# Electronic Supplementary Material (ESI) for Chemical Communications # 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_www _database_code_depnum_ccdc_archive 'CCDC 927114' #TrackingRef '927114.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H36 Cu5 I8 N6 O34 Sm2' _chemical_formula_sum 'C42 H36 Cu5 I8 N6 O34 Sm2' _chemical_formula_weight 2802.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.3970(10) _cell_length_b 13.5897(13) _cell_length_c 22.542(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.7390(10) _cell_angle_gamma 90.00 _cell_volume 3672.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 17913 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2590 _exptl_absorpt_coefficient_mu 6.440 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2852 _exptl_absorpt_correction_T_max 0.3071 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17913 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_unetI/netI 0.0423 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6465 _reflns_number_gt 5226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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. During the refinement, the command 'omit -3 50' was used to omit the weak reflections above 50 degree. During the refinement, the command 'ISOR' was used to restrain some non-H atoms with NPD and/or ADP problems. These atoms are as follows: CU3A CU3B CU2A CU2B C2 O5 C10 O1 O6 O9 O10 C3 C9 C19. All above refinement led to a relatively high restraint value (84). ; _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^)+(0.0384P)^2^+8.0809P] 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 6465 _refine_ls_number_parameters 496 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.133 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.25732(2) 0.490960(19) 0.486852(12) 0.01364(9) Uani 1 1 d . . . Cu1 Cu 0.01318(5) 0.39788(5) 0.52810(3) 0.01737(16) Uani 1 1 d . . . Cu2A Cu 0.6140(4) 0.3172(3) 0.2435(2) 0.0335(9) Uani 0.50 1 d PU . 1 Cu2B Cu 0.6215(4) 0.2860(3) 0.2557(2) 0.0322(9) Uani 0.50 1 d PU . 2 Cu3A Cu 0.5063(5) 0.0008(5) 0.51237(14) 0.0153(14) Uani 0.40 1 d PU . 1 Cu3B Cu 0.4802(13) -0.0010(12) 0.4634(6) 0.016(3) Uani 0.10 1 d PU . 2 I1A I 0.0726(3) 0.5583(3) 0.1709(2) 0.0773(7) Uani 0.50 1 d P A 1 I2A I 0.3463(2) 0.59676(18) 0.17689(17) 0.0794(8) Uani 0.40 1 d P B 1 I3A I 0.58746(18) 0.56799(13) 0.17231(11) 0.0669(5) Uani 0.50 1 d P B 1 I4A I 0.8162(3) 0.5687(4) 0.1739(3) 0.0942(10) Uani 0.50 1 d P B 1 I1B I 0.1053(3) 0.5480(5) 0.1688(3) 0.1090(14) Uani 0.50 1 d P C 2 I2B I 0.33480(15) 0.54813(13) 0.17307(9) 0.0737(5) Uani 0.60 1 d P C 2 I3B I 0.57932(16) 0.51519(15) 0.16911(11) 0.0746(5) Uani 0.50 1 d P . 2 I4B I 0.8507(3) 0.5507(3) 0.1736(2) 0.0740(7) Uani 0.50 1 d P D 2 C1 C 0.3904(5) 0.2837(6) 0.2260(3) 0.0399(18) Uani 1 1 d . . . C2 C 0.2811(7) 0.2882(7) 0.2274(4) 0.060(2) Uani 1 1 d U . . H2A H 0.2252 0.2622 0.1957 0.073 Uiso 1 1 calc R . . C3 C 0.2562(6) 0.3322(6) 0.2772(4) 0.057(2) Uani 1 1 d U . . H3A H 0.1824 0.3371 0.2791 0.069 Uiso 1 1 calc R . . C4 C 0.3397(5) 0.3691(5) 0.3241(3) 0.0324(16) Uani 1 1 d . . . C5 C 0.4475(5) 0.3637(5) 0.3183(3) 0.0317(15) Uani 1 1 d . . . H5A H 0.5046 0.3904 0.3491 0.038 Uiso 1 1 calc R . . C6 C 0.4267(5) 0.2355(6) 0.1740(3) 0.0388(17) Uani 1 1 d . . . C7 C 0.3099(5) 0.4142(5) 0.3788(3) 0.0270(14) Uani 1 1 d . . . C8 C 0.1551(5) 0.8214(5) 0.2355(3) 0.0334(16) Uani 1 1 d . . . C9 C 0.0500(6) 0.8156(6) 0.2423(4) 0.053(2) Uani 1 1 d U . . H9A H -0.0092 0.8451 0.2142 0.063 Uiso 1 1 calc R . . C10 C 0.0327(6) 0.7647(6) 0.2923(3) 0.0474(19) Uani 1 1 d U . . H10A H -0.0384 0.7603 0.2985 0.057 Uiso 1 1 calc R . . C11 C 0.1220(5) 0.7203(5) 0.3328(3) 0.0271(14) Uani 1 1 d . . . C12 C 0.2264(5) 0.7302(5) 0.3217(3) 0.0350(17) Uani 1 1 d . . . H12A H 0.2875 0.7007 0.3485 0.042 Uiso 1 1 calc R . . C13 C 0.1859(5) 0.8720(6) 0.1830(3) 0.0418(19) Uani 1 1 d . . . C14 C 0.1095(5) 0.6613(4) 0.3865(3) 0.0230(13) Uani 1 1 d . . . C15 C 0.2820(5) -0.0351(5) 0.4998(4) 0.0367(17) Uani 1 1 d . . . C16 C 0.1733(6) -0.0220(5) 0.5004(4) 0.054(2) Uani 1 1 d . . . H16A H 0.1267 -0.0757 0.4999 0.065 Uiso 1 1 calc R . . C17 C 0.1342(6) 0.0723(5) 0.5017(4) 0.046(2) Uani 1 1 d . . . H17A H 0.0608 0.0826 0.5031 0.055 Uiso 1 1 calc R . . C18 C 0.2024(5) 0.1515(4) 0.5009(3) 0.0253(14) Uani 1 1 d . . . C19 C 0.3115(5) 0.1330(5) 0.5004(3) 0.0349(16) Uani 1 1 d U . . H19A H 0.3592 0.1858 0.5003 0.042 Uiso 1 1 calc R . . C20 C 0.1650(5) 0.2561(4) 0.5015(3) 0.0222(13) Uani 1 1 d . . . C21 C 0.3368(5) -0.1331(5) 0.4984(4) 0.0415(19) Uani 1 1 d . . . N1 N 0.4730(4) 0.3213(4) 0.2699(2) 0.0327(13) Uani 1 1 d . . . N2 N 0.2420(4) 0.7804(4) 0.2744(2) 0.0353(14) Uani 1 1 d . . . N3 N 0.3503(4) 0.0425(4) 0.5003(3) 0.0413(16) Uani 1 1 d . . . O1 O 0.5301(4) 0.2370(4) 0.1783(2) 0.0503(14) Uani 1 1 d U . . O2 O 0.3561(4) 0.1984(5) 0.1315(2) 0.0607(17) Uani 1 1 d . . . O3 O 0.3874(3) 0.4476(4) 0.42237(19) 0.0338(11) Uani 1 1 d . . . O4 O 0.2115(3) 0.4163(3) 0.38031(19) 0.0296(10) Uani 1 1 d . . . O5 O 0.1130(4) 0.9140(5) 0.1440(3) 0.0634(16) Uani 1 1 d U . . O6 O 0.2861(4) 0.8693(4) 0.1810(2) 0.0451(13) Uani 1 1 d U . . O7 O 0.1946(3) 0.6166(3) 0.41539(19) 0.0264(10) Uani 1 1 d . . . O8 O 0.0163(3) 0.6632(3) 0.3990(2) 0.0317(11) Uani 1 1 d . . . O9 O 0.2827(4) -0.2089(3) 0.4976(3) 0.0536(14) Uani 1 1 d U . . O10 O 0.4383(4) -0.1307(3) 0.4985(3) 0.0535(14) Uani 1 1 d U . . O11 O 0.0685(3) 0.2702(3) 0.5086(2) 0.0315(11) Uani 1 1 d . . . O12 O 0.2324(3) 0.3201(3) 0.4947(2) 0.0261(10) Uani 1 1 d . . . O13 O 0.0555(3) 0.4734(2) 0.46201(16) 0.0140(8) Uani 1 1 d . . . H9 H 0.0325 0.4440 0.4204 0.021 Uiso 1 1 d R . . O1W O 0.3996(3) 0.6204(3) 0.5112(2) 0.0414(12) Uani 1 1 d . . . H1 H 0.4004 0.6567 0.4731 0.062 Uiso 1 1 d R . . H2 H 0.3819 0.6666 0.5415 0.062 Uiso 1 1 d R . . O2W O 0.4261(4) 0.4291(4) 0.5588(2) 0.0434(13) Uani 1 1 d . . . H3 H 0.4903 0.4712 0.5565 0.065 Uiso 1 1 d R . . H4 H 0.4160 0.4312 0.6011 0.065 Uiso 1 1 d R . . O3W O 0.2024(3) 0.4465(3) 0.58520(18) 0.0293(10) Uani 1 1 d . . . H5 H 0.2039 0.5033 0.6131 0.044 Uiso 1 1 d R . . H6 H 0.2468 0.3915 0.6083 0.044 Uiso 1 1 d R . . O4W O 0.1780(4) 0.6369(3) 0.5344(2) 0.0329(10) Uani 1 1 d . . . H7 H 0.2075 0.7018 0.5257 0.049 Uiso 1 1 d R . . H8 H 0.1866 0.6302 0.5792 0.049 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 Sm1 0.01248(15) 0.01423(15) 0.01687(15) 0.00085(12) 0.00862(10) 0.00092(11) Cu1 0.0173(4) 0.0145(3) 0.0252(4) 0.0059(3) 0.0145(3) 0.0035(3) Cu2A 0.0217(12) 0.050(2) 0.0335(17) -0.0237(15) 0.0159(12) -0.0051(16) Cu2B 0.0224(12) 0.0452(19) 0.0347(17) -0.0192(14) 0.0181(12) -0.0031(14) Cu3A 0.014(2) 0.0142(8) 0.018(4) -0.001(4) 0.006(3) 0.0025(12) Cu3B 0.016(4) 0.017(3) 0.015(5) -0.001(4) 0.004(4) 0.004(3) I1A 0.059(2) 0.0896(16) 0.0867(14) -0.0057(11) 0.0256(14) -0.0043(14) I2A 0.0474(11) 0.0700(16) 0.130(2) -0.0216(16) 0.0391(11) -0.0154(13) I3A 0.0552(9) 0.0698(11) 0.0807(10) -0.0028(11) 0.0264(7) 0.0037(10) I4A 0.0562(19) 0.122(2) 0.1125(16) 0.0058(15) 0.0352(16) 0.0185(14) I1B 0.059(2) 0.136(2) 0.143(2) -0.0184(16) 0.0451(17) 0.0079(16) I2B 0.0521(9) 0.0935(13) 0.0790(9) 0.0005(11) 0.0233(7) 0.0068(10) I3B 0.0413(8) 0.0900(14) 0.0983(12) 0.0055(14) 0.0283(7) -0.0014(11) I4B 0.0595(19) 0.0880(17) 0.0793(12) 0.0102(11) 0.0265(14) 0.0071(13) C1 0.024(4) 0.064(5) 0.035(4) -0.027(4) 0.014(3) -0.009(3) C2 0.046(4) 0.084(4) 0.056(4) -0.031(3) 0.020(3) -0.004(3) C3 0.037(4) 0.083(4) 0.058(4) -0.029(4) 0.023(3) -0.003(3) C4 0.019(3) 0.050(4) 0.031(4) -0.020(3) 0.011(3) -0.004(3) C5 0.022(3) 0.046(4) 0.032(4) -0.021(3) 0.015(3) -0.006(3) C6 0.029(4) 0.059(5) 0.031(4) -0.026(3) 0.011(3) -0.010(3) C7 0.021(3) 0.035(4) 0.027(3) -0.004(3) 0.012(3) 0.000(3) C8 0.024(3) 0.054(4) 0.025(3) 0.022(3) 0.010(3) 0.004(3) C9 0.038(4) 0.076(4) 0.047(4) 0.035(3) 0.016(3) 0.004(3) C10 0.030(3) 0.065(4) 0.051(3) 0.022(3) 0.018(3) 0.002(3) C11 0.025(3) 0.033(3) 0.028(3) 0.013(3) 0.015(3) 0.004(3) C12 0.020(3) 0.053(4) 0.035(4) 0.027(3) 0.012(3) 0.010(3) C13 0.026(4) 0.071(5) 0.031(4) 0.033(4) 0.011(3) 0.008(3) C14 0.023(3) 0.021(3) 0.028(3) 0.008(3) 0.012(3) 0.002(2) C15 0.027(4) 0.019(3) 0.069(5) 0.004(3) 0.023(3) 0.002(3) C16 0.030(4) 0.017(3) 0.122(8) 0.002(4) 0.034(4) -0.001(3) C17 0.026(4) 0.022(4) 0.099(7) -0.002(4) 0.032(4) 0.003(3) C18 0.022(3) 0.018(3) 0.040(4) 0.004(3) 0.015(3) 0.003(2) C19 0.029(3) 0.019(3) 0.062(4) 0.001(3) 0.022(3) 0.002(2) C20 0.026(3) 0.017(3) 0.026(3) 0.003(2) 0.011(3) 0.007(3) C21 0.025(4) 0.018(3) 0.086(6) -0.002(3) 0.022(4) -0.004(3) N1 0.019(3) 0.051(4) 0.031(3) -0.019(3) 0.013(2) -0.005(2) N2 0.026(3) 0.053(4) 0.033(3) 0.020(3) 0.019(2) 0.006(3) N3 0.026(3) 0.014(3) 0.091(5) 0.005(3) 0.027(3) 0.002(2) O1 0.032(3) 0.075(3) 0.048(3) -0.036(2) 0.019(2) -0.008(2) O2 0.032(3) 0.101(5) 0.054(3) -0.054(3) 0.019(3) -0.018(3) O3 0.019(2) 0.057(3) 0.028(2) -0.021(2) 0.0117(19) -0.005(2) O4 0.019(2) 0.045(3) 0.030(2) -0.010(2) 0.0144(18) -0.0026(19) O5 0.045(3) 0.095(3) 0.053(3) 0.040(3) 0.016(2) 0.003(3) O6 0.033(3) 0.067(3) 0.041(3) 0.029(2) 0.021(2) 0.004(2) O7 0.020(2) 0.028(2) 0.036(3) 0.0163(19) 0.0152(19) 0.0062(18) O8 0.024(2) 0.037(3) 0.040(3) 0.024(2) 0.021(2) 0.0094(19) O9 0.043(3) 0.023(2) 0.101(4) -0.003(2) 0.029(3) -0.005(2) O10 0.038(3) 0.024(2) 0.104(4) -0.002(2) 0.028(3) 0.005(2) O11 0.026(2) 0.015(2) 0.061(3) 0.003(2) 0.026(2) 0.0041(17) O12 0.024(2) 0.0127(19) 0.047(3) 0.0036(18) 0.020(2) -0.0003(17) O13 0.0132(19) 0.0146(18) 0.0159(19) -0.0007(15) 0.0066(15) 0.0013(15) O1W 0.027(3) 0.020(2) 0.077(4) -0.005(2) 0.010(2) -0.0021(19) O2W 0.023(2) 0.061(3) 0.044(3) 0.028(3) 0.005(2) -0.006(2) O3W 0.039(3) 0.031(2) 0.022(2) 0.0045(19) 0.0137(19) 0.009(2) O4W 0.047(3) 0.023(2) 0.036(3) -0.003(2) 0.024(2) -0.001(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 Sm1 O7 2.341(4) . ? Sm1 O12 2.354(4) . ? Sm1 O13 2.432(3) . ? Sm1 O2W 2.447(4) . ? Sm1 O1W 2.453(4) . ? Sm1 O3 2.501(4) . ? Sm1 O4 2.535(4) . ? Sm1 O3W 2.552(4) . ? Sm1 O4W 2.567(4) . ? Sm1 C7 2.873(6) . ? Cu1 O11 1.957(4) . ? Cu1 O8 1.957(4) 3_566 ? Cu1 O13 1.983(3) 3_566 ? Cu1 O13 1.986(3) . ? Cu1 Cu1 3.0341(13) 3_566 ? Cu2A O1 1.912(7) . ? Cu2A O6 1.964(7) 2_645 ? Cu2A N1 1.984(7) . ? Cu2A N2 1.993(7) 2_645 ? Cu2B O1 1.941(7) . ? Cu2B O6 1.947(7) 2_645 ? Cu2B N2 1.979(7) 2_645 ? Cu2B N1 2.005(7) . ? Cu3A Cu3A 0.540(6) 3_656 ? Cu3A O10 1.933(8) 3_656 ? Cu3A N3 1.960(8) 3_656 ? Cu3A O10 1.967(8) . ? Cu3A N3 1.966(8) . ? Cu3B Cu3B 1.60(2) 3_656 ? Cu3B O10 2.053(17) . ? Cu3B N3 2.076(16) . ? Cu3B O10 2.126(17) 3_656 ? Cu3B N3 2.128(16) 3_656 ? Cu3B I3B 2.897(12) 2_645 ? I2A I3A 3.042(4) . ? I3A I4A 2.827(4) . ? I1B I2B 2.822(4) . ? I2B I3B 3.088(3) . ? I3B Cu3B 2.897(12) 2_655 ? C1 N1 1.331(8) . ? C1 C2 1.365(9) . ? C1 C6 1.509(8) . ? C2 C3 1.373(10) . ? C2 H2A 0.9300 . ? C3 C4 1.372(10) . ? C3 H3A 0.9300 . ? C4 C5 1.377(8) . ? C4 C7 1.505(8) . ? C5 N1 1.341(7) . ? C5 H5A 0.9300 . ? C6 O2 1.230(7) . ? C6 O1 1.260(7) . ? C7 O4 1.229(7) . ? C7 O3 1.271(7) . ? C8 N2 1.328(8) . ? C8 C9 1.353(9) . ? C8 C13 1.499(8) . ? C9 C10 1.384(9) . ? C9 H9A 0.9300 . ? C10 C11 1.382(9) . ? C10 H10A 0.9300 . ? C11 C12 1.386(8) . ? C11 C14 1.492(8) . ? C12 N2 1.320(7) . ? C12 H12A 0.9300 . ? C13 O5 1.229(8) . ? C13 O6 1.254(7) . ? C14 O7 1.247(7) . ? C14 O8 1.256(7) . ? C15 N3 1.350(8) . ? C15 C16 1.362(9) . ? C15 C21 1.500(9) . ? C16 C17 1.373(9) . ? C16 H16A 0.9300 . ? C17 C18 1.371(9) . ? C17 H17A 0.9300 . ? C18 C19 1.379(8) . ? C18 C20 1.497(8) . ? C19 N3 1.322(8) . ? C19 H19A 0.9300 . ? C20 O12 1.242(7) . ? C20 O11 1.261(7) . ? C21 O9 1.226(7) . ? C21 O10 1.258(8) . ? N2 Cu2B 1.979(7) 2_655 ? N2 Cu2A 1.993(7) 2_655 ? N3 Cu3A 1.960(8) 3_656 ? N3 Cu3B 2.128(16) 3_656 ? O6 Cu2B 1.947(7) 2_655 ? O6 Cu2A 1.964(7) 2_655 ? O8 Cu1 1.957(4) 3_566 ? O10 Cu3A 1.933(8) 3_656 ? O10 Cu3B 2.126(17) 3_656 ? O13 Cu1 1.983(3) 3_566 ? O13 H9 0.9925 . ? O1W H1 0.9929 . ? O1W H2 0.9931 . ? O2W H3 0.9930 . ? O2W H4 0.9929 . ? O3W H5 0.9930 . ? O3W H6 0.9929 . ? O4W H7 0.9930 . ? O4W H8 0.9929 . ? 