# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_a1 _database_code_depnum_ccdc_archive 'CCDC 882312' #TrackingRef '1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H50 Cl2 Cu4 Gd N7 O43' _chemical_formula_weight 1534.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.565(5) _cell_length_b 20.273(7) _cell_length_c 16.053(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4740(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4585 _cell_measurement_theta_min 2.0090 _cell_measurement_theta_max 27.4719 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.2300 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3060 _exptl_absorpt_coefficient_mu 3.388 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6330 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35828 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.45 _reflns_number_total 5556 _reflns_number_gt 4976 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+0.7238P] 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 5556 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1232 _refine_ls_wR_factor_gt 0.1126 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_restrained_S_all 1.180 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.12858(2) 0.7500 0.103427(19) 0.02699(11) Uani 1 2 d S . . Cu1 Cu 0.02315(5) 0.7500 -0.09224(5) 0.02712(18) Uani 1 2 d S . . Cu2 Cu -0.04603(3) 0.64255(3) 0.03032(3) 0.02638(14) Uani 1 1 d . . . Cu3 Cu -0.10818(5) 0.7500 0.15097(5) 0.02733(17) Uani 1 2 d S . . Cl1 Cl 0.42252(9) 0.55125(8) 0.20305(11) 0.0600(4) Uani 1 1 d . . . C1 C -0.2674(3) 0.5454(2) -0.0651(3) 0.0318(10) Uani 1 1 d . . . C2 C -0.3203(3) 0.6176(2) -0.1763(3) 0.0384(11) Uani 1 1 d . . . C3 C -0.3949(4) 0.6208(3) -0.0400(4) 0.0420(12) Uani 1 1 d . . . C4 C -0.1880(3) 0.5475(2) -0.2017(3) 0.0375(11) Uani 1 1 d . . . H4A H -0.2168 0.5319 -0.2524 0.045 Uiso 1 1 calc R . . H4B H -0.1576 0.5102 -0.1757 0.045 Uiso 1 1 calc R . . C5 C -0.1159(3) 0.5993(3) -0.2242(3) 0.0375(11) Uani 1 1 d . . . H5A H -0.0690 0.5785 -0.2580 0.045 Uiso 1 1 calc R . . H5B H -0.1450 0.6330 -0.2581 0.045 Uiso 1 1 calc R . . C6 C -0.0699(3) 0.6326(2) -0.1510(3) 0.0281(9) Uani 1 1 d . . . C7 C -0.3380(4) 0.5513(3) 0.0744(3) 0.0397(11) Uani 1 1 d . . . H7A H -0.2984 0.5134 0.0821 0.048 Uiso 1 1 calc R . . H7B H -0.4006 0.5375 0.0857 0.048 Uiso 1 1 calc R . . C8 C -0.3110(3) 0.6047(2) 0.1365(3) 0.0353(10) Uani 1 1 d . . . H8A H -0.3564 0.6396 0.1337 0.042 Uiso 1 1 calc R . . H8B H -0.3139 0.5860 0.1920 0.042 Uiso 1 1 calc R . . C9 C -0.2186(3) 0.6349(2) 0.1253(3) 0.0284(9) Uani 1 1 d . . . N1 N -0.3850(3) 0.6403(2) -0.1216(3) 0.0428(10) Uani 1 1 d . . . H1A H -0.4230 0.6695 -0.1398 0.051 Uiso 1 1 calc R . . N2 N -0.2596(3) 0.57227(18) -0.1450(2) 0.0330(8) Uani 1 1 d . . . N3 N -0.3314(3) 0.57397(19) -0.0130(3) 0.0336(8) Uani 1 1 d . . . N4 N -0.2060(4) 0.7500 -0.0375(3) 0.0297(11) Uani 1 2 d S . . O1 O -0.2201(2) 0.49849(16) -0.0436(2) 0.0395(8) Uani 1 1 d . . . O1W O -0.5045(4) 0.7500 -0.1667(3) 0.0520(14) Uani 1 2 d S . . O2 O -0.3166(3) 0.63656(19) -0.2481(2) 0.0507(9) Uani 1 1 d . . . O2W O -0.0176(5) 0.7500 0.3791(5) 0.080(2) Uani 1 2 d S . . O3 O -0.4550(2) 0.6412(2) 0.0052(3) 0.0555(11) Uani 1 1 d . . . O3WA O 0.1417(9) 0.5770(8) -0.0860(10) 0.064(4) Uani 0.50 1 d P A 1 O3WB O 0.1832(9) 0.5944(8) -0.0865(10) 0.057(3) Uani 0.50 1 d P B 2 O4 O -0.0797(2) 0.60720(16) -0.0789(2) 0.0344(7) Uani 1 1 d . . . O4WA O 0.3726(8) 0.6643(8) -0.0691(10) 0.101(4) Uani 0.50 1 d P . . O4WB O 0.3530(10) 0.6277(9) -0.0145(17) 0.158(8) Uani 0.50 1 d P . . O5 O -0.0242(2) 0.68366(16) -0.1684(2) 0.0347(7) Uani 1 1 d . . . O6 O -0.1648(2) 0.61112(16) 0.0724(2) 0.0332(7) Uani 1 1 d . . . O7 O -0.2015(2) 0.68423(16) 0.1722(2) 0.0369(8) Uani 1 1 d . . . O8 O 0.0657(2) 0.68456(15) -0.01057(18) 0.0275(6) Uani 1 1 d . . . H8C H 0.1100 0.6531 -0.0338 0.033 Uiso 1 1 calc R . . O9 O -0.01090(19) 0.68518(14) 0.13690(18) 0.0259(6) Uani 1 1 d . . . H9A H -0.0038 0.6546 0.1838 0.031 Uiso 1 1 calc R . . O10 O 0.0227(3) 0.5417(2) 0.0791(3) 0.0581(11) Uani 1 1 d . . . H10A H 0.0741 0.5240 0.0678 0.070 Uiso 1 1 d R . . H10B H -0.0203 0.5295 0.1115 0.070 Uiso 1 1 d R . . O11 O 0.1670(3) 0.7500 -0.1615(3) 0.0418(12) Uani 1 2 d S . . H11 H 0.1782 0.7152 -0.1892 0.050 Uiso 1 1 d R . . O12 O 0.2855(4) 0.7500 0.1623(4) 0.077(2) Uani 1 2 d S . . H12 H 0.2984 0.7835 0.1918 0.092 Uiso 1 1 d R . . O13 O 0.2437(3) 0.7500 -0.0056(3) 0.0577(16) Uani 1 2 d S . . H13A H 0.2316 0.7500 -0.0575 0.069 Uiso 1 2 d SR . . H13B H 0.2958 0.7500 -0.0005 0.069 Uiso 1 2 d SR . . O14 O 0.1251(3) 0.7500 0.2544(3) 0.0418(12) Uani 1 2 d S . . H14A H 0.0785 0.7500 0.2863 0.050 Uiso 1 2 d SR . . H14B H 0.1769 0.7500 0.2802 0.050 Uiso 1 2 d SR . . O15 O 0.1770(3) 0.6360(2) 0.1268(3) 0.0578(11) Uani 1 1 d . . . H15A H 0.2347 0.6309 0.1224 0.069 Uiso 1 1 d R . . H15B H 0.1393 0.6079 0.1078 0.069 Uiso 1 1 d R . . O16 O -0.2083(4) 0.7500 -0.1111(4) 0.081(2) Uani 1 2 d S . . O17 O -0.1231(3) 0.7500 -0.0007(3) 0.0318(10) Uani 1 2 d S . . O18 O -0.2719(4) 0.7500 0.0089(4) 0.072(2) Uani 1 2 d S . . O19 O 0.4515(3) 0.5058(3) 0.1424(4) 0.093(2) Uani 1 1 d . . . O20 O 0.4929(3) 0.5938(3) 0.2274(3) 0.0794(16) Uani 1 1 d . . . O21 O 0.3473(6) 0.5827(5) 0.1784(9) 0.224(7) Uani 1 1 d . . . O22 O 0.3942(7) 0.5153(5) 0.2760(5) 0.176(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.02625(18) 0.03005(18) 0.02468(18) 0.000 -0.00277(10) 0.000 Cu1 0.0313(4) 0.0260(4) 0.0241(4) 0.000 -0.0014(3) 0.000 Cu2 0.0284(3) 0.0269(3) 0.0238(3) -0.0023(2) 0.00007(19) -0.0020(2) Cu3 0.0298(4) 0.0247(4) 0.0274(4) 0.000 0.0048(3) 0.000 Cl1 0.0384(7) 0.0700(10) 0.0716(11) -0.0341(8) 0.0058(6) -0.0085(7) C1 0.033(2) 0.028(2) 0.034(3) -0.0003(18) -0.0054(18) -0.0078(18) C2 0.043(3) 0.035(2) 0.037(3) 0.002(2) -0.011(2) -0.004(2) C3 0.037(3) 0.041(3) 0.048(3) 0.000(2) -0.011(2) -0.003(2) C4 0.051(3) 0.033(2) 0.029(3) -0.0016(19) -0.007(2) -0.006(2) C5 0.043(3) 0.043(3) 0.026(3) -0.004(2) -0.0024(18) -0.007(2) C6 0.029(2) 0.029(2) 0.026(2) -0.0025(17) 0.0009(16) 0.0002(17) C7 0.039(3) 0.040(3) 0.041(3) 0.004(2) 0.004(2) -0.009(2) C8 0.033(2) 0.041(3) 0.032(3) 0.000(2) 0.0075(18) -0.003(2) C9 0.029(2) 0.028(2) 0.029(2) 0.0054(17) 0.0015(17) -0.0025(17) N1 0.038(2) 0.043(2) 0.047(3) 0.002(2) -0.0090(19) 0.0084(19) N2 0.037(2) 0.033(2) 0.028(2) 0.0028(16) -0.0052(15) -0.0054(16) N3 0.035(2) 0.031(2) 0.035(2) -0.0001(16) -0.0030(16) -0.0004(16) N4 0.031(3) 0.028(3) 0.030(3) 0.000 0.003(2) 0.000 O1 0.049(2) 0.0336(17) 0.0361(19) 0.0046(14) -0.0028(15) 0.0047(15) O1W 0.055(3) 0.063(4) 0.038(3) 0.000 -0.006(2) 0.000 O2 0.069(3) 0.047(2) 0.035(2) 0.0100(17) -0.0110(17) 0.0060(19) O2W 0.071(5) 0.076(5) 0.091(6) 0.000 0.001(4) 0.000 O3 0.035(2) 0.069(3) 0.062(3) 0.003(2) 0.0032(17) 0.0082(19) O3WA 0.077(10) 0.068(10) 0.047(6) 0.006(6) 0.011(7) 0.030(7) O3WB 0.066(9) 0.058(8) 0.049(6) 0.005(5) 0.022(7) 0.020(6) O4 0.0413(18) 0.0374(17) 0.0244(17) 0.0002(14) -0.0034(13) -0.0089(14) O4WA 0.077(8) 0.114(12) 0.112(12) 0.014(9) -0.004(7) 0.027(8) O4WB 0.089(11) 0.118(14) 0.27(3) 0.015(15) -0.046(14) 0.016(10) O5 0.0410(18) 0.0361(17) 0.0269(17) 0.0008(13) -0.0006(13) -0.0086(14) O6 