# Supplementary Material (ESI) for Chemical Science # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address S.K.Langley ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; L.Ungur ; Department of quantum and physical chemistry, Katholieke Universiteit Leuven, Celestijnenlaan 200F, 3001 Heverlee, Belgium ; N.F.Chilton ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; B.Moubaraki ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; L.F.Chibotaru ; Department of quantum and physical chemistry, Katholieke Universiteit Leuven, Celestijnenlaan 200F, 3001 Heverlee, Belgium ; ; K.S.Murray ; ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; _publ_contact_author_address ; School of Chemistry, 171 Monash university, Vic 3800, Australia ; _publ_contact_author_email Keith.murray@sci.monash.edu.au _publ_contact_author_fax +61-3-9905-4597 _publ_contact_author_phone +61-3-9905-4512 #========================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Keith. S. Murray' _publ_contact_letter ; ; _publ_requested_category ? _publ_section_title ; Structure, magnetism and theory of a nonanuclear family of CuII5LnIII4 triethanolamine clusters displaying single molecule magnet behaviour. ; data_Cu5Gd4final _database_code_depnum_ccdc_archive 'CCDC 809026' #TrackingRef '- 1 Cu5Gd4final.CIF' #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; The crystal was run on the Australian synchrotron in which We were restricted to only one 185 degree phi scan. The asymmetric unit contains half the cluster which lies upon an inversion centre as well as solvent MeOH and Et2O molecules. All non H-atoms are refined anisotropically and H-atoms are placed in calculated positions. ; _publ_section_references ;Bruker (1997) SMART (Version 5.054) and SAINT-Plus (Version 6.45). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2001) XCIF (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA. Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M., Macrae, C. F., McCabe, P., Pearson, J. and Taylor, R. (2002) Acta Cryst., B58, 389--397. Farrugia, L. J. (1997) J. Appl. Cryst., 30, 565--565. Sheldrick, G. M. (1990) Acta Cryst., A46, 467--473. Sheldrick, G. M. (1997) SHELXL97., University of Gottingen, Germany. Sheldrick, G. M. (1996) SADABS., University of Gottingen, Germany. ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H82 Cu5 Gd4 N8 O34, 2(C4 H10 O), 2(C H4 O)' _chemical_formula_sum 'C48 H110 Cu5 Gd4 N8 O38' _chemical_formula_weight 2354.