? O17 Gd3 O11 83.89(12) . . ? O16 Gd3 O27 146.13(12) 2_665 . ? O28 Gd3 O27 72.94(12) . . ? O17 Gd3 O27 68.93(12) . . ? O11 Gd3 O27 91.65(12) . . ? O16 Gd3 N11 82.64(12) 2_665 . ? O28 Gd3 N11 75.92(13) . . ? O17 Gd3 N11 136.91(13) . . ? O11 Gd3 N11 132.41(12) . . ? O27 Gd3 N11 121.73(13) . . ? O16 Gd3 N9 87.95(13) 2_665 . ? O28 Gd3 N9 118.93(13) . . ? O17 Gd3 N9 64.23(13) . . ? O11 Gd3 N9 148.09(12) . . ? O27 Gd3 N9 76.47(13) . . ? N11 Gd3 N9 77.47(13) . . ? O16 Gd3 O21 71.97(11) 2_665 . ? O28 Gd3 O21 68.47(11) . . ? O17 Gd3 O21 138.54(11) . . ? O11 Gd3 O21 67.11(11) . . ? O27 Gd3 O21 137.21(12) . . ? N11 Gd3 O21 65.41(12) . . ? N9 Gd3 O21 139.35(12) . . ? O10 Gd4 O29 141.01(13) 1_554 . ? O10 Gd4 O31 70.17(13) 1_554 . ? O29 Gd4 O31 148.78(13) . . ? O10 Gd4 O32 74.73(13) 1_554 . ? O29 Gd4 O32 95.10(14) . . ? O31 Gd4 O32 93.18(14) . . ? O10 Gd4 O4 81.38(12) 1_554 2_655 ? O29 Gd4 O4 85.79(13) . 2_655 ? O31 Gd4 O4 105.14(13) . 2_655 ? O32 Gd4 O4 142.79(13) . 2_655 ? O10 Gd4 O30 127.22(13) 1_554 . ? O29 Gd4 O30 83.27(13) . . ? O31 Gd4 O30 72.23(13) . . ? O32 Gd4 O30 142.93(13) . . ? O4 Gd4 O30 74.20(12) 2_655 . ? O10 Gd4 O24 130.46(12) 1_554 . ? O29 Gd4 O24 76.56(12) . . ? O31 Gd4 O24 78.17(12) . . ? O32 Gd4 O24 69.96(12) . . ? O4 Gd4 O24 144.82(11) 2_655 . ? O30 Gd4 O24 73.69(12) . . ? O10 Gd4 O5 71.14(12) 1_554 1_554 ? O29 Gd4 O5 69.88(12) . 1_554 ? O31 Gd4 O5 141.21(12) . 1_554 ? O32 Gd4 O5 73.99(12) . 1_554 ? O4 Gd4 O5 71.47(11) 2_655 1_554 ? O30 Gd4 O5 137.40(12) . 1_554 ? O24 Gd4 O5 127.43(11) . 1_554 ? N3 Cu1 N1 96.23(18) . . ? N3 Cu1 O5 83.41(16) . . ? N1 Cu1 O5 175.18(17) . . ? N3 Cu1 O1 159.68(18) . . ? N1 Cu1 O1 82.65(16) . . ? O5 Cu1 O1 99.37(15) . . ? N7 Cu2 N5 95.91(18) . . ? N7 Cu2 O13 82.59(16) . . ? N5 Cu2 O13 169.60(17) . . ? N7 Cu2 O9 163.37(17) . . ? N5 Cu2 O9 83.37(16) . . ? O13 Cu2 O9 95.11(14) . . ? N7 Cu2 O25 104.33(16) . . ? N5 Cu2 O25 98.92(16) . . ? O13 Cu2 O25 91.41(14) . . ? O9 Cu2 O25 92.17(14) . . ? N10 Cu3 N12 98.29(18) . . ? N10 Cu3 O23 173.51(17) . . ? N12 Cu3 O23 82.48(16) . . ? N10 Cu3 O19 83.22(16) . . ? N12 Cu3 O19 177.90(17) . . ? O23 Cu3 O19 95.86(15) . . ? O2 C1 O1 124.0(5) . . ? O2 C1 C2 120.5(5) . . ? O1 C1 C2 115.5(4) . . ? N1 C2 C3 108.8(4) . . ? N1 C2 C1 113.1(4) . . ? C3 C2 C1 138.1(5) . . ? C2 C3 C4 104.0(4) . . ? C2 C3 H3 128.0 . . ? C4 C3 H3 128.0 . . ? N2 C4 C3 110.1(5) . . ? N2 C4 C5 115.5(4) . . ? C3 C4 C5 134.3(5) . . ? O3 C5 O4 123.8(5) . . ? O3 C5 C4 116.3(4) . . ? O4 C5 C4 119.9(4) . . ? O6 C6 O5 123.2(5) . . ? O6 C6 C7 123.3(4) . . ? O5 C6 C7 113.5(4) . . ? N3 C7 C8 109.1(5) . . ? N3 C7 C6 115.1(4) . . ? C8 C7 C6 135.9(5) . . ? C9 C8 C7 103.1(4) . . ? C9 C8 H8 128.5 . . ? C7 C8 H8 128.5 . . ? N4 C9 C8 111.6(4) . . ? N4 C9 C10 116.5(4) . . ? C8 C9 C10 131.8(4) . . ? O8 C10 O7 124.3(5) . . ? O8 C10 C9 119.2(4) . . ? O7 C10 C9 116.5(4) . . ? O10 C11 O9 124.8(5) . . ? O10 C11 C12 119.3(5) . . ? O9 C11 C12 115.9(4) . . ? N5 C12 C13 110.1(5) . . ? N5 C12 C11 115.4(5) . . ? C13 C12 C11 134.4(5) . . ? C12 C13 C14 103.3(4) . . ? C12 