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 O7 Sm1 O12 138.05(15) . . ? O7 Sm1 O13 76.76(12) . . ? O12 Sm1 O13 76.90(12) . . ? O7 Sm1 O2W 141.75(14) . . ? O12 Sm1 O2W 73.64(15) . . ? O13 Sm1 O2W 140.77(13) . . ? O7 Sm1 O1W 74.05(15) . . ? O12 Sm1 O1W 142.28(14) . . ? O13 Sm1 O1W 139.57(13) . . ? O2W Sm1 O1W 69.68(15) . . ? O7 Sm1 O3 85.56(15) . . ? O12 Sm1 O3 85.85(14) . . ? O13 Sm1 O3 128.37(12) . . ? O2W Sm1 O3 74.66(16) . . ? O1W Sm1 O3 76.44(15) . . ? O7 Sm1 O4 71.63(15) . . ? O12 Sm1 O4 70.98(15) . . ? O13 Sm1 O4 76.89(12) . . ? O2W Sm1 O4 116.00(16) . . ? O1W Sm1 O4 118.31(16) . . ? O3 Sm1 O4 51.49(13) . . ? O7 Sm1 O3W 130.94(13) . . ? O12 Sm1 O3W 68.42(14) . . ? O13 Sm1 O3W 71.97(12) . . ? O2W Sm1 O3W 73.43(14) . . ? O1W Sm1 O3W 108.13(16) . . ? O3 Sm1 O3W 143.44(15) . . ? O4 Sm1 O3W 133.09(14) . . ? O7 Sm1 O4W 68.17(14) . . ? O12 Sm1 O4W 131.24(13) . . ? O13 Sm1 O4W 72.01(13) . . ? O2W Sm1 O4W 110.01(16) . . ? O1W Sm1 O4W 71.49(14) . . ? O3 Sm1 O4W 142.86(14) . . ? O4 Sm1 O4W 133.45(14) . . ? O3W Sm1 O4W 66.73(13) . . ? O7 Sm1 C7 77.80(16) . . ? O12 Sm1 C7 76.58(16) . . ? O13 Sm1 C7 102.19(14) . . ? O2W Sm1 C7 95.59(17) . . ? O1W Sm1 C7 98.32(17) . . ? O3 Sm1 C7 26.20(15) . . ? O4 Sm1 C7 25.30(14) . . ? O3W Sm1 C7 144.97(16) . . ? O4W Sm1 C7 145.93(16) . . ? O11 Cu1 O8 87.95(18) . 3_566 ? O11 Cu1 O13 173.12(17) . 3_566 ? O8 Cu1 O13 95.87(16) 3_566 3_566 ? O11 Cu1 O13 96.58(16) . . ? O8 Cu1 O13 172.07(17) 3_566 . ? O13 Cu1 O13 80.30(15) 3_566 . ? O11 Cu1 Cu1 136.38(13) . 3_566 ? O8 Cu1 Cu1 135.66(13) 3_566 3_566 ? O13 Cu1 Cu1 40.19(10) 3_566 3_566 ? O13 Cu1 Cu1 40.11(10) . 3_566 ? O1 Cu2A O6 166.3(3) . 2_645 ? O1 Cu2A N1 84.2(3) . . ? O6 Cu2A N1 98.1(3) 2_645 . ? O1 Cu2A N2 92.3(3) . 2_645 ? O6 Cu2A N2 82.3(3) 2_645 2_645 ? N1 Cu2A N2 166.1(3) . 2_645 ? O1 Cu2B O6 163.3(3) . 2_645 ? O1 Cu2B N2 91.9(3) . 2_645 ? O6 Cu2B N2 83.1(3) 2_645 2_645 ? O1 Cu2B N1 82.8(3) . . ? O6 Cu2B N1 97.9(3) 2_645 . ? N2 Cu2B N1 164.6(3) 2_645 . ? Cu3A Cu3A O10 85.6(15) 3_656 3_656 ? Cu3A Cu3A N3 82.7(13) 3_656 3_656 ? O10 Cu3A N3 83.7(3) 3_656 3_656 ? Cu3A Cu3A O10 78.5(14) 3_656 . ? O10 Cu3A O10 164.11(18) 3_656 . ? N3 Cu3A O10 94.1(4) 3_656 . ? Cu3A Cu3A N3 81.5(13) 3_656 . ? O10 Cu3A N3 95.0(4) 3_656 . ? N3 Cu3A N3 164.19(18) 3_656 . ? O10 Cu3A N3 82.7(3) . . ? Cu3B Cu3B O10 70.0(11) 3_656 . ? Cu3B Cu3B N3 69.4(11) 3_656 . ? O10 Cu3B N3 78.0(6) . . ? Cu3B Cu3B O10 65.1(11) 3_656 3_656 ? O10 Cu3B O10 135.1(6) . 3_656 ? N3 Cu3B O10 86.3(6) . 3_656 ? Cu3B Cu3B N3 66.0(10) 3_656 3_656 ? O10 Cu3B N3 86.9(6) . 3_656 ? N3 Cu3B N3 135.3(6) . 3_656 ? O10 Cu3B N3 75.3(5) 3_656 3_656 ? Cu3B Cu3B I3B 173.9(15) 3_656 2_645 ? O10 Cu3B I3B 116.1(6) . 2_645 ? N3 Cu3B I3B 111.8(6) . 2_645 ? O10 Cu3B I3B 108.8(6) 3_656 2_645 ? N3 Cu3B I3B 112.6(6) 3_656 2_645 ? I4A I3A I2A 171.98(14) . . ? I1B I2B I3B 170.93(16) . . ? Cu3B I3B I2B 92.7(3) 2_655 . ? N1 C1 C2 123.1(6) . . ? N1 C1 C6 114.7(5) . . ? C2 C1 C6 122.1(6) . . ? C1 C2 C3 118.0(7) . . ? C1 C2 H2A 121.0 . . ? C3 C2 H2A 121.0 . . ? C4 C3 C2 120.4(7) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C3 C4 C5 117.9(6) . . ? C3 C4 C7 119.1(6) . . ? C5 C4 C7 123.1(5) . . ? N1 C5 C4 122.4(6) . . ? N1 C5 H5A 118.8 . . ? C4 C5 H5A 118.8 . . ? O2 C6 O1 125.1(6) . . ? O2 C6 C1 119.3(6) . . ? O1 C6 C1 115.6(5) . . ? O4 C7 O3 122.1(5) . . ? O4 C7 C4 119.0(5) . . ? O3 C7 C4 118.9(5) . . ? O4 C7 Sm1 61.8(3) . . ? O3 C7 Sm1 60.3(3) . . ? C4 C7 Sm1 176.9(5) . . ? N2 C8 C9 122.9(6) . . ? N2 C8 C13 112.8(5) . . ? C9 C8 C13 124.3(6) . . ? C8 C9 C10 118.3(7) . . ? C8 C9 H9A 120.8 . . ? C10 C9 H9A 120.8 . . ? C9 C10 C11 119.6(6) . . ? C9 C10 H10A 120.2 . . ? C11 C10 H10A 120.2 . . ? C10 C11 C12 117.7(6) . . ? C10 C11 C14 122.7(6) . . ? C12 C11 C14 119.6(5) . . ? N2 C12 C11 122.1(6) . . ? N2 C12 H12A 119.0 . . ? C11 C12 H12A 119.0 . . ? O5 C13 O6 122.9(6) . . ? O5 C13 C8 119.2(6) . . ? O6 C13 C8 117.9(5) . . ? O7 C14 O8 126.7(5) . . ? O7 C14 C11 115.8(5) . . ? O8 C14 C11 117.5(5) . . ? N3 C15 C16 121.2(6) . . ? N3 C15 C21 114.0(5) . . ? C16 C15 C21 124.8(6) . . ? C15 C16 C17 118.5(6) . . ? C15 C16 H16A 120.7 . . ? C17 C16 H16A 120.7 . . ? C18 C17 C16 120.7(6) . . ? C18 C17 H17A 119.6 . . ? C16 C17 H17A 119.6 . . ? C17 C18 C19 117.8(6) . . ? C17 C18 C20 123.6(5) . . ? C19 C18 C20 118.7(5) . . ? N3 C19 C18 121.9(6) . . ? N3 C19 H19A 119.0 . . ? C18 C19 H19A 119.0 . . ? O12 C20 O11 126.8(5) . . ? O12 C20 C18 116.4(5) . . ? O11 C20 C18 116.8(5) . . ? O9 C21 O10 124.4(6) . . ? O9 C21 C15 119.8(6) . . ? O10 C21 C15 115.8(5) . . ? C1 N1 C5 118.2(5) . . ? C1 N1 Cu2A 109.7(4) . . ? C5 N1 Cu2A 131.6(4) . . ? C1 N1 Cu2B 110.8(4) . . ? C5 N1 Cu2B 130.4(4) . . ? Cu2A N1 Cu2B 14.43(17) . . ? C12 N2 C8 119.4(5) . . ? C12 N2 Cu2B 127.7(5) . 2_655 ? C8 N2 Cu2B 112.1(4) . 2_655 ? C12 N2 Cu2A 128.0(5) . 2_655 ? C8 N2 Cu2A 112.2(4) . 2_655 ? Cu2B N2 Cu2A 14.50(17) 2_655 2_655 ? C19 N3 C15 119.9(6) . . ? C19 N3 Cu3A 128.6(5) . 3_656 ? C15 N3 Cu3A 110.8(5) . 3_656 ? C19 N3 Cu3A 127.9(5) . . ? C15 N3 Cu3A 111.7(5) . . ? Cu3A N3 Cu3A 15.81(18) 3_656 . ? C19 N3 Cu3B 125.9(6) . . ? C15 N3 Cu3B 108.9(6) . . ? Cu3A N3 Cu3B 14.7(3) 3_656 . ? Cu3A N3 Cu3B 30.5(4) . . ? C19 N3 Cu3B 124.8(6) . 3_656 ? C15 N3 Cu3B 110.6(6) . 3_656 ? Cu3A N3 Cu3B 30.0(4) 3_656 3_656 ? Cu3A N3 Cu3B 14.2(3) . 3_656 ? Cu3B N3 Cu3B 44.7(6) . 3_656 ? C6 O1 Cu2A 114.3(4) . . ? C6 O1 Cu2B 115.1(4) . . ? Cu2A O1 Cu2B 14.93(17) . . ? C7 O3 Sm1 93.5(3) . . ? C7 O4 Sm1 92.9(4) . . ? C13 O6 Cu2B 113.2(4) . 2_655 ? C13 O6 Cu2A 113.1(4) . 2_655 ? Cu2B O6 Cu2A 14.73(17) 2_655 2_655 ? C14 O7 Sm1 143.4(4) . . ? C14 O8 Cu1 123.9(4) . 3_566 ? C21 O10 Cu3A 114.3(5) . 3_656 ? C21 O10 Cu3A 114.3(4) . . ? Cu3A O10 Cu3A 15.89(18) 3_656 . ? C21 O10 Cu3B 111.9(6) . . ? Cu3A O10 Cu3B 14.9(3) 3_656 . ? Cu3A O10 Cu3B 30.8(4) . . ? C21 O10 Cu3B 113.3(6) . 3_656 ? Cu3A O10 Cu3B 30.1(4) 3_656 3_656 ? Cu3A O10 Cu3B 14.2(3) . 3_656 ? Cu3B O10 Cu3B 44.9(6) . 3_656 ? C20 O11 Cu1 124.1(4) . . ? C20 O12 Sm1 143.6(4) . . ? Cu1 O13 Cu1 99.70(15) 3_566 . ? Cu1 O13 Sm1 109.47(15) 3_566 . ? Cu1 O13 Sm1 109.31(15) . . ? Cu1 O13 H9 115.6 3_566 . ? Cu1 O13 H9 115.7 . . ? Sm1 O13 H9 106.8 . . ? Sm1 O1W H1 109.1 . . ? Sm1 O1W H2 109.5 . . ? H1 O1W H2 109.5 . . ? Sm1 O2W H3 109.2 . . ? Sm1 O2W H4 109.4 . . ? H3 O2W H4 109.5 . . ? Sm1 O3W H5 113.6 . . ? Sm1 O3W H6 113.5 . . ? H5 O3W H6 109.5 . . ? Sm1 O4W H7 113.9 . . ? Sm1 O4W H8 113.6 . . ? H7 O4W H8 109.5 . . ? 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 I1B I2B I3B Cu3B 63.0(10) . . . 2_655 ? N1 C1 C2 C3 -1.1(14) . . . . ? C6 C1 C2 C3 179.0(8) . . . . ? C1 C2 C3 C4 -0.9(14) . . . . ? C2 C3 C4 C5 2.4(13) . . . . ? C2 C3 C4 C7 -178.2(8) . . . . ? C3 C4 C5 N1 -2.2(11) . . . . ? C7 C4 C5 N1 178.5(6) . . . . ? N1 C1 C6 O2 179.7(7) . . . . ? C2 C1 C6 O2 -0.4(13) . . . . ? N1 C1 C6 O1 -0.3(11) . . . . ? C2 C1 C6 O1 179.6(8) . . . . ? C3 C4 C7 O4 0.5(10) . . . . ? C5 C4 C7 O4 179.9(7) . . . . ? C3 C4 C7 O3 179.5(7) . . . . ? C5 C4 C7 O3 -1.2(10) . . . . ? C3 C4 C7 Sm1 104(8) . . . . ? C5 C4 C7 Sm1 -77(8) . . . . ? O7 Sm1 C7 O4 -72.7(4) . . . . ? O12 Sm1 C7 O4 73.8(4) . . . . ? O13 Sm1 C7 O4 0.6(4) . . . . ? O2W Sm1 C7 O4 145.5(4) . . . . ? O1W Sm1 C7 O4 -144.3(4) . . . . ? O3 Sm1 C7 O4 -177.8(6) . . . . ? O3W Sm1 C7 O4 76.5(5) . . . . ? O4W Sm1 C7 O4 -75.2(5) . . . . ? O7 Sm1 C7 O3 105.1(4) . . . . ? O12 Sm1 C7 O3 -108.4(4) . . . . ? O13 Sm1 C7 O3 178.4(4) . . . . ? O2W Sm1 C7 O3 -36.8(4) . . . . ? O1W Sm1 C7 O3 33.5(4) . . . . ? O4 Sm1 C7 O3 177.8(6) . . . . ? O3W Sm1 C7 O3 -105.7(4) . . . . ? O4W Sm1 C7 O3 102.6(4) . . . . ? O7 Sm1 C7 C4 -178(100) . . . . ? O12 Sm1 C7 C4 -31(8) . . . . ? O13 Sm1 C7 C4 -105(8) . . . . ? O2W Sm1 C7 C4 40(8) . . . . ? O1W Sm1 C7 C4 110(8) . . . . ? O3 Sm1 C7 C4 77(8) . . . . ? O4 Sm1 C7 C4 -105(8) . . . . ? O3W Sm1 C7 C4 -29(8) . . . . ? O4W Sm1 C7 C4 180(100) . . . . ? N2 C8 C9 C10 0.1(13) . . . . ? C13 C8 C9 C10 178.5(8) . . . . ? C8 C9 C10 C11 -1.0(13) . . . . ? C9 C10 C11 C12 0.9(11) . . . . ? C9 C10 C11 C14 -177.9(7) . . . . ? C10 C11 C12 N2 0.2(11) . . . . ? C14 C11 C12 N2 179.0(6) . . . . ? N2 C8 C13 O5 -179.2(7) . . . . ? C9 C8 C13 O5 2.3(13) . . . . ? N2 C8 C13 O6 0.8(10) . . . . ? C9 C8 C13 O6 -177.7(8) . . . . ? C10 C11 C14 O7 172.5(7) . . . . ? C12 C11 C14 O7 -6.3(9) . . . . ? C10 C11 C14 O8 -9.1(10) . . . . ? C12 C11 C14 O8 172.2(6) . . . . ? N3 C15 C16 C17 -0.2(13) . . . . ? C21 C15 C16 C17 180.0(8) . . . . ? C15 C16 C17 C18 1.5(14) . . . . ? C16 C17 C18 C19 -1.7(12) . . . . ? C16 C17 C18 C20 179.3(8) . . . . ? C17 C18 C19 N3 0.5(11) . . . . ? C20 C18 C19 N3 179.6(7) . . . . ? C17 C18 C20 O12 -173.2(7) . . . . ? C19 C18 C20 O12 7.7(9) . . . . ? C17 C18 C20 O11 6.5(10) . . . . ? C19 C18 C20 O11 -172.6(6) . . . . ? N3 C15 C21 O9 -179.7(8) . . . . ? C16 C15 C21 O9 0.1(13) . . . . ? N3 C15 C21 O10 0.7(11) . . . . ? C16 C15 C21 O10 -179.5(8) . . . . ? C2 C1 N1 C5 1.4(12) . . . . ? C6 C1 N1 C5 -178.7(7) . . . . ? C2 C1 N1 Cu2A -171.2(7) . . . . ? C6 C1 N1 Cu2A 8.7(8) . . . . ? C2 C1 N1 Cu2B 173.4(7) . . . . ? C6 C1 N1 Cu2B -6.7(8) . . . . ? C4 C5 N1 C1 0.3(11) . . . . ? C4 C5 N1 Cu2A 171.0(5) . . . . ? C4 C5 N1 Cu2B -169.9(5) . . . . ? O1 Cu2A N1 C1 -10.5(5) . . . . ? O6 Cu2A N1 C1 -176.9(5) 2_645 . . . ? N2 Cu2A N1 C1 -86.5(15) 2_645 . . . ? O1 Cu2A N1 C5 178.1(7) . . . . ? O6 Cu2A N1 C5 11.8(7) 2_645 . . . ? N2 Cu2A N1 C5 102.2(15) 2_645 . . . ? O1 Cu2A N1 Cu2B 86.4(11) . . . . ? O6 Cu2A N1 Cu2B -80.0(11) 2_645 . . . ? N2 Cu2A N1 Cu2B 10.5(9) 2_645 . . . ? O1 Cu2B N1 C1 8.3(5) . . . . ? O6 Cu2B N1 C1 171.4(5) 2_645 . . . ? N2 Cu2B N1 C1 78.9(14) 2_645 . . . ? O1 Cu2B N1 C5 179.0(7) . . . . ? O6 Cu2B N1 C5 -17.9(7) 2_645 . . . ? N2 Cu2B N1 C5 -110.4(13) 2_645 . . . ? O1 Cu2B N1 Cu2A -80.1(11) . . . . ? O6 Cu2B N1 Cu2A 83.0(10) 2_645 . . . ? N2 Cu2B N1 Cu2A -9.5(8) 2_645 . . . ? C11 C12 N2 C8 -1.1(11) . . . . ? C11 C12 N2 Cu2B -170.0(5) . . . 2_655 ? C11 C12 N2 Cu2A 171.6(5) . . . 2_655 ? C9 C8 N2 C12 0.9(12) . . . . ? C13 C8 N2 C12 -177.6(7) . . . . ? C9 C8 N2 Cu2B 171.5(7) . . . 2_655 ? C13 C8 N2 Cu2B -7.1(8) . . . 2_655 ? C9 C8 N2 Cu2A -172.8(7) . . . 2_655 ? C13 C8 N2 Cu2A 8.6(8) . . . 2_655 ? C18 C19 N3 C15 0.8(12) . . . . ? C18 C19 N3 Cu3A 170.2(5) . . . 3_656 ? C18 C19 N3 Cu3A -169.7(5) . . . . ? C18 C19 N3 Cu3B 152.0(7) . . . . ? C18 C19 N3 Cu3B -152.5(7) . . . 3_656 ? C16 C15 N3 C19 -1.0(12) . . . . ? C21 C15 N3 C19 178.9(7) . . . . ? C16 C15 N3 Cu3A -172.1(7) . . . 3_656 ? C21 C15 N3 Cu3A 7.7(8) . . . 3_656 ? C16 C15 N3 Cu3A 171.0(7) . . . . ? C21 C15 N3 Cu3A -9.2(9) . . . . ? C16 C15 N3 Cu3B -156.6(8) . . . . ? C21 C15 N3 Cu3B 23.2(9) . . . . ? C16 C15 N3 Cu3B 155.8(8) . . . 3_656 ? C21 C15 N3 Cu3B -24.4(9) . . . 3_656 ? Cu3A Cu3A N3 C19 -98.9(16) 3_656 . . . ? O10 Cu3A N3 C19 -14.1(7) 3_656 . . . ? N3 Cu3A N3 C19 -98.9(16) 3_656 . . . ? O10 Cu3A N3 C19 -178.3(7) . . . . ? Cu3A Cu3A N3 C15 90.0(16) 3_656 . . . ? O10 Cu3A N3 C15 174.8(6) 3_656 . . . ? N3 Cu3A N3 C15 90.0(16) 3_656 . . . ? O10 Cu3A N3 C15 10.6(6) . . . . ? O10 Cu3A N3 Cu3A 84.8(15) 3_656 . . 3_656 ? N3 Cu3A N3 Cu3A 0.000(2) 3_656 . . 3_656 ? O10 Cu3A N3 Cu3A -79.4(15) . . . 3_656 ? Cu3A Cu3A N3 Cu3B -0.7(11) 3_656 . . . ? O10 Cu3A N3 Cu3B 84.1(11) 3_656 . . . ? N3 Cu3A N3 Cu3B -0.7(11) 3_656 . . . ? O10 Cu3A N3 Cu3B -80.1(11) . . . . ? Cu3A Cu3A N3 Cu3B 179(2) 3_656 . . 3_656 ? O10 Cu3A N3 Cu3B -96.6(17) 3_656 . . 3_656 ? N3 Cu3A N3 Cu3B 179(2) 3_656 . . 3_656 ? O10 Cu3A N3 Cu3B 99.2(16) . . . 3_656 ? Cu3B Cu3B N3 C19 105.6(12) 3_656 . . . ? O10 Cu3B N3 C19 178.5(7) . . . . ? O10 Cu3B N3 C19 40.9(8) 3_656 . . . ? N3 Cu3B N3 C19 105.6(12) 3_656 . . . ? I3B Cu3B N3 C19 -68.0(10) 2_645 . . . ? Cu3B Cu3B N3 C15 -100.6(12) 3_656 . . . ? O10 Cu3B N3 C15 -27.7(6) . . . . ? O10 Cu3B N3 C15 -165.3(6) 3_656 . . . ? N3 Cu3B N3 C15 -100.6(12) 3_656 . . . ? I3B Cu3B N3 C15 85.8(8) 2_645 . . . ? Cu3B Cu3B N3 Cu3A -0.5(8) 3_656 . . 3_656 ? O10 Cu3B N3 Cu3A 72.4(15) . . . 3_656 ? O10 Cu3B N3 Cu3A -65.2(14) 3_656 . . 3_656 ? N3 Cu3B N3 Cu3A -0.5(8) 3_656 . . 3_656 ? I3B Cu3B N3 Cu3A -174(2) 2_645 . . 3_656 ? Cu3B Cu3B N3 Cu3A 0.2(4) 3_656 . . . ? O10 Cu3B N3 Cu3A 73.1(10) . . . . ? O10 Cu3B N3 Cu3A -64.5(9) 3_656 . . . ? N3 Cu3B N3 Cu3A 0.2(4) 3_656 . . . ? I3B Cu3B N3 Cu3A -173.3(15) 2_645 . . . ? O10 Cu3B N3 Cu3B 72.9(10) . . . 3_656 ? O10 Cu3B N3 Cu3B -64.7(10) 3_656 . . 3_656 ? N3 Cu3B N3 Cu3B 0.0 3_656 . . 