0.0295(16) 0.0372(17) 0.0330(18) -0.0045(14) 0.0026(13) -0.0035(13) O7 0.0417(18) 0.0322(16) 0.0369(19) -0.0032(14) 0.0133(14) -0.0072(14) O8 0.0277(14) 0.0282(15) 0.0265(16) 0.0005(12) 0.0010(12) 0.0026(12) O9 0.0297(15) 0.0226(14) 0.0253(16) 0.0001(12) -0.0015(11) 0.0020(12) O10 0.060(3) 0.045(2) 0.070(3) 0.007(2) 0.012(2) 0.0210(19) O11 0.056(3) 0.038(3) 0.031(3) 0.000 0.011(2) 0.000 O12 0.040(3) 0.160(7) 0.032(3) 0.000 -0.008(2) 0.000 O13 0.031(3) 0.102(5) 0.040(3) 0.000 -0.001(2) 0.000 O14 0.036(3) 0.061(3) 0.028(3) 0.000 -0.0075(19) 0.000 O15 0.067(3) 0.046(2) 0.061(3) -0.004(2) -0.018(2) 0.020(2) O16 0.046(4) 0.161(8) 0.036(4) 0.000 -0.005(2) 0.000 O17 0.029(2) 0.031(2) 0.035(3) 0.000 -0.0035(17) 0.000 O18 0.039(3) 0.125(6) 0.053(4) 0.000 0.006(3) 0.000 O19 0.078(3) 0.096(4) 0.105(4) -0.061(4) 0.039(3) -0.037(3) O20 0.062(3) 0.098(4) 0.079(3) -0.051(3) 0.020(2) -0.036(3) O21 0.119(6) 0.204(10) 0.348(16) -0.150(10) -0.126(8) 0.108(7) O22 0.233(9) 0.189(9) 0.105(6) -0.045(6) 0.067(6) -0.155(8) _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 O14 2.425(5) . ? Gd1 O13 2.423(5) . ? Gd1 O8 2.438(3) . ? Gd1 O8 2.438(3) 7_575 ? Gd1 O15 2.445(4) . ? Gd1 O15 2.445(4) 7_575 ? Gd1 O12 2.473(5) . ? Gd1 O9 2.478(3) . ? Gd1 O9 2.478(3) 7_575 ? Gd1 Cu1 3.4963(13) . ? Gd1 Cu3 3.5318(13) . ? Gd1 Cu2 3.5483(9) . ? Cu1 O5 1.944(3) . ? Cu1 O5 1.944(3) 7_575 ? Cu1 O8 1.966(3) 7_575 ? Cu1 O8 1.966(3) . ? Cu1 O11 2.372(5) . ? Cu2 O8 1.951(3) . ? Cu2 O4 1.957(3) . ? Cu2 O6 1.963(3) . ? Cu2 O9 1.984(3) . ? Cu2 O10 2.407(4) . ? Cu2 Cu3 3.0523(10) . ? Cu3 O7 1.934(3) . ? Cu3 O7 1.934(3) 7_575 ? Cu3 O9 1.946(3) . ? Cu3 O9 1.946(3) 7_575 ? Cu3 Cu2 3.0523(10) 7_575 ? Cl1 O21 1.328(7) . ? Cl1 O20 1.395(4) . ? Cl1 O19 1.406(5) . ? Cl1 O22 1.440(8) . ? C1 O1 1.223(5) . ? C1 N3 1.381(6) . ? C1 N2 1.399(6) . ? C2 O2 1.216(6) . ? C2 N1 1.368(7) . ? C2 N2 1.372(6) . ? C3 O3 1.211(7) . ? C3 N1 1.376(7) . ? C3 N3 1.393(6) . ? C4 N2 1.472(6) . ? C4 C5 1.529(7) . ? C5 C6 1.512(6) . ? C6 O5 1.261(5) . ? C6 O4 1.274(5) . ? C7 N3 1.480(6) . ? C7 C8 1.523(7) . ? C8 C9 1.488(6) . ? C9 O6 1.252(5) . ? C9 O7 1.276(6) . ? N4 O16 1.183(8) . ? N4 O18 1.215(8) . ? N4 O17 1.345(7) . ? O4WA O4WB 1.18(2) . ? 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 O14 Gd1 O13 137.42(17) . . ? O14 Gd1 O8 137.94(9) . . ? O13 Gd1 O8 73.61(13) . . ? O14 Gd1 O8 137.94(9) . 7_575 ? O13 Gd1 O8 73.61(13) . 7_575 ? O8 Gd1 O8 65.92(14) . 7_575 ? O14 Gd1 O15 81.50(11) . . ? O13 Gd1 O15 84.91(12) . . ? O8 Gd1 O15 73.12(12) . . ? O8 Gd1 O15 137.55(12) 7_575 . ? O14 Gd1 O15 81.50(11) . 7_575 ? O13 Gd1 O15 84.91(12) . 7_575 ? O8 Gd1 O15 137.55(12) . 7_575 ? O8 Gd1 O15 73.12(12) 7_575 7_575 ? O15 Gd1 O15 141.8(2) . 7_575 ? O14 Gd1 O12 68.72(18) . . ? O13 Gd1 O12 68.70(19) . . ? O8 Gd1 O12 129.32(12) . . ? O8 Gd1 O12 129.32(12) 7_575 . ? O15 Gd1 O12 71.00(10) . . ? O15 Gd1 O12 71.00(10) 7_575 . ? O14 Gd1 O9 76.48(11) . . ? O13 Gd1 O9 136.35(10) . . ? O8 Gd1 O9 64.32(10) . . ? O8 Gd1 O9 98.25(10) 7_575 . ? O15 Gd1 O9 72.68(13) . . ? O15 Gd1 O9 134.77(13) 7_575 . ? O12 Gd1 O9 132.42(12) . . ? O14 Gd1 O9 76.48(11) . 7_575 ? O13 Gd1 O9 136.35(10) . 7_575 ? O8 Gd1 O9 98.25(10) . 7_575 ? O8 Gd1 O9 64.32(10) 7_575 7_575 ? O15 Gd1 O9 134.77(13) . 7_575 ? O15 Gd1 O9 72.68(13) 7_575 7_575 ? O12 Gd1 O9 132.42(12) . 7_575 ? O9 Gd1 O9 64.04(13) . 7_575 ? O14 Gd1 Cu1 152.75(11) . . ? O13 Gd1 Cu1 69.83(13) . . ? O8 Gd1 Cu1 32.96(7) . . ? O8 Gd1 Cu1 32.96(7) 7_575 . ? O15 Gd1 Cu1 105.37(10) . . ? O15 Gd1 Cu1 105.37(10) 7_575 . ? O12 Gd1 Cu1 138.53(14) . . ? O9 Gd1 Cu1 80.49(7) . . ? O9 Gd1 Cu1 80.49(7) 7_575 . ? O14 Gd1 Cu3 76.32(10) . . ? O13 Gd1 Cu3 146.26(13) . . ? O8 Gd1 Cu3 78.22(7) . . ? O8 Gd1 Cu3 78.22(7) 7_575 . ? O15 Gd1 Cu3 104.40(11) . . ? O15 Gd1 Cu3 104.40(11) 7_575 . ? O12 Gd1 Cu3 145.04(14) . . ? O9 Gd1 Cu3 32.10(7) . . ? O9 Gd1 Cu3 32.10(7) 7_575 . ? Cu1 Gd1 Cu3 76.43(2) . . ? O14 Gd1 Cu2 108.41(8) . . ? O13 Gd1 Cu2 104.89(10) . . ? O8 Gd1 Cu2 31.66(7) . . ? O8 Gd1 Cu2 79.44(7) 7_575 . ? O15 Gd1 Cu2 71.19(11) . . ? O15 Gd1 Cu2 146.92(10) 7_575 . ? O12 Gd1 Cu2 142.067(16) . . ? O9 Gd1 Cu2 32.73(7) . . ? O9 Gd1 Cu2 79.03(7) 7_575 . ? Cu1 Gd1 Cu2 52.271(14) . . ? Cu3 Gd1 Cu2 51.075(18) . . ? O5 Cu1 O5 87.6(2) . 7_575 ? O5 Cu1 O8 176.70(13) . 7_575 ? O5 Cu1 O8 93.69(13) 7_575 7_575 ? O5 Cu1 O8 93.69(13) . . ? O5 Cu1 O8 176.70(13) 7_575 . ? O8 Cu1 O8 84.89(18) 7_575 . ? O5 Cu1 O11 91.11(13) . . ? O5 Cu1 O11 91.11(13) 7_575 . ? O8 Cu1 O11 91.92(13) 7_575 . ? O8 Cu1 O11 91.92(13) . . ? O5 Cu1 Gd1 136.11(10) . . ? O5 Cu1 Gd1 136.11(10) 7_575 . ? O8 Cu1 Gd1 42.45(9) 7_575 . ? O8 Cu1 Gd1 42.45(9) . . ? O11 Cu1 Gd1 91.88(13) . . ? O8 Cu2 O4 93.87(13) . . ? O8 Cu2 O6 173.03(13) . . ? O4 Cu2 O6 88.22(14) . . ? O8 Cu2 O9 83.38(12) . . ? O4 Cu2 O9 175.55(13) . . ? O6 Cu2 O9 94.11(13) . . ? O8 Cu2 O10 97.65(14) . . ? O4 Cu2 O10 94.88(15) . . ? O6 Cu2 O10 88.79(14) . . ? O9 Cu2 O10 88.97(14) . . ? O8 Cu2 Cu3 98.59(9) . . ? O4 Cu2 Cu3 139.09(10) . . ? O6 Cu2 Cu3 75.63(9) . . ? O9 Cu2 Cu3 38.59(8) . . ? O10 Cu2 Cu3 121.53(11) . . ? O8 Cu2 Gd1 40.99(9) . . ? O4 Cu2 Gd1 134.49(10) . . ? O6 Cu2 Gd1 135.79(10) . . ? O9 Cu2 Gd1 42.48(8) . . ? O10 Cu2 Gd1 96.63(11) . . ? Cu3 Cu2 Gd1 64.18(2) . . ? O7 Cu3 O7 87.1(2) . 7_575 ? O7 Cu3 O9 93.82(13) . . ? O7 Cu3 O9 176.18(14) 7_575 . ? O7 Cu3 O9 176.18(14) . 7_575 ? O7 Cu3 O9 93.82(13) 7_575 7_575 ? O9 Cu3 O9 84.97(17) . 7_575 ? O7 Cu3 Cu2 80.11(10) . . ? O7 Cu3 Cu2 144.30(11) 7_575 . ? O9 Cu3 Cu2 39.49(8) . . ? O9 Cu3 Cu2 101.09(9) 7_575 . ? O7 Cu3 Cu2 144.30(11) . 7_575 ? O7 Cu3 Cu2 80.11(10) 7_575 7_575 ? O9 Cu3 Cu2 101.09(9) . 7_575 ? O9 Cu3 Cu2 39.49(8) 7_575 7_575 ? Cu2 Cu3 Cu2 91.07(4) . 7_575 ? O7 Cu3 Gd1 136.40(10) . . ? O7 Cu3 Gd1 136.40(10) 7_575 . ? O9 Cu3 Gd1 42.60(9) . . ? O9 Cu3 Gd1 42.60(9) 7_575 . ? Cu2 Cu3 Gd1 64.743(17) . . ? Cu2 Cu3 Gd1 64.743(17) 7_575 . ? O21 Cl1 O20 113.1(5) . . ? O21 Cl1 O19 110.8(5) . . ? O20 Cl1 O19 112.3(3) . . ? O21 Cl1 O22 104.4(8) . . ? O20 Cl1 O22 107.2(4) . . ? O19 Cl1 O22 108.5(5) . . ? O1 C1 N3 122.4(4) . . ? O1 C1 N2 121.1(4) . . ? N3 C1 N2 116.5(4) . . ? O2 C2 N1 122.3(5) . . ? O2 C2 N2 122.0(5) . . ? N1 C2 N2 115.7(5) . . ? O3 C3 N1 123.2(5) . . ? O3 C3 N3 121.8(5) . . ? N1 C3 N3 115.0(5) . . ? N2 C4 C5 113.5(4) . . ? C6 C5 C4 115.3(4) . . ? O5 C6 O4 126.3(4) . . ? O5 C6 C5 115.4(4) . . ? O4 C6 C5 118.4(4) . . ? N3 C7 C8 112.5(4) . . ? C9 C8 C7 116.6(4) . . ? O6 C9 O7 125.4(4) . . ? O6 C9 C8 119.3(4) . . ? O7 C9 C8 115.3(4) . . ? C2 N1 C3 125.9(4) . . ? C2 N2 C1 123.1(4) . . ? C2 N2 C4 117.4(4) . . ? C1 N2 C4 119.4(4) . . ? C1 N3 C3 123.1(4) . . ? C1 N3 C7 119.2(4) . . ? C3 N3 C7 117.6(4) . . ? O16 N4 O18 126.2(6) . . ? O16 N4 O17 117.7(5) . . ? O18 N4 O17 116.1(6) . . ? C6 O4 Cu2 129.6(3) . . ? C6 O5 Cu1 128.0(3) . . ? C9 O6 Cu2 131.3(3) . . ? C9 O7 Cu3 125.0(3) . . ? Cu2 O8 Cu1 104.81(14) . . ? Cu2 O8 Gd1 107.35(13) . . ? Cu1 O8 Gd1 104.59(13) . . ? Cu3 O9 Cu2 101.92(13) . . ? Cu3 O9 Gd1 105.30(12) . . ? Cu2 O9 Gd1 104.80(12) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.145 _refine_diff_density_min -0.952 _refine_diff_density_rms 0.167 data_a2 _database_code_depnum_ccdc_archive 'CCDC 882313' #TrackingRef '2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H50 Cl2 Cu4 N7 O43 Tb' _chemical_formula_weight 1536.