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.050(2) _cell_length_b 13.830(3) _cell_length_c 14.030(3) _cell_angle_alpha 78.80(3) _cell_angle_beta 83.81(3) _cell_angle_gamma 69.28(3) _cell_volume 1965.4(8) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12139 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.989 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1159 _exptl_absorpt_coefficient_mu 4.737 _exptl_absorpt_correction_type MULTi-scan _exptl_absorpt_correction_T_min 0.786 _exptl_absorpt_correction_T_max 0.899 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71082 _diffrn_radiation_type synchrotron _diffrn_radiation_source '3BM1 dipole' _diffrn_radiation_monochromator 'double crystal' _diffrn_measurement_device_type synchrotron _diffrn_measurement_method 'scans in phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12139 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7056 _reflns_number_gt 6876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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. The crystal was run on the Australian synchrotron in which We were restricted to only one 185 degree phi scan. The asymmetric unit contains half the cluster which lies upon an inversion centre as well as solvent MeOH and Et2O molecules. All non H-atoms are refined anisotropically and H-atoms are placed in calculated positions. ; _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^)+(0.0000P)^2^+20.5732P] 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 7056 _refine_ls_number_parameters 477 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0999 _refine_ls_wR_factor_gt 0.0992 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _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 0.16746(3) 0.47562(2) 0.30188(2) 0.00891(11) Uani 1 1 d . . . Gd2 Gd 0.13931(3) 0.67966(2) 0.45069(2) 0.01088(11) Uani 1 1 d . . . Cu1 Cu 0.0000 0.5000 0.5000 0.0076(2) Uani 1 2 d S . . Cu2 Cu 0.09850(7) 0.58197(6) 0.68482(5) 0.01224(18) Uani 1 1 d . . . Cu3 Cu -0.14134(7) 0.74542(6) 0.57703(6) 0.01054(18) Uani 1 1 d . . . O1 O -0.0180(4) 0.6035(3) 0.5833(3) 0.0110(9) Uani 1 1 d . . . O2 O 0.0045(4) 0.6058(3) 0.3837(3) 0.0106(9) Uani 1 1 d . . . O3 O 0.2343(4) 0.5041(3) 0.4408(3) 0.0147(9) Uani 1 1 d . . . O4 O 0.2700(5) 0.4205(4) 0.1422(4) 0.0197(10) Uani 1 1 d . . . O5 O 0.4032(4) 0.4375(4) 0.2354(3) 0.0172(10) Uani 1 1 d . . . O6 O 0.4767(5) 0.3737(5) 0.1022(4) 0.0276(12) Uani 1 1 d . . . O7 O 0.1803(6) 0.6303(4) 0.2116(5) 0.0406(17) Uani 1 1 d . . . O8 O 0.1322(6) 0.7670(5) 0.2880(4) 0.0359(14) Uani 1 1 d . . . O9 O 0.3665(5) 0.6782(4) 0.4157(5) 