3_656 ? I3B Cu3B N3 Cu3B -173.6(16) 2_645 . . 3_656 ? O2 C6 O1 Cu2A 171.1(7) . . . . ? C1 C6 O1 Cu2A -8.9(9) . . . . ? O2 C6 O1 Cu2B -172.5(7) . . . . ? C1 C6 O1 Cu2B 7.5(9) . . . . ? O6 Cu2A O1 C6 111.0(16) 2_645 . . . ? N1 Cu2A O1 C6 10.9(6) . . . . ? N2 Cu2A O1 C6 177.4(6) 2_645 . . . ? O6 Cu2A O1 Cu2B 14.6(9) 2_645 . . . ? N1 Cu2A O1 Cu2B -85.5(12) . . . . ? N2 Cu2A O1 Cu2B 81.0(12) 2_645 . . . ? O6 Cu2B O1 C6 -102.5(13) 2_645 . . . ? N2 Cu2B O1 C6 -174.3(6) 2_645 . . . ? N1 Cu2B O1 C6 -8.9(6) . . . . ? O6 Cu2B O1 Cu2A -12.1(7) 2_645 . . . ? N2 Cu2B O1 Cu2A -83.9(12) 2_645 . . . ? N1 Cu2B O1 Cu2A 81.6(12) . . . . ? O4 C7 O3 Sm1 2.3(7) . . . . ? C4 C7 O3 Sm1 -176.6(5) . . . . ? O7 Sm1 O3 C7 -71.2(4) . . . . ? O12 Sm1 O3 C7 67.7(4) . . . . ? O13 Sm1 O3 C7 -2.0(5) . . . . ? O2W Sm1 O3 C7 141.9(4) . . . . ? O1W Sm1 O3 C7 -145.8(4) . . . . ? O4 Sm1 O3 C7 -1.2(4) . . . . ? O3W Sm1 O3 C7 111.9(4) . . . . ? O4W Sm1 O3 C7 -115.1(4) . . . . ? O3 C7 O4 Sm1 -2.3(7) . . . . ? C4 C7 O4 Sm1 176.6(5) . . . . ? O7 Sm1 O4 C7 100.4(4) . . . . ? O12 Sm1 O4 C7 -98.9(4) . . . . ? O13 Sm1 O4 C7 -179.4(4) . . . . ? O2W Sm1 O4 C7 -38.9(4) . . . . ? O1W Sm1 O4 C7 41.0(4) . . . . ? O3 Sm1 O4 C7 1.2(4) . . . . ? O3W Sm1 O4 C7 -130.1(4) . . . . ? O4W Sm1 O4 C7 131.7(4) . . . . ? O5 C13 O6 Cu2B -174.0(7) . . . 2_655 ? C8 C13 O6 Cu2B 6.0(9) . . . 2_655 ? O5 C13 O6 Cu2A 170.0(7) . . . 2_655 ? C8 C13 O6 Cu2A -10.0(9) . . . 2_655 ? O8 C14 O7 Sm1 17.9(11) . . . . ? C11 C14 O7 Sm1 -163.8(5) . . . . ? O12 Sm1 O7 C14 61.8(7) . . . . ? O13 Sm1 O7 C14 9.4(7) . . . . ? O2W Sm1 O7 C14 -161.3(6) . . . . ? O1W Sm1 O7 C14 -142.3(7) . . . . ? O3 Sm1 O7 C14 140.6(7) . . . . ? O4 Sm1 O7 C14 89.8(7) . . . . ? O3W Sm1 O7 C14 -41.9(7) . . . . ? O4W Sm1 O7 C14 -66.3(7) . . . . ? C7 Sm1 O7 C14 115.2(7) . . . . ? O7 C14 O8 Cu1 4.6(9) . . . 3_566 ? C11 C14 O8 Cu1 -173.6(4) . . . 3_566 ? O9 C21 O10 Cu3A 171.3(7) . . . 3_656 ? C15 C21 O10 Cu3A -9.1(9) . . . 3_656 ? O9 C21 O10 Cu3A -171.2(7) . . . . ? C15 C21 O10 Cu3A 8.3(9) . . . . ? O9 C21 O10 Cu3B 155.3(8) . . . . ? C15 C21 O10 Cu3B -25.1(9) . . . . ? O9 C21 O10 Cu3B -155.8(8) . . . 3_656 ? C15 C21 O10 Cu3B 23.8(10) . . . 3_656 ? Cu3A Cu3A O10 C21 -93.4(14) 3_656 . . . ? O10 Cu3A O10 C21 -93.4(14) 3_656 . . . ? N3 Cu3A O10 C21 -175.1(6) 3_656 . . . ? N3 Cu3A O10 C21 -10.6(6) . . . . ? O10 Cu3A O10 Cu3A 0.000(3) 3_656 . . 3_656 ? N3 Cu3A O10 Cu3A -81.6(13) 3_656 . . 3_656 ? N3 Cu3A O10 Cu3A 82.8(13) . . . 3_656 ? Cu3A Cu3A O10 Cu3B -1.1(9) 3_656 . . . ? O10 Cu3A O10 Cu3B -1.1(9) 3_656 . . . ? N3 Cu3A O10 Cu3B -82.8(11) 3_656 . . . ? N3 Cu3A O10 Cu3B 81.6(11) . . . . ? Cu3A Cu3A O10 Cu3B 177.7(18) 3_656 . . 3_656 ? O10 Cu3A O10 Cu3B 177.7(18) 3_656 . . 3_656 ? N3 Cu3A O10 Cu3B 96.1(15) 3_656 . . 3_656 ? N3 Cu3A O10 Cu3B -99.5(15) . . . 3_656 ? Cu3B Cu3B O10 C21 101.6(11) 3_656 . . . ? N3 Cu3B O10 C21 29.4(7) . . . . ? O10 Cu3B O10 C21 101.6(11) 3_656 . . . ? N3 Cu3B O10 C21 167.1(6) 3_656 . . . ? I3B Cu3B O10 C21 -79.2(8) 2_645 . . . ? Cu3B Cu3B O10 Cu3A -0.8(6) 3_656 . . 3_656 ? N3 Cu3B O10 Cu3A -73.0(14) . . . 3_656 ? O10 Cu3B O10 Cu3A -0.8(6) 3_656 . . 3_656 ? N3 Cu3B O10 Cu3A 64.7(13) 3_656 . . 3_656 ? I3B Cu3B O10 Cu3A 178.4(19) 2_645 . . 3_656 ? Cu3B Cu3B O10 Cu3A 0.4(3) 3_656 . . . ? N3 Cu3B O10 Cu3A -71.8(9) . . . . ? O10 Cu3B O10 Cu3A 0.4(3) 3_656 . . . ? N3 Cu3B O10 Cu3A 65.9(9) 3_656 . . . ? I3B Cu3B O10 Cu3A 179.6(15) 2_645 . . . ? N3 Cu3B O10 Cu3B -72.2(10) . . . 3_656 ? O10 Cu3B O10 Cu3B 0.0 3_656 . . 3_656 ? N3 Cu3B O10 Cu3B 65.5(9) 3_656 . . 3_656 ? I3B Cu3B O10 Cu3B 179.2(16) 2_645 . . 3_656 ? O12 C20 O11 Cu1 -13.8(9) . . . . ? C18 C20 O11 Cu1 166.5(4) . . . . ? O8 Cu1 O11 C20 -122.8(5) 3_566 . . . ? O13 Cu1 O11 C20 113.3(13) 3_566 . . . ? O13 Cu1 O11 C20 50.7(5) . . . . ? Cu1 Cu1 O11 C20 56.5(6) 3_566 . . . ? O11 C20 O12 Sm1 -1.2(11) . . . . ? C18 C20 O12 Sm1 178.4(4) . . . . ? O7 Sm1 O12 C20 -72.6(7) . . . . ? O13 Sm1 O12 C20 -20.3(7) . . . . ? O2W Sm1 O12 C20 133.5(7) . . . . ? O1W Sm1 O12 C20 147.3(6) . . . . ? O3 Sm1 O12 C20 -151.2(7) . . . . ? O4 Sm1 O12 C20 -100.7(7) . . . . ? O3W Sm1 O12 C20 55.3(7) . . . . ? O4W Sm1 O12 C20 31.0(7) . . . . ? C7 Sm1 O12 C20 -126.4(7) . . . . ? O11 Cu1 O13 Cu1 173.81(17) . . . 3_566 ? O8 Cu1 O13 Cu1 -61.6(11) 3_566 . . 3_566 ? O13 Cu1 O13 Cu1 0.0 3_566 . . 3_566 ? O11 Cu1 O13 Sm1 -71.47(18) . . . . ? O8 Cu1 O13 Sm1 53.1(11) 3_566 . . . ? O13 Cu1 O13 Sm1 114.7(2) 3_566 . . . ? Cu1 Cu1 O13 Sm1 114.7(2) 3_566 . . . ? O7 Sm1 O13 Cu1 -51.84(16) . . . 3_566 ? O12 Sm1 O13 Cu1 161.10(19) . . . 3_566 ? O2W Sm1 O13 Cu1 119.0(2) . . . 3_566 ? O1W Sm1 O13 Cu1 -7.2(3) . . . 3_566 ? O3 Sm1 O13 Cu1 -125.11(18) . . . 3_566 ? O4 Sm1 O13 Cu1 -125.73(18) . . . 3_566 ? O3W Sm1 O13 Cu1 89.84(17) . . . 3_566 ? O4W Sm1 O13 Cu1 19.17(15) . . . 3_566 ? C7 Sm1 O13 Cu1 -126.00(18) . . . 3_566 ? O7 Sm1 O13 Cu1 -160.10(18) . . . . ? O12 Sm1 O13 Cu1 52.84(16) . . . . ? O2W Sm1 O13 Cu1 10.8(3) . . . . ? O1W Sm1 O13 Cu1 -115.5(2) . . . . ? O3 Sm1 O13 Cu1 126.63(18) . . . . ? O4 Sm1 O13 Cu1 126.02(18) . . . . ? O3W Sm1 O13 Cu1 -18.42(15) . . . . ? O4W Sm1 O13 Cu1 -89.08(17) . . . . ? C7 Sm1 O13 Cu1 125.74(18) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.089 _refine_diff_density_min -1.202 _refine_diff_density_rms 0.144 data_www1 _database_code_depnum_ccdc_archive 'CCDC 927115' #TrackingRef '927115.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H36 Cu5 I8 N6 O34 Eu2' _chemical_formula_sum 'C42 H36 Cu5 Eu2 I8 N6 O34' _chemical_formula_weight 2805.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.380(2) _cell_length_b 13.575(5) _cell_length_c 22.507(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.799(5) _cell_angle_gamma 90.00 _cell_volume 3657.0(17) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 17820 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2594 _exptl_absorpt_coefficient_mu 6.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2603 _exptl_absorpt_correction_T_max 0.2901 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17820 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_unitI/netI 0.0536 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6443 _reflns_number_gt 4982 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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. During the refinement, the command 'omit -3 50' was used to omit the weak reflections above 50 degree. During the refinement, the command 'ISOR' was used to restrain some non-H atoms with NPD and/or ADP problems. These atoms are as follows: CU3A CU3B CU2A CU2B O1 O2 O9 O10 C2 C3 C10 N3 O5 c19. All above refinement led to a relatively high restraint value (84). ; _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^)+(0.0383P)^2^+5.7899P] 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 6443 _refine_ls_number_parameters 496 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0959 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.130 _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 0.25707(2) 0.49079(2) 0.486865(13) 0.01361(10) Uani 1 1 d . . . Cu1 Cu 0.01316(6) 0.39810(6) 0.52801(3) 0.01732(18) Uani 1 1 d . . . Cu2A Cu 0.6143(5) 0.3170(3) 0.2437(2) 0.0320(9) Uani 0.50 1 d PU . 1 Cu2B Cu 0.6215(5) 0.2853(3) 0.2564(2) 0.0306(9) Uani 0.50 1 d PU . 2 Cu3A Cu 0.5065(3) 0.0004(3) 0.51251(12) 0.0151(7) Uani 0.40 1 d PU . 1 Cu3B Cu 0.4820(7) -0.0016(7) 0.4631(4) 0.013(2) Uani 0.10 1 d PU . 2 I1A I 0.0723(3) 0.5575(4) 0.1709(2) 0.0763(8) Uani 0.50 1 d P A 1 I2A I 0.3460(3) 0.5964(2) 0.1766(2) 0.0800(10) Uani 0.40 1 d P B 1 I3A I 0.5876(2) 0.56773(15) 0.17214(13) 0.0673(6) Uani 0.50 1 d P B 1 I4A I 0.8168(4) 0.5690(5) 0.1746(3) 0.0917(11) Uani 0.50 1 d P B 1 I1B I 0.1054(4) 0.5492(5) 0.1684(3) 0.1067(15) Uani 0.50 1 d P C 2 I2B I 0.33469(18) 0.54816(15) 0.17286(10) 0.0729(5) Uani 0.60 1 d P C 2 I3B I 0.5793(2) 0.51535(17) 0.16939(13) 0.0737(6) Uani 0.50 1 d P . 2 I4B I 0.8508(3) 0.5505(4) 0.1734(2) 0.0738(8) Uani 0.50 1 d P D 2 C1 C 0.3911(6) 0.2828(7) 0.2262(3) 0.039(2) Uani 1 1 d . . . C2 C 0.2826(8) 0.2900(8) 0.2277(4) 0.064(3) Uani 1 1 d U . . H2A H 0.2260 0.2670 0.1950 0.077 Uiso 1 1 calc R . . C3 C 0.2574(7) 0.3319(7) 0.2780(4) 0.057(2) Uani 1 1 d U . . H3A H 0.1836 0.3346 0.2804 0.069 Uiso 1 1 calc R . . C4 C 0.3404(6) 0.3696(6) 0.3247(3) 0.0313(18) Uani 1 1 d . . . C5 C 0.4486(6) 0.3636(6) 0.3194(3) 0.0307(18) Uani 1 1 d . . . H5A H 0.5060 0.3894 0.3506 0.037 Uiso 1 1 calc R . . C6 C 0.4266(6) 0.2362(7) 0.1746(3) 0.042(2) Uani 1 1 d . . . C7 C 0.3098(6) 0.4133(5) 0.3789(3) 0.0236(15) Uani 1 1 d . . . C8 C 0.1551(6) 0.8208(6) 0.2353(3) 0.0358(19) Uani 1 1 d . . . C9 C 0.0504(6) 0.8158(8) 0.2426(4) 0.060(3) Uani 1 1 d . . . H9A H -0.0090 0.8459 0.2148 0.073 Uiso 1 1 calc R . . C10 C 0.0341(6) 0.7645(7) 0.2929(4) 0.046(2) Uani 1 1 d U . . H10A H -0.0371 0.7603 0.2993 0.055 Uiso 1 1 calc R . . C11 C 0.1224(5) 0.7201(5) 0.3331(3) 0.0260(16) Uani 1 1 d . . . C12 C 0.2270(6) 0.7300(6) 0.3226(3) 0.0333(19) Uani 1 1 d . . . H12A H 0.2882 0.7012 0.3499 0.040 Uiso 1 1 calc R . . C13 C 0.1849(6) 0.8714(7) 0.1827(3) 0.043(2) Uani 1 1 d . . . C14 C 0.1111(6) 0.6608(5) 0.3872(3) 0.0231(15) Uani 1 1 d . . . C15 C 0.2815(6) -0.0354(5) 0.4992(4) 0.0344(18) Uani 1 1 d . . . C16 C 0.1731(6) -0.0225(6) 0.4998(5) 0.052(3) Uani 1 1 d . . . H16A H 0.1264 -0.0763 0.4993 0.062 Uiso 1 1 calc R . . C17 C 0.1336(7) 0.0729(6) 0.5012(4) 0.046(2) Uani 1 1 d . . . H17A H 0.0598 0.0834 0.5021 0.055 Uiso 1 1 calc R . . C18 C 0.2027(5) 0.1516(5) 0.5011(3) 0.0241(15) Uani 1 1 d . . . C19 C 0.3104(6) 0.1327(6) 0.5001(4) 0.0374(19) Uani 1 1 d U . . H19A H 0.3578 0.1857 0.4997 0.045 Uiso 1 1 calc R . . C20 C 0.1650(5) 0.2569(5) 0.5015(3) 0.0200(14) Uani 1 1 d . . . C21 C 0.3368(6) -0.1323(5) 0.4987(4) 0.042(2) Uani 1 1 d . . . N1 N 0.4740(5) 0.3217(5) 0.2705(3) 0.0325(15) Uani 1 1 d . . . N2 N 0.2428(5) 0.7800(5) 0.2743(3) 0.0325(15) Uani 1 1 d . . . N3 N 0.3507(5) 0.0424(4) 0.4997(3) 0.0379(16) Uani 1 1 d U . . O1 O 0.5295(4) 0.2365(5) 0.1781(2) 0.0479(15) Uani 1 1 d U . . O2 O 0.3556(4) 0.1985(5) 0.1317(3) 0.0553(17) Uani 1 1 d U . . O3 O 0.3873(4) 0.4475(4) 0.4228(2) 0.0323(12) Uani 1 1 d . . . O4 O 0.2116(4) 0.4159(4) 0.3807(2) 0.0312(12) Uani 1 1 d . . . O5 O 0.1120(5) 0.9152(5) 0.1441(3) 0.0609(17) Uani 1 1 d U . . O6 O 0.2855(4) 0.8679(4) 0.1806(2) 0.0450(15) Uani 1 1 d . . . O7 O 0.1948(4) 0.6155(3) 0.4154(2) 0.0261(11) Uani 1 1 d . . . O8 O 0.0168(4) 0.6627(4) 0.3994(2) 0.0311(12) Uani 1 1 d . . . O9 O 0.2830(4) -0.2089(4) 0.4970(3) 0.0526(16) Uani 1 1 d U . . O10 O 0.4378(5) -0.1315(4) 0.4980(3) 0.0553(16) Uani 1 1 d U . . O11 O 0.0695(4) 0.2705(3) 0.5089(2) 0.0303(12) Uani 1 1 d . . . O12 O 0.2323(4) 0.3201(3) 0.4947(2) 0.0253(11) Uani 1 1 d . . . O13 O 0.0559(3) 0.4739(3) 0.46216(17) 0.0147(9) Uani 1 1 d . . . H9 H 0.0329 0.4445 0.4205 0.022 Uiso 1 1 d R . . O1W O 0.3997(4) 0.6199(4) 0.5109(3) 0.0402(13) Uani 1 1 d . . . H1 H 0.4004 0.6562 0.4728 0.060 Uiso 1 1 d R . . H2 H 0.3819 0.6661 0.5412 0.060 Uiso 1 1 d R . . O2W O 0.4260(4) 0.4294(4) 0.5593(2) 0.0426(15) Uani 1 1 d . . . H3 H 0.4903 0.4715 0.5569 0.064 Uiso 1 1 d R . . H4 H 0.4160 0.4315 0.6016 0.064 Uiso 1 1 d R . . O3W O 0.2030(4) 0.4469(3) 0.58509(19) 0.0274(11) Uani 1 1 d . . . H5 H 0.2045 0.5038 0.6130 0.041 Uiso 1 1 d R . . H6 H 0.2474 0.3920 0.6082 0.041 Uiso 1 1 d R . . O4W O 0.1788(4) 0.6370(3) 0.5344(2) 0.0326(12) Uani 1 1 d . . . H7 H 0.2083 0.7019 0.5257 0.049 Uiso 1 1 d R . . H8 H 0.1874 0.6302 0.5792 0.049 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 0.01319(17) 0.01418(17) 0.01498(16) 0.00065(14) 0.00636(11) 0.00085(14) Cu1 0.0181(4) 0.0142(4) 0.0234(4) 0.0062(3) 0.0121(3) 0.0037(3) Cu2A 0.0237(14) 0.045(2) 0.0318(18) -0.0201(15) 0.0149(13) -0.0049(16) Cu2B 0.0230(13) 0.042(2) 0.0310(17) -0.0175(14) 0.0145(12) -0.0039(15) Cu3A 0.0154(9) 0.0139(8) 0.0158(14) -0.0005(11) 0.0038(10) 0.0019(6) Cu3B 0.013(2) 0.013(2) 0.013(2) -0.0001(11) 0.0031(12) 0.0001(10) I1A 0.059(2) 0.0867(18) 0.0864(15) -0.0038(12) 0.0242(16) -0.0069(17) I2A 0.0484(13) 0.0709(19) 0.129(2) -0.0259(19) 0.0369(13) -0.0166(15) I3A 0.0542(11) 0.0706(14) 0.0803(11) -0.0030(13) 0.0233(8) 0.0030(12) I4A 0.058(2) 0.117(3) 