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.564(5) _cell_length_b 20.278(6) _cell_length_c 16.024(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4732(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4663 _cell_measurement_theta_min 2.0085 _cell_measurement_theta_max 27.4526 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.2400 _exptl_crystal_size_mid 0.1900 _exptl_crystal_size_min 0.1800 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3064 _exptl_absorpt_coefficient_mu 3.487 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7267 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35602 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.45 _reflns_number_total 5548 _reflns_number_gt 5030 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+0.2785P] 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 5548 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.172 _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 0.127922(18) 0.7500 0.103246(15) 0.02720(10) Uani 1 2 d S . . Cu1 Cu 0.02343(5) 0.7500 -0.09214(4) 0.02676(16) Uani 1 2 d S . . Cu2 Cu -0.04586(3) 0.64262(2) 0.03041(3) 0.02589(13) Uani 1 1 d . . . Cu3 Cu -0.10816(5) 0.7500 0.15138(4) 0.02700(15) Uani 1 2 d S . . Cl1 Cl 0.42222(9) 0.55128(7) 0.20330(9) 0.0593(4) Uani 1 1 d . . . C1 C -0.2669(3) 0.54510(19) -0.0653(2) 0.0323(8) Uani 1 1 d . . . C2 C -0.3208(3) 0.6177(2) -0.1762(3) 0.0378(9) Uani 1 1 d . . . C3 C -0.3950(3) 0.6204(2) -0.0399(3) 0.0413(10) Uani 1 1 d . . . C4 C -0.1873(3) 0.5474(2) -0.2018(2) 0.0358(9) Uani 1 1 d . . . H4A H -0.2158 0.5316 -0.2527 0.043 Uiso 1 1 calc R . . H4B H -0.1569 0.5103 -0.1754 0.043 Uiso 1 1 calc R . . C5 C -0.1158(3) 0.5990(2) -0.2241(3) 0.0386(10) Uani 1 1 d . . . H5A H -0.0690 0.5783 -0.2582 0.046 Uiso 1 1 calc R . . H5B H -0.1451 0.6327 -0.2579 0.046 Uiso 1 1 calc R . . C6 C -0.0691(3) 0.63246(18) -0.1510(2) 0.0293(8) Uani 1 1 d . . . C7 C -0.3380(3) 0.5518(2) 0.0741(3) 0.0368(9) Uani 1 1 d . . . H7A H -0.2981 0.5140 0.0818 0.044 Uiso 1 1 calc R . . H7B H -0.4004 0.5377 0.0852 0.044 Uiso 1 1 calc R . . C8 C -0.3116(3) 0.6048(2) 0.1365(3) 0.0365(9) Uani 1 1 d . . . H8A H -0.3571 0.6397 0.1338 0.044 Uiso 1 1 calc R . . H8B H -0.3146 0.5859 0.1921 0.044 Uiso 1 1 calc R . . C9 C -0.2186(3) 0.63508(19) 0.1251(2) 0.0294(8) Uani 1 1 d . . . N1 N -0.3851(3) 0.6403(2) -0.1218(3) 0.0432(9) Uani 1 1 d . . . H1A H -0.4229 0.6695 -0.1400 0.052 Uiso 1 1 calc R . . N2 N -0.2596(2) 0.57237(16) -0.1452(2) 0.0325(7) Uani 1 1 d . . . N3 N -0.3315(2) 0.57405(17) -0.0135(2) 0.0350(7) Uani 1 1 d . . . N4 N -0.2062(3) 0.7500 -0.0375(3) 0.0299(10) Uani 1 2 d S . . O1 O -0.2199(2) 0.49850(14) -0.04389(18) 0.0390(7) Uani 1 1 d . . . O1W O -0.5036(4) 0.7500 -0.1666(3) 0.0508(12) Uani 1 2 d S . . O2 O -0.3167(3) 0.63630(16) -0.2484(2) 0.0504(8) Uani 1 1 d . . . O2W O -0.0172(5) 0.7500 0.3788(4) 0.0814(19) Uani 1 2 d S . . O3 O -0.4551(2) 0.64139(19) 0.0047(3) 0.0560(9) Uani 1 1 d . . . O3WA O 0.1422(9) 0.5769(7) -0.0881(8) 0.065(3) Uani 0.50 1 d P A 1 O3WB O 0.1840(8) 0.5959(6) -0.0836(8) 0.055(3) Uani 0.50 1 d P B 2 O4 O -0.0792(2) 0.60711(14) -0.07937(17) 0.0337(6) Uani 1 1 d . . . O4WA O 0.3729(8) 0.6658(7) -0.0686(9) 0.100(4) Uani 0.50 1 d P . . O4WB O 0.3515(9) 0.6282(8) -0.0172(15) 0.158(7) Uani 0.50 1 d P . . O5 O -0.0239(2) 0.68348(14) -0.16863(17) 0.0349(6) Uani 1 1 d . . . O6 O -0.16480(19) 0.61113(13) 0.07252(17) 0.0316(6) Uani 1 1 d . . . O7 O -0.2016(2) 0.68417(14) 0.17261(19) 0.0376(7) Uani 1 1 d . . . O8 O 0.06569(18) 0.68485(13) -0.01036(16) 0.0272(5) Uani 1 1 d . . . H8C H 0.1101 0.6535 -0.0335 0.033 Uiso 1 1 calc R . . O9 O -0.01030(17) 0.68550(12) 0.13702(15) 0.0261(5) Uani 1 1 d . . . H9A H -0.0029 0.6550 0.1840 0.031 Uiso 1 1 calc R . . O10 O 0.0232(3) 0.54199(17) 0.0798(2) 0.0555(9) Uani 1 1 d . . . H10A H 0.0325 0.5146 0.0405 0.067 Uiso 1 1 d R . . H10B H -0.0197 0.5298 0.1121 0.067 Uiso 1 1 d R . . O11 O 0.1675(3) 0.7500 -0.1610(3) 0.0401(10) Uani 1 2 d S . . H11 H 0.1787 0.7152 -0.1887 0.048 Uiso 1 1 d R . . O12 O 0.2842(4) 0.7500 0.1624(3) 0.0757(19) Uani 1 2 d S . . H12 H 0.2972 0.7835 0.1919 0.091 Uiso 1 1 d R . . O13 O 0.2431(3) 0.7500 -0.0048(3) 0.0579(14) Uani 1 2 d S . . H13A H 0.2310 0.7500 -0.0567 0.069 Uiso 1 2 d SR . . H13B H 0.2952 0.7500 0.0003 0.069 Uiso 1 2 d SR . . O14 O 0.1245(3) 0.7500 0.2535(3) 0.0432(11) Uani 1 2 d S . . H14A H 0.0778 0.7500 0.2854 0.052 Uiso 1 2 d SR . . H14B H 0.1763 0.7500 0.2792 0.052 Uiso 1 2 d SR . . O15 O 0.1769(3) 0.63658(17) 0.1269(2) 0.0569(10) Uani 1 1 d . . . H15A H 0.2346 0.6315 0.1225 0.068 Uiso 1 1 d R . . H15B H 0.1392 0.6084 0.1078 0.068 Uiso 1 1 d R . . O16 O -0.2088(4) 0.7500 -0.1111(3) 0.080(2) Uani 1 2 d S . . O17 O -0.1226(3) 0.7500 -0.0010(3) 0.0320(9) Uani 1 2 d S . . O18 O -0.2719(4) 0.7500 0.0083(3) 0.0697(17) Uani 1 2 d S . . O19 O 0.4513(3) 0.5061(2) 0.1424(3) 0.0905(17) Uani 1 1 d . . . O20 O 0.4930(3) 0.5938(2) 0.2274(3) 0.0798(14) Uani 1 1 d . . . O21 O 0.3476(5) 0.5835(5) 0.1776(7) 0.217(6) Uani 1 1 d . . . O22 O 0.3963(7) 0.5150(4) 0.2760(4) 0.176(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.02531(16) 0.03175(16) 0.02453(15) 0.000 -0.00296(9) 0.000 Cu1 0.0293(4) 0.0273(3) 0.0236(3) 0.000 -0.0012(2) 0.000 Cu2 0.0268(3) 0.0275(2) 0.0234(2) -0.00195(17) 0.00037(17) -0.00180(17) Cu3 0.0284(3) 0.0257(3) 0.0269(3) 0.000 0.0049(3) 0.000 Cl1 0.0366(6) 0.0712(8) 0.0700(8) -0.0342(7) 0.0042(6) -0.0087(6) C1 0.034(2) 0.0311(19) 0.032(2) -0.0028(16) -0.0028(16) -0.0066(16) C2 0.041(2) 0.035(2) 0.038(2) 0.0009(18) -0.0118(18) -0.0008(18) C3 0.033(2) 0.043(2) 0.047(3) 0.000(2) -0.0045(19) -0.0035(19) C4 0.043(2) 0.035(2) 0.0288(19) -0.0042(17) -0.0081(17) -0.0035(18) C5 0.045(3) 0.045(2) 0.026(2) -0.0042(18) -0.0032(17) -0.0051(19) C6 0.031(2) 0.0287(18) 0.0279(18) -0.0043(16) -0.0004(15) 0.0033(15) C7 0.036(2) 0.037(2) 0.037(2) 0.0016(19) 0.0051(18) -0.0087(18) C8 0.031(2) 0.043(2) 0.035(2) 0.0016(19) 0.0051(17) -0.0044(18) C9 0.034(2) 0.0276(18) 0.0269(18) 0.0044(15) 0.0012(16) -0.0003(16) N1 0.042(2) 0.042(2) 0.046(2) 0.0021(18) -0.0070(17) 0.0094(17) N2 0.0332(18) 0.0343(17) 0.0300(17) 0.0028(14) -0.0044(14) -0.0016(14) N3 0.0319(18) 0.0360(18) 0.0372(18) 0.0016(15) -0.0023(15) -0.0005(14) N4 0.035(3) 0.024(2) 0.031(2) 0.000 0.0081(19) 0.000 O1 0.0477(18) 0.0325(14) 0.0368(15) 0.0056(12) -0.0034(14) 0.0031(13) O1W 0.055(3) 0.063(3) 0.035(2) 0.000 -0.008(2) 0.000 O2 0.067(2) 0.0488(19) 0.0358(17) 0.0065(15) -0.0109(16) 0.0070(17) O2W 0.077(5) 0.075(4) 0.093(5) 0.000 0.003(4) 0.000 O3 0.0349(19) 0.073(3) 0.060(2) 0.0003(19) 0.0048(16) 0.0102(17) O3WA 0.080(9) 0.072(9) 0.042(5) 0.002(5) 0.001(6) 0.030(6) O3WB 0.064(8) 0.052(6) 0.048(5) -0.001(4) 0.008(6) 0.017(5) O4 0.0413(17) 0.0344(14) 0.0254(13) -0.0001(12) -0.0029(12) -0.0066(12) O4WA 0.073(8) 0.111(10) 0.118(10) 0.018(8) -0.001(6) 0.009(7) O4WB 0.070(9) 0.123(12) 0.28(2) 0.010(14) -0.031(12) 0.001(8) O5 0.0417(16) 0.0352(15) 0.0278(13) -0.0021(12) 0.0006(12) -0.0084(13) O6 0.0293(15) 0.0344(14) 0.0313(14) -0.0058(12) 0.0026(11) -0.0032(11) O7 0.0398(17) 