0.0295(13) Uani 1 1 d . . . O10 O 0.2289(5) 0.8221(4) 0.4517(4) 0.0243(11) Uani 1 1 d . . . O11 O 0.4318(6) 0.8049(5) 0.4321(6) 0.0478(19) Uani 1 1 d . . . O12 O -0.0468(4) 0.8090(3) 0.4770(3) 0.0159(10) Uani 1 1 d . . . O13 O -0.0622(5) 0.7740(4) 0.7215(4) 0.0257(11) Uani 1 1 d . . . H13 H -0.0818 0.7616 0.7810 0.031 Uiso 1 1 calc R . . O14 O -0.2717(4) 0.6977(3) 0.6505(3) 0.0148(9) Uani 1 1 d . . . O15 O 0.0016(4) 0.5168(4) 0.7796(3) 0.0165(10) Uani 1 1 d . . . O16 O 0.2033(5) 0.6521(4) 0.6041(3) 0.0186(10) Uani 1 1 d . . . O17 O 0.3899(6) 0.3465(4) 0.9317(4) 0.0329(13) Uani 1 1 d . . . H17 H 0.4431 0.3229 0.9761 0.040 Uiso 1 1 calc R . . O1S O 0.5928(14) 0.9838(11) 0.2131(10) 0.119(5) Uani 1 1 d . . . O2S O -0.1850(6) 0.7395(5) 0.8967(4) 0.0384(15) Uani 1 1 d . . . H2S H -0.2141 0.6899 0.9042 0.046 Uiso 1 1 calc R . . N1 N 0.3863(5) 0.4104(4) 0.1591(4) 0.0159(12) Uani 1 1 d . . . N2 N 0.3441(6) 0.7690(5) 0.4336(5) 0.0279(15) Uani 1 1 d . . . N3 N -0.2651(5) 0.8920(4) 0.5795(4) 0.0144(11) Uani 1 1 d . . . N4 N 0.2231(5) 0.5533(5) 0.7885(4) 0.0185(12) Uani 1 1 d . . . C1 C -0.1161(6) 0.6707(5) 0.3438(5) 0.0167(14) Uani 1 1 d . . . H1A H -0.1537 0.6283 0.3163 0.025 Uiso 1 1 calc R . . H1B H -0.1027 0.7256 0.2924 0.025 Uiso 1 1 calc R . . H1C H -0.1752 0.7032 0.3950 0.025 Uiso 1 1 calc R . . C2 C 0.3522(7) 0.4405(6) 0.4843(5) 0.0206(15) Uani 1 1 d . . . H2A H 0.3830 0.3726 0.4621 0.031 Uiso 1 1 calc R . . H2B H 0.3384 0.4298 0.5552 0.031 Uiso 1 1 calc R . . H2C H 0.4168 0.4752 0.4658 0.031 Uiso 1 1 calc R . . C3 C 0.1511(6) 0.7278(6) 0.2128(6) 0.0210(15) Uani 1 1 d . A . C4 C 0.1352(9) 0.7980(7) 0.1119(6) 0.0322(18) Uani 1 1 d . . . C5 C 0.1142(13) 0.9088(9) 0.1196(9) 0.061(3) Uani 1 1 d . A 1 H5A H 0.1091 0.9507 0.0543 0.091 Uiso 1 1 calc R A 1 H5B H 0.1865 0.9114 0.1526 0.091 Uiso 1 1 calc R A 1 H5C H 0.0331 0.9370 0.1570 0.091 Uiso 1 1 calc R A 1 C6 C 0.0189(15) 0.7909(11) 0.0646(10) 0.070(4) Uani 1 1 d . A 1 H6A H 0.0152 0.8263 -0.0033 0.104 Uiso 1 1 calc R A 1 H6B H -0.0615 0.8249 0.1002 0.104 Uiso 1 1 calc R A 1 H6C H 0.0295 0.7171 0.0669 0.104 Uiso 1 1 calc R A 1 C7 C 0.2549(15) 0.7552(12) 0.0484(9) 0.083(5) Uani 1 1 d . A 1 H7A H 0.2795 0.6789 0.0562 0.125 Uiso 1 1 calc R A 1 H7B H 0.3261 0.7731 0.0676 0.125 Uiso 1 1 calc R A 1 H7C H 0.2367 0.7862 -0.0198 0.125 Uiso 1 1 calc R A 1 C8 C -0.1051(7) 0.9183(5) 0.4497(5) 0.0179(14) Uani 1 1 d . . . H8A H -0.0944 0.9384 0.3785 0.021 Uiso 1 1 calc R . . H8B H -0.0633 0.9552 0.4820 0.021 Uiso 1 1 calc R . . C9 C -0.2488(7) 0.9490(5) 0.4801(5) 0.0180(14) Uani 