0.1072(17) 0.0019(17) 0.0334(17) 0.0173(16) I1B 0.055(2) 0.136(3) 0.137(2) -0.0196(18) 0.0386(18) 0.0049(19) I2B 0.0525(10) 0.0933(15) 0.0746(10) -0.0009(12) 0.0195(7) 0.0069(11) I3B 0.0410(9) 0.0902(16) 0.0943(13) 0.0052(16) 0.0253(8) -0.0009(13) I4B 0.062(2) 0.086(2) 0.0775(13) 0.0075(13) 0.0261(17) 0.0072(16) C1 0.022(4) 0.065(6) 0.035(4) -0.029(4) 0.014(3) -0.011(4) C2 0.049(4) 0.091(5) 0.054(4) -0.029(4) 0.016(4) -0.003(4) C3 0.039(4) 0.081(5) 0.057(4) -0.026(4) 0.022(3) -0.001(4) C4 0.022(4) 0.047(5) 0.027(4) -0.015(4) 0.011(3) -0.001(3) C5 0.023(4) 0.046(5) 0.025(4) -0.020(3) 0.009(3) -0.005(3) C6 0.025(4) 0.063(6) 0.039(4) -0.033(4) 0.011(4) -0.012(4) C7 0.024(4) 0.028(4) 0.021(4) -0.005(3) 0.010(3) -0.001(3) C8 0.027(4) 0.056(5) 0.027(4) 0.026(4) 0.012(3) 0.004(4) C9 0.023(4) 0.111(9) 0.050(5) 0.051(6) 0.013(4) 0.010(5) C10 0.031(4) 0.065(4) 0.044(4) 0.026(3) 0.013(3) -0.001(3) C11 0.020(4) 0.038(4) 0.022(4) 0.011(3) 0.011(3) 0.006(3) C12 0.020(4) 0.055(5) 0.027(4) 0.017(4) 0.010(3) 0.005(4) C13 0.024(4) 0.077(7) 0.029(4) 0.030(4) 0.008(3) 0.012(4) C14 0.029(4) 0.022(4) 0.022(4) 0.010(3) 0.013(3) 0.000(3) C15 0.027(4) 0.020(4) 0.061(5) 0.002(4) 0.020(4) 0.000(3) C16 0.025(4) 0.020(4) 0.115(8) -0.004(5) 0.029(5) -0.002(3) C17 0.027(4) 0.021(4) 0.097(7) 0.000(4) 0.029(5) 0.001(3) C18 0.019(4) 0.013(3) 0.044(4) 0.000(3) 0.017(3) 0.007(3) C19 0.036(3) 0.028(3) 0.050(3) -0.001(2) 0.014(2) -0.001(2) C20 0.022(4) 0.014(3) 0.026(4) 0.001(3) 0.011(3) 0.001(3) C21 0.024(4) 0.019(4) 0.086(6) 0.002(4) 0.020(4) -0.003(3) N1 0.023(3) 0.049(4) 0.029(3) -0.018(3) 0.013(3) -0.008(3) N2 0.023(3) 0.049(4) 0.027(3) 0.020(3) 0.008(3) 0.006(3) N3 0.029(3) 0.020(3) 0.068(4) 0.002(3) 0.019(3) 0.003(2) O1 0.033(3) 0.069(3) 0.045(3) -0.032(3) 0.017(2) -0.005(3) O2 0.042(3) 0.076(4) 0.050(3) -0.038(3) 0.016(3) -0.012(3) O3 0.020(3) 0.052(3) 0.026(3) -0.020(2) 0.006(2) -0.005(2) O4 0.022(3) 0.048(3) 0.026(3) -0.011(2) 0.011(2) -0.004(2) O5 0.051(3) 0.080(3) 0.053(3) 0.028(2) 0.015(2) 0.000(2) O6 0.031(3) 0.072(4) 0.035(3) 0.034(3) 0.014(2) 0.009(3) O7 0.023(3) 0.028(3) 0.030(3) 0.014(2) 0.011(2) 0.009(2) O8 0.024(3) 0.038(3) 0.038(3) 0.020(2) 0.019(2) 0.009(2) O9 0.044(3) 0.026(3) 0.092(4) -0.001(3) 0.025(3) -0.003(2) O10 0.037(3) 0.030(3) 0.102(4) 0.000(3) 0.025(3) 0.003(2) O11 0.028(3) 0.014(2) 0.056(3) 0.006(2) 0.024(2) 0.006(2) O12 0.027(3) 0.013(2) 0.040(3) -0.001(2) 0.017(2) -0.002(2) O13 0.015(2) 0.017(2) 0.013(2) -0.0021(17) 0.0055(17) 0.0021(18) O1W 0.030(3) 0.019(3) 0.068(4) -0.002(3) 0.007(3) 0.001(2) O2W 0.025(3) 0.061(4) 0.038(3) 0.029(3) 0.001(2) -0.006(3) O3W 0.038(3) 0.027(3) 0.019(2) 0.004(2) 0.011(2) 0.011(2) O4W 0.049(3) 0.020(3) 0.036(3) -0.006(2) 0.023(2) -0.008(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 Eu1 O7 2.326(4) . ? Eu1 O12 2.350(4) . ? Eu1 O13 2.420(4) . ? Eu1 O2W 2.447(5) . ? Eu1 O1W 2.448(5) . ? Eu1 O3 2.493(4) . ? Eu1 O4 2.524(4) . ? Eu1 O3W 2.539(4) . ? Eu1 O4W 2.559(5) . ? Eu1 C7 2.871(6) . ? Eu1 Cu1 3.6038(9) . ? Eu1 Cu1 3.6065(10) 3_566 ? Cu1 O8 1.949(4) 3_566 ? Cu1 O11 1.956(4) . ? Cu1 O13 1.974(4) 3_566 ? Cu1 O13 1.984(4) . ? Cu1 Cu1 3.0231(17) 3_566 ? Cu1 Eu1 3.6065(10) 3_566 ? Cu2A O1 1.919(7) . ? Cu2A O6 1.959(7) 2_645 ? Cu2A N2 1.979(8) 2_645 ? Cu2A N1 1.979(8) . ? Cu2B O6 1.939(7) 2_645 ? Cu2B O1 1.952(7) . ? Cu2B N2 1.974(8) 2_645 ? Cu2B N1 1.994(8) . ? Cu3A Cu3A 0.545(5) 3_656 ? Cu3A O10 1.945(7) 3_656 ? Cu3A N3 1.946(7) 3_656 ? Cu3A N3 1.961(7) . ? Cu3A O10 1.974(7) . ? Cu3B Cu3B 1.607(19) 3_656 ? Cu3B O10 2.061(11) . ? Cu3B N3 2.089(11) . ? Cu3B N3 2.101(11) 3_656 ? Cu3B O10 2.139(11) 3_656 ? Cu3B I3B 2.892(10) 2_645 ? I2A I3A 3.044(4) . ? I3A I4A 2.823(5) . ? I1B I2B 2.814(5) . ? I2B I3B 3.082(3) . ? I3B Cu3B 2.892(10) 2_655 ? C1 N1 1.343(8) . ? C1 C2 1.356(10) . ? C1 C6 1.484(9) . ? C2 C3 1.372(11) . ? C2 H2A 0.9300 . ? C3 C4 1.368(11) . ? C3 H3A 0.9300 . ? C4 C5 1.378(9) . ? C4 C7 1.490(9) . ? C5 N1 1.346(8) . ? C5 H5A 0.9300 . ? C6 O2 1.239(8) . ? C6 O1 1.256(8) . ? C7 O4 1.227(7) . ? C7 O3 1.274(7) . ? C8 N2 1.330(9) . ? C8 C9 1.349(10) . ? C8 C13 1.494(9) . ? C9 C10 1.386(10) . ? C9 H9A 0.9300 . ? C10 C11 1.368(10) . ? C10 H10A 0.9300 . ? C11 C12 1.381(9) . ? C11 C14 1.496(9) . ? C12 N2 1.338(8) . ? C12 H12A 0.9300 . ? C13 O5 1.234(9) . ? C13 O6 1.259(8) . ? C14 O7 1.232(8) . ? C14 O8 1.267(7) . ? C15 C16 1.356(10) . ? C15 N3 1.358(9) . ? C15 C21 1.485(10) . ? C16 C17 1.388(10) . ? C16 H16A 0.9300 . ? C17 C18 1.369(10) . ? C17 H17A 0.9300 . ? C18 C19 1.364(9) . ? C18 C20 1.504(9) . ? C19 N3 1.325(9) . ? C19 H19A 0.9300 . ? C20 O12 1.232(7) . ? C20 O11 1.250(7) . ? C21 O9 1.230(9) . ? C21 O10 1.254(8) . ? N2 Cu2B 1.974(8) 2_655 ? N2 Cu2A 1.979(8) 2_655 ? N3 Cu3A 1.946(7) 3_656 ? N3 Cu3B 2.101(11) 3_656 ? O6 Cu2B 1.939(7) 2_655 ? O6 Cu2A 1.959(7) 2_655 ? O8 Cu1 1.949(4) 3_566 ? O10 Cu3A 1.945(7) 3_656 ? O10 Cu3B 2.139(11) 3_656 ? O13 Cu1 1.974(4) 3_566 ? O13 H9 0.9907 . ? O1W H1 0.9915 . ? O1W H2 0.9919 . ? O2W H3 0.9917 . ? O2W H4 0.9916 . ? O3W H5 0.9918 . ? O3W H6 0.9914 . ? O4W H7 0.9919 . ? O4W H8 0.9912 . ? 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 O7 Eu1 O12 137.97(16) . . ? O7 Eu1 O13 76.73(14) . . ? O12 Eu1 O13 77.13(14) . . ? O7 Eu1 O2W 141.65(16) . . ? O12 Eu1 O2W 73.74(17) . . ? O13 Eu1 O2W 140.84(15) . . ? O7 Eu1 O1W 74.02(17) . . ? O12 Eu1 O1W 142.18(16) . . ? O13 Eu1 O1W 139.50(15) . . ? O2W Eu1 O1W 69.56(17) . . ? O7 Eu1 O3 85.44(16) . . ? O12 Eu1 O3 85.82(16) . . ? O13 Eu1 O3 128.63(14) . . ? O2W Eu1 O3 74.70(17) . . ? O1W Eu1 O3 76.14(17) . . ? O7 Eu1 O4 71.61(17) . . ? O12 Eu1 O4 70.86(16) . . ? O13 Eu1 O4 77.10(14) . . ? O2W Eu1 O4 116.07(18) . . ? O1W Eu1 O4 118.13(18) . . ? O3 Eu1 O4 51.53(14) . . ? O7 Eu1 O3W 131.14(15) . . ? O12 Eu1 O3W 68.58(15) . . ? O13 Eu1 O3W 72.12(14) . . ? O2W Eu1 O3W 73.19(15) . . ? O1W Eu1 O3W 108.13(17) . . ? O3 Eu1 O3W 143.33(16) . . ? O4 Eu1 O3W 133.24(16) . . ? O7 Eu1 O4W 68.34(16) . . ? O12 Eu1 O4W 131.49(15) . . ? O13 Eu1 O4W 72.09(14) . . ? O2W Eu1 O4W 109.62(18) . . ? O1W Eu1 O4W 71.40(16) . . ? O3 Eu1 O4W 142.62(16) . . ? O4 Eu1 O4W 133.74(16) . . ? O3W Eu1 O4W 66.76(15) . . ? O7 Eu1 C7 77.78(18) . . ? O12 Eu1 C7 76.40(17) . . ? O13 Eu1 C7 102.36(16) . . ? O2W Eu1 C7 95.65(19) . . ? O1W Eu1 C7 98.17(19) . . ? O3 Eu1 C7 26.29(16) . . ? O4 Eu1 C7 25.26(15) . . ? O3W Eu1 C7 144.93(18) . . ? O4W Eu1 C7 146.08(17) . . ? O7 Eu1 Cu1 106.28(11) . . ? O12 Eu1 Cu1 60.15(11) . . ? O13 Eu1 Cu1 31.27(9) . . ? O2W Eu1 Cu1 109.87(12) . . ? O1W Eu1 Cu1 142.89(13) . . ? O3 Eu1 Cu1 140.76(11) . . ? O4 Eu1 Cu1 95.95(11) . . ? O3W Eu1 Cu1 43.09(11) . . ? O4W Eu1 Cu1 74.45(11) . . ? C7 Eu1 Cu1 118.44(14) . . ? O7 Eu1 Cu1 59.73(11) . 3_566 ? O12 Eu1 Cu1 106.47(11) . 3_566 ? O13 Eu1 Cu1 30.97(10) . 3_566 ? O2W Eu1 Cu1 145.01(13) . 3_566 ? O1W Eu1 Cu1 108.70(11) . 3_566 ? O3 Eu1 Cu1 140.05(11) . 3_566 ? O4 Eu1 Cu1 95.93(11) . 3_566 ? O3W Eu1 Cu1 74.58(10) . 3_566 ? O4W Eu1 Cu1 43.40(11) . 3_566 ? C7 Eu1 Cu1 118.73(14) . 3_566 ? Cu1 Eu1 Cu1 49.58(3) . 3_566 ? O8 Cu1 O11 88.0(2) 3_566 . ? O8 Cu1 O13 95.63(18) 3_566 3_566 ? O11 Cu1 O13 173.36(19) . 3_566 ? O8 Cu1 O13 171.9(2) 3_566 . ? O11 Cu1 O13 96.69(18) . . ? O13 Cu1 O13 80.39(17) 3_566 . ? O8 Cu1 Cu1 135.54(15) 3_566 3_566 ? O11 Cu1 Cu1 136.47(14) . 3_566 ? O13 Cu1 Cu1 40.32(11) 3_566 3_566 ? O13 Cu1 Cu1 40.08(11) . 3_566 ? O8 Cu1 Eu1 135.60(14) 3_566 . ? O11 Cu1 Eu1 83.30(13) . . ? O13 Cu1 Eu1 97.86(12) 3_566 . ? O13 Cu1 Eu1 39.29(11) . . ? Cu1 Cu1 Eu1 65.26(3) 3_566 . ? O8 Cu1 Eu1 83.36(13) 3_566 3_566 ? O11 Cu1 Eu1 136.41(14) . 3_566 ? O13 Cu1 Eu1 39.12(12) 3_566 3_566 ? O13 Cu1 Eu1 97.58(11) . 3_566 ? Cu1 Cu1 Eu1 65.16(3) 3_566 3_566 ? Eu1 Cu1 Eu1 130.42(3) . 3_566 ? O1 Cu2A O6 165.9(3) . 2_645 ? O1 Cu2A N2 92.3(3) . 2_645 ? O6 Cu2A N2 82.3(3) 2_645 2_645 ? O1 Cu2A N1 84.4(3) . . ? O6 Cu2A N1 97.7(3) 2_645 . ? N2 Cu2A N1 166.2(3) 2_645 . ? O6 Cu2B O1 163.1(3) 2_645 . ? O6 Cu2B N2 83.0(3) 2_645 2_645 ? O1 Cu2B N2 91.4(3) . 2_645 ? O6 Cu2B N1 97.9(3) 2_645 . ? O1 Cu2B N1 83.2(3) . . ? N2 Cu2B N1 163.9(3) 2_645 . ? Cu3A Cu3A O10 85.1(8) 3_656 3_656 ? Cu3A Cu3A N3 83.5(7) 3_656 3_656 ? O10 Cu3A N3 83.8(3) 3_656 3_656 ? Cu3A Cu3A N3 80.4(7) 3_656 . ? O10 Cu3A N3 94.7(3) 3_656 . ? N3 Cu3A N3 163.98(16) 3_656 . ? Cu3A Cu3A O10 79.0(8) 3_656 . ? O10 Cu3A O10 164.04(16) 3_656 . ? N3 Cu3A O10 94.3(3) 3_656 . ? N3 Cu3A O10 82.7(3) . . ? Cu3B Cu3B O10 70.1(7) 3_656 . ? Cu3B Cu3B N3 67.8(6) 3_656 . ? O10 Cu3B N3 77.6(4) . . ? Cu3B Cu3B N3 67.0(6) 3_656 3_656 ? O10 Cu3B N3 87.3(4) . 3_656 ? N3 Cu3B N3 134.9(5) . 3_656 ? Cu3B Cu3B O10 65.0(6) 3_656 3_656 ? O10 Cu3B O10 135.1(5) . 3_656 ? N3 Cu3B O10 85.6(4) . 3_656 ? N3 Cu3B O10 75.6(4) 3_656 3_656 ? Cu3B Cu3B I3B 173.8(9) 3_656 2_645 ? O10 Cu3B I3B 115.8(4) . 2_645 ? N3 Cu3B I3B 111.0(4) . 2_645 ? N3 Cu3B I3B 113.8(4) 3_656 2_645 ? O10 Cu3B I3B 109.1(4) 3_656 2_645 ? I4A I3A I2A 171.76(16) . . ? I1B I2B I3B 171.29(18) . . ? Cu3B I3B I2B 92.11(19) 2_655 . ? N1 C1 C2 121.8(7) . . ? N1 C1 C6 115.2(6) . . ? C2 C1 C6 122.9(7) . . ? C1 C2 C3 119.0(8) . . ? C1 C2 H2A 120.5 . . ? C3 C2 H2A 120.5 . . ? C4 C3 C2 120.4(8) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C3 C4 C5 117.8(6) . . ? C3 C4 C7 118.7(6) . . ? C5 C4 C7 123.4(6) . . ? N1 C5 C4 122.1(6) . . ? N1 C5 H5A 118.9 . . ? C4 C5 H5A 118.9 . . ? O2 C6 O1 123.9(7) . . ? O2 C6 C1 119.6(7) . . ? O1 C6 C1 116.6(6) . . ? O4 C7 O3 121.3(6) . . ? O4 C7 C4 119.9(6) . . ? O3 C7 C4 118.7(6) . . ? O4 C7 Eu1 61.3(3) . . ? O3 C7 Eu1 60.1(3) . . ? C4 C7 Eu1 177.4(5) . . ? N2 C8 C9 123.1(6) . . ? N2 C8 C13 112.9(6) . . ? C9 C8 C13 124.0(7) . . ? C8 C9 C10 118.0(7) . . ? C8 C9 H9A 121.0 . . ? C10 C9 H9A 121.0 . . ? C11 C10 C9 120.2(7) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C10 C11 C12 118.0(6) . . ? C10 C11 C14 123.4(6) . . ? C12 C11 C14 118.5(6) . . ? N2 C12 C11 121.7(6) . . ? N2 C12 H12A 119.1 . . ? C11 C12 H12A 119.1 . . ? O5 C13 O6 123.0(7) . . ? O5 C13 C8 119.7(7) . . ? O6 C13 C8 117.3(6) . . ? O7 C14 O8 126.8(6) . . ? O7 C14 C11 116.6(6) . . ? O8 C14 C11 116.6(6) . . ? C16 C15 N3 121.5(7) . . ? C16 C15 C21 125.0(7) . . ? N3 C15 C21 113.4(6) . . ? C15 C16 C17 118.4(7) . . ? C15 C16 H16A 120.8 . . ? C17 C16 H16A 120.8 . . ? C18 C17 C16 120.3(7) . . ? C18 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? C19 C18 C17 117.8(6) . . ? C19 C18 C20 119.0(6) . . ? C17 C18 C20 123.1(6) . . ? N3 C19 C18 123.1(7) . . ? N3 C19 H19A 118.5 . . ? C18 C19 H19A 118.5 . . ? O12 C20 O11 127.3(6) . . ? O12 C20 C18 116.2(6) . . ? O11 C20 C18 116.5(6) . . ? O9 C21 O10 122.8(7) . . ? O9 C21 C15 120.1(7) . . ? O10 C21 C15 117.1(6) . . ? C1 N1 C5 118.7(6) . . ? C1 N1 Cu2A 109.0(5) . . ? C5 N1 Cu2A 132.0(5) . . ? C1 N1 Cu2B 110.0(5) . . ? C5 N1 Cu2B 130.5(5) . . ? Cu2A N1 Cu2B 14.75(17) . . ? C8 N2 C12 119.0(6) . . ? C8 N2 Cu2B 112.2(5) . 2_655 ? C12 N2 Cu2B 128.1(5) . 2_655 ? C8 N2 Cu2A 112.4(5) . 2_655 ? C12 N2 Cu2A 128.3(5) . 2_655 ? Cu2B N2 Cu2A 14.83(17) 2_655 2_655 ? C19 N3 C15 118.8(7) . . ? C19 N3 Cu3A 129.4(5) . 3_656 ? C15 N3 Cu3A 111.1(5) . 3_656 ? C19 N3 Cu3A 128.7(5) . . ? C15 N3 Cu3A 111.7(5) . . ? Cu3A N3 Cu3A 16.02(16) 3_656 . ? C19 N3 Cu3B 126.8(6) . . ? C15 N3 Cu3B 109.1(5) . . ? Cu3A N3 Cu3B 14.6(2) 3_656 . ? Cu3A N3 Cu3B 30.6(3) . . ? C19 N3 Cu3B 125.2(6) . 3_656 ? C15 N3 Cu3B 110.7(5) . 3_656 ? Cu3A N3 Cu3B 30.5(3) 3_656 3_656 ? Cu3A N3 Cu3B 14.5(2) . 3_656 ? Cu3B N3 Cu3B 45.1(5) . 3_656 ? C6 O1 Cu2A 113.4(5) . . ? C6 O1 Cu2B 114.0(5) . . ? Cu2A O1 Cu2B 15.12(17) . . ? C7 O3 Eu1 93.7(4) . . ? C7 O4 Eu1 93.4(4) . . ? C13 O6 Cu2B 113.8(5) . 2_655 ? C13 O6 Cu2A 113.2(4) . 2_655 ? Cu2B O6 Cu2A 15.03(17) 2_655 2_655 ? C14 O7 Eu1 143.7(4) . . ? C14 O8 Cu1 123.8(4) . 3_566 ? C21 O10 Cu3A 113.3(5) . 3_656 ? C21 O10 Cu3A 113.3(5) . . ? Cu3A O10 Cu3A 15.96(16) 3_656 . ? C21 O10 Cu3B 112.0(5) . . ? Cu3A O10 Cu3B 14.9(2) 3_656 . ? Cu3A O10 Cu3B 30.8(3) . . ? C21 O10 Cu3B 111.3(6) . 3_656 ? Cu3A O10 Cu3B 30.1(3) 3_656 3_656 ? Cu3A O10 Cu3B 14.1(2) . 3_656 ? Cu3B O10 Cu3B 44.9(5) . 