C13 H13 128.4 . . ? C14 C13 H13 128.4 . . ? N6 C14 C13 110.4(4) . . ? N6 C14 C15 119.9(4) . . ? C13 C14 C15 129.6(5) . . ? O12 C15 O11 124.7(5) . . ? O12 C15 C14 117.4(4) . . ? O11 C15 C14 118.0(5) . . ? O14 C16 O13 124.4(5) . . ? O14 C16 C17 121.7(5) . . ? O13 C16 C17 113.9(5) . . ? N7 C17 C18 109.3(5) . . ? N7 C17 C16 113.5(4) . . ? C18 C17 C16 137.2(5) . . ? C17 C18 C19 104.2(5) . . ? C17 C18 H18 127.9 . . ? C19 C18 H18 127.9 . . ? N8 C19 C18 110.4(5) . . ? N8 C19 C20 116.2(5) . . ? C18 C19 C20 133.0(4) . . ? O16 C20 O15 123.8(5) . . ? O16 C20 C19 119.8(5) . . ? O15 C20 C19 116.3(4) . . ? O18 C21 O17 119.3(5) . . ? O18 C21 C22 124.4(5) . . ? O17 C21 C22 116.3(4) . . ? O18 C21 Gd1 61.8(3) . . ? O17 C21 Gd1 57.9(2) . . ? C22 C21 Gd1 171.7(4) . . ? N9 C22 C23 112.3(4) . . ? N9 C22 C21 114.9(5) . . ? C23 C22 C21 132.5(5) . . ? C22 C23 C24 102.7(4) . . ? C22 C23 H23 128.6 . . ? C24 C23 H23 128.6 . . ? N10 C24 C23 108.9(5) . . ? N10 C24 C25 114.6(4) . . ? C23 C24 C25 136.5(5) . . ? O20 C25 O19 124.7(5) . . ? O20 C25 C24 121.5(5) . . ? O19 C25 C24 113.8(4) . . ? O22 C26 O21 123.0(5) . . ? O22 C26 C27 120.0(4) . . ? O21 C26 C27 117.0(4) . . ? N11 C27 C28 110.0(5) . . ? N11 C27 C26 119.5(4) . . ? C28 C27 C26 130.4(5) . . ? C29 C28 C27 103.5(4) . . ? C29 C28 H28 128.2 . . ? C27 C28 H28 128.2 . . ? N12 C29 C28 109.7(4) . . ? N12 C29 C30 113.2(4) . . ? C28 C29 C30 137.1(5) . . ? O24 C30 O23 122.2(5) . . ? O24 C30 C29 123.1(5) . . ? O23 C30 C29 114.8(4) . . ? N2 N1 C2 110.2(4) . . ? N2 N1 Cu1 135.0(3) . . ? C2 N1 Cu1 113.9(3) . . ? N1 N2 C4 106.9(4) . . ? N1 N2 Gd1 134.0(3) . . ? C4 N2 Gd1 114.7(3) . . ? N4 N3 C7 110.5(4) . . ? N4 N3 Cu1 134.9(3) . . ? C7 N3 Cu1 113.9(3) . . ? N3 N4 C9 105.8(4) . . ? N3 N4 Gd1 137.0(3) . . ? C9 N4 Gd1 115.9(3) . . ? N6 N5 C12 109.0(4) . . ? N6 N5 Cu2 138.4(3) . . ? C12 N5 Cu2 112.5(3) . . ? N5 N6 C14 107.2(4) . . ? N5 N6 Gd2 133.1(3) . . ? C14 N6 Gd2 119.6(3) . . ? N8 N7 C17 109.9(4) . . ? N8 N7 Cu2 134.5(3) . . ? C17 N7 Cu2 114.9(3) . . ? N7 N8 C19 106.2(4) . . ? N7 N8 Gd2 135.7(3) . . ? C19 N8 Gd2 116.4(3) . . ? N10 N9 C22 105.5(4) . . ? N10 N9 Gd3 135.1(3) . . ? C22 N9 Gd3 118.3(3) . . ? N9 N10 C24 110.6(4) . . ? N9 N10 Cu3 135.0(3) . . ? C24 N10 Cu3 114.1(3) . . ? N12 N11 C27 107.0(4) . . ? N12 N11 Gd3 135.0(3) . . ? C27 N11 Gd3 117.9(3) . . ? N11 N12 C29 109.7(4) . . ? N11 N12 Cu3 136.0(3) . . ? C29 N12 Cu3 113.7(3) . . ? C1 O1 Cu1 113.9(3) . . ? C1 O2 Gd1 124.2(3) . 2_756 ? C5 O3 Gd1 123.9(3) . . ? C5 O4 Gd4 136.4(3) . 2_655 ? C6 O5 Cu1 112.6(3) . . ? C6 O5 Gd4 123.0(3) . 1_556 ? Cu1 O5 Gd4 108.54(15) . 1_556 ? C10 O7 Gd1 124.6(3) . . ? C10 O8 Gd2 145.2(3) . 1_655 ? C11 O9 Cu2 112.6(3) . . ? C11 O10 Gd4 174.6(4) . 1_556 ? C15 O11 Gd3 128.5(3) . . ? C15 O11 Gd2 118.7(3) . . ? Gd3 O11 Gd2 111.90(13) . . ? C15 O12 Gd1 137.4(3) . . ? C16 O13 Cu2 114.0(3) . . ? C20 O15 Gd2 123.2(3) . . ? C20 O16 Gd3 142.9(3) . 2_665 ? C21 O17 Gd3 123.6(3) . . ? C21 O17 Gd1 95.2(3) . . ? Gd3 O17 Gd1 138.83(16) . . ? C21 O18 Gd1 92.2(3) . . ? C25 O19 Cu3 114.0(3) . . ? C26 O21 Gd2 125.3(3) . . ? C26 O21 Gd3 118.3(3) . . ? Gd2 O21 Gd3 115.14(13) . . ? C26 O22 Gd2 154.9(3) . 