0.0330(14) 0.0399(16) -0.0048(13) 0.0148(13) -0.0087(12) O8 0.0247(13) 0.0312(13) 0.0256(12) 0.0007(11) -0.0005(10) 0.0030(10) O9 0.0291(14) 0.0248(12) 0.0245(12) -0.0008(10) -0.0029(10) 0.0007(10) O10 0.064(2) 0.0405(18) 0.062(2) 0.0033(17) 0.0107(19) 0.0155(17) O11 0.050(3) 0.038(2) 0.033(2) 0.000 0.0081(19) 0.000 O12 0.039(3) 0.154(6) 0.034(2) 0.000 -0.011(2) 0.000 O13 0.029(2) 0.105(4) 0.040(3) 0.000 -0.0004(19) 0.000 O14 0.037(3) 0.059(3) 0.033(2) 0.000 -0.0085(18) 0.000 O15 0.061(2) 0.0464(19) 0.063(2) -0.0048(18) -0.0161(19) 0.0220(17) O16 0.038(3) 0.163(7) 0.038(3) 0.000 -0.005(2) 0.000 O17 0.029(2) 0.031(2) 0.036(2) 0.000 -0.0050(16) 0.000 O18 0.032(3) 0.128(5) 0.050(3) 0.000 0.004(2) 0.000 O19 0.074(3) 0.095(3) 0.103(4) -0.059(3) 0.034(3) -0.033(3) O20 0.063(3) 0.102(3) 0.074(3) -0.048(2) 0.019(2) -0.039(2) O21 0.123(6) 0.211(9) 0.318(12) -0.153(9) -0.131(7) 0.112(6) O22 0.242(9) 0.192(7) 0.092(4) -0.040(5) 0.056(5) -0.154(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O14 2.408(4) . ? Tb1 O13 2.410(5) . ? Tb1 O8 2.425(3) . ? Tb1 O8 2.425(3) 7_575 ? Tb1 O15 2.438(3) 7_575 ? Tb1 O15 2.438(3) . ? Tb1 O9 2.461(3) . ? Tb1 O9 2.461(3) 7_575 ? Tb1 O12 2.466(5) . ? Tb1 Cu1 3.4811(11) . ? Tb1 Cu3 3.5237(13) . ? Tb1 Cu2 3.5368(9) . ? Cu1 O5 1.948(3) 7_575 ? Cu1 O5 1.948(3) . ? Cu1 O8 1.960(3) 7_575 ? Cu1 O8 1.960(3) . ? Cu1 O11 2.371(4) . ? Cu2 O8 1.949(3) . ? Cu2 O4 1.962(3) . ? Cu2 O6 1.966(3) . ? Cu2 O9 1.986(2) . ? Cu2 O10 2.409(3) . ? Cu2 Cu3 3.0532(9) . ? Cu3 O7 1.936(3) . ? Cu3 O7 1.936(3) 7_575 ? Cu3 O9 1.948(3) 7_575 ? Cu3 O9 1.948(3) . ? Cu3 Cu2 3.0532(9) 7_575 ? Cl1 O21 1.333(6) . ? Cl1 O20 1.398(4) . ? Cl1 O19 1.403(4) . ? Cl1 O22 1.429(7) . ? C1 O1 1.216(5) . ? C1 N3 1.385(5) . ? C1 N2 1.400(5) . ? C2 O2 1.218(5) . ? C2 N1 1.358(6) . ? C2 N2 1.372(5) . ? C3 O3 1.207(6) . ? C3 N1 1.381(6) . ? C3 N3 1.384(6) . ? C4 N2 1.479(5) . ? C4 C5 1.519(6) . ? C5 C6 1.514(5) . ? C6 O5 1.258(5) . ? C6 O4 1.267(5) . ? C7 N3 1.477(6) . ? C7 C8 1.518(6) . ? C8 C9 1.498(6) . ? C9 O6 1.249(5) . ? C9 O7 1.277(5) . ? N4 O16 1.179(7) . ? N4 O18 1.206(7) . ? N4 O17 1.351(6) . ? O4WA O4WB 1.17(2) . ? 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 O14 Tb1 O13 137.11(15) . . ? O14 Tb1 O8 137.96(8) . . ? O13 Tb1 O8 73.79(11) . . ? O14 Tb1 O8 137.96(8) . 7_575 ? O13 Tb1 O8 73.79(11) . 7_575 ? O8 Tb1 O8 66.02(12) . 7_575 ? O14 Tb1 O15 81.41(10) . 7_575 ? O13 Tb1 O15 84.72(11) . 7_575 ? O8 Tb1 O15 137.75(11) . 7_575 ? O8 Tb1 O15 73.27(11) 7_575 7_575 ? O14 Tb1 O15 81.41(10) . . ? O13 Tb1 O15 84.72(11) . . ? O8 Tb1 O15 73.27(11) . . ? O8 Tb1 O15 137.75(11) 7_575 . ? O15 Tb1 O15 141.27(19) 7_575 . ? O14 Tb1 O9 76.30(10) . . ? O13 Tb1 O9 136.64(9) . . ? O8 Tb1 O9 64.52(8) . . ? O8 Tb1 O9 98.56(9) 7_575 . ? O15 Tb1 O9 134.97(12) 7_575 . ? O15 Tb1 O9 72.78(12) . . ? O14 Tb1 O9 76.30(10) . 7_575 ? O13 Tb1 O9 136.64(9) . 7_575 ? O8 Tb1 O9 98.56(9) . 7_575 ? O8 Tb1 O9 64.52(8) 7_575 7_575 ? O15 Tb1 O9 72.78(12) 7_575 7_575 ? O15 Tb1 O9 134.97(12) . 7_575 ? O9 Tb1 O9 64.21(12) . 7_575 ? O14 Tb1 O12 68.59(16) . . ? O13 Tb1 O12 68.51(16) . . ? O8 Tb1 O12 129.31(11) . . ? O8 Tb1 O12 129.31(11) 7_575 . ? O15 Tb1 O12 70.72(10) 7_575 . ? O15 Tb1 O12 70.72(10) . . ? O9 Tb1 O12 132.12(10) . . ? O9 Tb1 O12 132.12(10) 7_575 . ? O14 Tb1 Cu1 152.88(10) . . ? O13 Tb1 Cu1 70.01(12) . . ? O8 Tb1 Cu1 33.02(6) . . ? O8 Tb1 Cu1 33.02(6) 7_575 . ? O15 Tb1 Cu1 105.54(9) 7_575 . ? O15 Tb1 Cu1 105.54(9) . . ? O9 Tb1 Cu1 80.80(6) . . ? O9 Tb1 Cu1 80.80(6) 7_575 . ? O12 Tb1 Cu1 138.52(12) . . ? O14 Tb1 Cu3 76.16(10) . . ? O13 Tb1 Cu3 146.73(11) . . ? O8 Tb1 Cu3 78.44(6) . . ? O8 Tb1 Cu3 78.44(6) 7_575 . ? O15 Tb1 Cu3 104.58(10) 7_575 . ? O15 Tb1 Cu3 104.58(10) . . ? O9 Tb1 Cu3 32.19(6) . . ? O9 Tb1 Cu3 32.19(6) 7_575 . ? O12 Tb1 Cu3 144.76(12) . . ? Cu1 Tb1 Cu3 76.72(2) . . ? O14 Tb1 Cu2 108.36(8) . . ? O13 Tb1 Cu2 105.12(9) . . ? O8 Tb1 Cu2 31.73(6) . . ? O8 Tb1 Cu2 79.65(6) 7_575 . ? O15 Tb1 Cu2 147.32(10) 7_575 . ? O15 Tb1 Cu2 71.34(10) . . ? O9 Tb1 Cu2 32.86(6) . . ? O9 Tb1 Cu2 79.31(6) 7_575 . ? O12 Tb1 Cu2 141.947(15) . . ? Cu1 Tb1 Cu2 52.440(12) . . ? Cu3 Tb1 Cu2 51.244(17) . . ? O5 Cu1 O5 87.63(17) 7_575 . ? O5 Cu1 O8 93.72(12) 7_575 7_575 ? O5 Cu1 O8 176.63(11) . 7_575 ? O5 Cu1 O8 176.63(11) 7_575 . ? O5 Cu1 O8 93.72(12) . . ? O8 Cu1 O8 84.76(16) 7_575 . ? O5 Cu1 O11 91.16(12) 7_575 . ? O5 Cu1 O11 91.16(12) . . ? O8 Cu1 O11 91.90(11) 7_575 . ? O8 Cu1 O11 91.90(11) . . ? O5 Cu1 Tb1 136.08(9) 7_575 . ? O5 Cu1 Tb1 136.08(9) . . ? O8 Cu1 Tb1 42.39(8) 7_575 . ? O8 Cu1 Tb1 42.39(8) . . ? O11 Cu1 Tb1 91.80(11) . . ? O8 Cu2 O4 93.84(11) . . ? O8 Cu2 O6 172.87(11) . . ? O4 Cu2 O6 88.31(12) . . ? O8 Cu2 O9 83.02(11) . . ? O4 Cu2 O9 175.37(11) . . ? O6 Cu2 O9 94.41(11) . . ? O8 Cu2 O10 97.70(12) . . ? O4 Cu2 O10 94.99(13) . . ? O6 Cu2 O10 88.87(13) . . ? O9 Cu2 O10 88.83(12) . . ? O8 Cu2 Cu3 98.46(8) . . ? O4 Cu2 Cu3 139.24(9) . . ? O6 Cu2 Cu3 75.64(8) . . ? O9 Cu2 Cu3 38.65(8) . . ? O10 Cu2 Cu3 121.32(9) . . ? O8 Cu2 Tb1 40.86(8) . . ? O4 Cu2 Tb1 134.34(9) . . ? O6 Cu2 Tb1 135.84(8) . . ? O9 Cu2 Tb1 42.25(7) . . ? O10 Cu2 Tb1 96.56(10) . . ? Cu3 Cu2 Tb1 64.16(2) . . ? O7 Cu3 O7 87.16(18) . 7_575 ? O7 Cu3 O9 176.17(12) . 7_575 ? O7 Cu3 O9 94.13(12) 7_575 7_575 ? O7 Cu3 O9 94.13(12) . . ? O7 Cu3 O9 176.17(12) 7_575 . ? O9 Cu3 O9 84.35(15) 7_575 . ? O7 Cu3 Cu2 144.30(10) . 7_575 ? O7 Cu3 Cu2 80.14(9) 7_575 7_575 ? O9 Cu3 Cu2 39.53(7) 7_575 7_575 ? O9 Cu3 Cu2 100.74(8) . 7_575 ? O7 Cu3 Cu2 80.14(9) . . ? O7 Cu3 Cu2 144.30(10) 7_575 . ? O9 Cu3 Cu2 100.74(8) 7_575 . ? O9 Cu3 Cu2 39.53(7) . . ? Cu2 Cu3 Cu2 90.99(3) 7_575 . ? O7 Cu3 Tb1 136.40(9) . . ? O7 Cu3 Tb1 136.40(9) 7_575 . ? O9 Cu3 Tb1 42.29(8) 7_575 . ? O9 Cu3 Tb1 42.29(8) . . ? Cu2 Cu3 Tb1 64.600(15) 7_575 . ? Cu2 Cu3 Tb1 64.600(15) . . ? O21 Cl1 O20 112.6(5) . . ? O21 Cl1 O19 110.5(4) . . ? O20 Cl1 O19 111.8(3) . . ? O21 Cl1 O22 106.8(7) . . ? O20 Cl1 O22 106.7(4) . . ? O19 Cl1 O22 108.1(4) . . ? O1 C1 N3 122.9(4) . . ? O1 C1 N2 121.5(4) . . ? N3 C1 N2 115.6(3) . . ? O2 C2 N1 122.5(4) . . ? O2 C2 N2 121.3(4) . . ? N1 C2 N2 116.2(4) . . ? O3 C3 N1 122.4(4) . . ? O3 C3 N3 122.9(4) . . ? N1 C3 N3 114.8(4) . . ? N2 C4 C5 113.4(3) . . ? C6 C5 C4 115.8(3) . . ? O5 C6 O4 126.7(4) . . ? O5 C6 C5 115.5(3) . . ? O4 C6 C5 117.8(4) . . ? N3 C7 C8 113.2(3) . . ? C9 C8 C7 116.0(4) . . ? O6 C9 O7 125.7(4) . . ? O6 C9 C8 119.3(4) . . ? O7 C9 C8 115.0(3) . . ? C2 N1 C3 125.7(4) . . ? C2 N2 C1 123.1(4) . . ? C2 N2 C4 118.1(3) . . ? C1 N2 C4 118.6(3) . . ? C3 N3 C1 123.9(4) . . ? C3 N3 C7 117.1(4) . . ? C1 N3 C7 118.9(3) . . ? O16 N4 O18 125.6(6) . . ? O16 N4 O17 117.6(5) . . ? O18 N4 O17 116.8(5) . . ? C6 O4 Cu2 129.4(3) . . ? C6 O5 Cu1 127.8(3) . . ? C9 O6 Cu2 131.2(3) . . ? C9 O7 Cu3 124.7(3) . . ? Cu2 O8 Cu1 104.98(12) . . ? Cu2 O8 Tb1 107.41(11) . . ? Cu1 O8 Tb1 104.60(11) . . ? Cu3 O9 Cu2 101.82(11) . . ? Cu3 O9 Tb1 105.52(11) . . ? Cu2 O9 Tb1 104.89(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.087 _refine_diff_density_min -0.941 _refine_diff_density_rms 0.162 data_a3 _database_code_depnum_ccdc_archive 'CCDC 882314' #TrackingRef '3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H50 Cl2 Cu4 N7 O43 Sm' _chemical_formula_weight 1528.