3_656 ? C20 O11 Cu1 124.3(4) . . ? C20 O12 Eu1 143.3(4) . . ? Cu1 O13 Cu1 99.61(17) 3_566 . ? Cu1 O13 Eu1 109.91(17) 3_566 . ? Cu1 O13 Eu1 109.44(17) . . ? Cu1 O13 H9 115.6 3_566 . ? Cu1 O13 H9 115.5 . . ? Eu1 O13 H9 106.6 . . ? Eu1 O1W H1 109.3 . . ? Eu1 O1W H2 109.3 . . ? H1 O1W H2 109.5 . . ? Eu1 O2W H3 109.2 . . ? Eu1 O2W H4 109.5 . . ? H3 O2W H4 109.5 . . ? Eu1 O3W H5 113.7 . . ? Eu1 O3W H6 113.5 . . ? H5 O3W H6 109.5 . . ? Eu1 O4W H7 114.1 . . ? Eu1 O4W H8 113.6 . . ? H7 O4W H8 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.337 _refine_diff_density_min -1.058 _refine_diff_density_rms 0.148 data_www3 _database_code_depnum_ccdc_archive 'CCDC 927116' #TrackingRef '927116.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H36 Cu5 I8 N6 O34 Gd2' _chemical_formula_sum 'C42 H36 Cu5 Gd2 I8 N6 O34' _chemical_formula_weight 2816.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.390(2) _cell_length_b 13.575(3) _cell_length_c 22.512(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.811(3) _cell_angle_gamma 90.00 _cell_volume 3660.6(13) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 17773 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2598 _exptl_absorpt_coefficient_mu 6.669 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2864 _exptl_absorpt_correction_T_max 0.2975 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17773 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_unitI/netI 0.0719 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6422 _reflns_number_gt 4882 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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. During the refinement, the command 'ISOR' was used to restrain some non-H atoms with NPD and/or ADP problems. These atoms are as follows: CU3A CU3B CU2A CU2B O1 N3 C2 C3 C13 O2 O5 O6 O9 O10 C9 C10 C16 C17. All above refinement led to a relatively high restraint value (108). ; _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^)+(0.0669P)^2^+7.6163P] 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 6422 _refine_ls_number_parameters 496 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1347 _refine_ls_wR_factor_gt 0.1219 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.085 _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 0.25688(3) 0.49062(3) 0.487000(17) 0.01268(14) Uani 1 1 d . . . Cu1 Cu 0.01292(8) 0.39812(7) 0.52802(5) 0.0168(2) Uani 1 1 d . . . Cu2A Cu 0.6131(5) 0.3167(3) 0.2440(2) 0.0312(11) Uani 0.50 1 d PU . 1 Cu2B Cu 0.6223(5) 0.2848(3) 0.2569(2) 0.0284(10) Uani 0.50 1 d PU . 2 Cu3A Cu 0.5069(3) 0.0003(3) 0.51284(15) 0.0133(8) Uani 0.40 1 d PU . 1 Cu3B Cu 0.4787(9) -0.0016(8) 0.4622(6) 0.013(3) Uani 0.10 1 d PU . 2 I1A I 0.0723(4) 0.5574(5) 0.1713(3) 0.0764(10) Uani 0.50 1 d P A 1 I2A I 0.3457(4) 0.5959(3) 0.1760(2) 0.0794(12) Uani 0.40 1 d P B 1 I3A I 0.5878(3) 0.56712(18) 0.17196(15) 0.0656(7) Uani 0.50 1 d P B 1 I4A I 0.8168(4) 0.5680(6) 0.1748(4) 0.0911(14) Uani 0.50 1 d P B 1 I1B I 0.1051(5) 0.5477(7) 0.1684(4) 0.1037(18) Uani 0.50 1 d P C 2 I2B I 0.3347(2) 0.54761(19) 0.17298(12) 0.0720(6) Uani 0.60 1 d P C 2 I3B I 0.5796(2) 0.5151(2) 0.16988(16) 0.0739(8) Uani 0.50 1 d P . 2 I4B I 0.8513(4) 0.5507(5) 0.1738(3) 0.0742(10) Uani 0.50 1 d P D 2 C1 C 0.3897(8) 0.2828(8) 0.2266(5) 0.038(3) Uani 1 1 d . . . C2 C 0.2793(10) 0.2883(10) 0.2277(6) 0.060(3) Uani 1 1 d U . . H2A H 0.2227 0.2633 0.1957 0.072 Uiso 1 1 calc R . . C3 C 0.2564(10) 0.3325(9) 0.2783(5) 0.057(3) Uani 1 1 d U . . H3A H 0.1826 0.3378 0.2803 0.068 Uiso 1 1 calc R . . C4 C 0.3395(7) 0.3688(7) 0.3255(4) 0.030(2) Uani 1 1 d . . . C5 C 0.4490(8) 0.3627(7) 0.3192(4) 0.031(2) Uani 1 1 d . . . H5A H 0.5065 0.3899 0.3497 0.037 Uiso 1 1 calc R . . C6 C 0.4268(8) 0.2352(8) 0.1746(5) 0.042(3) Uani 1 1 d . . . C7 C 0.3107(7) 0.4129(6) 0.3802(4) 0.0232(19) Uani 1 1 d . . . C8 C 0.1546(8) 0.8213(7) 0.2356(4) 0.035(2) Uani 1 1 d . . . C9 C 0.0495(9) 0.8136(8) 0.2413(5) 0.047(3) Uani 1 1 d U . . H9A H -0.0104 0.8406 0.2123 0.056 Uiso 1 1 calc R . . C10 C 0.0340(9) 0.7635(8) 0.2928(5) 0.049(3) Uani 1 1 d U . . H10A H -0.0369 0.7598 0.2995 0.058 Uiso 1 1 calc R . . C11 C 0.1230(7) 0.7197(6) 0.3334(4) 0.0238(19) Uani 1 1 d . . . C12 C 0.2263(8) 0.7294(7) 0.3217(4) 0.033(2) Uani 1 1 d . . . H12A H 0.2872 0.6994 0.3484 0.039 Uiso 1 1 calc R . . C13 C 0.1858(8) 0.8719(7) 0.1829(4) 0.035(2) Uani 1 1 d U . . C14 C 0.1122(7) 0.6599(6) 0.3869(4) 0.0212(19) Uani 1 1 d . . . C15 C 0.2814(8) -0.0344(6) 0.4996(5) 0.034(2) Uani 1 1 d . . . C16 C 0.1743(9) -0.0221(7) 0.4997(6) 0.045(3) Uani 1 1 d U . . H16A H 0.1276 -0.0760 0.4987 0.054 Uiso 1 1 calc R . . C17 C 0.1347(8) 0.0737(7) 0.5014(5) 0.038(2) Uani 1 1 d U . . H17A H 0.0613 0.0841 0.5029 0.046 Uiso 1 1 calc R . . C18 C 0.2027(7) 0.1514(6) 0.5008(4) 0.026(2) Uani 1 1 d . . . C19 C 0.3120(8) 0.1326(6) 0.5007(5) 0.036(2) Uani 1 1 d . . . H19A H 0.3602 0.1853 0.5014 0.043 Uiso 1 1 calc R . . C20 C 0.1653(7) 0.2562(6) 0.5016(4) 0.0209(19) Uani 1 1 d . . . C21 C 0.3357(8) -0.1326(7) 0.4978(6) 0.048(3) Uani 1 1 d . . . N1 N 0.4737(6) 0.3196(6) 0.2715(3) 0.0325(19) Uani 1 1 d . . . N2 N 0.2429(6) 0.7795(6) 0.2742(3) 0.0306(18) Uani 1 1 d . . . N3 N 0.3503(7) 0.0419(5) 0.4997(4) 0.0355(19) Uani 1 1 d U . . O1 O 0.5294(6) 0.2360(5) 0.1787(3) 0.0446(18) Uani 1 1 d U . . O2 O 0.3546(6) 0.1977(6) 0.1321(3) 0.052(2) Uani 1 1 d U . . O3 O 0.3872(5) 0.4473(5) 0.4236(3) 0.0311(15) Uani 1 1 d . . . O4 O 0.2107(5) 0.4166(5) 0.3812(3) 0.0301(15) Uani 1 1 d . . . O5 O 0.1117(7) 0.9161(7) 0.1441(4) 0.066(2) Uani 1 1 d U . . O6 O 0.2848(6) 0.8678(5) 0.1801(3) 0.0418(17) Uani 1 1 d U . . O7 O 0.1961(5) 0.6153(4) 0.4149(3) 0.0251(14) Uani 1 1 d . . . O8 O 0.0173(5) 0.6624(4) 0.3997(3) 0.0317(15) Uani 1 1 d . . . O9 O 0.2823(6) -0.2093(5) 0.4964(4) 0.0492(19) Uani 1 1 d U . . O10 O 0.4384(6) -0.1315(5) 0.4975(4) 0.052(2) Uani 1 1 d U . . O11 O 0.0682(5) 0.2703(4) 0.5087(3) 0.0314(15) Uani 1 1 d . . . O12 O 0.2325(5) 0.3209(4) 0.4950(3) 0.0247(14) Uani 1 1 d . . . O13 O 0.0563(4) 0.4731(4) 0.4624(2) 0.0153(12) Uani 1 1 d . . . H9 H 0.0333 0.4438 0.4208 0.023 Uiso 1 1 d R . . O1W O 0.3991(5) 0.6194(4) 0.5099(4) 0.0394(17) Uani 1 1 d . . . H1 H 0.3998 0.6558 0.4718 0.059 Uiso 1 1 d R . . H2 H 0.3814 0.6656 0.5402 0.059 Uiso 1 1 d R . . O2W O 0.4250(5) 0.4300(5) 0.5591(3) 0.0422(18) Uani 1 1 d . . . H3 H 0.4893 0.4720 0.5567 0.063 Uiso 1 1 d R . . H4 H 0.4150 0.4321 0.6014 0.063 Uiso 1 1 d R . . O3W O 0.2038(5) 0.4473(4) 0.5850(3) 0.0289(14) Uani 1 1 d . . . H5 H 0.2054 0.5041 0.6129 0.043 Uiso 1 1 d R . . H6 H 0.2482 0.3924 0.6081 0.043 Uiso 1 1 d R . . O4W O 0.1803(5) 0.6366(4) 0.5344(3) 0.0324(16) Uani 1 1 d . . . H7 H 0.2097 0.7015 0.5257 0.049 Uiso 1 1 d R . . H8 H 0.1888 0.6298 0.5792 0.049 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 0.0150(2) 0.0107(2) 0.0163(2) 0.00077(16) 0.01119(16) 0.00110(16) Cu1 0.0196(5) 0.0108(5) 0.0261(5) 0.0060(4) 0.0170(4) 0.0042(4) Cu2A 0.0248(16) 0.043(2) 0.031(2) -0.0182(16) 0.0171(15) -0.0015(18) Cu2B 0.0226(16) 0.038(2) 0.0303(19) -0.0151(15) 0.0174(14) -0.0010(16) Cu3A 0.0141(10) 0.0120(9) 0.0136(14) -0.0006(10) 0.0029(10) 0.0019(7) Cu3B 0.014(3) 0.013(3) 0.013(3) 0.0001(11) 0.0030(12) 0.0002(11) I1A 0.059(3) 0.087(2) 0.089(2) -0.0071(15) 0.030(2) -0.005(2) I2A 0.0523(16) 0.067(2) 0.129(3) -0.025(2) 0.0426(17) -0.0167(19) I3A 0.0553(13) 0.0670(16) 0.0799(15) -0.0017(15) 0.0270(11) 0.0028(15) I4A 0.058(3) 0.116(3) 0.109(2) 0.003(2) 0.039(2) 0.015(2) I1B 0.057(3) 0.134(3) 0.132(3) -0.019(2) 0.046(2) 0.006(2) I2B 0.0551(13) 0.0893(18) 0.0758(13) -0.0002(14) 0.0245(10) 0.0081(14) I3B 0.0446(11) 0.087(2) 0.0980(18) 0.0049(19) 0.0318(12) -0.0026(16) I4B 0.060(3) 0.091(2) 0.0784(17) 0.0092(15) 0.032(2) 0.008(2) C1 0.024(5) 0.053(6) 0.043(6) -0.024(5) 0.017(5) -0.010(5) C2 0.051(5) 0.079(5) 0.053(5) -0.025(4) 0.021(4) 0.000(4) C3 0.043(5) 0.076(5) 0.056(5) -0.019(4) 0.023(4) 0.001(4) C4 0.022(5) 0.043(6) 0.027(5) -0.021(4) 0.010(4) -0.004(4) C5 0.023(5) 0.042(6) 0.032(5) -0.016(4) 0.017(4) -0.004(4) C6 0.029(5) 0.061(7) 0.039(6) -0.032(5) 0.015(5) -0.009(5) C7 0.024(5) 0.028(5) 0.025(5) 0.001(4) 0.018(4) 0.004(4) C8 0.030(5) 0.049(6) 0.029(5) 0.021(5) 0.014(5) -0.001(5) C9 0.038(4) 0.059(5) 0.046(4) 0.024(4) 0.014(4) 0.000(4) C10 0.040(4) 0.062(5) 0.050(5) 0.020(4) 0.022(4) -0.003(4) C11 0.027(5) 0.026(5) 0.021(5) 0.013(4) 0.012(4) 0.005(4) C12 0.025(5) 0.047(6) 0.029(5) 0.024(4) 0.014(4) 0.010(5) C13 0.032(4) 0.049(4) 0.029(4) 0.019(3) 0.012(3) 0.002(4) C14 0.025(5) 0.022(4) 0.021(4) 0.004(3) 0.015(4) 0.004(4) C15 0.036(5) 0.012(4) 0.060(7) 0.000(4) 0.026(5) 0.000(4) C16 0.038(4) 0.033(4) 0.067(5) 0.003(4) 0.020(4) -0.004(4) C17 0.029(4) 0.029(4) 0.058(5) -0.001(4) 0.013(4) 0.003(3) C18 0.024(5) 0.017(4) 0.042(6) 0.001(4) 0.019(4) 0.003(4) C19 0.032(5) 0.012(4) 0.072(7) 0.002(4) 0.031(5) 0.002(4) C20 0.026(5) 0.010(4) 0.033(5) 0.002(3) 0.019(4) 0.007(4) C21 0.030(6) 0.015(5) 0.110(10) -0.003(5) 0.041(6) -0.003(4) N1 0.031(4) 0.040(5) 0.031(5) -0.014(4) 0.017(4) -0.004(4) N2 0.025(4) 0.045(5) 0.027(4) 0.017(4) 0.016(4) 0.004(4) N3 0.030(3) 0.021(3) 0.060(4) 0.002(3) 0.019(3) 0.001(3) O1 0.034(3) 0.063(4) 0.043(3) -0.026(3) 0.021(3) -0.004(3) O2 0.043(4) 0.068(4) 0.049(4) -0.030(3) 0.021(3) -0.006(3) O3 0.017(3) 0.051(4) 0.028(4) -0.018(3) 0.012(3) -0.006(3) O4 0.027(3) 0.040(4) 0.028(3) -0.015(3) 0.015(3) -0.007(3) O5 0.052(4) 0.092(4) 0.059(4) 0.036(4) 0.023(3) 0.000(4) O6 0.032(3) 0.059(4) 0.041(3) 0.019(3) 0.021(3) -0.001(3) O7 0.024(3) 0.025(3) 0.032(3) 0.018(3) 0.017(3) 0.007(3) O8 0.026(3) 0.037(4) 0.038(4) 0.022(3) 0.021(3) 0.009(3) O9 0.042(3) 0.029(3) 0.080(4) 0.000(3) 0.023(3) 0.000(3) O10 0.042(4) 0.030(3) 0.089(4) -0.001(3) 0.025(3) 0.005(3) O11 0.030(4) 0.015(3) 0.058(4) 0.002(3) 0.028(3) 0.002(3) O12 0.027(3) 0.008(3) 0.046(4) -0.002(2) 0.023(3) 0.000(2) O13 0.020(3) 0.015(3) 0.015(3) -0.002(2) 0.011(2) -0.003(2) O1W 0.026(3) 0.014(3) 0.075(5) -0.003(3) 0.008(4) -0.002(3) O2W 0.023(3) 0.057(5) 0.046(4) 0.031(4) 0.008(3) -0.004(3) O3W 0.038(4) 0.027(3) 0.028(3) 0.002(3) 0.020(3) 0.011(3) O4W 0.051(4) 0.020(3) 0.036(4) -0.002(3) 0.029(4) -0.006(3) _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 O7 2.332(5) . ? Gd1 O12 2.336(5) . ? Gd1 O13 2.415(5) . ? Gd1 O2W 2.434(6) . ? Gd1 O1W 2.442(6) . ? Gd1 O3 2.484(5) . ? Gd1 O4 2.514(6) . ? Gd1 O3W 2.527(6) . ? Gd1 O4W 2.546(6) . ? Gd1 C7 2.857(8) . ? Cu1 O8 1.943(5) 3_566 ? Cu1 O11 1.955(6) . ? Cu1 O13 1.978(5) . ? Cu1 O13 1.983(5) 3_566 ? Cu1 Cu1 3.0229(19) 3_566 ? Cu2A O1 1.912(8) . ? Cu2A O6 1.974(8) 2_645 ? Cu2A N1 1.978(9) . ? Cu2A N2 1.995(9) 2_645 ? Cu2B O6 1.942(8) 2_645 ? Cu2B O1 1.956(8) . ? Cu2B N2 1.971(9) 2_645 ? Cu2B N1 2.008(9) . ? Cu3A Cu3A 0.559(7) 3_656 ? Cu3A O10 1.942(8) 3_656 ? Cu3A N3 1.948(9) 3_656 ? Cu3A N3 1.969(9) . ? Cu3A O10 1.973(8) . ? Cu3B Cu3B 1.65(3) 3_656 ? Cu3B O10 2.049(13) . ? Cu3B N3 2.070(13) . ? Cu3B N3 2.143(14) 3_656 ? Cu3B O10 2.160(13) 3_656 ? Cu3B I3B 2.883(14) 2_645 ? I2A I3A 3.049(5) . ? I3A I4A 2.822(5) . ? I1B I2B 2.820(5) . ? I2B I3B 3.085(4) . ? I3B Cu3B 2.883(14) 2_655 ? C1 N1 1.348(12) . ? C1 C2 1.376(14) . ? C1 C6 1.509(12) . ? C2 C3 1.380(15) . ? C2 H2A 0.9300 . ? C3 C4 1.369(14) . ? C3 H3A 0.9300 . ? C4 C5 1.401(12) . ? C4 C7 1.493(11) . ? C5 N1 1.326(11) . ? C5 H5A 0.9300 . ? C6 O2 1.240(11) . ? C6 O1 1.250(11) . ? C7 O4 1.246(10) . ? C7 O3 1.264(10) . ? C8 N2 1.337(12) . ? C8 C9 1.346(14) . ? C8 C13 1.504(12) . ? C9 C10 1.398(14) . ? C9 H9A 0.9300 . ? C10 C11 1.375(13) . ? C10 H10A 0.9300 . ? C11 C12 1.377(12) . ? C11 C14 1.487(10) . ? C12 N2 1.327(10) . ? C12 H12A 0.9300 . ? C13 O5 1.247(12) . ? C13 O6 1.246(11) . ? C14 O7 1.229(10) . ? C14 O8 1.281(10) . ? C15 C16 1.338(14) . ? C15 N3 1.342(11) . ? C15 C21 1.499(12) . ? C16 C17 1.393(13) . ? C16 H16A 0.9300 . ? C17 C18 1.353(12) . ? C17 H17A 0.9300 . ? C18 C19 1.378(12) . ? C18 C20 1.498(11) . ? C19 N3 1.322(11) . ? C19 H19A 0.9300 . ? C20 O12 1.245(9) . ? C20 O11 1.268(10) . ? C21 O9 1.230(11) . ? C21 O10 1.274(11) . ? N2 Cu2B 1.971(9) 2_655 ? N2 Cu2A 1.995(9) 2_655 ? N3 Cu3A 1.948(9) 3_656 ? N3 Cu3B 2.143(14) 3_656 ? O6 Cu2B 1.942(8) 2_655 ? O6 Cu2A 1.974(8) 2_655 ? O8 Cu1 1.943(5) 3_566 ? O10 Cu3A 1.942(8) 3_656 ? O10 Cu3B 2.160(13) 3_656 ? O13 Cu1 1.983(5) 3_566 ? O13 H9 0.9909 . ? O1W H1 0.9917 . ? O1W H2 0.9921 . ? O2W H3 0.9923 . ? O2W H4 0.9918 . ? O3W H5 0.9918 . ? O3W H6 0.9916 . ? O4W H7 0.9921 . ? O4W H8 0.9914 . ? 