2_565 ? C30 O23 Cu3 115.4(3) . . ? C30 O24 Gd4 132.2(3) . . ? Cu2 O25 H25A 105.0 . . ? Cu2 O25 H25B 102.3 . . ? H25A O25 H25B 118.6 . . ? Gd2 O26 H26A 109.3 . . ? Gd2 O26 H26C 109.3 . . ? H26A O26 H26C 109.5 . . ? Gd3 O27 H27A 128.9 . . ? Gd3 O27 H27B 111.1 . . ? H27A O27 H27B 105.3 . . ? Gd3 O28 H28C 110.1 . . ? Gd3 O28 H28A 105.9 . . ? H28C O28 H28A 110.6 . . ? Gd4 O29 H29A 116.5 . . ? Gd4 O29 H29B 125.8 . . ? H29A O29 H29B 112.8 . . ? Gd4 O30 H30A 123.2 . . ? Gd4 O30 H30B 117.4 . . ? H30A O30 H30B 118.5 . . ? Gd4 O31 H31A 127.9 . . ? Gd4 O31 H31B 124.4 . . ? H31A O31 H31B 107.1 . . ? Gd4 O32 H32A 111.4 . . ? Gd4 O32 H32B 143.8 . . ? H32A O32 H32B 96.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 N1 -167.3(5) . . . . ? O1 C1 C2 N1 10.4(6) . . . . ? O2 C1 C2 C3 11.9(9) . . . . ? O1 C1 C2 C3 -170.3(6) . . . . ? N1 C2 C3 C4 -0.6(6) . . . . ? C1 C2 C3 C4 -179.9(6) . . . . ? C2 C3 C4 N2 1.7(6) . . . . ? C2 C3 C4 C5 -174.0(6) . . . . ? N2 C4 C5 O3 12.5(7) . . . . ? C3 C4 C5 O3 -172.1(6) . . . . ? N2 C4 C5 O4 -164.3(5) . . . . ? C3 C4 C5 O4 11.2(9) . . . . ? O6 C6 C7 N3 177.6(5) . . . . ? O5 C6 C7 N3 -1.3(7) . . . . ? O6 C6 C7 C8 -4.0(10) . . . . ? O5 C6 C7 C8 177.1(6) . . . . ? N3 C7 C8 C9 -1.0(6) . . . . ? C6 C7 C8 C9 -179.5(6) . . . . ? C7 C8 C9 N4 0.5(6) . . . . ? C7 C8 C9 C10 -175.5(5) . . . . ? N4 C9 C10 O8 -175.6(5) . . . . ? C8 C9 C10 O8 0.2(9) . . . . ? N4 C9 C10 O7 5.4(7) . . . . ? C8 C9 C10 O7 -178.8(5) . . . . ? O10 C11 C12 N5 178.7(5) . . . . ? O9 C11 C12 N5 -1.6(7) . . . . ? O10 C11 C12 C13 -4.7(9) . . . . ? O9 C11 C12 C13 175.0(5) . . . . ? N5 C12 C13 C14 -0.2(6) . . . . ? C11 C12 C13 C14 -176.9(6) . . . . ? C12 C13 C14 N6 0.3(5) . . . . ? C12 C13 C14 C15 177.2(5) . . . . ? N6 C14 C15 O12 175.9(4) . . . . ? C13 C14 C15 O12 -0.8(8) . . . . ? N6 C14 C15 O11 -4.3(7) . . . . ? C13 C14 C15 O11 179.0(5) . . . . ? O14 C16 C17 N7 -168.4(5) . . . . ? O13 C16 C17 N7 11.0(7) . . . . ? O14 C16 C17 C18 14.3(10) . . . . ? O13 C16 C17 C18 -166.3(6) . . . . ? N7 C17 C18 C19 -0.8(6) . . . . ? C16 C17 C18 C19 176.6(6) . . . . ? C17 C18 C19 N8 1.2(6) . . . . ? C17 C18 C19 C20 -171.0(5) . . . . ? N8 C19 C20 O16 -160.9(4) . . . . ? C18 C19 C20 O16 10.9(9) . . . . ? N8 C19 C20 O15 15.9(7) . . . . ? C18 C19 C20 O15 -172.3(5) . . . . ? O12 Gd1 C21 O18 -158.5(3) . . . . ? O2 Gd1 C21 O18 33.9(3) 2_756 . . . ? O7 Gd1 C21 O18 113.2(3) . . . . ? O17 Gd1 C21 O18 172.4(5) . . . . ? O3 Gd1 C21 O18 -66.8(3) . . . . ? N4 Gd1 C21 O18 118.5(3) . . . . ? N2 Gd1 C21 O18 -54.8(4) . . . . ? O12 Gd1 C21 O17 29.1(3) . . . . ? O2 Gd1 C21 O17 -138.5(3) 2_756 . . . ? O7 Gd1 C21 O17 -59.2(3) . . . . ? O3 Gd1 C21 O17 120.8(3) . . . . ? O18 Gd1 C21 O17 -172.4(5) . . . . ? N4 Gd1 C21 O17 -53.9(4) . . . . ? N2 Gd1 C21 O17 132.8(3) . . . . ? O18 C21 C22 N9 -172.8(5) . . . . ? O17 C21 C22 N9 6.3(7) . . . . ? O18 C21 C22 C23 1.7(9) . . . . ? O17 C21 C22 C23 -179.2(5) . . . . ? N9 C22 C23 C24 