1 1 d . . . H9A H -0.2859 1.0256 0.4796 0.022 Uiso 1 1 calc R . . H9B H -0.2955 0.9313 0.4335 0.022 Uiso 1 1 calc R . . C10 C -0.2347(8) 0.9375(5) 0.6577(6) 0.0239(16) Uani 1 1 d . . . H10A H -0.2944 0.9313 0.7146 0.029 Uiso 1 1 calc R . . H10B H -0.2508 1.0132 0.6344 0.029 Uiso 1 1 calc R . . C11 C -0.0963(8) 0.8859(6) 0.6901(6) 0.0272(17) Uani 1 1 d . . . H11A H -0.0365 0.8994 0.6356 0.033 Uiso 1 1 calc R . . H11B H -0.0851 0.9179 0.7443 0.033 Uiso 1 1 calc R . . C12 C -0.3945(7) 0.8786(5) 0.5972(6) 0.0228(16) Uani 1 1 d . . . H12A H -0.4240 0.8704 0.5360 0.027 Uiso 1 1 calc R . . H12B H -0.4587 0.9413 0.6198 0.027 Uiso 1 1 calc R . . C13 C -0.3828(7) 0.7819(5) 0.6738(6) 0.0200(15) Uani 1 1 d . . . H13A H -0.3748 0.7968 0.7386 0.024 Uiso 1 1 calc R . . H13B H -0.4613 0.7627 0.6759 0.024 Uiso 1 1 calc R . . C14 C 0.1445(8) 0.5448(7) 0.8805(5) 0.0255(16) Uani 1 1 d . . . H14A H 0.0883 0.6154 0.8926 0.031 Uiso 1 1 calc R . . H14B H 0.2019 0.5105 0.9359 0.031 Uiso 1 1 calc R . . C15 C 0.0614(7) 0.4789(6) 0.8702(5) 0.0226(16) Uani 1 1 d . . . H15A H 0.1165 0.4043 0.8737 0.027 Uiso 1 1 calc R . . H15B H -0.0055 0.4843 0.9238 0.027 Uiso 1 1 calc R . . C16 C 0.2597(7) 0.6497(6) 0.7665(6) 0.0241(16) Uani 1 1 d . . . H16A H 0.3360 0.6394 0.8034 0.029 Uiso 1 1 calc R . . H16B H 0.1872 0.7101 0.7858 0.029 Uiso 1 1 calc R . . C17 C 0.2916(8) 0.6716(7) 0.6562(5) 0.0265(17) Uani 1 1 d . . . H17A H 0.2869 0.7455 0.6365 0.032 Uiso 1 1 calc R . . H17B H 0.3808 0.6260 0.6411 0.032 Uiso 1 1 calc R . . C18 C 0.3360(7) 0.4584(6) 0.7772(6) 0.0253(16) Uani 1 1 d . . . H18A H 0.3839 0.4736 0.7156 0.030 Uiso 1 1 calc R . . H18B H 0.3036 0.4018 0.7708 0.030 Uiso 1 1 calc R . . C19 C 0.4301(8) 0.4178(6) 0.8582(6) 0.0267(16) Uani 1 1 d . . . H19A H 0.5180 0.3815 0.8320 0.032 Uiso 1 1 calc R . . H19B H 0.4330 0.4771 0.8865 0.032 Uiso 1 1 calc R . . C1S C 0.486(2) 0.8724(18) 0.184(2) 0.146(10) Uani 1 1 d . . . H1S1 H 0.4339 0.8626 0.2441 0.219 Uiso 1 1 calc R . . H1S2 H 0.5029 0.8138 0.1495 0.219 Uiso 1 1 calc R . . H1S3 H 0.4396 0.9383 0.1430 0.219 Uiso 1 1 calc R . . C2S C 0.597(2) 0.876(2) 0.2069(19) 0.146(11) Uani 1 1 d . . . H2S1 H 0.6644 0.8475 0.1573 0.175 Uiso 1 1 calc R . . H2S2 H 0.6224 0.8300 0.2702 0.175 Uiso 1 1 calc R . . C3S C 0.7042(18) 1.0011(14) 0.1915(12) 0.094(6) Uani 1 1 d . . . H3S1 H 0.7235 1.0036 0.1206 0.113 Uiso 1 1 calc R . . H3S2 H 0.7740 0.9410 0.2251 0.113 Uiso 1 1 calc R . . C4S C 0.7068(14) 1.0938(10) 0.2167(10) 0.070(4) Uani 1 1 d . . . H4S1 H 0.6563 1.1543 0.1710 0.104 Uiso 1 1 calc R . . H4S2 H 