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.5762(4) _cell_length_b 20.2376(6) _cell_length_c 15.9957(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4718.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12963 _cell_measurement_theta_min 2.1403 _cell_measurement_theta_max 27.4856 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.1900 _exptl_crystal_size_mid 0.1700 _exptl_crystal_size_min 0.1600 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3052 _exptl_absorpt_coefficient_mu 3.242 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7667 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35469 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5555 _reflns_number_gt 5385 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+9.7632P] 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 5555 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0999 _refine_ls_wR_factor_gt 0.0991 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 0.126626(14) 0.7500 0.102972(13) 0.01942(8) Uani 1 2 d S . . Cu1 Cu 0.02275(4) 0.7500 -0.09188(3) 0.02320(13) Uani 1 2 d S . . Cu2 Cu -0.04623(3) 0.64260(2) 0.03075(2) 0.02247(11) Uani 1 1 d . . . Cu3 Cu -0.10796(4) 0.7500 0.15208(4) 0.02353(13) Uani 1 2 d S . . Cl1 Cl 0.42191(7) 0.55166(7) 0.20219(8) 0.0559(3) Uani 1 1 d . . . C1 C -0.2674(2) 0.54518(17) -0.0647(2) 0.0282(7) Uani 1 1 d . . . C2 C -0.3205(3) 0.61761(19) -0.1756(2) 0.0346(8) Uani 1 1 d . . . C3 C -0.3943(3) 0.6203(2) -0.0396(3) 0.0365(8) Uani 1 1 d . . . C4 C -0.1875(3) 0.54727(19) -0.2017(2) 0.0326(7) Uani 1 1 d . . . H4A H -0.2161 0.5315 -0.2527 0.039 Uiso 1 1 calc R . . H4B H -0.1571 0.5100 -0.1755 0.039 Uiso 1 1 calc R . . C5 C -0.1162(3) 0.5990(2) -0.2240(2) 0.0356(8) Uani 1 1 d . . . H5A H -0.0693 0.5783 -0.2581 0.043 Uiso 1 1 calc R . . H5B H -0.1454 0.6327 -0.2578 0.043 Uiso 1 1 calc R . . C6 C -0.0696(2) 0.63258(17) -0.1506(2) 0.0256(6) Uani 1 1 d . . . C7 C -0.3377(3) 0.5516(2) 0.0745(2) 0.0340(8) Uani 1 1 d . . . H7A H -0.2978 0.5136 0.0821 0.041 Uiso 1 1 calc R . . H7B H -0.4001 0.5375 0.0856 0.041 Uiso 1 1 calc R . . C8 C -0.3112(2) 0.6048(2) 0.1370(2) 0.0329(8) Uani 1 1 d . . . H8A H -0.3564 0.6399 0.1338 0.039 Uiso 1 1 calc R . . H8B H -0.3147 0.5860 0.1927 0.039 Uiso 1 1 calc R . . C9 C -0.2177(2) 0.63501(17) 0.1263(2) 0.0254(6) Uani 1 1 d . . . N1 N -0.3847(2) 0.64074(19) -0.1213(2) 0.0406(8) Uani 1 1 d . . . H1A H -0.4221 0.6704 -0.1392 0.049 Uiso 1 1 calc R . . N2 N -0.2597(2) 0.57237(15) -0.14478(18) 0.0299(6) Uani 1 1 d . . . N3 N -0.3311(2) 0.57421(16) -0.01307(19) 0.0311(6) Uani 1 1 d . . . N4 N -0.2057(3) 0.7500 -0.0369(3) 0.0274(8) Uani 1 2 d S . . O1 O -0.2202(2) 0.49850(14) -0.04344(17) 0.0365(6) Uani 1 1 d . . . O1W O -0.5036(3) 0.7500 -0.1661(3) 0.0484(11) Uani 1 2 d S . . O2 O -0.3165(2) 0.63664(15) -0.24819(19) 0.0478(7) Uani 1 1 d . . . O2W O -0.0183(5) 0.7500 0.3785(4) 0.0758(17) Uani 1 2 d S . . O3 O -0.4545(2) 0.64151(18) 0.0054(2) 0.0511(8) Uani 1 1 d . . . O3WA O 0.1408(8) 0.5770(8) -0.0867(8) 0.067(4) Uani 0.50 1 d P A 1 O3WB O 0.1818(8) 0.5953(7) -0.0847(9) 0.058(3) Uani 0.50 1 d P B 2 O4 O -0.07983(18) 0.60701(13) -0.07908(15) 0.0308(5) Uani 1 1 d . . . O4WA O 0.3734(7) 0.6650(7) -0.0680(8) 0.096(4) Uani 0.50 1 d P . . O4WB O 0.3516(8) 0.6296(8) -0.0127(14) 0.143(6) Uani 0.50 1 d P . . O5 O -0.02417(18) 0.68336(13) -0.16837(15) 0.0321(5) Uani 1 1 d . . . O6 O -0.16472(16) 0.61120(13) 0.07292(15) 0.0285(5) Uani 1 1 d . . . O7 O -0.20103(19) 0.68409(13) 0.17345(16) 0.0344(6) Uani 1 1 d . . . O8 O 0.06560(15) 0.68497(12) -0.01012(14) 0.0242(5) Uani 1 1 d . . . H8C H 0.1101 0.6536 -0.0333 0.029 Uiso 1 1 calc R . . O9 O -0.01041(15) 0.68557(11) 0.13707(13) 0.0231(4) Uani 1 1 d . . . H9A H -0.0026 0.6550 0.1841 0.028 Uiso 1 1 calc R . . O10 O 0.0234(2) 0.54243(16) 0.0802(2) 0.0529(8) Uani 1 1 d . . . H10A H 0.0326 0.5150 0.0409 0.063 Uiso 1 1 d R . . H10B H -0.0196 0.5302 0.1125 0.063 Uiso 1 1 d R . . O11 O 0.1665(3) 0.7500 -0.1608(2) 0.0379(9) Uani 1 2 d S . . H11 H 0.1777 0.7152 -0.1885 0.046 Uiso 1 1 d R . . O12 O 0.2824(3) 0.7500 0.1617(3) 0.0745(19) Uani 1 2 d S . . H12 H 0.2954 0.7835 0.1912 0.089 Uiso 1 1 d R . . O13 O 0.2410(3) 0.7500 -0.0042(3) 0.0512(12) Uani 1 2 d S . . H13A H 0.2289 0.7500 -0.0561 0.061 Uiso 1 2 d SR . . H13B H 0.2931 0.7500 0.0009 0.061 Uiso 1 2 d SR . . O14 O 0.1243(3) 0.7500 0.2525(2) 0.0386(9) Uani 1 2 d S . . H14A H 0.0776 0.7500 0.2844 0.046 Uiso 1 2 d SR . . H14B H 0.1761 0.7500 0.2782 0.046 Uiso 1 2 d SR . . O15 O 0.1757(3) 0.63693(17) 0.1265(2) 0.0547(9) Uani 1 1 d . . . H15A H 0.2334 0.6318 0.1221 0.066 Uiso 1 1 d R . . H15B H 0.1379 0.6087 0.1074 0.066 Uiso 1 1 d R . . O16 O -0.2080(4) 0.7500 -0.1105(3) 0.079(2) Uani 1 2 d S . . O17 O -0.1229(2) 0.7500 -0.0005(2) 0.0288(7) Uani 1 2 d S . . O18 O -0.2720(3) 0.7500 0.0091(3) 0.0662(16) Uani 1 2 d S . . O19 O 0.4506(3) 0.5064(2) 0.1410(3) 0.0882(17) Uani 1 1 d . . . O20 O 0.4925(3) 0.5943(2) 0.2264(2) 0.0743(13) Uani 1 1 d . . . O21 O 0.3477(5) 0.5847(5) 0.1762(8) 0.232(6) Uani 1 1 d . . . O22 O 0.3961(6) 0.5155(4) 0.2753(4) 0.174(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.01838(12) 0.02514(14) 0.01473(12) 0.000 -0.00304(7) 0.000 Cu1 0.0266(3) 0.0253(3) 0.0177(2) 0.000 -0.0016(2) 0.000 Cu2 0.0239(2) 0.0255(2) 0.01802(19) -0.00207(14) 0.00013(14) -0.00185(14) Cu3 0.0252(3) 0.0233(3) 0.0222(3) 0.000 0.0052(2) 0.000 Cl1 0.0344(5) 0.0696(8) 0.0637(7) -0.0338(6) 0.0064(5) -0.0095(5) C1 0.0330(17) 0.0271(16) 0.0243(15) 0.0002(13) -0.0050(13) -0.0056(13) C2 0.0389(19) 0.0317(19) 0.0330(18) 0.0026(15) -0.0104(15) -0.0017(15) C3 0.0320(18) 0.041(2) 0.0370(19) 0.0008(16) -0.0064(15) -0.0035(16) C4 0.0404(19) 0.0328(18) 0.0247(16) -0.0037(14) -0.0044(14) -0.0037(15) C5 0.042(2) 0.046(2) 0.0188(15) -0.0035(15) -0.0035(13) -0.0082(17) C6 0.0278(15) 0.0264(16) 0.0226(14) -0.0046(12) 0.0022(12) 0.0014(13) C7 0.0330(18) 0.036(2) 0.0327(18) 0.0052(15) 0.0019(15) -0.0100(15) C8 0.0285(17) 0.042(2) 0.0281(17) -0.0007(15) 0.0061(13) -0.0062(15) C9 0.0275(15) 0.0269(16) 0.0219(14) 0.0028(12) 0.0017(12) -0.0011(13) N1 0.0393(18) 0.041(2) 0.0419(18) 0.0035(15) -0.0086(15) 0.0085(14) N2 0.0337(15) 0.0310(15) 0.0250(14) 0.0018(12) -0.0062(11) -0.0022(12) N3 0.0290(14) 0.0318(16) 0.0325(15) 0.0004(12) -0.0031(12) -0.0032(12) N4 0.031(2) 0.026(2) 0.0247(19) 0.000 0.0022(16) 0.000 O1 0.0458(15) 0.0332(14) 0.0306(12) 0.0041(11) -0.0018(11) 0.0064(12) O1W 0.054(3) 0.062(3) 0.0291(19) 0.000 -0.0087(18) 0.000 O2 0.065(2) 0.0470(17) 0.0309(14) 0.0079(13) -0.0110(14) 0.0055(15) O2W 0.074(4) 0.070(4) 0.084(4) 0.000 0.002(3) 0.000 O3 0.0350(15) 0.064(2) 0.0545(19) 0.0019(16) 0.0049(13) 0.0109(14) O3WA 0.084(9) 0.083(10) 0.035(4) 0.007(5) 0.014(6) 0.040(7) O3WB 0.073(7) 0.061(7) 0.041(4) 0.010(4) 0.019(6) 0.030(6) O4 0.0401(14) 0.0338(13) 0.0184(10) -0.0035(10) -0.0028(10) -0.0074(11) O4WA 0.069(6) 0.120(10) 0.100(9) 0.017(8) -0.008(5) 0.019(6) O4WB 0.069(7) 0.119(12) 0.24(2) -0.007(13) -0.006(10) 0.016(7) O5 0.0411(14) 0.0324(13) 0.0228(11) -0.0020(10) 0.0002(10) -0.0076(11) O6 0.0265(11) 0.0339(13) 0.0250(11) -0.0027(10) 0.0035(9) -0.0046(10) O7 0.0394(14) 0.0308(13) 