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 O7 Gd1 O12 138.1(2) . . ? O7 Gd1 O13 77.40(18) . . ? O12 Gd1 O13 76.99(18) . . ? O7 Gd1 O2W 141.1(2) . . ? O12 Gd1 O2W 73.8(2) . . ? O13 Gd1 O2W 140.77(19) . . ? O7 Gd1 O1W 73.4(2) . . ? O12 Gd1 O1W 142.2(2) . . ? O13 Gd1 O1W 139.75(18) . . ? O2W Gd1 O1W 69.7(2) . . ? O7 Gd1 O3 85.0(2) . . ? O12 Gd1 O3 85.8(2) . . ? O13 Gd1 O3 128.83(18) . . ? O2W Gd1 O3 74.4(2) . . ? O1W Gd1 O3 75.6(2) . . ? O7 Gd1 O4 71.1(2) . . ? O12 Gd1 O4 71.1(2) . . ? O13 Gd1 O4 76.83(18) . . ? O2W Gd1 O4 116.4(2) . . ? O1W Gd1 O4 117.6(2) . . ? O3 Gd1 O4 52.00(19) . . ? O7 Gd1 O3W 131.80(19) . . ? O12 Gd1 O3W 68.60(19) . . ? O13 Gd1 O3W 72.25(19) . . ? O2W Gd1 O3W 73.1(2) . . ? O1W Gd1 O3W 108.5(2) . . ? O3 Gd1 O3W 143.0(2) . . ? O4 Gd1 O3W 133.4(2) . . ? O7 Gd1 O4W 68.8(2) . . ? O12 Gd1 O4W 131.71(18) . . ? O13 Gd1 O4W 72.57(19) . . ? O2W Gd1 O4W 109.3(2) . . ? O1W Gd1 O4W 71.4(2) . . ? O3 Gd1 O4W 142.3(2) . . ? O4 Gd1 O4W 133.6(2) . . ? O3W Gd1 O4W 66.89(18) . . ? O7 Gd1 C7 77.6(2) . . ? O12 Gd1 C7 76.3(2) . . ? O13 Gd1 C7 102.6(2) . . ? O2W Gd1 C7 95.3(2) . . ? O1W Gd1 C7 97.5(2) . . ? O3 Gd1 C7 26.2(2) . . ? O4 Gd1 C7 25.8(2) . . ? O3W Gd1 C7 144.8(2) . . ? O4W Gd1 C7 146.4(2) . . ? O8 Cu1 O11 88.0(3) 3_566 . ? O8 Cu1 O13 172.0(3) 3_566 . ? O11 Cu1 O13 96.5(2) . . ? O8 Cu1 O13 95.8(2) 3_566 3_566 ? O11 Cu1 O13 172.9(3) . 3_566 ? O13 Cu1 O13 80.5(2) . 3_566 ? O8 Cu1 Cu1 135.54(19) 3_566 3_566 ? O11 Cu1 Cu1 136.46(18) . 3_566 ? O13 Cu1 Cu1 40.31(14) . 3_566 ? O13 Cu1 Cu1 40.19(14) 3_566 3_566 ? O1 Cu2A O6 165.6(4) . 2_645 ? O1 Cu2A N1 84.6(4) . . ? O6 Cu2A N1 98.1(4) 2_645 . ? O1 Cu2A N2 92.0(4) . 2_645 ? O6 Cu2A N2 81.8(3) 2_645 2_645 ? N1 Cu2A N2 165.4(4) . 2_645 ? O6 Cu2B O1 162.9(4) 2_645 . ? O6 Cu2B N2 83.3(3) 2_645 2_645 ? O1 Cu2B N2 91.4(4) . 2_645 ? O6 Cu2B N1 98.1(4) 2_645 . ? O1 Cu2B N1 82.7(3) . . ? N2 Cu2B N1 164.3(4) 2_645 . ? Cu3A Cu3A O10 84.9(8) 3_656 3_656 ? Cu3A Cu3A N3 84.0(8) 3_656 3_656 ? O10 Cu3A N3 83.9(3) 3_656 3_656 ? Cu3A Cu3A N3 79.6(8) 3_656 . ? O10 Cu3A N3 94.6(3) 3_656 . ? N3 Cu3A N3 163.6(2) 3_656 . ? Cu3A Cu3A O10 78.6(8) 3_656 . ? O10 Cu3A O10 163.6(2) 3_656 . ? N3 Cu3A O10 94.3(3) 3_656 . ? N3 Cu3A O10 82.6(3) . . ? Cu3B Cu3B O10 70.5(8) 3_656 . ? Cu3B Cu3B N3 69.3(8) 3_656 . ? O10 Cu3B N3 78.3(5) . . ? Cu3B Cu3B N3 64.6(7) 3_656 3_656 ? O10 Cu3B N3 86.5(5) . 3_656 ? N3 Cu3B N3 133.9(7) . 3_656 ? Cu3B Cu3B O10 63.4(7) 3_656 3_656 ? O10 Cu3B O10 133.9(7) . 3_656 ? N3 Cu3B O10 85.5(5) . 3_656 ? N3 Cu3B O10 74.4(5) 3_656 3_656 ? Cu3B Cu3B I3B 172.8(10) 3_656 2_645 ? O10 Cu3B I3B 116.5(5) . 2_645 ? N3 Cu3B I3B 112.5(5) . 2_645 ? N3 Cu3B I3B 113.2(5) 3_656 2_645 ? O10 Cu3B I3B 109.5(5) 3_656 2_645 ? I4A I3A I2A 171.9(2) . . ? I1B I2B I3B 171.2(2) . . ? Cu3B I3B I2B 92.6(2) 2_655 . ? N1 C1 C2 123.2(9) . . ? N1 C1 C6 114.2(8) . . ? C2 C1 C6 122.6(9) . . ? C1 C2 C3 116.9(11) . . ? C1 C2 H2A 121.5 . . ? C3 C2 H2A 121.5 . . ? C4 C3 C2 121.6(11) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C3 C4 C5 117.2(8) . . ? C3 C4 C7 119.5(8) . . ? C5 C4 C7 123.3(8) . . ? N1 C5 C4 122.5(9) . . ? N1 C5 H5A 118.7 . . ? C4 C5 H5A 118.7 . . ? O2 C6 O1 125.5(9) . . ? O2 C6 C1 118.1(8) . . ? O1 C6 C1 116.4(8) . . ? O4 C7 O3 121.6(7) . . ? O4 C7 C4 118.7(8) . . ? O3 C7 C4 119.7(7) . . ? O4 C7 Gd1 61.5(4) . . ? O3 C7 Gd1 60.2(4) . . ? C4 C7 Gd1 178.0(6) . . ? N2 C8 C9 123.8(8) . . ? N2 C8 C13 112.0(8) . . ? C9 C8 C13 124.1(9) . . ? C8 C9 C10 117.3(10) . . ? C8 C9 H9A 121.4 . . ? C10 C9 H9A 121.4 . . ? C11 C10 C9 120.3(10) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C10 C11 C12 117.3(8) . . ? C10 C11 C14 123.5(8) . . ? C12 C11 C14 119.1(8) . . ? N2 C12 C11 123.1(8) . . ? N2 C12 H12A 118.4 . . ? C11 C12 H12A 118.4 . . ? O5 C13 O6 122.9(8) . . ? O5 C13 C8 118.7(8) . . ? O6 C13 C8 118.3(8) . . ? O7 C14 O8 127.0(7) . . ? O7 C14 C11 116.5(7) . . ? O8 C14 C11 116.5(8) . . ? C16 C15 N3 122.3(8) . . ? C16 C15 C21 124.3(8) . . ? N3 C15 C21 113.4(8) . . ? C15 C16 C17 118.2(9) . . ? C15 C16 H16A 120.9 . . ? C17 C16 H16A 120.9 . . ? C18 C17 C16 120.2(9) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? C17 C18 C19 118.0(8) . . ? C17 C18 C20 123.0(8) . . ? C19 C18 C20 118.9(8) . . ? N3 C19 C18 122.0(8) . . ? N3 C19 H19A 119.0 . . ? C18 C19 H19A 119.0 . . ? O12 C20 O11 126.4(7) . . ? O12 C20 C18 116.7(7) . . ? O11 C20 C18 116.8(7) . . ? O9 C21 O10 122.7(9) . . ? O9 C21 C15 120.8(8) . . ? O10 C21 C15 116.5(8) . . ? C5 N1 C1 118.5(8) . . ? C5 N1 Cu2A 131.5(7) . . ? C1 N1 Cu2A 109.1(6) . . ? C5 N1 Cu2B 130.4(7) . . ? C1 N1 Cu2B 110.8(6) . . ? Cu2A N1 Cu2B 14.91(18) . . ? C12 N2 C8 118.1(8) . . ? C12 N2 Cu2B 128.7(7) . 2_655 ? C8 N2 Cu2B 112.3(6) . 2_655 ? C12 N2 Cu2A 128.8(7) . 2_655 ? C8 N2 Cu2A 112.6(6) . 2_655 ? Cu2B N2 Cu2A 14.99(18) 2_655 2_655 ? C19 N3 C15 119.2(8) . . ? C19 N3 Cu3A 128.3(6) . 3_656 ? C15 N3 Cu3A 112.0(6) . 3_656 ? C19 N3 Cu3A 127.5(7) . . ? C15 N3 Cu3A 112.4(6) . . ? Cu3A N3 Cu3A 16.4(2) 3_656 . ? C19 N3 Cu3B 126.1(7) . . ? C15 N3 Cu3B 109.5(7) . . ? Cu3A N3 Cu3B 15.2(3) 3_656 . ? Cu3A N3 Cu3B 31.6(4) . . ? C19 N3 Cu3B 123.6(7) . 3_656 ? C15 N3 Cu3B 111.5(7) . 3_656 ? Cu3A N3 Cu3B 30.9(4) 3_656 3_656 ? Cu3A N3 Cu3B 14.5(3) . 3_656 ? Cu3B N3 Cu3B 46.1(7) . 3_656 ? C6 O1 Cu2A 113.8(6) . . ? C6 O1 Cu2B 115.1(6) . . ? Cu2A O1 Cu2B 15.33(18) . . ? C7 O3 Gd1 93.6(4) . . ? C7 O4 Gd1 92.7(5) . . ? C13 O6 Cu2B 113.3(6) . 2_655 ? C13 O6 Cu2A 113.2(6) . 2_655 ? Cu2B O6 Cu2A 15.17(18) 2_655 2_655 ? C14 O7 Gd1 142.7(5) . . ? C14 O8 Cu1 124.2(5) . 3_566 ? C21 O10 Cu3A 113.0(6) . 3_656 ? C21 O10 Cu3A 113.3(6) . . ? Cu3A O10 Cu3A 16.4(2) 3_656 . ? C21 O10 Cu3B 110.8(7) . . ? Cu3A O10 Cu3B 15.4(3) 3_656 . ? Cu3A O10 Cu3B 31.8(4) . . ? C21 O10 Cu3B 112.1(7) . 3_656 ? Cu3A O10 Cu3B 30.7(4) 3_656 3_656 ? Cu3A O10 Cu3B 14.3(3) . 3_656 ? Cu3B O10 Cu3B 46.1(7) . 3_656 ? C20 O11 Cu1 124.0(5) . . ? C20 O12 Gd1 144.0(5) . . ? Cu1 O13 Cu1 99.5(2) . 3_566 ? Cu1 O13 Gd1 109.9(2) . . ? Cu1 O13 Gd1 109.7(2) 3_566 . ? Cu1 O13 H9 115.6 . . ? Cu1 O13 H9 115.4 3_566 . ? Gd1 O13 H9 106.7 . . ? Gd1 O1W H1 109.9 . . ? Gd1 O1W H2 108.8 . . ? H1 O1W H2 109.5 . . ? Gd1 O2W H3 109.4 . . ? Gd1 O2W H4 109.5 . . ? H3 O2W H4 109.5 . . ? Gd1 O3W H5 113.9 . . ? Gd1 O3W H6 113.6 . . ? H5 O3W H6 109.5 . . ? Gd1 O4W H7 114.4 . . ? Gd1 O4W H8 113.6 . . ? H7 O4W H8 109.5 . . ? 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 I1B I2B I3B Cu3B 63.9(15) . . . 2_655 ? N1 C1 C2 C3 -1(2) . . . . ? C6 C1 C2 C3 179.2(11) . . . . ? C1 C2 C3 C4 0(2) . . . . ? C2 C3 C4 C5 2.5(18) . . . . ? C2 C3 C4 C7 -177.9(11) . . . . ? C3 C4 C5 N1 -3.3(16) . . . . ? C7 C4 C5 N1 177.1(9) . . . . ? N1 C1 C6 O2 178.5(10) . . . . ? C2 C1 C6 O2 -1.8(19) . . . . ? N1 C1 C6 O1 -0.5(16) . . . . ? C2 C1 C6 O1 179.2(12) . . . . ? C3 C4 C7 O4 -0.8(14) . . . . ? C5 C4 C7 O4 178.8(9) . . . . ? C3 C4 C7 O3 -179.3(10) . . . . ? C5 C4 C7 O3 0.3(15) . . . . ? C3 C4 C7 Gd1 94(18) . . . . ? C5 C4 C7 Gd1 -87(18) . . . . ? O7 Gd1 C7 O4 -72.0(5) . . . . ? O12 Gd1 C7 O4 74.8(5) . . . . ? O13 Gd1 C7 O4 1.8(5) . . . . ? O2W Gd1 C7 O4 146.7(5) . . . . ? O1W Gd1 C7 O4 -143.1(5) . . . . ? O3 Gd1 C7 O4 -176.2(9) . . . . ? O3W Gd1 C7 O4 78.8(6) . . . . ? O4W Gd1 C7 O4 -75.7(7) . . . . ? O7 Gd1 C7 O3 104.2(5) . . . . ? O12 Gd1 C7 O3 -109.0(5) . . . . ? O13 Gd1 C7 O3 178.0(5) . . . . ? O2W Gd1 C7 O3 -37.1(5) . . . . ? O1W Gd1 C7 O3 33.1(5) . . . . ? O4 Gd1 C7 O3 176.2(9) . . . . ? O3W Gd1 C7 O3 -104.9(6) . . . . ? O4W Gd1 C7 O3 100.6(6) . . . . ? O7 Gd1 C7 C4 -168(18) . . . . ? O12 Gd1 C7 C4 -21(18) . . . . ? O13 Gd1 C7 C4 -94(18) . . . . ? O2W Gd1 C7 C4 51(18) . . . . ? O1W Gd1 C7 C4 121(18) . . . . ? O3 Gd1 C7 C4 88(18) . . . . ? O4 Gd1 C7 C4 -96(18) . . . . ? O3W Gd1 C7 C4 -17(18) . . . . ? O4W Gd1 C7 C4 -171(17) . . . . ? N2 C8 C9 C10 3.7(18) . . . . ? C13 C8 C9 C10 179.4(10) . . . . ? C8 C9 C10 C11 -3.5(17) . . . . ? C9 C10 C11 C12 1.3(16) . . . . ? C9 C10 C11 C14 -176.0(10) . . . . ? C10 C11 C12 N2 0.9(16) . . . . ? C14 C11 C12 N2 178.4(9) . . . . ? N2 C8 C13 O5 -178.3(10) . . . . ? C9 C8 C13 O5 5.5(18) . . . . ? N2 C8 C13 O6 1.6(14) . . . . ? C9 C8 C13 O6 -174.6(11) . . . . ? C10 C11 C14 O7 171.4(9) . . . . ? C12 C11 C14 O7 -5.9(13) . . . . ? C10 C11 C14 O8 -10.2(14) . . . . ? C12 C11 C14 O8 172.4(9) . . . . ? N3 C15 C16 C17 -1.5(17) . . . . ? C21 C15 C16 C17 -179.9(11) . . . . ? C15 C16 C17 C18 2.2(17) . . . . ? C16 C17 C18 C19 -2.3(16) . . . . ? C16 C17 C18 C20 179.1(10) . . . . ? C17 C18 C19 N3 1.7(16) . . . . ? C20 C18 C19 N3 -179.6(9) . . . . ? C17 C18 C20 O12 -173.4(9) . . . . ? C19 C18 C20 O12 8.0(13) . . . . ? C17 C18 C20 O11 6.4(14) . . . . ? C19 C18 C20 O11 -172.2(9) . . . . ? C16 C15 C21 O9 0(2) . . . . ? N3 C15 C21 O9 -178.7(11) . . . . ? C16 C15 C21 O10 179.5(12) . . . . ? N3 C15 C21 O10 1.0(16) . . . . ? C4 C5 N1 C1 1.9(15) . . . . ? C4 C5 N1 Cu2A 169.7(8) . . . . ? C4 C5 N1 Cu2B -170.6(8) . . . . ? C2 C1 N1 C5 0.4(17) . . . . ? C6 C1 N1 C5 -179.9(9) . . . . ? C2 C1 N1 Cu2A -170.0(11) . . . . ? C6 C1 N1 Cu2A 9.8(12) . . . . ? C2 C1 N1 Cu2B 174.3(10) . . . . ? C6 C1 N1 Cu2B -6.0(12) . . . . ? O1 Cu2A N1 C5 179.6(10) . . . . ? O6 Cu2A N1 C5 13.9(10) 2_645 . . . ? N2 Cu2A N1 C5 102.4(18) 2_645 . . . ? O1 Cu2A N1 C1 -11.7(7) . . . . ? O6 Cu2A N1 C1 -177.5(7) 2_645 . . . ? N2 Cu2A N1 C1 -88.9(18) 2_645 . . . ? O1 Cu2A N1 Cu2B 87.5(11) . . . . ? O6 Cu2A N1 Cu2B -78.2(11) 2_645 . . . ? N2 Cu2A N1 Cu2B 10.3(12) 2_645 . . . ? O6 Cu2B N1 C5 -16.7(10) 2_645 . . . ? O1 Cu2B N1 C5 -179.5(9) . . . . ? N2 Cu2B N1 C5 -110.7(16) 2_645 . . . ? O6 Cu2B N1 C1 170.3(7) 2_645 . . . ? O1 Cu2B N1 C1 7.5(7) . . . . ? N2 Cu2B N1 C1 76.4(17) 2_645 . . . ? O6 Cu2B N1 Cu2A 84.2(11) 2_645 . . . ? O1 Cu2B N1 Cu2A -78.6(11) . . . . ? N2 Cu2B N1 Cu2A -9.8(11) 2_645 . . . ? C11 C12 N2 C8 -0.9(15) . . . . ? C11 C12 N2 Cu2B -169.7(7) . . . 2_655 ? C11 C12 N2 Cu2A 171.0(7) . . . 2_655 ? C9 C8 N2 C12 -1.5(16) . . . . ? C13 C8 N2 C12 -177.7(9) . . . . ? C9 C8 N2 Cu2B 169.1(10) . . . 2_655 ? C13 C8 N2 Cu2B -7.2(11) . . . 2_655 ? C9 C8 N2 Cu2A -174.7(10) . . . 2_655 ? C13 C8 N2 Cu2A 9.1(11) . . . 2_655 ? C18 C19 N3 C15 -1.0(16) . . . . ? C18 C19 N3 Cu3A 169.9(8) . . . 3_656 ? C18 C19 N3 Cu3A -169.3(8) . . . . ? C18 C19 N3 Cu3B 151.0(9) . . . . ? C18 C19 N3 Cu3B -152.1(9) . . . 3_656 ? C16 C15 N3 C19 0.9(16) . . . . ? C21 C15 N3 C19 179.4(10) . . . . ? C16 C15 N3 Cu3A -171.4(10) . . . 3_656 ? C21 C15 N3 Cu3A 7.2(12) . . . 3_656 ? C16 C15 N3 Cu3A 170.9(10) . . . . ? C21 C15 N3 Cu3A -10.6(12) . . . . ? C16 C15 N3 Cu3B -155.3(10) . . . . ? C21 C15 N3 Cu3B 23.2(12) . . . . ? C16 C15 N3 Cu3B 155.3(10) . . . 3_656 ? C21 C15 N3 Cu3B -26.1(12) . . . 3_656 ? Cu3A Cu3A N3 C19 -99.1(12) 3_656 . . . ? O10 Cu3A N3 C19 -15.1(10) 3_656 . . . ? N3 Cu3A N3 C19 -99.1(12) 3_656 . . . ? O10 Cu3A N3 C19 -178.9(10) . . . . ? Cu3A Cu3A N3 C15 91.9(10) 3_656 . . . ? O10 Cu3A N3 C15 175.9(7) 3_656 . . . ? N3 Cu3A N3 C15 91.9(10) 3_656 . . . ? O10 Cu3A N3 C15 12.1(7) . . . . ? O10 Cu3A N3 Cu3A 84.0(8) 3_656 . . 3_656 ? N3 Cu3A N3 Cu3A 0.000(1) 3_656 . . 3_656 ? O10 Cu3A N3 Cu3A -79.8(8) . . . 3_656 ? Cu3A Cu3A N3 Cu3B 0.7(9) 3_656 . . . ? O10 Cu3A N3 Cu3B 84.7(6) 3_656 . . . ? N3 Cu3A N3 Cu3B 0.7(9) 3_656 . . . ? O10 Cu3A N3 Cu3B -79.1(6) . . . . ? Cu3A Cu3A N3 Cu3B -178.6(18) 3_656 . . 3_656 ? O10 Cu3A N3 Cu3B -94.6(14) 3_656 . . 3_656 ? N3 Cu3A N3 Cu3B -178.6(18) 3_656 . . 3_656 ? O10 Cu3A N3 Cu3B 101.7(13) . . . 3_656 ? Cu3B Cu3B N3 C19 104.4(11) 3_656 . . . ? O10 Cu3B N3 C19 177.8(10) . . . . ? N3 Cu3B N3 C19 104.4(11) 3_656 . . . ? O10 Cu3B N3 C19 41.2(11) 3_656 . . . ? I3B Cu3B N3 C19 -68.1(11) 2_645 . . . ? Cu3B Cu3B N3 C15 -101.5(10) 3_656 . . . ? O10 Cu3B N3 C15 -28.1(8) . . . . ? N3 Cu3B N3 C15 -101.5(10) 3_656 . . . ? O10 Cu3B N3 C15 -164.7(8) 3_656 . . . ? I3B Cu3B N3 C15 86.0(8) 2_645 . . . ? Cu3B Cu3B N3 Cu3A 0.5(7) 3_656 . . 3_656 ? O10 Cu3B N3 Cu3A 73.9(12) . . . 3_656 ? N3 Cu3B N3 Cu3A 0.5(7) 3_656 . . 3_656 ? O10 Cu3B N3 Cu3A -62.7(12) 3_656 . . 3_656 ? I3B Cu3B N3 Cu3A -172.0(16) 2_645 . . 3_656 ? Cu3B Cu3B N3 Cu3A -0.3(3) 3_656 . . . ? O10 Cu3B N3 Cu3A 73.1(6) . . . . ? N3 Cu3B N3 Cu3A -0.3(3) 3_656 . . . ? O10 Cu3B N3 Cu3A -63.5(5) 3_656 . . . ? I3B Cu3B N3 Cu3A -172.8(8) 2_645 . . . ? O10 Cu3B N3 Cu3B 73.4(7) . . . 