0.7965 1.0921 0.2139 0.104 Uiso 1 1 calc R . . H4S3 H 0.6693 1.0998 0.2828 0.104 Uiso 1 1 calc R . . C5S C -0.2711(12) 0.8210(9) 0.9412(8) 0.054(3) Uani 1 1 d . . . H5S1 H -0.2806 0.7957 1.0109 0.081 Uiso 1 1 calc R . . H5S2 H -0.3556 0.8454 0.9119 0.081 Uiso 1 1 calc R . . H5S3 H -0.2375 0.8791 0.9320 0.081 Uiso 1 1 calc 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 0.00881(17) 0.01166(17) 0.00805(17) -0.00346(11) 0.00282(12) -0.00565(12) Gd2 0.01062(17) 0.01135(17) 0.01375(18) -0.00469(12) 0.00241(12) -0.00698(12) Cu1 0.0093(5) 0.0088(5) 0.0063(5) -0.0024(4) 0.0020(4) -0.0052(4) Cu2 0.0106(4) 0.0194(4) 0.0098(4) -0.0045(3) 0.0002(3) -0.0081(3) Cu3 0.0095(4) 0.0091(3) 0.0140(4) -0.0037(3) 0.0038(3) -0.0045(3) O1 0.012(2) 0.012(2) 0.010(2) -0.0052(17) 0.0014(18) -0.0040(17) O2 0.011(2) 0.011(2) 0.011(2) -0.0028(17) 0.0015(18) -0.0057(17) O3 0.016(2) 0.015(2) 0.014(2) -0.0031(18) -0.0053(19) -0.0050(18) O4 0.014(2) 0.030(3) 0.020(3) -0.011(2) 0.007(2) -0.013(2) O5 0.015(2) 0.026(2) 0.015(2) -0.008(2) 0.003(2) -0.012(2) O6 0.014(2) 0.051(3) 0.023(3) -0.017(3) 0.010(2) -0.014(2) O7 0.033(3) 0.016(3) 0.058(4) 0.009(3) 0.022(3) -0.006(2) O8 0.049(4) 0.056(4) 0.017(3) -0.001(3) 0.004(3) -0.039(3) O9 0.017(3) 0.016(2) 0.052(4) -0.002(2) 0.006(3) -0.005(2) O10 0.024(3) 0.019(2) 0.035(3) -0.005(2) 0.001(2) -0.014(2) O11 0.024(3) 0.030(3) 0.093(6) 0.007(3) -0.014(3) -0.020(3) O12 0.015(2) 0.014(2) 0.020(2) -0.0037(19) 0.004(2) -0.0072(18) O13 0.025(3) 0.028(3) 0.027(3) -0.012(2) 0.002(2) -0.010(2) O14 0.010(2) 0.013(2) 0.020(2) -0.0053(18) 0.0033(19) -0.0025(17) O15 0.014(2) 0.030(3) 0.007(2) -0.0025(19) -0.0010(19) -0.010(2) O16 0.016(2) 0.035(3) 0.012(2) -0.003(2) -0.003(2) -0.017(2) O17 0.041(3) 0.032(3) 0.031(3) 0.003(2) -0.010(3) -0.020(3) O1S 0.130(11) 0.116(9) 0.134(11) -0.067(9) 0.073(9) -0.069(9) O2S 0.049(4) 0.050(4) 0.034(3) -0.018(3) 0.010(3) -0.036(3) N1 0.010(3) 0.024(3) 0.017(3) -0.009(2) 0.005(2) -0.008(2) N2 0.016(3) 0.022(3) 0.048(4) 0.002(3) -0.009(3) -0.011(3) N3 0.011(3) 0.010(2) 0.019(3) -0.001(2) 0.005(2) -0.002(2) N4 0.013(3) 0.024(3) 0.020(3) -0.002(2) 0.000(2) -0.009(2) C1 0.014(3) 0.017(3) 0.018(3) -0.002(3) -0.003(3) -0.004(3) C2 0.018(3) 0.022(3) 0.023(4) -0.006(3) -0.006(3) -0.006(3) C3 0.010(3) 0.026(4) 0.026(4) 0.006(3) -0.002(3) -0.010(3) C4 0.043(5) 0.034(4) 0.019(4) 0.005(3) -0.005(4) -0.017(4) C5 0.079(8) 0.047(6) 0.052(7) 0.017(5) -0.019(6) -0.025(6) C6 0.089(10) 0.069(8) 0.054(7) 0.019(6) -0.030(7) -0.039(7) C7 0.081(10) 0.096(10) 0.036(6) 0.012(6) 0.017(7) -0.003(8) C8 