0.0331(13) -0.0043(11) 0.0143(11) -0.0077(11) O8 0.0241(10) 0.0279(12) 0.0207(10) 0.0002(9) -0.0003(8) 0.0028(9) O9 0.0260(11) 0.0235(11) 0.0198(10) -0.0005(8) -0.0020(8) 0.0019(9) O10 0.060(2) 0.0409(17) 0.0576(19) 0.0009(15) 0.0092(16) 0.0170(15) O11 0.048(2) 0.038(2) 0.0276(18) 0.000 0.0075(16) 0.000 O12 0.040(3) 0.151(6) 0.032(2) 0.000 -0.0118(19) 0.000 O13 0.0266(19) 0.098(4) 0.030(2) 0.000 0.0008(16) 0.000 O14 0.038(2) 0.056(3) 0.0227(18) 0.000 -0.0081(15) 0.000 O15 0.061(2) 0.0490(19) 0.0543(19) -0.0049(16) -0.0147(16) 0.0255(16) O16 0.038(3) 0.162(7) 0.037(3) 0.000 -0.008(2) 0.000 O17 0.0274(17) 0.0307(18) 0.0282(17) 0.000 -0.0028(13) 0.000 O18 0.033(2) 0.118(5) 0.047(3) 0.000 0.002(2) 0.000 O19 0.075(3) 0.092(3) 0.098(3) -0.060(3) 0.036(2) -0.033(3) O20 0.057(2) 0.096(3) 0.069(2) -0.046(2) 0.0166(19) -0.035(2) O21 0.115(5) 0.226(10) 0.355(14) -0.168(10) -0.131(8) 0.109(6) O22 0.238(9) 0.193(8) 0.091(4) -0.052(5) 0.071(5) -0.158(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O14 2.392(4) . ? Sm1 O13 2.391(4) . ? Sm1 O8 2.407(2) . ? Sm1 O8 2.407(2) 7_575 ? Sm1 O15 2.427(3) 7_575 ? Sm1 O15 2.427(3) . ? Sm1 O9 2.447(2) . ? Sm1 O9 2.447(2) 7_575 ? Sm1 O12 2.457(5) . ? Sm1 Cu1 3.4651(6) . ? Sm1 Cu3 3.5084(6) . ? Sm1 Cu2 3.5224(4) . ? Cu1 O5 1.945(3) 7_575 ? Cu1 O5 1.945(3) . ? Cu1 O8 1.958(2) 7_575 ? Cu1 O8 1.958(2) . ? Cu1 O11 2.368(4) . ? Cu2 O8 1.954(2) . ? Cu2 O4 1.961(2) . ? Cu2 O6 1.960(2) . ? Cu2 O9 1.980(2) . ? Cu2 O10 2.401(3) . ? Cu2 Cu3 3.0496(5) . ? Cu3 O7 1.933(3) . ? Cu3 O7 1.933(3) 7_575 ? Cu3 O9 1.944(2) 7_575 ? Cu3 O9 1.944(2) . ? Cu3 Cu2 3.0496(5) 7_575 ? Cl1 O21 1.337(7) . ? Cl1 O20 1.399(4) . ? Cl1 O19 1.404(4) . ? Cl1 O22 1.430(7) . ? C1 O1 1.217(4) . ? C1 N3 1.375(5) . ? C1 N2 1.398(4) . ? C2 O2 1.224(5) . ? C2 N1 1.360(6) . ? C2 N2 1.367(5) . ? C3 O3 1.214(5) . ? C3 N1 1.378(5) . ? C3 N3 1.378(5) . ? C4 N2 1.481(5) . ? C4 C5 1.519(5) . ? C5 C6 1.516(5) . ? C6 O5 1.255(4) . ? C6 O4 1.265(4) . ? C7 N3 1.477(5) . ? C7 C8 1.520(5) . ? C8 C9 1.503(5) . ? C9 O6 1.249(4) . ? C9 O7 1.270(4) . ? N4 O16 1.178(6) . ? N4 O18 1.214(6) . ? N4 O17 1.340(5) . ? O4WA O4WB 1.181(19) . ? 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 O14 Sm1 O13 136.61(14) . . ? O14 Sm1 O8 138.25(8) . . ? O13 Sm1 O8 73.68(10) . . ? O14 Sm1 O8 138.25(8) . 7_575 ? O13 Sm1 O8 73.68(10) . 7_575 ? O8 Sm1 O8 66.28(11) . 7_575 ? O14 Sm1 O15 81.33(9) . 7_575 ? O13 Sm1 O15 84.58(10) . 7_575 ? O8 Sm1 O15 137.80(10) . 7_575 ? O8 Sm1 O15 73.13(10) 7_575 7_575 ? O14 Sm1 O15 81.34(9) . . ? O13 Sm1 O15 84.58(10) . . ? O8 Sm1 O15 73.13(10) . . ? O8 Sm1 O15 137.80(10) 7_575 . ? O15 Sm1 O15 141.11(18) 7_575 . ? O14 Sm1 O9 76.43(9) . . ? O13 Sm1 O9 136.80(8) . . ? O8 Sm1 O9 64.82(7) . . ? O8 Sm1 O9 99.04(7) 7_575 . ? O15 Sm1 O9 135.11(11) 7_575 . ? O15 Sm1 O9 72.76(11) . . ? O14 Sm1 O9 76.43(9) . 7_575 ? O13 Sm1 O9 136.80(8) . 7_575 ? O8 Sm1 O9 99.04(7) . 7_575 ? O8 Sm1 O9 64.82(7) 7_575 7_575 ? O15 Sm1 O9 72.76(11) 7_575 7_575 ? O15 Sm1 O9 135.11(11) . 7_575 ? O9 Sm1 O9 64.40(11) . 7_575 ? O14 Sm1 O12 68.36(15) . . ? O13 Sm1 O12 68.25(15) . . ? O8 Sm1 O12 128.94(10) . . ? O8 Sm1 O12 128.94(10) 7_575 . ? O15 Sm1 O12 70.64(9) 7_575 . ? O15 Sm1 O12 70.64(9) . . ? O9 Sm1 O12 132.01(10) . . ? O9 Sm1 O12 132.01(10) 7_575 . ? O14 Sm1 Cu1 153.27(9) . . ? O13 Sm1 Cu1 70.12(10) . . ? O8 Sm1 Cu1 33.14(6) . . ? O8 Sm1 Cu1 33.14(6) 7_575 . ? O15 Sm1 Cu1 105.55(8) 7_575 . ? O15 Sm1 Cu1 105.55(8) . . ? O9 Sm1 Cu1 81.01(5) . . ? O9 Sm1 Cu1 81.01(5) 7_575 . ? O12 Sm1 Cu1 138.37(12) . . ? O14 Sm1 Cu3 76.24(9) . . ? O13 Sm1 Cu3 147.15(10) . . ? O8 Sm1 Cu3 78.94(5) . . ? O8 Sm1 Cu3 78.94(5) 7_575 . ? O15 Sm1 Cu3 104.63(10) 7_575 . ? O15 Sm1 Cu3 104.63(10) . . ? O9 Sm1 Cu3 32.28(5) . . ? O9 Sm1 Cu3 32.28(5) 7_575 . ? O12 Sm1 Cu3 144.60(12) . . ? Cu1 Sm1 Cu3 77.028(14) . . ? O14 Sm1 Cu2 108.52(7) . . ? O13 Sm1 Cu2 105.29(8) . . ? O8 Sm1 Cu2 31.99(5) . . ? O8 Sm1 Cu2 80.01(6) 7_575 . ? O15 Sm1 Cu2 147.51(9) 7_575 . ? O15 Sm1 Cu2 71.32(9) . . ? O9 Sm1 Cu2 32.90(5) . . ? O9 Sm1 Cu2 79.51(5) 7_575 . ? O12 Sm1 Cu2 141.846(9) . . ? Cu1 Sm1 Cu2 52.586(9) . . ? Cu3 Sm1 Cu2 51.412(9) . . ? O5 Cu1 O5 87.79(16) 7_575 . ? O5 Cu1 O8 93.80(10) 7_575 7_575 ? O5 Cu1 O8 176.85(10) . 7_575 ? O5 Cu1 O8 176.85(10) 7_575 . ? O5 Cu1 O8 93.80(10) . . ? O8 Cu1 O8 84.48(14) 7_575 . ? O5 Cu1 O11 91.04(11) 7_575 . ? O5 Cu1 O11 91.04(11) . . ? O8 Cu1 O11 91.65(10) 7_575 . ? O8 Cu1 O11 91.65(10) . . ? O5 Cu1 Sm1 136.01(8) 7_575 . ? O5 Cu1 Sm1 136.01(8) . . ? O8 Cu1 Sm1 42.24(7) 7_575 . ? O8 Cu1 Sm1 42.24(7) . . ? O11 Cu1 Sm1 91.84(10) . . ? O8 Cu2 O4 94.00(10) . . ? O8 Cu2 O6 172.88(11) . . ? O4 Cu2 O6 88.23(11) . . ? O8 Cu2 O9 82.80(10) . . ? O4 Cu2 O9 175.30(10) . . ? O6 Cu2 O9 94.54(10) . . ? O8 Cu2 O10 97.35(11) . . ? O4 Cu2 O10 95.18(12) . . ? O6 Cu2 O10 89.17(12) . . ? O9 Cu2 O10 88.66(11) . . ? O8 Cu2 Cu3 98.41(7) . . ? O4 Cu2 Cu3 139.32(8) . . ? O6 Cu2 Cu3 75.65(7) . . ? O9 Cu2 Cu3 38.58(7) . . ? O10 Cu2 Cu3 121.13(9) . . ? O8 Cu2 Sm1 40.74(7) . . ? O4 Cu2 Sm1 134.36(8) . . ? O6 Cu2 Sm1 135.85(7) . . ? O9 Cu2 Sm1 42.16(7) . . ? O10 Cu2 Sm1 96.35(9) . . ? Cu3 Cu2 Sm1 64.057(13) . . ? O7 Cu3 O7 87.27(16) . 7_575 ? O7 Cu3 O9 176.33(11) . 7_575 ? O7 Cu3 O9 94.15(11) 7_575 7_575 ? O7 Cu3 O9 94.15(11) . . ? O7 Cu3 O9 176.33(11) 7_575 . ? O9 Cu3 O9 84.24(14) 7_575 . ? O7 Cu3 Cu2 144.23(9) . 7_575 ? O7 Cu3 Cu2 80.08(8) 7_575 7_575 ? O9 Cu3 Cu2 39.43(6) 7_575 7_575 ? O9 Cu3 Cu2 100.58(7) . 7_575 ? O7 Cu3 Cu2 80.08(8) . . ? O7 Cu3 Cu2 144.23(9) 7_575 . ? O9 Cu3 Cu2 100.58(7) 7_575 . ? O9 Cu3 Cu2 39.43(6) . . ? Cu2 Cu3 Cu2 90.91(2) 7_575 . ? O7 Cu3 Sm1 136.35(8) . . ? O7 Cu3 Sm1 136.35(8) 7_575 . ? O9 Cu3 Sm1 42.23(7) 7_575 . ? O9 Cu3 Sm1 42.23(7) . . ? Cu2 Cu3 Sm1 64.531(12) 7_575 . ? Cu2 Cu3 Sm1 64.531(12) . . ? O21 Cl1 O20 111.9(5) . . ? O21 Cl1 O19 110.5(5) . . ? O20 Cl1 O19 112.1(2) . . ? O21 Cl1 O22 107.3(7) . . ? O20 Cl1 O22 106.5(3) . . ? O19 Cl1 O22 108.3(4) . . ? O1 C1 N3 123.1(3) . . ? O1 C1 N2 121.1(3) . . ? N3 C1 N2 115.9(3) . . ? O2 C2 N1 122.1(4) . . ? O2 C2 N2 121.5(4) . . ? N1 C2 N2 116.5(3) . . ? O3 C3 N1 122.0(4) . . ? O3 C3 N3 122.7(4) . . ? N1 C3 N3 115.3(4) . . ? N2 C4 C5 113.2(3) . . ? C6 C5 C4 115.8(3) . . ? O5 C6 O4 127.0(3) . . ? O5 C6 C5 115.3(3) . . ? O4 C6 C5 117.7(3) . . ? N3 C7 C8 112.8(3) . . ? C9 C8 C7 116.4(3) . . ? O6 C9 O7 126.1(3) . . ? O6 C9 C8 118.8(3) . . ? O7 C9 C8 115.1(3) . . ? C2 N1 C3 125.0(4) . . ? C2 N2 C1 122.8(3) . . ? C2 N2 C4 117.9(3) . . ? C1 N2 C4 119.0(3) . . ? C3 N3 C1 123.8(3) . . ? C3 N3 C7 117.3(3) . . ? C1 N3 C7 118.7(3) . . ? O16 N4 O18 125.7(5) . . ? O16 N4 O17 117.3(4) . . ? O18 N4 O17 117.0(4) . . ? C6 O4 Cu2 129.1(2) . . ? C6 O5 Cu1 127.7(2) . . ? C9 O6 Cu2 131.0(2) . . ? C9 O7 Cu3 124.7(2) . . ? Cu2 O8 Cu1 104.61(11) . . ? Cu2 O8 Sm1 107.26(9) . . ? Cu1 O8 Sm1 104.62(10) . . ? Cu3 O9 Cu2 101.99(10) . . ? Cu3 O9 Sm1 105.50(10) . . ? Cu2 O9 Sm1 104.94(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.033 _refine_diff_density_min -0.973 _refine_diff_density_rms 0.115 data_a4 _database_code_depnum_ccdc_archive 'CCDC 882315' #TrackingRef '4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H50 Cl2 Cu4 Eu N7 O43' _chemical_formula_weight 1529.