3_656 ? N3 Cu3B N3 Cu3B 0.0 3_656 . . 3_656 ? O10 Cu3B N3 Cu3B -63.2(7) 3_656 . . 3_656 ? I3B Cu3B N3 Cu3B -172.5(10) 2_645 . . 3_656 ? O2 C6 O1 Cu2A 171.4(10) . . . . ? C1 C6 O1 Cu2A -9.7(13) . . . . ? O2 C6 O1 Cu2B -171.8(10) . . . . ? C1 C6 O1 Cu2B 7.1(14) . . . . ? O6 Cu2A O1 C6 113.6(18) 2_645 . . . ? N1 Cu2A O1 C6 12.1(9) . . . . ? N2 Cu2A O1 C6 177.8(8) 2_645 . . . ? O6 Cu2A O1 Cu2B 15.5(11) 2_645 . . . ? N1 Cu2A O1 Cu2B -86.0(12) . . . . ? N2 Cu2A O1 Cu2B 79.7(12) 2_645 . . . ? O6 Cu2B O1 C6 -102.2(16) 2_645 . . . ? N2 Cu2B O1 C6 -173.6(9) 2_645 . . . ? N1 Cu2B O1 C6 -8.3(9) . . . . ? O6 Cu2B O1 Cu2A -13.3(9) 2_645 . . . ? N2 Cu2B O1 Cu2A -84.8(12) 2_645 . . . ? N1 Cu2B O1 Cu2A 80.6(12) . . . . ? O4 C7 O3 Gd1 3.9(9) . . . . ? C4 C7 O3 Gd1 -177.7(7) . . . . ? O7 Gd1 O3 C7 -71.9(5) . . . . ? O12 Gd1 O3 C7 67.1(5) . . . . ? O13 Gd1 O3 C7 -2.5(6) . . . . ? O2W Gd1 O3 C7 141.4(6) . . . . ? O1W Gd1 O3 C7 -146.0(6) . . . . ? O4 Gd1 O3 C7 -2.1(5) . . . . ? O3W Gd1 O3 C7 112.3(6) . . . . ? O4W Gd1 O3 C7 -116.9(5) . . . . ? O3 C7 O4 Gd1 -3.9(9) . . . . ? C4 C7 O4 Gd1 177.7(7) . . . . ? O7 Gd1 O4 C7 100.8(5) . . . . ? O12 Gd1 O4 C7 -97.6(5) . . . . ? O13 Gd1 O4 C7 -178.2(5) . . . . ? O2W Gd1 O4 C7 -37.6(6) . . . . ? O1W Gd1 O4 C7 42.2(6) . . . . ? O3 Gd1 O4 C7 2.1(5) . . . . ? O3W Gd1 O4 C7 -128.9(5) . . . . ? O4W Gd1 O4 C7 132.2(5) . . . . ? O5 C13 O6 Cu2B -175.2(9) . . . 2_655 ? C8 C13 O6 Cu2B 5.0(12) . . . 2_655 ? O5 C13 O6 Cu2A 168.3(9) . . . 2_655 ? C8 C13 O6 Cu2A -11.6(12) . . . 2_655 ? O8 C14 O7 Gd1 16.4(16) . . . . ? C11 C14 O7 Gd1 -165.5(6) . . . . ? O12 Gd1 O7 C14 64.3(10) . . . . ? O13 Gd1 O7 C14 10.8(9) . . . . ? O2W Gd1 O7 C14 -160.0(9) . . . . ? O1W Gd1 O7 C14 -141.2(10) . . . . ? O3 Gd1 O7 C14 142.4(10) . . . . ? O4 Gd1 O7 C14 91.0(10) . . . . ? O3W Gd1 O7 C14 -41.0(11) . . . . ? O4W Gd1 O7 C14 -65.2(9) . . . . ? C7 Gd1 O7 C14 116.9(10) . . . . ? O7 C14 O8 Cu1 4.8(13) . . . 3_566 ? C11 C14 O8 Cu1 -173.4(6) . . . 3_566 ? O9 C21 O10 Cu3A 171.0(10) . . . 3_656 ? C15 C21 O10 Cu3A -8.7(14) . . . 3_656 ? O9 C21 O10 Cu3A -171.2(10) . . . . ? C15 C21 O10 Cu3A 9.2(14) . . . . ? O9 C21 O10 Cu3B 154.5(11) . . . . ? C15 C21 O10 Cu3B -25.1(14) . . . . ? O9 C21 O10 Cu3B -155.8(11) . . . 3_656 ? C15 C21 O10 Cu3B 24.6(14) . . . 3_656 ? Cu3A Cu3A O10 C21 -92.6(11) 3_656 . . . ? O10 Cu3A O10 C21 -92.6(11) 3_656 . . . ? N3 Cu3A O10 C21 -175.6(9) 3_656 . . . ? N3 Cu3A O10 C21 -11.8(9) . . . . ? O10 Cu3A O10 Cu3A 0.000(2) 3_656 . . 3_656 ? N3 Cu3A O10 Cu3A -83.0(8) 3_656 . . 3_656 ? N3 Cu3A O10 Cu3A 80.8(8) . . . 3_656 ? Cu3A Cu3A O10 Cu3B -0.3(9) 3_656 . . . ? O10 Cu3A O10 Cu3B -0.3(9) 3_656 . . . ? N3 Cu3A O10 Cu3B -83.3(6) 3_656 . . . ? N3 Cu3A O10 Cu3B 80.5(6) . . . . ? Cu3A Cu3A O10 Cu3B 179.3(18) 3_656 . . 3_656 ? O10 Cu3A O10 Cu3B 179.3(18) 3_656 . . 3_656 ? N3 Cu3A O10 Cu3B 96.3(13) 3_656 . . 3_656 ? N3 Cu3A O10 Cu3B -99.9(13) . . . 3_656 ? Cu3B Cu3B O10 C21 101.1(11) 3_656 . . . ? N3 Cu3B O10 C21 29.1(9) . . . . ? N3 Cu3B O10 C21 165.4(9) 3_656 . . . ? O10 Cu3B O10 C21 101.1(11) 3_656 . . . ? I3B Cu3B O10 C21 -80.4(9) 2_645 . . . ? Cu3B Cu3B O10 Cu3A -0.2(6) 3_656 . . 3_656 ? N3 Cu3B O10 Cu3A -72.2(12) . . . 3_656 ? N3 Cu3B O10 Cu3A 64.0(12) 3_656 . . 3_656 ? O10 Cu3B O10 Cu3A -0.2(6) 3_656 . . 3_656 ? I3B Cu3B O10 Cu3A 178.3(16) 2_645 . . 3_656 ? Cu3B Cu3B O10 Cu3A 0.1(3) 3_656 . . . ? N3 Cu3B O10 Cu3A -71.8(6) . . . . ? N3 Cu3B O10 Cu3A 64.4(5) 3_656 . . . ? O10 Cu3B O10 Cu3A 0.1(3) 3_656 . . . ? I3B Cu3B O10 Cu3A 178.7(8) 2_645 . . . ? N3 Cu3B O10 Cu3B -72.0(7) . . . 3_656 ? N3 Cu3B O10 Cu3B 64.3(7) 3_656 . . 3_656 ? O10 Cu3B O10 Cu3B 0.0 3_656 . . 3_656 ? I3B Cu3B O10 Cu3B 178.6(11) 2_645 . . 3_656 ? O12 C20 O11 Cu1 -13.4(13) . . . . ? C18 C20 O11 Cu1 166.9(6) . . . . ? O8 Cu1 O11 C20 -123.2(7) 3_566 . . . ? O13 Cu1 O11 C20 50.2(7) . . . . ? O13 Cu1 O11 C20 114.5(18) 3_566 . . . ? Cu1 Cu1 O11 C20 56.2(8) 3_566 . . . ? O11 C20 O12 Gd1 -2.1(16) . . . . ? C18 C20 O12 Gd1 177.7(7) . . . . ? O7 Gd1 O12 C20 -73.1(10) . . . . ? O13 Gd1 O12 C20 -19.4(10) . . . . ? O2W Gd1 O12 C20 134.1(10) . . . . ? O1W Gd1 O12 C20 149.2(9) . . . . ? O3 Gd1 O12 C20 -150.9(10) . . . . ? O4 Gd1 O12 C20 -99.8(10) . . . . ? O3W Gd1 O12 C20 56.3(10) . . . . ? O4W Gd1 O12 C20 32.4(11) . . . . ? C7 Gd1 O12 C20 -126.1(10) . . . . ? O8 Cu1 O13 Cu1 -62.6(17) 3_566 . . 3_566 ? O11 Cu1 O13 Cu1 173.6(3) . . . 3_566 ? O13 Cu1 O13 Cu1 0.0 3_566 . . 3_566 ? O8 Cu1 O13 Gd1 52.4(17) 3_566 . . . ? O11 Cu1 O13 Gd1 -71.4(3) . . . . ? O13 Cu1 O13 Gd1 115.1(3) 3_566 . . . ? Cu1 Cu1 O13 Gd1 115.1(3) 3_566 . . . ? O7 Gd1 O13 Cu1 -160.7(3) . . . . ? O12 Gd1 O13 Cu1 52.8(2) . . . . ? O2W Gd1 O13 Cu1 10.2(4) . . . . ? O1W Gd1 O13 Cu1 -116.5(3) . . . . ? O3 Gd1 O13 Cu1 126.4(3) . . . . ? O4 Gd1 O13 Cu1 126.1(3) . . . . ? O3W Gd1 O13 Cu1 -18.6(2) . . . . ? O4W Gd1 O13 Cu1 -89.2(2) . . . . ? C7 Gd1 O13 Cu1 125.3(2) . . . . ? O7 Gd1 O13 Cu1 -52.3(2) . . . 3_566 ? O12 Gd1 O13 Cu1 161.2(3) . . . 3_566 ? O2W Gd1 O13 Cu1 118.6(4) . . . 3_566 ? O1W Gd1 O13 Cu1 -8.1(4) . . . 3_566 ? O3 Gd1 O13 Cu1 -125.2(3) . . . 3_566 ? O4 Gd1 O13 Cu1 -125.5(3) . . . 3_566 ? O3W Gd1 O13 Cu1 89.8(2) . . . 3_566 ? O4W Gd1 O13 Cu1 19.2(2) . . . 3_566 ? C7 Gd1 O13 Cu1 -126.3(3) . . . 3_566 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.228 _refine_diff_density_min -1.494 _refine_diff_density_rms 0.224 data_www4 _database_code_depnum_ccdc_archive 'CCDC 927117' #TrackingRef '927117.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H36 Cu5 I8 N6 O34 Tb2' _chemical_formula_sum 'C42 H36 Cu5 I8 N6 O34 Tb2' _chemical_formula_weight 2819.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.3775(10) _cell_length_b 13.5563(12) _cell_length_c 22.4534(19) _cell_angle_alpha 90.00 _cell_angle_beta 105.0040(10) _cell_angle_gamma 90.00 _cell_volume 3639.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 18293 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2602 _exptl_absorpt_coefficient_mu 6.830 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2697 _exptl_absorpt_correction_T_max 0.2910 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18293 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_unitI/netI 0.0381 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6386 _reflns_number_gt 5345 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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. During the refinement, the command 'omit -3 50' was used to omit the weak reflections above 50 degree. During the refinement, the command 'ISOR' was used to restrain some non-H atoms with NPD and/or ADP problems. These atoms are as follows: CU3A CU3B CU2A CU2B O5 C2 C3 O1 O2 O6 O9 O10 C9 C13. All above refinement led to a relatively high restraint value (84). ; _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^)+(0.0350P)^2^+18.4637P] 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 6386 _refine_ls_number_parameters 496 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0812 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.25667(2) 0.490474(18) 0.486903(12) 0.01159(9) Uani 1 1 d . . . Cu1 Cu 0.01277(6) 0.39807(5) 0.52781(3) 0.01615(16) Uani 1 1 d . . . Cu2A Cu 0.6141(5) 0.3157(3) 0.2446(2) 0.0320(9) Uani 0.50 1 d PU . 1 Cu2B Cu 0.6219(4) 0.2855(3) 0.2571(2) 0.0289(9) Uani 0.50 1 d PU . 2 Cu3A Cu 0.5060(8) 0.0008(8) 0.5127(2) 0.015(3) Uani 0.40 1 d PU . 1 Cu3B Cu 0.481(3) -0.002(3) 0.4629(10) 0.016(4) Uani 0.10 1 d PU . 2 I1A I 0.0725(3) 0.5581(3) 0.1714(2) 0.0713(7) Uani 0.50 1 d P A 1 I2A I 0.3456(2) 0.59602(18) 0.17559(17) 0.0749(8) Uani 0.40 1 d P B 1 I3A I 0.58769(17) 0.56763(13) 0.17184(10) 0.0621(5) Uani 0.50 1 d P B 1 I4A I 0.8170(3) 0.5691(4) 0.1747(3) 0.0868(10) Uani 0.50 1 d P B 1 I1B I 0.1050(3) 0.5473(5) 0.1680(3) 0.0990(13) Uani 0.50 1 d P C 2 I2B I 0.33432(15) 0.54763(14) 0.17289(9) 0.0681(4) Uani 0.60 1 d P C 2 I3B I 0.57952(15) 0.51544(15) 0.17034(11) 0.0692(5) Uani 0.50 1 d P . 2 I4B I 0.8515(3) 0.5511(3) 0.1744(2) 0.0705(7) Uani 0.50 1 d P D 2 C1 C 0.3903(6) 0.2833(6) 0.2265(3) 0.0386(18) Uani 1 1 d . . . C2 C 0.2808(7) 0.2895(8) 0.2280(4) 0.061(2) Uani 1 1 d U . . H2A H 0.2242 0.2652 0.1955 0.074 Uiso 1 1 calc R . . C3 C 0.2560(7) 0.3323(7) 0.2784(4) 0.055(2) Uani 1 1 d U . . H3A H 0.1822 0.3361 0.2806 0.066 Uiso 1 1 calc R . . C4 C 0.3395(5) 0.3692(5) 0.3250(3) 0.0301(16) Uani 1 1 d . . . C5 C 0.4484(5) 0.3635(5) 0.3200(3) 0.0302(16) Uani 1 1 d . . . H5A H 0.5059 0.3897 0.3512 0.036 Uiso 1 1 calc R . . C6 C 0.4265(6) 0.2355(6) 0.1746(3) 0.0391(19) Uani 1 1 d . . . C7 C 0.3100(5) 0.4136(5) 0.3800(3) 0.0224(14) Uani 1 1 d . . . C8 C 0.1545(5) 0.8213(6) 0.2350(3) 0.0348(17) Uani 1 1 d . . . C9 C 0.0502(7) 0.8159(7) 0.2425(4) 0.052(2) Uani 1 1 d U . . H9A H -0.0094 0.8459 0.2145 0.063 Uiso 1 1 calc R . . C10 C 0.0334(6) 0.7646(7) 0.2930(4) 0.053(2) Uani 1 1 d . . . H10A H -0.0375 0.7608 0.2998 0.063 Uiso 1 1 calc R . . C11 C 0.1228(5) 0.7197(5) 0.3326(3) 0.0259(14) Uani 1 1 d . . . C12 C 0.2271(5) 0.7292(5) 0.3218(3) 0.0309(16) Uani 1 1 d . . . H12A H 0.2884 0.7000 0.3490 0.037 Uiso 1 1 calc R . . C13 C 0.1845(6) 0.8722(6) 0.1821(3) 0.0372(17) Uani 1 1 d U . . C14 C 0.1113(5) 0.6607(4) 0.3872(3) 0.0214(13) Uani 1 1 d . . . C15 C 0.2809(6) -0.0346(5) 0.4987(4) 0.0333(17) Uani 1 1 d . . . C16 C 0.1731(6) -0.0215(5) 0.4986(5) 0.048(2) Uani 1 1 d . . . H16A H 0.1261 -0.0755 0.4972 0.057 Uiso 1 1 calc R . . C17 C 0.1332(6) 0.0735(5) 0.5006(4) 0.044(2) Uani 1 1 d . . . H17A H 0.0597 0.0840 0.5022 0.053 Uiso 1 1 calc R . . C18 C 0.2022(5) 0.1515(4) 0.5003(3) 0.0258(14) Uani 1 1 d . . . C19 C 0.3120(6) 0.1339(4) 0.5001(4) 0.0356(18) Uani 1 1 d . . . H19A H 0.3599 0.1868 0.5002 0.043 Uiso 1 1 calc R . . C20 C 0.1651(5) 0.2571(4) 0.5012(3) 0.0217(13) Uani 1 1 d . . . C21 C 0.3361(6) -0.1326(5) 0.4972(4) 0.0378(19) Uani 1 1 d . . . N1 N 0.4732(4) 0.3209(4) 0.2709(3) 0.0308(13) Uani 1 1 d . . . N2 N 0.2426(4) 0.7789(4) 0.2736(3) 0.0311(14) Uani 1 1 d . . . N3 N 0.3502(5) 0.0421(4) 0.4998(3) 0.0406(17) Uani 1 1 d . . . O1 O 0.5291(4) 0.2359(4) 0.1786(2) 0.0473(14) Uani 1 1 d U . . O2 O 0.3548(4) 0.1982(4) 0.1317(2) 0.0506(15) Uani 1 1 d U . . O3 O 0.3874(3) 0.4470(4) 0.4242(2) 0.0317(11) Uani 1 1 d . . . O4 O 0.2106(3) 0.4157(3) 0.3813(2) 0.0276(10) Uani 1 1 d . . . O5 O 0.1115(5) 0.9170(5) 0.1443(3) 0.0613(16) Uani 1 1 d U . . O6 O 0.2842(4) 0.8681(4) 0.1796(2) 0.0414(13) Uani 1 1 d U . . O7 O 0.1959(3) 0.6143(3) 0.41512(19) 0.0235(10) Uani 1 1 d . . . O8 O 0.0177(4) 0.6629(3) 0.3996(2) 0.0319(11) Uani 1 1 d . . . O9 O 0.2817(4) -0.2092(3) 0.4955(3) 0.0484(14) Uani 1 1 d U . . O10 O 0.4377(4) -0.1313(4) 0.4974(3) 0.0529(15) Uani 1 1 d U . . O11 O 0.0688(4) 0.2706(3) 0.5083(2) 0.0308(11) Uani 1 1 d . . . O12 O 0.2331(3) 0.3216(3) 0.4949(2) 0.0226(10) Uani 1 1 d . . . O13 O 0.0575(3) 0.4740(3) 0.46257(17) 0.0134(8) Uani 1 1 d . . . H9 H 0.0344 0.4446 0.4209 0.020 Uiso 1 1 d R . . O1W O 0.3981(4) 0.6181(3) 0.5097(3) 0.0389(13) Uani 1 1 d . . . H1 H 0.3989 0.6545 0.4716 0.058 Uiso 1 1 d R . . H2 H 0.3804 0.6643 0.5400 0.058 Uiso 1 1 d R . . O2W O 0.4239(4) 0.4306(4) 0.5590(2) 0.0391(13) Uani 1 1 d . . . H3 H 0.4881 0.4727 0.5566 0.059 Uiso 1 1 d R . . H4 H 0.4138 0.4327 0.6013 0.059 Uiso 1 1 d R . . O3W O 0.2027(4) 0.4469(3) 0.5846(2) 0.0286(10) Uani 1 1 d . . . H5 H 0.2042 0.5037 0.6125 0.043 Uiso 1 1 d R . . H6 H 0.2471 0.3920 0.6077 0.043 Uiso 1 1 d R . . O4W O 0.1808(4) 0.6354(3) 0.5342(2) 0.0325(11) Uani 1 1 d . . . H7 H 0.2103 0.7003 0.5255 0.049 Uiso 1 1 d R . . H8 H 0.1894 0.6286 0.5790 0.049 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 Tb1 0.00985(14) 0.01251(14) 0.01430(15) 0.00075(11) 0.00655(10) 0.00072(10) Cu1 0.0156(4) 0.0134(3) 0.0241(4) 0.0066(3) 0.0134(3) 0.0037(3) Cu2A 0.0201(12) 0.049(2) 0.0317(19) -0.0226(15) 0.0147(12) -0.0049(15) Cu2B 0.0175(12) 0.0442(19) 0.0296(17) -0.0184(13) 0.0146(11) -0.0036(14) Cu3A 0.014(4) 0.0120(10) 0.023(9) -0.003(8) 0.009(7) 0.002(2) Cu3B 0.017(6) 0.018(4) 0.016(10) -0.001(8) 0.008(7) 0.003(4) I1A 0.0494(19) 0.0886(15) 0.0795(13) -0.0065(10) 0.0229(13) -0.0040(14) I2A 0.0423(10) 0.0682(15) 0.122(2) -0.0248(16) 0.0356(11) -0.0165(12) I3A 