1.3(6) . . . . ? C21 C22 C23 C24 -173.2(5) . . . . ? C22 C23 C24 N10 -0.6(6) . . . . ? C22 C23 C24 C25 176.1(6) . . . . ? N10 C24 C25 O20 -173.9(5) . . . . ? C23 C24 C25 O20 9.6(10) . . . . ? N10 C24 C25 O19 5.8(7) . . . . ? C23 C24 C25 O19 -170.7(5) . . . . ? O22 C26 C27 N11 -166.2(4) . . . . ? O21 C26 C27 N11 13.9(7) . . . . ? O22 C26 C27 C28 12.4(8) . . . . ? O21 C26 C27 C28 -167.5(5) . . . . ? N11 C27 C28 C29 0.8(6) . . . . ? C26 C27 C28 C29 -178.0(5) . . . . ? C27 C28 C29 N12 0.4(6) . . . . ? C27 C28 C29 C30 179.6(6) . . . . ? N12 C29 C30 O24 177.1(5) . . . . ? C28 C29 C30 O24 -2.1(10) . . . . ? N12 C29 C30 O23 -2.4(7) . . . . ? C28 C29 C30 O23 178.3(6) . . . . ? C3 C2 N1 N2 -0.7(6) . . . . ? C1 C2 N1 N2 178.8(4) . . . . ? C3 C2 N1 Cu1 170.4(3) . . . . ? C1 C2 N1 Cu1 -10.1(5) . . . . ? N3 Cu1 N1 N2 -26.4(5) . . . . ? O1 Cu1 N1 N2 174.0(5) . . . . ? N3 Cu1 N1 C2 165.5(4) . . . . ? O1 Cu1 N1 C2 5.9(4) . . . . ? C2 N1 N2 C4 1.8(6) . . . . ? Cu1 N1 N2 C4 -166.7(4) . . . . ? C2 N1 N2 Gd1 -152.5(4) . . . . ? Cu1 N1 N2 Gd1 39.1(7) . . . . ? C3 C4 N2 N1 -2.2(6) . . . . ? C5 C4 N2 N1 174.4(4) . . . . ? C3 C4 N2 Gd1 157.7(3) . . . . ? C5 C4 N2 Gd1 -25.8(6) . . . . ? O12 Gd1 N2 N1 -95.3(5) . . . . ? O2 Gd1 N2 N1 66.3(4) 2_756 . . . ? O7 Gd1 N2 N1 -1.5(6) . . . . ? O17 Gd1 N2 N1 -155.4(4) . . . . ? O3 Gd1 N2 N1 173.8(5) . . . . ? O18 Gd1 N2 N1 135.9(4) . . . . ? N4 Gd1 N2 N1 -15.4(4) . . . . ? C21 Gd1 N2 N1 160.7(4) . . . . ? O12 Gd1 N2 C4 112.0(4) . . . . ? O2 Gd1 N2 C4 -86.5(4) 2_756 . . . ? O7 Gd1 N2 C4 -154.2(3) . . . . ? O17 Gd1 N2 C4 51.9(5) . . . . ? O3 Gd1 N2 C4 21.1(3) . . . . ? O18 Gd1 N2 C4 -16.8(4) . . . . ? N4 Gd1 N2 C4 -168.2(4) . . . . ? C21 Gd1 N2 C4 8.0(5) . . . . ? C8 C7 N3 N4 1.2(6) . . . . ? C6 C7 N3 N4 -179.9(4) . . . . ? C8 C7 N3 Cu1 173.2(4) . . . . ? C6 C7 N3 Cu1 -7.9(6) . . . . ? N1 Cu1 N3 N4 -5.1(5) . . . . ? O5 Cu1 N3 N4 179.7(5) . . . . ? O1 Cu1 N3 N4 80.5(7) . . . . ? N1 Cu1 N3 C7 -174.6(4) . . . . ? O5 Cu1 N3 C7 10.2(4) . . . . ? O1 Cu1 N3 C7 -88.9(6) . . . . ? C7 N3 N4 C9 -0.9(6) . . . . ? Cu1 N3 N4 C9 -170.6(4) . . . . ? C7 N3 N4 Gd1 -166.8(4) . . . . ? Cu1 N3 N4 Gd1 23.5(8) . . . . ? C8 C9 N4 N3 0.2(6) . . . . ? C10 C9 N4 N3 176.8(4) . . . . ? C8 C9 N4 Gd1 169.6(3) . . . . ? C10 C9 N4 Gd1 -13.8(6) . . . . ? O12 Gd1 N4 N3 83.8(5) . . . . ? O2 Gd1 N4 N3 -98.8(5) 2_756 . . . ? O7 Gd1 N4 N3 176.9(5) . . . . ? O17 Gd1 N4 N3 144.1(4) . . . . ? O3 Gd1 N4 N3 -1.3(6) . . . . ? O18 Gd1 N4 N3 -139.5(4) . . . . ? N2 Gd1 N4 N3 -13.5(5) . . . . ? C21 Gd1 N4 N3 171.0(4) . . . . ? O12 Gd1 N4 C9 -81.1(4) . . . . ? O2 Gd1 N4 C9 96.3(4) 2_756 . . . ? O7 Gd1 N4 C9 12.0(3) . . . . ? O17 Gd1 N4 C9 -20.8(4) . . . . ? O3 Gd1 N4 C9 -166.3(3) . . . . ? O18 Gd1 N4 C9 55.6(5) . . . . ? N2 Gd1 N4 C9 -178.4(4) . . . . ? C21 Gd1 N4 C9 6.1(5) . . . . ? C13 C12 N5 N6 0.0(6) . . . . ? C11 C12 N5 N6 177.3(4) . . . . ? C13 C12 N5 Cu2 -178.5(3) . . . . ? C11 C12 N5 Cu2 -1.2(6) . . . . ? N7 Cu2 N5 N6 -12.3(5) . . . . ? O13 Cu2 N5 N6 -93.5(10) . . . . ? O9 Cu2 N5 N6 -175.6(5) . . . . ? O25 