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.5743(4) _cell_length_b 20.2763(6) _cell_length_c 16.0214(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4734.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13078 _cell_measurement_theta_min 2.0087 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.2200 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1700 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3056 _exptl_absorpt_coefficient_mu 3.316 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6386 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35994 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5576 _reflns_number_gt 5463 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+6.8487P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5576 _refine_ls_number_parameters 375 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0860 _refine_ls_wR_factor_gt 0.0854 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl -0.42248(6) 0.44870(6) -0.20288(7) 0.0551(3) Uani 1 1 d . . . Eu1 Eu 0.128673(13) 0.7500 0.103595(12) 0.02416(7) Uani 1 2 d S . . N1 N -0.3847(2) 0.64027(16) -0.1214(2) 0.0413(7) Uani 1 1 d . . . H1A H -0.4225 0.6695 -0.1394 0.050 Uiso 1 1 calc R . . N2 N -0.25957(18) 0.57247(13) -0.14507(16) 0.0309(5) Uani 1 1 d . . . N3 N -0.33115(18) 0.57412(13) -0.01353(17) 0.0319(5) Uani 1 1 d . . . N4 N -0.2066(3) 0.7500 -0.0377(2) 0.0276(7) Uani 1 2 d S . . C1 C -0.2670(2) 0.54515(15) -0.06557(19) 0.0305(6) Uani 1 1 d . . . C2 C -0.3204(2) 0.61794(17) -0.1758(2) 0.0363(7) Uani 1 1 d . . . C3 C -0.3945(2) 0.62018(18) -0.0401(2) 0.0378(7) Uani 1 1 d . . . C4 C -0.1875(2) 0.54752(16) -0.20202(19) 0.0342(7) Uani 1 1 d . . . H4A H -0.2162 0.5319 -0.2529 0.041 Uiso 1 1 calc R . . H4B H -0.1570 0.5103 -0.1759 0.041 Uiso 1 1 calc R . . C5 C -0.1161(2) 0.59946(18) -0.2242(2) 0.0358(7) Uani 1 1 d . . . H5A H -0.0692 0.5789 -0.2583 0.043 Uiso 1 1 calc R . . H5B H -0.1454 0.6332 -0.2578 0.043 Uiso 1 1 calc R . . C6 C -0.0698(2) 0.63258(14) -0.15099(18) 0.0268(6) Uani 1 1 d . . . C7 C -0.3377(2) 0.55150(17) 0.0741(2) 0.0352(7) Uani 1 1 d . . . H7A H -0.2977 0.5137 0.0817 0.042 Uiso 1 1 calc R . . H7B H -0.4000 0.5373 0.0852 0.042 Uiso 1 1 calc R . . C8 C -0.3115(2) 0.60444(17) 0.1363(2) 0.0338(7) Uani 1 1 d . . . H8A H -0.3571 0.6392 0.1335 0.041 Uiso 1 1 calc R . . H8B H -0.3146 0.5855 0.1919 0.041 Uiso 1 1 calc R . . C9 C -0.2181(2) 0.63507(14) 0.12528(18) 0.0260(5) Uani 1 1 d . . . O1 O -0.22018(17) 0.49844(11) -0.04403(15) 0.0376(5) Uani 1 1 d . . . O1W O -0.5034(3) 0.7500 -0.1663(2) 0.0507(9) Uani 1 2 d S . . O2 O -0.3170(2) 0.63658(13) -0.24824(17) 0.0494(6) Uani 1 1 d . . . O2W O -0.0170(4) 0.7500 0.3805(3) 0.0714(13) Uani 1 2 d S . . O3 O -0.45468(18) 0.64114(16) 0.0051(2) 0.0532(7) Uani 1 1 d . . . O3W O 0.1624(4) 0.5865(2) -0.0862(2) 0.111(2) Uani 1 1 d . . . O4 O -0.07977(16) 0.60731(11) -0.07950(13) 0.0314(5) Uani 1 1 d . . . O4WA O 0.3734(6) 0.6638(6) -0.0703(7) 0.093(3) Uani 0.50 1 d P . . O4WB O 0.3512(7) 0.6285(6) -0.0173(11) 0.129(5) Uani 0.50 1 d P . . O5 O -0.02412(16) 0.68344(11) -0.16842(13) 0.0326(5) Uani 1 1 d . . . O6 O -0.16464(14) 0.61102(11) 0.07224(13) 0.0301(4) Uani 1 1 d . . . O7 O -0.20177(16) 0.68425(11) 0.17181(14) 0.0346(5) Uani 1 1 d . . . O8 O 0.06539(14) 0.68477(11) -0.01058(13) 0.0248(4) Uani 1 1 d . . . O9 O -0.01107(14) 0.68528(10) 0.13676(12) 0.0238(4) Uani 1 1 d . . . O10 O 0.0230(2) 0.54212(14) 0.07950(19) 0.0534(7) Uani 1 1 d . . . H10A H 0.0322 0.5147 0.0402 0.064 Uiso 1 1 d R . . H10B H -0.0200 0.5299 0.1119 0.064 Uiso 1 1 d R . . O11 O 0.1669(2) 0.7500 -0.1613(2) 0.0387(7) Uani 1 2 d S . . H11 H 0.1780 0.7152 -0.1890 0.046 Uiso 1 1 d R . . O12 O 0.2858(3) 0.7500 0.1626(3) 0.0785(17) Uani 1 2 d S . . H12 H 0.2987 0.7835 0.1922 0.094 Uiso 1 1 d R . . O13 O 0.2445(2) 0.7500 -0.0061(2) 0.0560(11) Uani 1 2 d S . . H13A H 0.2323 0.7500 -0.0580 0.067 Uiso 1 2 d SR . . H13B H 0.2966 0.7500 -0.0010 0.067 Uiso 1 2 d SR . . O14 O 0.1254(2) 0.7500 0.2553(2) 0.0393(8) Uani 1 2 d S . . H14A H 0.0787 0.7500 0.2871 0.047 Uiso 1 2 d SR . . H14B H 0.1772 0.7500 0.2810 0.047 Uiso 1 2 d SR . . O15 O 0.1776(2) 0.63538(14) 0.12705(19) 0.0567(8) Uani 1 1 d . . . H15A H 0.2353 0.6303 0.1227 0.068 Uiso 1 1 d R . . H15B H 0.1399 0.6072 0.1080 0.068 Uiso 1 1 d R . . O16 O -0.2083(3) 0.7500 -0.1112(3) 0.0816(18) Uani 1 2 d S . . O17 O -0.1230(2) 0.7500 -0.0006(2) 0.0300(6) Uani 1 2 d S . . O18 O -0.2719(3) 0.7500 0.0082(3) 0.0691(14) Uani 1 2 d S . . O19 O -0.3477(5) 0.4172(4) -0.1781(6) 0.220(5) Uani 1 1 d . . . O20 O -0.4510(3) 0.4937(2) -0.1420(3) 0.0881(14) Uani 1 1 d . . . O21 O -0.4936(2) 0.4060(2) -0.2268(2) 0.0800(12) Uani 1 1 d . . . O22 O -0.3949(6) 0.4847(4) -0.2751(4) 0.176(4) Uani 1 1 d . . . Cu1 Cu 0.02292(4) 0.7500 -0.09210(3) 0.02443(11) Uani 1 2 d S . . Cu2 Cu -0.04616(2) 0.642537(17) 0.03025(2) 0.02366(9) Uani 1 1 d . . . Cu3 Cu -0.10851(3) 0.7500 0.15074(3) 0.02409(11) Uani 1 2 d S . . H8 H 0.089(3) 0.6612(19) -0.030(2) 0.023(10) Uiso 1 1 d . . . H9 H -0.011(3) 0.662(2) 0.172(2) 0.031(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0354(4) 0.0664(6) 0.0634(6) -0.0327(5) 0.0047(4) -0.0079(4) Eu1 0.02335(11) 0.02841(12) 0.02071(11) 0.000 -0.00264(7) 0.000 N1 0.0399(15) 0.0425(17) 0.0415(16) 0.0041(13) -0.0096(13) 0.0088(13) N2 0.0347(13) 0.0303(13) 0.0276(12) 0.0010(10) -0.0048(10) -0.0023(10) N3 0.0305(13) 0.0328(13) 0.0323(13) 0.0013(11) -0.0035(10) -0.0018(10) N4 0.0317(18) 0.0252(17) 0.0259(17) 0.000 0.0049(14) 0.000 C1 0.0351(15) 0.0263(14) 0.0299(15) 0.0003(12) -0.0065(12) -0.0055(12) C2 0.0399(17) 0.0339(16) 0.0352(16) 0.0018(13) -0.0101(13) -0.0023(13) C3 0.0313(16) 0.0389(17) 0.0433(18) 0.0012(15) -0.0057(14) -0.0017(14) C4 0.0427(17) 0.0329(16) 0.0269(14) -0.0055(12) -0.0060(13) -0.0054(13) C5 0.0430(17) 0.0412(18) 0.0233(14) -0.0050(13) -0.0020(12) -0.0071(14) C6 0.0288(14) 0.0272(14) 0.0243(13) -0.0042(11) 0.0010(11) 0.0012(11) C7 0.0340(16) 0.0370(17) 0.0346(16) 0.0053(14) 0.0024(13) -0.0090(13) C8 0.0295(15) 0.0406(17) 0.0314(15) -0.0011(13) 0.0064(12) -0.0058(13) C9 0.0281(14) 0.0260(13) 0.0241(13) 0.0033(11) 0.0017(11) -0.0013(11) O1 0.0485(14) 0.0307(11) 0.0337(11) 0.0046(9) -0.0024(10) 0.0040(10) O1W 0.055(2) 0.063(3) 0.0339(18) 0.000 -0.0101(17) 0.000 O2 0.0647(17) 0.0482(15) 0.0352(13) 0.0087(11) -0.0116(12) 0.0061(13) O2W 0.067(3) 0.070(3) 0.078(3) 0.000 0.002(3) 0.000 O3 0.0367(14) 0.068(2) 0.0547(16) 0.0022(14) 0.0034(12) 0.0095(13) O3W 0.185(5) 0.108(3) 0.0410(17) 0.009(2) 0.016(2) 0.099(3) O4 0.0394(12) 0.0325(11) 0.0222(9) -0.0022(9) -0.0014(9) -0.0073(9) O4WA 0.070(6) 0.118(8) 0.091(7) 0.006(6) -0.007(4) 0.019(5) O4WB 0.066(6) 0.112(9) 0.209(15) -0.010(9) -0.012(8) 0.011(6) O5 0.0414(12) 0.0323(11) 0.0241(10) -0.0019(8) -0.0017(9) -0.0070(9) O6 0.0277(10) 0.0327(11) 0.0299(10) -0.0050(9) 0.0044(8) -0.0047(9) O7 0.0380(12) 0.0310(11) 0.0349(11) -0.0054(9) 0.0138(9) -0.0065(9) O8 0.0266(10) 0.0261(10) 0.0216(9) -0.0013(8) 0.0015(8) 0.0038(8) O9 0.0284(10) 0.0236(10) 0.0194(9) 0.0018(8) -0.0014(8) 0.0009(8) O10 0.0614(18) 0.0390(14) 0.0596(16) 0.0015(13) 0.0109(14) 0.0157(13) O11 0.049(2) 0.0376(18) 