0.023(4) 0.015(3) 0.017(3) -0.001(3) 0.004(3) -0.010(3) C9 0.018(3) 0.011(3) 0.021(4) 0.006(3) -0.005(3) -0.003(3) C10 0.032(4) 0.011(3) 0.025(4) -0.008(3) 0.010(3) -0.004(3) C11 0.044(5) 0.025(4) 0.019(4) -0.008(3) 0.003(4) -0.019(4) C12 0.010(3) 0.017(3) 0.036(4) 0.000(3) 0.002(3) -0.002(3) C13 0.012(3) 0.017(3) 0.029(4) 0.000(3) 0.003(3) -0.005(3) C14 0.026(4) 0.044(4) 0.014(3) -0.008(3) 0.001(3) -0.019(4) C15 0.025(4) 0.042(4) 0.006(3) -0.004(3) -0.001(3) -0.018(3) C16 0.022(4) 0.036(4) 0.022(4) -0.005(3) -0.005(3) -0.019(3) C17 0.032(4) 0.041(4) 0.019(4) -0.001(3) -0.003(3) -0.029(4) C18 0.017(4) 0.032(4) 0.022(4) -0.002(3) -0.002(3) -0.004(3) C19 0.024(4) 0.033(4) 0.024(4) -0.002(3) -0.007(3) -0.011(3) C1S 0.107(15) 0.134(18) 0.21(3) -0.12(2) -0.032(16) -0.005(13) C2S 0.090(13) 0.23(3) 0.17(2) -0.16(2) 0.030(14) -0.059(16) C3S 0.112(13) 0.114(13) 0.081(10) -0.057(10) 0.050(10) -0.062(11) C4S 0.069(8) 0.055(7) 0.070(8) -0.005(6) 0.023(7) -0.014(6) C5S 0.065(7) 0.054(6) 0.050(6) -0.021(5) 0.012(6) -0.025(6) _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 O15 2.254(5) 2_566 ? Gd1 O14 2.260(5) 2_566 ? Gd1 O3 2.305(5) . ? Gd1 O7 2.306(5) . ? Gd1 O2 2.422(4) . ? Gd1 O4 2.528(5) . ? Gd1 O1 2.557(4) 2_566 ? Gd1 O5 2.574(4) . ? Gd1 N1 2.965(5) . ? Gd1 Cu2 3.2842(10) 2_566 ? Gd1 Cu3 3.2887(12) 2_566 ? Gd2 O12 2.249(5) . ? Gd2 O16 2.258(5) . ? Gd2 O3 2.305(4) . ? Gd2 O8 2.361(6) . ? Gd2 O2 2.428(4) . ? Gd2 O9 2.499(5) . ? Gd2 O10 2.501(5) . ? Gd2 O1 2.726(4) . ? Gd2 N2 2.907(6) . ? Cu1 O1 1.964(4) . ? Cu1 O1 1.964(4) 2_566 ? Cu1 O2 1.978(4) 2_566 ? Cu1 O2 1.978(4) . ? Cu1 Gd1 3.1747(10) 2_566 ? Cu1 Gd2 3.2910(9) 2_566 ? Cu2 O15 1.907(5) . ? Cu2 O16 1.910(5) . ? Cu2 O1 1.932(4) . ? Cu2 N4 1.997(6) . ? Cu2 Gd1 3.2842(10) 2_566 ? Cu3 O14 1.914(4) . ? Cu3 O12 1.920(4) . ? Cu3 O1 1.945(4) . ? Cu3 N3 2.009(5) . ? Cu3 Gd1 3.2887(13) 2_566 ? O1 Gd1 2.557(4) 2_566 ? O2 C1 1.419(8) . ? O3 C2 1.412(9) . ? O4 N1 1.286(8) . ? O5 N1 1.253(7) . ? O6 N1 1.233(7) . ? O7 C3 1.274(9) . ? O8 C3 1.243(10) . ? O9 N2 1.261(8) . ? O10 N2 1.251(8) . ? O11 N2 1.232(8) . ? O12 C8 1.409(8) . ? O13 C11 1.445(9) . ? O13 H13 0.8400 . ? O14 C13 1.421(8) . ? O14 Gd1 2.260(5) 2_566 ? O15 C15 1.417(9) . ? O15 Gd1 2.254(5) 2_566 ? O16 C17 1.405(9) . ? O17 C19 1.431(9) . ? O17 H17 0.8400 . ? O1S C3S 1.328(19) . ? O1S C2S 1.50(3) . ? O2S C5S 1.397(12) . ? O2S H2S 0.8400 . ? N3 C10 1.487(9) . ? N3 C9 1.489(9) . ? N3 C12 1.494(8) . ? N4 C18 1.478(10) . ? N4 C14 1.485(9) . ? N4 C16 1.494(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.542(10) . ? C4 