Cu2 N5 N6 93.2(5) . . . . ? N7 Cu2 N5 C12 165.6(4) . . . . ? O13 Cu2 N5 C12 84.4(10) . . . . ? O9 Cu2 N5 C12 2.3(3) . . . . ? O25 Cu2 N5 C12 -88.9(4) . . . . ? C12 N5 N6 C14 0.2(5) . . . . ? Cu2 N5 N6 C14 178.2(4) . . . . ? C12 N5 N6 Gd2 179.6(3) . . . . ? Cu2 N5 N6 Gd2 -2.5(8) . . . . ? C13 C14 N6 N5 -0.3(5) . . . . ? C15 C14 N6 N5 -177.6(4) . . . . ? C13 C14 N6 Gd2 -179.8(3) . . . . ? C15 C14 N6 Gd2 2.9(6) . . . . ? O8 Gd2 N6 N5 -106.0(4) 1_455 . . . ? O22 Gd2 N6 N5 -45.9(5) 2_565 . . . ? O26 Gd2 N6 N5 101.4(4) . . . . ? O21 Gd2 N6 N5 171.5(4) . . . . ? O15 Gd2 N6 N5 50.7(5) . . . . ? N8 Gd2 N6 N5 18.0(4) . . . . ? O11 Gd2 N6 N5 179.8(5) . . . . ? O8 Gd2 N6 C14 73.3(4) 1_455 . . . ? O22 Gd2 N6 C14 133.4(3) 2_565 . . . ? O26 Gd2 N6 C14 -79.3(4) . . . . ? O21 Gd2 N6 C14 -9.1(4) . . . . ? O15 Gd2 N6 C14 -130.0(3) . . . . ? N8 Gd2 N6 C14 -162.7(4) . . . . ? O11 Gd2 N6 C14 -0.9(3) . . . . ? C18 C17 N7 N8 0.1(6) . . . . ? C16 C17 N7 N8 -178.0(4) . . . . ? C18 C17 N7 Cu2 172.3(3) . . . . ? C16 C17 N7 Cu2 -5.8(6) . . . . ? N5 Cu2 N7 N8 0.2(5) . . . . ? O13 Cu2 N7 N8 169.9(5) . . . . ? O9 Cu2 N7 N8 86.9(7) . . . . ? O25 Cu2 N7 N8 -100.6(5) . . . . ? N5 Cu2 N7 C17 -169.4(4) . . . . ? O13 Cu2 N7 C17 0.3(4) . . . . ? O9 Cu2 N7 C17 -82.8(7) . . . . ? O25 Cu2 N7 C17 89.8(4) . . . . ? C17 N7 N8 C19 0.6(5) . . . . ? Cu2 N7 N8 C19 -169.4(4) . . . . ? C17 N7 N8 Gd2 -163.2(4) . . . . ? Cu2 N7 N8 Gd2 26.9(7) . . . . ? C18 C19 N8 N7 -1.2(6) . . . . ? C20 C19 N8 N7 172.5(4) . . . . ? C18 C19 N8 Gd2 166.3(3) . . . . ? C20 C19 N8 Gd2 -20.1(5) . . . . ? O8 Gd2 N8 N7 37.3(5) 1_455 . . . ? O22 Gd2 N8 N7 96.5(5) 2_565 . . . ? O26 Gd2 N8 N7 -106.8(5) . . . . ? O21 Gd2 N8 N7 -171.5(4) . . . . ? O15 Gd2 N8 N7 175.7(5) . . . . ? N6 Gd2 N8 N7 -30.2(4) . . . . ? O11 Gd2 N8 N7 -53.6(5) . . . . ? O8 Gd2 N8 C19 -125.3(3) 1_455 . . . ? O22 Gd2 N8 C19 -66.0(3) 2_565 . . . ? O26 Gd2 N8 C19 90.6(4) . . . . ? O21 Gd2 N8 C19 25.9(5) . . . . ? O15 Gd2 N8 C19 13.1(3) . . . . ? N6 Gd2 N8 C19 167.2(4) . . . . ? O11 Gd2 N8 C19 143.9(3) . . . . ? C23 C22 N9 N10 -1.6(6) . . . . ? C21 C22 N9 N10 174.0(4) . . . . ? C23 C22 N9 Gd3 167.9(3) . . . . ? C21 C22 N9 Gd3 -16.5(6) . . . . ? O16 Gd3 N9 N10 -103.2(4) 2_665 . . . ? O28 Gd3 N9 N10 45.6(5) . . . . ? O17 Gd3 N9 N10 180.0(5) . . . . ? O11 Gd3 N9 N10 177.8(4) . . . . ? O27 Gd3 N9 N10 107.1(4) . . . . ? N11 Gd3 N9 N10 -20.3(4) . . . . ? O21 Gd3 N9 N10 -44.4(5) . . . . ? O16 Gd3 N9 C22 91.3(4) 2_665 . . . ? O28 Gd3 N9 C22 -119.9(3) . . . . ? O17 Gd3 N9 C22 14.5(3) . . . . ? O11 Gd3 N9 C22 12.3(5) . . . . ? O27 Gd3 N9 C22 -58.4(4) . . . . ? N11 Gd3 N9 C22 174.2(4) . . . . ? O21 Gd3 N9 C22 150.1(3) . . . . ? C22 N9 N10 C24 1.1(6) . . . . ? Gd3 N9 N10 C24 -165.6(3) . . . . ? C22 N9 N10 Cu3 -171.3(4) . . . . ? Gd3 N9 N10 Cu3 21.9(7) . . . . ? C23 C24 N10 N9 -0.3(6) . . . . ? C25 C24 N10 N9 -177.8(4) . . . . ? C23 C24 N10 Cu3 173.8(3) . . . . ? C25 C24 N10 Cu3 -3.6(6) . . . . ? N12 Cu3 N10 N9 -5.5(5) . . . . ? O19 Cu3 N10 N9 173.0(5) . . . . ? N12 Cu3 N10 C24 -177.8(4) . . . . ? O19 Cu3 N10 C24 0.8(4) . . . . ? C28 C27 N11 N12 -1.6(5) . . . . ? C26 C27 N11 N12 177.3(4) . . . . ? C28 C27 N11 Gd3 176.6(3) . . . . ? C26 C27 N11 Gd3 -4.5(6) . . . . ? O16 Gd3 N11 N12 101.8(5) 2_665 . . . ? O28 Gd3 N11 N12 -112.2(5) . . . . ? O17 Gd3 N11 N12 39.5(5) . . . . ? O11 Gd3 N11 N12 179.4(4) . . . . ? O27 Gd3 N11 N12 -52.9(5) . . . . ? N9 Gd3 N11 N12 12.3(4) . . . . ? O21 Gd3 N11 N12 175.3(5) . . . . ? O16 Gd3 N11 C27 -75.8(4) 2_665 . . . ? O28 Gd3 N11 C27 70.2(3) . . . . ? O17 Gd3 N11 C27 -138.1(3) . . . . ? O11 Gd3 N11 C27 1.8(4) . . . . ? O27 Gd3 N11 C27 129.5(3) . . . . ? N9 Gd3 N11 C27 -165.3(4) . . . . ? O21 Gd3 N11 C27 -2.3(3) . . . . ? C27 N11 N12 C29 1.8(6) . . . . ? Gd3 N11 N12 C29 -176.0(3) . . . . ? C27 N11 N12 Cu3 172.6(4) . . . . ? Gd3 N11 N12 Cu3 -5.1(8) . . . . ? C28 C29 N12 N11 -1.4(6) . . . . ? C30 C29 N12 N11 179.2(4) . . . . ? C28 C29 N12 Cu3 -174.4(3) . . . . ? C30 C29 N12 Cu3 6.1(5) . . . . ? N10 Cu3 N12 N11 -3.0(5) . . . . ? O23 Cu3 N12 N11 -176.4(5) . . . . ? N10 Cu3 N12 C29 167.6(4) . . . . ? O23 Cu3 N12 C29 -5.9(4) . . . . ? O2 C1 O1 Cu1 172.1(4) . . . . ? C2 C1 O1 Cu1 -5.5(5) . . . . ? N3 Cu1 O1 C1 -88.1(6) . . . . ? N1 Cu1 O1 C1 0.0(3) . . . . ? O5 Cu1 O1 C1 175.6(3) . . . . ? O1 C1 O2 Gd1 -78.0(6) . . . 2_756 ? C2 C1 O2 Gd1 99.6(5) . . . 2_756 ? O4 C5 O3 Gd1 -174.2(4) . . . . ? C4 C5 O3 Gd1 9.1(7) . . . . ? O12 Gd1 O3 C5 -109.9(4) . . . . ? O2 Gd1 O3 C5 59.3(4) 2_756 . . . ? O7 Gd1 O3 C5 155.2(4) . . . . ? O17 Gd1 O3 C5 178.1(4) . . . . ? O18 Gd1 O3 C5 129.5(4) . . . . ? N4 Gd1 O3 C5 -29.2(5) . . . . ? N2 Gd1 O3 C5 -16.1(4) . . . . ? C21 Gd1 O3 C5 155.2(4) . . . . ? O3 C5 O4 Gd4 30.5(8) . . . 2_655 ? C4 C5 O4 Gd4 -152.9(4) . . . 2_655 ? O6 C6 O5 Cu1 -169.4(4) . . . . ? C7 C6 O5 Cu1 9.5(5) . . . . ? O6 C6 O5 Gd4 57.5(6) . . . 1_556 ? C7 C6 O5 Gd4 -123.6(4) . . . 1_556 ? N3 Cu1 O5 C6 -11.0(3) . . . . ? O1 Cu1 O5 C6 148.6(3) . . . . ? N3 Cu1 O5 Gd4 128.71(18) . . . 1_556 ? O1 Cu1 O5 Gd4 -71.63(16) . . . 1_556 ? O8 C10 O7 Gd1 -171.9(4) . . . . ? C9 C10 O7 Gd1 7.0(6) . . . . ? O12 Gd1 O7 C10 70.9(4) . . . . ? O2 Gd1 O7 C10 -93.5(4) 2_756 . . . ? O17 Gd1 O7 C10 141.9(4) . . . . ? O3 Gd1 O7 C10 166.5(4) . . . . ? O18 Gd1 O7 C10 -169.7(4) . . . . ? N4 Gd1 O7 C10 -10.1(4) . . . . ? N2 Gd1 O7 C10 -25.0(5) . . . . ? C21 Gd1 O7 C10 166.5(4) . . . . ? O7 C10 O8 Gd2 -94.3(7) . . . 1_655 ? C9 C10 O8 Gd2 86.8(7) . . . 1_655 ? O10 C11 O9 Cu2 -176.9(4) . . . . ? C12 C11 O9 Cu2 3.4(6) . . . . ? N7 Cu2 O9 C11 -91.7(7) . . . . ? N5 Cu2 O9 C11 -3.2(4) . . . . ? O13 Cu2 O9 C11 -172.9(4) . . . . ? O25 Cu2 O9 C11 95.5(4) . . . . ? O12 C15 O11 Gd3 -8.2(7) . . . . ? C14 C15 O11 Gd3 172.0(3) . . . . ? O12 C15 O11 Gd2 -176.7(4) . . . . ? C14 C15 O11 Gd2 3.4(6) . . . . ? O16 Gd3 O11 C15 -98.1(4) 2_665 . . . ? O28 Gd3 O11 C15 120.7(4) . . . . ? O17 Gd3 O11 C15 -20.5(4) . . . . ? O27 Gd3 O11 C15 48.1(4) . . . . ? N11 Gd3 O11 C15 -174.3(4) . . . . ? N9 Gd3 O11 C15 -18.6(5) . . . . ? O21 Gd3 O11 C15 -170.2(4) . . . . ? O16 Gd3 O11 Gd2 71.12(14) 2_665 . . . ? O28 Gd3 O11 Gd2 -70.03(14) . . . . ? O17 Gd3 O11 Gd2 148.69(15) . . . . ? O27 Gd3 O11 Gd2 -142.70(14) . . . . ? N11 Gd3 O11 Gd2 -5.1(2) . . . . ? N9 Gd3 O11 Gd2 150.65(19) . . . . ? O21 Gd3 O11 Gd2 -1.00(11) . . . . ? O8 Gd2 O11 C15 -87.5(3) 1_455 . . . ? O22 Gd2 O11 C15 -107.5(4) 2_565 . . . ? O26 Gd2 O11 C15 79.4(3) . . . . ? O21 Gd2 O11 C15 171.5(4) . . . . ? O15 Gd2 O11 C15 124.1(3) . . . . ? N8 Gd2 O11 C15 23.9(4) . . . . ? N6 Gd2 O11 C15 -1.5(3) . . . . ? O8 Gd2 O11 Gd3 102.08(15) 1_455 . . . ? O22 Gd2 O11 Gd3 82.0(2) 2_565 . . . ? O26 Gd2 O11 Gd3 -91.00(15) . . . . ? O21 Gd2 O11 Gd3 1.09(12) . . . . ? O15 Gd2 O11 Gd3 -46.3(2) . . . . ? N8 Gd2 O11 Gd3 -146.50(15) . . . . ? N6 Gd2 O11 Gd3 -171.87(18) . . . . ? O11 C15 O12 Gd1 82.7(7) . . . . ? C14 C15 O12 Gd1 -97.4(5) . . . . ? O2 Gd1 O12 C15 52.1(7) 2_756 . . . ? O7 Gd1 O12 C15 -4.3(5) . . . . ? O17 Gd1 O12 C15 -72.4(5) . . . . ? O3 Gd1 O12 C15 -163.0(5) . . . . ? O18 Gd1 O12 C15 -96.4(5) . . . . ? N4 Gd1 O12 C15 60.1(5) . . . . ? N2 Gd1 O12 C15 133.5(5) . . . . ? C21 Gd1 O12 C15 -85.8(5) . . . . ? O14 C16 O13 Cu2 168.7(4) . . . . ? C17 C16 O13 Cu2 -10.7(6) . . . . ? N7 Cu2 O13 C16 6.1(4) . . . . ? N5 Cu2 O13 C16 88.5(10) . . . . ? O9 Cu2 O13 C16 169.6(4) . . . . ? O25 Cu2 O13 C16 -98.1(4) . . . . ? O16 C20 O15 Gd2 173.2(3) . . . . ? C19 C20 O15 Gd2 -3.4(6) . . . . ? O8 Gd2 O15 C20 100.0(4) 1_455 . . . ? O22 Gd2 O15 C20 76.6(4) 2_565 . . . ? O26 Gd2 O15 C20 -90.8(4) . . . . ? O21 Gd2 O15 C20 -177.8(4) . . . . ? N8 Gd2 O15 C20 -4.9(3) . . . . ? N6 Gd2 O15 C20 -40.1(4) . . . . ? O11 Gd2 O15 C20 -135.2(3) . . . . ? O15 C20 O16 Gd3 -107.3(6) . . . 2_665 ? C19 C20 O16 Gd3 69.2(7) . . . 2_665 ? O18 C21 O17 Gd3 -173.1(3) . . . . ? C22 C21 O17 Gd3 7.8(6) . . . . ? Gd1 C21 O17 Gd3 -165.4(3) . . . . ? O18 C21 O17 Gd1 -7.7(5) . . . . ? C22 C21 O17 Gd1 173.2(4) . . . . ? O16 Gd3 O17 C21 -105.6(4) 2_665 . . . ? O28 Gd3 O17 C21 93.6(4) . . . . ? O11 Gd3 O17 C21 167.2(4) . . . . ? O27 Gd3 O17 C21 73.1(4) . . . . ? N11 Gd3 O17 C21 -41.3(4) . . . . ? N9 Gd3 O17 C21 -11.6(4) . . . . ? O21 Gd3 O17 C21 -148.2(3) . . . . ? O16 Gd3 O17 Gd1 96.9(2) 2_665 . . . ? O28 Gd3 O17 Gd1 -64.0(3) . . . . ? O11 Gd3 O17 Gd1 9.7(2) . . . . ? O27 Gd3 O17 Gd1 -84.5(2) . . . . ? N11 Gd3 O17 Gd1 161.11(19) . . . . ? N9 Gd3 O17 Gd1 -169.2(3) . . . . ? O21 Gd3 O17 Gd1 54.3(3) . . . . ? O12 Gd1 O17 C21 -149.4(3) . . . . ? O2 Gd1 O17 C21 47.8(3) 2_756 . . . ? O7 Gd1 O17 C21 114.4(3) . . . . ? O3 Gd1 O17 C21 -56.9(3) . . . . ? O18 Gd1 O17 C21 4.2(3) . . . . ? N4 Gd1 O17 C21 146.0(3) . . . . ? N2 Gd1 O17 C21 -84.1(4) . . . . ? O12 Gd1 O17 Gd3 12.0(2) . . . . ? O2 Gd1 O17 Gd3 -150.8(2) 2_756 . . . ? O7 Gd1 O17 Gd3 -84.2(2) . . . . ? O3 Gd1 O17 Gd3 104.5(2) . . . . ? O18 Gd1 O17 Gd3 165.6(3) . . . . ? N4 Gd1 O17 Gd3 -52.6(3) . . . . ? N2 Gd1 O17 Gd3 77.3(4) . . . . ? C21 Gd1 O17 Gd3 161.4(4) . . . . ? O17 C21 O18 Gd1 7.4(5) . . . . ? C22 C21 O18 Gd1 -173.5(4) . . . . ? O12 Gd1 O18 C21 24.7(3) . . . . ? O2 Gd1 O18 C21 -145.5(3) 2_756 . . . ? O7 Gd1 O18 C21 -65.5(3) . . . . ? O17 Gd1 O18 C21 -4.3(3) . . . . ? O3 Gd1 O18 C21 105.3(3) . . . . ? N4 Gd1 O18 C21 -104.1(3) . . . . ? N2 Gd1 O18 C21 141.6(3) . . . . ? O20 C25 O19 Cu3 174.6(4) . . . . ? C24 C25 O19 Cu3 -5.1(5) . . . . ? N10 Cu3 O19 C25 2.6(4) . . . . ? O23 Cu3 O19 C25 176.1(3) . . . . ? O22 C26 O21 Gd2 -2.3(7) . . . . ? C27 C26 O21 Gd2 177.5(3) . . . . ? O22 C26 O21 Gd3 164.2(4) . . . . ? C27 C26 O21 Gd3 -15.9(5) . . . . ? O8 Gd2 O21 C26 97.9(4) 1_455 . . . ? O22 Gd2 O21 C26 26.7(4) 2_565 . . . ? O26 Gd2 O21 C26 -120.4(4) . . . . ? O15 Gd2 O21 C26 -45.3(4) . . . . ? N8 Gd2 O21 C26 -57.0(4) . . . . ? N6 Gd2 O21 C26 174.0(3) . . . . ? O11 Gd2 O21 C26 165.9(4) . . . . ? O8 Gd2 O21 Gd3 -69.02(15) 1_455 . . . ? O22 Gd2 O21 Gd3 -140.25(14) 2_565 . . . ? O26 Gd2 O21 Gd3 72.67(15) . . . . ? O15 Gd2 O21 Gd3 147.77(16) . . . . ? N8 Gd2 O21 Gd3 136.05(19) . . . . ? N6 Gd2 O21 Gd3 7.1(2) . . . . ? O11 Gd2 O21 Gd3 -1.04(12) . . . . ? O16 Gd3 O21 C26 100.0(3) 2_665 . . . ? O28 Gd3 O21 C26 -73.9(3) . . . . ? O17 Gd3 O21 C26 144.0(3) . . . . ? O11 Gd3 O21 C26 -166.8(4) . . . . ? O27 Gd3 O21 C26 -101.0(3) . . . . ? N11 Gd3 O21 C26 9.9(3) . . . . ? N9 Gd3 O21 C26 35.9(4) . . . . ? O16 Gd3 O21 Gd2 -92.11(16) 2_665 . . . ? O28 Gd3 O21 Gd2 93.99(16) . . . . ? O17 Gd3 O21 Gd2 -48.1(2) . . . . ? O11 Gd3 O21 Gd2 1.14(13) . . . . ? O27 Gd3 O21 Gd2 66.9(2) . . . . ? N11 Gd3 O21 Gd2 177.85(19) . . . . ? N9 Gd3 O21 Gd2 -156.20(16) . . . . ? O21 C26 O22 Gd2 -104.8(8) . . . 2_565 ? C27 C26 O22 Gd2 75.3(9) . . . 2_565 ? O24 C30 O23 Cu3 178.0(4) . . . . ? C29 C30 O23 Cu3 -2.5(6) . . . . ? N12 Cu3 O23 C30 4.6(4) . . . . ? O19 Cu3 O23 C30 -174.1(4) . . . . ? O23 C30 O24 Gd4 3.6(8) . . . . ? C29 C30 O24 Gd4 -176.0(3) . . . . ? O10 Gd4 O24 C30 -176.4(4) 1_554 . . . ? O29 Gd4 O24 C30 -28.6(4) . . . . ? O31 Gd4 O24 C30 132.9(5) . . . . ? O32 Gd4 O24 C30 -129.2(5) . . . . ? O4 Gd4 O24 C30 33.3(5) 2_655 . . . ? O30 Gd4 O24 C30 58.2(4) . . . . ? O5 Gd4 O24 C30 -79.7(5) 1_554 . . . ? 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 O29 H29A O23 0.84 1.89 2.645(5) 149.1 . O25 H25A O6 0.85 1.98 2.796(5) 163.4 1_455 O28 H28C O7 0.85 1.89 2.741(5) 175.3 1_455 O26 H26A O22 0.85 2.50 3.063(5) 124.9 2_665 O26 H26C O15 0.85 1.95 2.648(5) 138.1 2_665 O26 H26C O16 0.85 2.41 3.219(5) 159.6 2_665 O27 H27B O19 0.91 1.89 2.751(5) 156.1 2_655 O27 H27B O20 0.91 2.53 3.170(5) 127.6 2_655 O28 H28A O20 0.85 1.91 2.678(5) 149.9 2_655 O29 H29B O1 0.85 1.92 2.707(5) 153.6 1_554 O32 H32A O6 0.85 1.93 2.739(5) 158.8 1_554 O25 H25B O24 0.84 1.97 2.785(5) 163.5 2_565 O30 H30B O14 0.83 1.92 2.724(5) 164.7 2_565 O31 H31B O13 0.84 1.79 2.627(5) 172.1 2_565 O30 H30A O3 0.84 2.09 2.788(5) 140.5 2_655 O30 H30A O18 0.84 2.38 3.093(5) 142.6 2_655 O32 H32B O9 0.85 2.06 2.860(5) 157.1 2_665 O31 H31A O6 0.84 2.59 3.296(6) 142.6 1_454 O27 H27A O2 0.79 2.30 3.065(5) 164.5 2_656 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.436 _refine_diff_density_min -1.068 _refine_diff_density_rms 0.211 _database_code_depnum_ccdc_archive 'CCDC 931531'