0.0292(16) 0.000 0.0069(14) 0.000 O12 0.040(2) 0.165(6) 0.0304(19) 0.000 -0.0092(16) 0.000 O13 0.0307(18) 0.104(4) 0.0333(18) 0.000 0.0014(14) 0.000 O14 0.0326(17) 0.060(2) 0.0254(16) 0.000 -0.0072(12) 0.000 O15 0.0670(19) 0.0467(16) 0.0565(17) -0.0061(14) -0.0158(15) 0.0240(14) O16 0.047(3) 0.162(6) 0.036(2) 0.000 -0.0054(18) 0.000 O17 0.0288(15) 0.0287(15) 0.0326(16) 0.000 -0.0043(12) 0.000 O18 0.036(2) 0.124(4) 0.047(2) 0.000 0.0007(18) 0.000 O19 0.123(5) 0.200(7) 0.337(12) -0.149(8) -0.136(6) 0.107(5) O20 0.076(2) 0.092(3) 0.097(3) -0.061(2) 0.033(2) -0.036(2) O21 0.0609(19) 0.103(3) 0.076(2) -0.052(2) 0.0191(17) -0.0394(19) O22 0.238(8) 0.199(7) 0.091(4) -0.040(4) 0.057(4) -0.159(6) Cu1 0.0287(2) 0.0248(2) 0.0198(2) 0.000 -0.00137(18) 0.000 Cu2 0.02570(18) 0.02500(18) 0.02028(17) -0.00215(12) 0.00019(12) -0.00188(13) Cu3 0.0257(2) 0.0229(2) 0.0237(2) 0.000 0.00425(18) 0.000 _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 Cl1 O19 1.324(5) . ? Cl1 O20 1.399(3) . ? Cl1 O21 1.404(3) . ? Cl1 O22 1.426(6) . ? Eu1 O14 2.431(3) . ? Eu1 O13 2.437(4) . ? Eu1 O8 2.438(2) . ? Eu1 O8 2.438(2) 7_575 ? Eu1 O15 2.460(3) 7_575 ? Eu1 O15 2.460(3) . ? Eu1 O12 2.477(4) . ? Eu1 O9 2.480(2) . ? Eu1 O9 2.480(2) 7_575 ? Eu1 Cu1 3.4936(5) . ? Eu1 Cu3 3.5383(5) . ? Eu1 Cu2 3.5526(4) . ? N1 C2 1.357(5) . ? N1 C3 1.372(5) . ? N2 C2 1.371(4) . ? N2 C1 1.393(4) . ? N2 C4 1.480(4) . ? N3 C3 1.380(4) . ? N3 C1 1.384(4) . ? N3 C7 1.480(4) . ? N4 O16 1.178(5) . ? N4 O18 1.202(6) . ? N4 O17 1.355(5) . ? C1 O1 1.217(4) . ? C2 O2 1.222(4) . ? C3 O3 1.214(5) . ? C4 C5 1.523(5) . ? C5 C6 1.510(4) . ? C6 O5 1.259(4) . ? C6 O4 1.263(4) . ? C7 C8 1.514(5) . ? C8 C9 1.507(4) . ? C9 O6 1.252(4) . ? C9 O7 1.268(4) . ? O4 Cu2 1.960(2) . ? O4WA O4WB 1.156(15) . ? O5 Cu1 1.946(2) . ? O6 Cu2 1.960(2) . ? O7 Cu3 1.934(2) . ? O8 Cu2 1.950(2) . ? O8 Cu1 1.959(2) . ? O9 Cu3 1.946(2) . ? O9 Cu2 1.981(2) . ? O10 Cu2 2.405(3) . ? O11 Cu1 2.373(3) . ? O17 Cu3 2.434(3) . ? Cu1 O5 1.946(2) 7_575 ? Cu1 O8 1.959(2) 7_575 ? Cu2 Cu3 3.0496(5) . ? Cu3 O7 1.934(2) 7_575 ? Cu3 O9 1.946(2) 7_575 ? Cu3 Cu2 3.0496(5) 7_575 ? 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 O19 Cl1 O20 110.4(4) . . ? O19 Cl1 O21 113.1(4) . . ? O20 Cl1 O21 112.0(2) . . ? O19 Cl1 O22 105.0(6) . . ? O20 Cl1 O22 108.4(4) . . ? O21 Cl1 O22 107.6(3) . . ? O14 Eu1 O13 137.30(12) . . ? O14 Eu1 O8 137.94(7) . . ? O13 Eu1 O8 73.79(9) . . ? O14 Eu1 O8 137.94(7) . 7_575 ? O13 Eu1 O8 73.79(9) . 7_575 ? O8 Eu1 O8 65.70(10) . 7_575 ? O14 Eu1 O15 81.55(8) . 7_575 ? O13 Eu1 O15 84.80(9) . 7_575 ? O8 Eu1 O15 137.46(9) . 7_575 ? O8 Eu1 O15 73.25(9) 7_575 7_575 ? O14 Eu1 O15 81.55(8) . . ? O13 Eu1 O15 84.80(9) . . ? O8 Eu1 O15 73.25(9) . . ? O8 Eu1 O15 137.46(9) 7_575 . ? O15 Eu1 O15 141.73(15) 7_575 . ? O14 Eu1 O12 68.68(12) . . ? O13 Eu1 O12 68.62(13) . . ? O8 Eu1 O12 129.50(9) . . ? O8 Eu1 O12 129.50(9) 7_575 . ? O15 Eu1 O12 70.95(8) 7_575 . ? O15 Eu1 O12 70.95(8) . . ? O14 Eu1 O9 76.68(8) . . ? O13 Eu1 O9 136.32(7) . . ? O8 Eu1 O9 64.10(7) . . ? O8 Eu1 O9 97.88(7) 7_575 . ? O15 Eu1 O9 134.85(10) 7_575 . ? O15 Eu1 O9 72.88(10) . . ? O12 Eu1 O9 132.61(8) . . ? O14 Eu1 O9 76.68(8) . 7_575 ? O13 Eu1 O9 136.32(7) . 7_575 ? O8 Eu1 O9 97.88(7) . 7_575 ? O8 Eu1 O9 64.10(7) 7_575 7_575 ? O15 Eu1 O9 72.88(10) 7_575 7_575 ? O15 Eu1 O9 134.85(10) . 7_575 ? O12 Eu1 O9 132.61(8) . 7_575 ? O9 Eu1 O9 63.88(9) . 7_575 ? O14 Eu1 Cu1 152.69(8) . . ? O13 Eu1 Cu1 70.01(9) . . ? O8 Eu1 Cu1 32.85(5) . . ? O8 Eu1 Cu1 32.85(5) 7_575 . ? O15 Eu1 Cu1 105.37(7) 7_575 . ? O15 Eu1 Cu1 105.37(7) . . ? O12 Eu1 Cu1 138.63(10) . . ? O9 Eu1 Cu1 80.21(5) . . ? O9 Eu1 Cu1 80.21(5) 7_575 . ? O14 Eu1 Cu3 76.54(8) . . ? O13 Eu1 Cu3 146.15(9) . . ? O8 Eu1 Cu3 77.91(5) . . ? O8 Eu1 Cu3 77.91(5) 7_575 . ? O15 Eu1 Cu3 104.52(8) 7_575 . ? O15 Eu1 Cu3 104.52(8) . . ? O12 Eu1 Cu3 145.22(10) . . ? O9 Eu1 Cu3 32.02(5) . . ? O9 Eu1 Cu3 32.02(5) 7_575 . ? Cu1 Eu1 Cu3 76.148(12) . . ? O14 Eu1 Cu2 108.45(6) . . ? O13 Eu1 Cu2 104.96(7) . . ? O8 Eu1 Cu2 31.56(5) . . ? O8 Eu1 Cu2 79.24(5) 7_575 . ? O15 Eu1 Cu2 146.93(8) 7_575 . ? O15 Eu1 Cu2 71.28(8) . . ? O12 Eu1 Cu2 142.109(8) . . ? O9 Eu1 Cu2 32.59(5) . . ? O9 Eu1 Cu2 78.84(5) 7_575 . ? Cu1 Eu1 Cu2 52.175(8) . . ? Cu3 Eu1 Cu2 50.943(8) . . ? C2 N1 C3 125.7(3) . . ? C2 N2 C1 123.1(3) . . ? C2 N2 C4 117.9(3) . . ? C1 N2 C4 118.9(3) . . ? C3 N3 C1 123.6(3) . . ? C3 N3 C7 117.3(3) . . ? C1 N3 C7 118.9(3) . . ? O16 N4 O18 126.5(5) . . ? O16 N4 O17 117.2(4) . . ? O18 N4 O17 116.3(4) . . ? O1 C1 N3 122.6(3) . . ? O1 C1 N2 121.7(3) . . ? N3 C1 N2 115.8(3) . . ? O2 C2 N1 122.4(3) . . ? O2 C2 N2 121.5(3) . . ? N1 C2 N2 116.1(3) . . ? O3 C3 N1 122.5(3) . . ? O3 C3 N3 122.4(3) . . ? N1 C3 N3 115.1(3) . . ? N2 C4 C5 113.1(3) . . ? C6 C5 C4 115.6(3) . . ? O5 C6 O4 126.5(3) . . ? O5 C6 C5 115.4(3) . . ? O4 C6 C5 118.2(3) . . ? N3 C7 C8 112.9(3) . . ? C9 C8 C7 116.3(3) . . ? O6 C9 O7 126.0(3) . . ? O6 C9 C8 118.8(3) . . ? O7 C9 C8 115.2(3) . . ? C6 O4 Cu2 129.5(2) . . ? C6 O5 Cu1 127.96(19) . . ? C9 O6 Cu2 130.9(2) . . ? C9 O7 Cu3 124.88(19) . . ? Cu2 O8 Cu1 104.87(10) . . ? Cu2 O8 Eu1 107.57(9) . . ? Cu1 O8 Eu1 104.68(9) . . ? Cu3 O9 Cu2 101.87(9) . . ? Cu3 O9 Eu1 105.48(9) . . ? Cu2 O9 Eu1 105.00(8) . . ? N4 O17 Cu3 121.0(2) . . ? O5 Cu1 O5 87.82(13) . 7_575 ? O5 Cu1 O8 176.79(9) . 7_575 ? O5 Cu1 O8 93.55(9) 7_575 7_575 ? O5 Cu1 O8 93.55(9) . . ? O5 Cu1 O8 176.79(9) 7_575 . ? O8 Cu1 O8 84.93(13) 7_575 . ? O5 Cu1 O11 91.03(9) . . ? O5 Cu1 O11 91.03(9) 7_575 . ? O8 Cu1 O11 91.84(9) 7_575 . ? O8 Cu1 O11 91.84(9) . . ? O5 Cu1 Eu1 136.00(7) . . ? O5 Cu1 Eu1 136.00(7) 7_575 . ? O8 Cu1 Eu1 42.47(7) 7_575 . ? O8 Cu1 Eu1 42.47(7) . . ? O11 Cu1 Eu1 91.67(8) . . ? O8 Cu2 O4 93.87(9) . . ? O8 Cu2 O6 172.96(9) . . ? O4 Cu2 O6 88.22(9) . . ? O8 Cu2 O9 83.21(9) . . ? O4 Cu2 O9 175.32(9) . . ? O6 Cu2 O9 94.26(9) . . ? O8 Cu2 O10 97.62(10) . . ? O4 Cu2 O10 95.19(10) . . ? O6 Cu2 O10 88.88(10) . . ? O9 Cu2 O10 88.83(10) . . ? O8 Cu2 Cu3 98.45(7) . . ? O4 Cu2 Cu3 138.92(7) . . ? O6 Cu2 Cu3 75.71(6) . . ? O9 Cu2 Cu3 38.66(6) . . ? O10 Cu2 Cu3 121.47(7) . . ? O8 Cu2 Eu1 40.87(6) . . ? O4 Cu2 Eu1 134.38(7) . . ? O6 Cu2 Eu1 135.91(6) . . ? O9 Cu2 Eu1 42.41(6) . . ? O10 Cu2 Eu1 96.33(8) . . ? Cu3 Cu2 Eu1 64.285(11) . . ? O7 Cu3 O7 87.17(14) . 7_575 ? O7 Cu3 O9 93.90(9) . . ? O7 Cu3 O9 176.16(10) 7_575 . ? O7 Cu3 O9 176.16(10) . 7_575 ? O7 Cu3 O9 93.90(9) 7_575 7_575 ? O9 Cu3 O9 84.79(12) . 7_575 ? O7 Cu3 O17 96.48(9) . . ? O7 Cu3 O17 96.48(9) 7_575 . ? O9 Cu3 O17 87.06(8) . . ? O9 Cu3 O17 87.06(8) 7_575 . ? O7 Cu3 Cu2 80.06(6) . . ? O7 Cu3 Cu2 144.35(8) 7_575 . ? O9 Cu3 Cu2 39.47(6) . . ? O9 Cu3 Cu2 101.04(7) 7_575 . ? O17 Cu3 Cu2 52.79(3) . . ? O7 Cu3 Cu2 144.35(8) . 7_575 ? O7 Cu3 Cu2 80.06(6) 7_575 7_575 ? O9 Cu3 Cu2 101.04(7) . 7_575 ? O9 Cu3 Cu2 39.47(6) 7_575 7_575 ? O17 Cu3 Cu2 52.79(3) . 7_575 ? Cu2 Cu3 Cu2 91.206(18) . 7_575 ? O7 Cu3 Eu1 136.39(7) . . ? O7 Cu3 Eu1 136.39(7) 7_575 . ? O9 Cu3 Eu1 42.50(6) . . ? O9 Cu3 Eu1 42.50(6) 7_575 . ? O17 Cu3 Eu1 82.65(7) . . ? Cu2 Cu3 Eu1 64.771(11) . . ? Cu2 Cu3 Eu1 64.771(11) 7_575 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.697 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.098