0.0504(9) 0.0657(11) 0.0741(10) -0.0015(11) 0.0230(7) 0.0031(9) I4A 0.0498(19) 0.118(2) 0.0998(16) 0.0033(15) 0.0316(16) 0.0155(14) I1B 0.0478(19) 0.129(2) 0.129(2) -0.0142(15) 0.0395(16) 0.0072(16) I2B 0.0466(8) 0.0893(12) 0.0703(9) -0.0014(10) 0.0188(6) 0.0056(9) I3B 0.0360(7) 0.0839(13) 0.0930(12) 0.0052(13) 0.0262(7) -0.0020(10) I4B 0.0537(19) 0.0861(16) 0.0763(12) 0.0087(11) 0.0253(15) 0.0054(13) C1 0.022(4) 0.063(5) 0.033(4) -0.026(4) 0.010(3) -0.009(3) C2 0.044(4) 0.091(5) 0.050(4) -0.037(4) 0.012(3) -0.004(4) C3 0.033(3) 0.084(5) 0.055(4) -0.029(4) 0.021(3) -0.004(3) C4 0.021(3) 0.049(4) 0.024(4) -0.017(3) 0.012(3) -0.003(3) C5 0.020(3) 0.043(4) 0.029(4) -0.021(3) 0.009(3) -0.004(3) C6 0.022(4) 0.065(5) 0.033(4) -0.029(4) 0.010(3) -0.008(3) C7 0.021(3) 0.026(3) 0.021(3) -0.004(3) 0.007(3) 0.000(3) C8 0.021(3) 0.057(5) 0.027(4) 0.025(3) 0.008(3) 0.007(3) C9 0.038(4) 0.074(4) 0.046(4) 0.031(3) 0.014(3) 0.009(3) C10 0.019(4) 0.091(7) 0.051(5) 0.046(5) 0.015(3) 0.010(4) C11 0.019(3) 0.033(3) 0.029(4) 0.014(3) 0.012(3) 0.004(3) C12 0.021(3) 0.050(4) 0.023(4) 0.022(3) 0.009(3) 0.006(3) C13 0.029(3) 0.055(4) 0.028(3) 0.024(3) 0.009(3) 0.004(3) C14 0.021(3) 0.019(3) 0.026(4) 0.008(3) 0.010(3) 0.002(2) C15 0.026(4) 0.016(3) 0.062(5) 0.000(3) 0.018(3) 0.000(3) C16 0.026(4) 0.015(3) 0.109(8) 0.001(4) 0.029(4) -0.003(3) C17 0.024(4) 0.018(3) 0.099(7) -0.003(4) 0.030(4) 0.002(3) C18 0.023(3) 0.017(3) 0.043(4) 0.003(3) 0.019(3) 0.003(3) C19 0.030(4) 0.010(3) 0.074(6) 0.004(3) 0.028(4) -0.001(3) C20 0.023(3) 0.013(3) 0.032(4) 0.000(3) 0.013(3) 0.004(2) C21 0.023(4) 0.014(3) 0.082(6) 0.002(3) 0.025(4) 0.001(3) N1 0.020(3) 0.046(3) 0.029(3) -0.018(3) 0.011(2) -0.002(2) N2 0.018(3) 0.051(4) 0.027(3) 0.022(3) 0.013(2) 0.006(3) N3 0.023(3) 0.017(3) 0.091(5) 0.005(3) 0.029(3) 0.002(2) O1 0.031(3) 0.072(3) 0.044(3) -0.033(3) 0.019(2) -0.007(2) O2 0.036(3) 0.073(3) 0.046(3) -0.036(3) 0.015(2) -0.011(2) O3 0.016(2) 0.054(3) 0.028(3) -0.021(2) 0.0121(19) -0.005(2) O4 0.017(2) 0.043(3) 0.028(3) -0.013(2) 0.0139(19) -0.0032(19) O5 0.054(2) 0.074(2) 0.057(2) 0.0199(19) 0.0186(18) 0.0007(18) O6 0.030(2) 0.065(3) 0.033(3) 0.027(2) 0.017(2) 0.006(2) O7 0.018(2) 0.029(2) 0.026(2) 0.0164(19) 0.0118(18) 0.0052(18) O8 0.023(2) 0.041(3) 0.039(3) 0.025(2) 0.020(2) 0.011(2) O9 0.041(3) 0.023(2) 0.086(4) -0.001(2) 0.025(3) -0.001(2) O10 0.036(3) 0.024(2) 0.104(4) 0.000(3) 0.028(3) 0.002(2) O11 0.025(2) 0.013(2) 0.063(3) 0.003(2) 0.026(2) 0.0037(18) O12 0.021(2) 0.0124(19) 0.038(3) 0.0012(18) 0.015(2) 0.0015(17) O13 0.0129(19) 0.0143(19) 0.015(2) -0.0002(15) 0.0073(16) 0.0006(15) O1W 0.023(2) 0.016(2) 0.075(4) -0.002(2) 0.007(2) -0.0020(19) O2W 0.019(2) 0.056(3) 0.039(3) 0.026(3) 0.001(2) -0.006(2) O3W 0.033(3) 0.032(2) 0.025(3) 0.005(2) 0.015(2) 0.010(2) O4W 0.046(3) 0.019(2) 0.042(3) -0.004(2) 0.027(2) -0.006(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 Tb1 O7 2.313(4) . ? Tb1 O12 2.321(4) . ? Tb1 O13 2.394(4) . ? Tb1 O2W 2.414(4) . ? Tb1 O1W 2.420(4) . ? Tb1 O3 2.476(4) . ? Tb1 O4 2.505(4) . ? Tb1 O3W 2.523(4) . ? Tb1 O4W 2.527(4) . ? Tb1 C7 2.847(6) . ? Cu1 O8 1.950(4) 3_566 ? Cu1 O11 1.953(4) . ? Cu1 O13 1.977(4) 3_566 ? Cu1 O13 1.983(4) . ? Cu1 Cu1 3.0153(13) 3_566 ? Cu2A O1 1.914(7) . ? Cu2A O6 1.969(7) 2_645 ? Cu2A N1 1.982(8) . ? Cu2A N2 1.984(7) 2_645 ? Cu2B O6 1.942(7) 2_645 ? Cu2B O1 1.956(7) . ? Cu2B N2 1.974(8) 2_645 ? Cu2B N1 2.002(8) . ? Cu3A Cu3A 0.550(9) 3_656 ? Cu3A O10 1.936(12) 3_656 ? Cu3A N3 1.956(11) . ? Cu3A N3 1.961(11) 3_656 ? Cu3A O10 1.972(12) . ? Cu3B Cu3B 1.61(4) 3_656 ? Cu3B O10 2.04(3) . ? Cu3B N3 2.09(3) . ? Cu3B N3 2.11(3) 3_656 ? Cu3B O10 2.15(3) 3_656 ? Cu3B I3B 2.90(2) 2_645 ? I2A I3A 3.044(3) . ? I3A I4A 2.823(4) . ? I1B I2B 2.812(4) . ? I2B I3B 3.081(3) . ? I3B Cu3B 2.90(2) 2_655 ? C1 N1 1.333(8) . ? C1 C2 1.367(11) . ? C1 C6 1.501(9) . ? C2 C3 1.376(11) . ? C2 H2A 0.9300 . ? C3 C4 1.361(10) . ? C3 H3A 0.9300 . ? C4 C5 1.385(9) . ? C4 C7 1.501(9) . ? C5 N1 1.347(8) . ? C5 H5A 0.9300 . ? C6 O2 1.236(8) . ? C6 O1 1.250(8) . ? C7 O4 1.238(7) . ? C7 O3 1.270(7) . ? C8 N2 1.335(8) . ? C8 C9 1.347(10) . ? C8 C13 1.502(9) . ? C9 C10 1.390(10) . ? C9 H9A 0.9300 . ? C10 C11 1.371(9) . ? C10 H10A 0.9300 . ? C11 C12 1.381(9) . ? C11 C14 1.500(8) . ? C12 N2 1.329(8) . ? C12 H12A 0.9300 . ? C13 O5 1.228(8) . ? C13 O6 1.252(8) . ? C14 O7 1.243(7) . ? C14 O8 1.261(7) . ? C15 N3 1.343(8) . ? C15 C16 1.346(10) . ? C15 C21 1.498(9) . ? C16 C17 1.385(9) . ? C16 H16A 0.9300 . ? C17 C18 1.360(9) . ? C17 H17A 0.9300 . ? C18 C19 1.381(9) . ? C18 C20 1.506(8) . ? C19 N3 1.332(8) . ? C19 H19A 0.9300 . ? C20 O12 1.247(7) . ? C20 O11 1.256(7) . ? C21 O9 1.233(8) . ? C21 O10 1.257(8) . ? N2 Cu2B 1.974(8) 2_655 ? N2 Cu2A 1.984(8) 2_655 ? N3 Cu3A 1.961(11) 3_656 ? N3 Cu3B 2.11(3) 3_656 ? O6 Cu2B 1.942(7) 2_655 ? O6 Cu2A 1.969(7) 2_655 ? O8 Cu1 1.950(4) 3_566 ? O10 Cu3A 1.936(12) 3_656 ? O10 Cu3B 2.15(3) 3_656 ? O13 Cu1 1.977(4) 3_566 ? O13 H9 0.9876 . ? O1W H1 0.9894 . ? O1W H2 0.9908 . ? O2W H3 0.9913 . ? O2W H4 0.9896 . ? O3W H5 0.9900 . ? O3W H6 0.9891 . ? O4W H7 0.9909 . ? O4W H8 0.9885 . ? 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 O7 Tb1 O12 138.12(15) . . ? O7 Tb1 O13 77.21(13) . . ? O12 Tb1 O13 77.44(13) . . ? O7 Tb1 O2W 141.15(15) . . ? O12 Tb1 O2W 73.73(16) . . ? O13 Tb1 O2W 140.82(14) . . ? O7 Tb1 O1W 73.49(16) . . ? O12 Tb1 O1W 141.96(14) . . ? O13 Tb1 O1W 139.56(13) . . ? O2W Tb1 O1W 69.56(16) . . ? O7 Tb1 O3 85.35(16) . . ? O12 Tb1 O3 85.58(15) . . ? O13 Tb1 O3 129.35(13) . . ? O2W Tb1 O3 74.25(17) . . ? O1W Tb1 O3 75.35(17) . . ? O7 Tb1 O4 71.37(15) . . ? O12 Tb1 O4 70.84(15) . . ? O13 Tb1 O4 77.14(13) . . ? O2W Tb1 O4 116.40(17) . . ? O1W Tb1 O4 117.67(17) . . ? O3 Tb1 O4 52.21(14) . . ? O7 Tb1 O3W 131.60(14) . . ? O12 Tb1 O3W 68.59(15) . . ? O13 Tb1 O3W 71.80(13) . . ? O2W Tb1 O3W 73.27(15) . . ? O1W Tb1 O3W 108.87(18) . . ? O3 Tb1 O3W 142.94(15) . . ? O4 Tb1 O3W 132.97(15) . . ? O7 Tb1 O4W 68.89(15) . . ? O12 Tb1 O4W 131.80(14) . . ? O13 Tb1 O4W 72.29(14) . . ? O2W Tb1 O4W 109.06(18) . . ? O1W Tb1 O4W 71.48(15) . . ? O3 Tb1 O4W 142.46(15) . . ? O4 Tb1 O4W 133.96(15) . . ? O3W Tb1 O4W 66.78(14) . . ? O7 Tb1 C7 77.44(16) . . ? O12 Tb1 C7 76.43(16) . . ? O13 Tb1 C7 102.90(15) . . ? O2W Tb1 C7 95.56(18) . . ? O1W Tb1 C7 97.30(18) . . ? O3 Tb1 C7 26.46(15) . . ? O4 Tb1 C7 25.76(15) . . ? O3W Tb1 C7 144.96(16) . . ? O4W Tb1 C7 146.25(16) . . ? O8 Cu1 O11 88.20(19) 3_566 . ? O8 Cu1 O13 95.46(17) 3_566 3_566 ? O11 Cu1 O13 172.90(18) . 3_566 ? O8 Cu1 O13 171.60(19) 3_566 . ? O11 Cu1 O13 96.34(17) . . ? O13 Cu1 O13 80.81(16) 3_566 . ? O8 Cu1 Cu1 135.47(14) 3_566 3_566 ? O11 Cu1 Cu1 136.33(14) . 3_566 ? O13 Cu1 Cu1 40.47(11) 3_566 3_566 ? O13 Cu1 Cu1 40.34(10) . 3_566 ? O1 Cu2A O6 166.7(3) . 2_645 ? O1 Cu2A N1 84.3(3) . . ? O6 Cu2A N1 98.3(3) 2_645 . ? O1 Cu2A N2 92.3(3) . 2_645 ? O6 Cu2A N2 82.2(3) 2_645 2_645 ? N1 Cu2A N2 166.6(3) . 2_645 ? O6 Cu2B O1 163.3(3) 2_645 . ? O6 Cu2B N2 83.1(3) 2_645 2_645 ? O1 Cu2B N2 91.3(3) . 2_645 ? O6 Cu2B N1 98.5(3) 2_645 . ? O1 Cu2B N1 82.7(3) . . ? N2 Cu2B N1 164.4(3) 2_645 . ? Cu3A Cu3A O10 86(2) 3_656 3_656 ? Cu3A Cu3A N3 82(2) 3_656 . ? O10 Cu3A N3 95.3(5) 3_656 . ? Cu3A Cu3A N3 81(2) 3_656 3_656 ? O10 Cu3A N3 83.5(4) 3_656 3_656 ? N3 Cu3A N3 163.9(3) . 3_656 ? Cu3A Cu3A O10 78(2) 3_656 . ? O10 Cu3A O10 163.9(3) 3_656 . ? N3 Cu3A O10 82.7(4) . . ? N3 Cu3A O10 94.0(5) 3_656 . ? Cu3B Cu3B O10 71(2) 3_656 . ? Cu3B Cu3B N3 68(2) 3_656 . ? O10 Cu3B N3 77.8(11) . . ? Cu3B Cu3B N3 67(2) 3_656 3_656 ? O10 Cu3B N3 87.6(12) . 3_656 ? N3 Cu3B N3 134.9(11) . 3_656 ? Cu3B Cu3B O10 64(2) 3_656 3_656 ? O10 Cu3B O10 134.9(11) . 3_656 ? N3 Cu3B O10 85.6(12) . 3_656 ? N3 Cu3B O10 75.1(10) 3_656 3_656 ? Cu3B Cu3B I3B 173(3) 3_656 2_645 ? O10 Cu3B I3B 116.0(12) . 2_645 ? N3 Cu3B I3B 111.5(11) . 2_645 ? N3 Cu3B I3B 113.2(12) 3_656 2_645 ? O10 Cu3B I3B 109.1(12) 3_656 2_645 ? I4A I3A I2A 171.84(14) . . ? I1B I2B I3B 171.18(15) . . ? Cu3B I3B I2B 92.2(7) 2_655 . ? N1 C1 C2 122.4(7) . . ? N1 C1 C6 114.8(6) . . ? C2 C1 C6 122.8(6) . . ? C1 C2 C3 118.6(8) . . ? C1 C2 H2A 120.7 . . ? C3 C2 H2A 120.7 . . ? C4 C3 C2 120.1(8) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C3 C4 C5 118.5(6) . . ? C3 C4 C7 118.8(6) . . ? C5 C4 C7 122.6(6) . . ? N1 C5 C4 121.6(6) . . ? N1 C5 H5A 119.2 . . ? C4 C5 H5A 119.2 . . ? O2 C6 O1 124.7(6) . . ? O2 C6 C1 118.9(6) . . ? O1 C6 C1 116.3(6) . . ? O4 C7 O3 121.8(6) . . ? O4 C7 C4 118.9(5) . . ? O3 C7 C4 119.3(5) . . ? O4 C7 Tb1 61.5(3) . . ? O3 C7 Tb1 60.3(3) . . ? C4 C7 Tb1 177.7(5) . . ? N2 C8 C9 123.0(6) . . ? N2 C8 C13 112.6(6) . . ? C9 C8 C13 124.4(6) . . ? C8 C9 C10 118.6(7) . . ? C8 C9 H9A 120.7 . . ? C10 C9 H9A 120.7 . . ? C11 C10 C9 119.0(7) . . ? C11 C10 H10A 120.5 . . ? C9 C10 H10A 120.5 . . ? C10 C11 C12 118.6(6) . . ? C10 C11 C14 122.4(6) . . ? C12 C11 C14 119.0(5) . . ? N2 C12 C11 122.0(6) . . ? N2 C12 H12A 119.0 . . ? C11 C12 H12A 119.0 . . ? O5 C13 O6 123.2(7) . . ? O5 C13 C8 119.1(7) . . ? O6 C13 C8 117.7(6) . . ? O7 C14 O8 127.1(6) . . ? O7 C14 C11 115.9(5) . . ? O8 C14 C11 117.1(5) . . ? N3 C15 C16 121.7(6) . . ? N3 C15 C21 113.2(6) . . ? C16 C15 C21 125.1(6) . . ? C15 C16 C17 119.0(6) . . ? C15 C16 H16A 120.5 . . ? C17 C16 H16A 120.5 . . ? C18 C17 C16 119.5(6) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C17 C18 C19 119.1(6) . . ? C17 C18 C20 123.0(6) . . ? C19 C18 C20 117.9(5) . . ? N3 C19 C18 120.8(6) . . ? N3 C19 H19A 119.6 . . ? C18 C19 H19A 119.6 . . ? O12 C20 O11 127.1(5) . . ? O12 C20 C18 116.6(5) . . ? O11 C20 C18 116.3(5) . . ? O9 C21 O10 123.3(6) . . ? O9 C21 C15 120.0(6) . . ? O10 C21 C15 116.7(6) . . ? C1 N1 C5 118.7(6) . . ? C1 N1 Cu2A 109.3(5) . . ? C5 N1 Cu2A 131.5(5) . . ? C1 N1 Cu2B 110.7(5) . . ? C5 N1 Cu2B 130.0(5) . . ? Cu2A N1 Cu2B 14.16(17) . . ? C12 N2 C8 118.7(6) . . ? C12 N2 Cu2B 128.5(5) . 2_655 ? C8 N2 Cu2B 112.3(5) . 2_655 ? C12 N2 Cu2A 128.3(5) . 2_655 ? C8 N2 Cu2A 112.4(4) . 2_655 ? Cu2B N2 Cu2A 14.26(17) 2_655 2_655 ? C19 N3 C15 119.9(6) . . ? C19 N3 Cu3A 127.1(6) . . ? C15 N3 Cu3A 112.4(5) . . ? C19 N3 Cu3A 127.9(6) . 3_656 ? C15 N3 Cu3A 111.5(5) . 3_656 ? Cu3A N3 Cu3A 16.1(3) . 3_656 ? C19 N3 Cu3B 125.6(11) . . ? C15 N3 Cu3B 109.2(11) . . ? Cu3A N3 Cu3B 30.8(7) . . ? Cu3A N3 Cu3B 14.6(5) 3_656 . ? C19 N3 Cu3B 123.7(11) . 3_656 ? C15 N3 Cu3B 111.6(11) . 3_656 ? Cu3A N3 Cu3B 14.3(5) . 3_656 ? Cu3A N3 Cu3B 30.5(7) 3_656 3_656 ? Cu3B N3 Cu3B 45.1(11) . 3_656 ? C6 O1 Cu2A 113.8(5) . . ? C6 O1 Cu2B 114.5(5) . . ? Cu2A O1 Cu2B 14.53(17) . . ? C7 O3 Tb1 93.3(4) . . ? C7 O4 Tb1 92.7(4) . . ? C13 O6 Cu2B 113.7(4) . 2_655 ? C13 O6 Cu2A 113.2(4) . 2_655 ? Cu2B O6 Cu2A 14.41(17) 2_655 2_655 ? C14 O7 Tb1 143.0(4) . . ? C14 O8 Cu1 124.2(4) . 3_566 ? C21 O10 Cu3A 113.7(5) . 3_656 ? C21 O10 Cu3A 113.4(5) . . ? Cu3A O10 Cu3A 16.1(3) 3_656 . ? C21 O10 Cu3B 111.7(10) . . ? Cu3A O10 Cu3B 15.0(5) 3_656 . ? Cu3A O10 Cu3B 31.1(7) . . ? C21 O10 Cu3B 112.0(10) . 3_656 ? Cu3A O10 Cu3B 30.1(7) 3_656 3_656 ? Cu3A O10 Cu3B 14.0(5) . 3_656 ? Cu3B O10 Cu3B 45.1(11) . 3_656 ? C20 O11 Cu1 124.1(4) . . ? C20 O12 Tb1 143.4(4) . . ? Cu1 O13 Cu1 99.19(16) 3_566 . ? Cu1 O13 Tb1 110.44(16) 3_566 . ? Cu1 O13 Tb1 110.35(16) . . ? Cu1 O13 H9 115.4 3_566 . ? Cu1 O13 H9 115.0 . . ? Tb1 O13 H9 106.4 . . ? Tb1 O1W H1 110.0 . . ? Tb1 O1W H2 108.7 . . ? H1 O1W H2 109.5 . . ? Tb1 O2W H3 109.4 . . ? Tb1 O2W H4 109.6 . . ? H3 O2W H4 109.7 . . ? Tb1 O3W H5 113.7 . . ? Tb1 O3W H6 113.4 . . ? H5 O3W H6 109.7 . . ? Tb1 O4W H7 114.3 . . ? Tb1 O4W H8 113.7 . . ? H7 O4W H8 109.6 . . ? 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 C12 H12A O1 0.93 2.54 3.020(8) 112.6 2_655 C19 H19A O10 0.93 2.60 3.084(8) 112.7 3_656 O13 H9 O5 0.99 2.04 2.851(7) 137.5 2_545 O1W H2 O9 0.99 2.19 2.724(6) 112.2 1_565 O2W H3 O3 0.99 1.84 2.810(6) 163.9 3_666 O2W H4 O2 0.99 2.10 2.677(7) 115.3 4_566 O3W H5 O5 0.99 1.85 2.694(7) 141.8 4_576 O3W H5 O6 0.99 2.34 3.278(7) 156.8 4_576 O3W H6 O2 0.99 1.79 2.739(7) 160.6 4_566 O4W H7 O9 0.99 1.75 2.705(7) 161.6 1_565 O4W H8 O5 0.99 2.05 2.907(8) 144.1 4_576 O4W H8 O6 0.99 2.26 3.183(7) 155.0 4_576 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.776 _refine_diff_density_min -1.019 _refine_diff_density_rms 0.147