C5 1.490(14) . ? C4 C7 1.513(15) . ? C4 C6 1.549(16) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.527(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.518(12) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.520(10) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.538(10) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.545(10) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.510(12) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C1S C2S 1.31(3) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S C4S 1.406(19) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S3 0.9800 . ? C5S H5S1 0.9800 . ? C5S H5S2 0.9800 . ? C5S H5S3 0.9800 . ? 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 O15 Gd1 O14 104.46(17) 2_566 2_566 ? O15 Gd1 O3 146.44(16) 2_566 . ? O14 Gd1 O3 87.97(17) 2_566 . ? O15 Gd1 O7 92.9(2) 2_566 . ? O14 Gd1 O7 146.30(17) 2_566 . ? O3 Gd1 O7 93.2(2) . . ? O15 Gd1 O2 83.71(16) 2_566 . ? O14 Gd1 O2 131.81(15) 2_566 . ? O3 Gd1 O2 65.47(16) . . ? O7 Gd1 O2 77.95(17) . . ? O15 Gd1 O4 76.34(16) 2_566 . ? O14 Gd1 O4 78.78(17) 2_566 . ? O3 Gd1 O4 137.15(16) . . ? O7 Gd1 O4 77.6(2) . . ? O2 Gd1 O4 147.38(16) . . ? O15 Gd1 O1 70.26(15) 2_566 2_566 ? O14 Gd1 O1 70.38(14) 2_566 2_566 ? O3 Gd1 O1 85.51(14) . 2_566 ? O7 Gd1 O1 143.31(17) . 2_566 ? O2 Gd1 O1 68.20(13) . 2_566 ? O4 Gd1 O1 126.04(14) . 2_566 ? O15 Gd1 O5 126.41(15) 2_566 . ? O14 Gd1 O5 73.47(16) 2_566 . ? O3 Gd1 O5 86.85(15) . . ? O7 Gd1 O5 72.98(18) . . ? O2 Gd1 O5 138.31(14) . . ? O4 Gd1 O5 50.35(15) . . ? O1 Gd1 O5 143.25(15) 2_566 . ? O15 Gd1 N1 101.84(16) 2_566 . ? O14 Gd1 N1 73.24(16) 2_566 . ? O3 Gd1 N1 111.63(16) . . ? O7 Gd1 N1 75.07(18) . . ? O2 Gd1 N1 152.66(15) . . ? O4 Gd1 N1 25.52(16) . . ? O1 Gd1 N1 138.99(14) 2_566 . ? O5 Gd1 N1 24.90(15) . . ? O15 Gd1 Cu2 34.31(11) 2_566 2_566 ? O14 Gd1 Cu2 86.63(12) 2_566 2_566 ? O3 Gd1 Cu2 118.64(11) . 2_566 ? O7 Gd1 Cu2 121.35(17) . 2_566 ? O2 Gd1 Cu2 73.97(10) . 2_566 ? O4 Gd1 Cu2 101.21(11) . 2_566 ? O1 Gd1 Cu2 35.97(10) 2_566 2_566 ? O5 Gd1 Cu2 147.38(10) . 2_566 ? N1 Gd1 Cu2 124.71(11) . 2_566 ? O15 Gd1 Cu3 84.63(13) 2_566 2_566 ? O14 Gd1 Cu3 34.43(11) 2_566 2_566 ? O3 Gd1 Cu3 89.23(11) . 2_566 ? O7 Gd1 Cu3 177.43(19) . 2_566 ? O2 Gd1 Cu3 102.49(10) . 2_566 ? O4 Gd1 Cu3 101.04(11) . 2_566 ? O1 Gd1 Cu3 36.20(9) 2_566 2_566 ? O5 Gd1 Cu3 107.90(11) . 2_566 ? N1 Gd1 Cu3 104.67(12) . 2_566 ? Cu2 Gd1 Cu3 56.62(3) 2_566 2_566 ? O12 Gd2 O16 93.89(18) . . ? O12 Gd2 O3 145.52(16) . . ? O16 Gd2 O3 91.70(18) . . ? O12 Gd2 O8 86.3(2) . . ? O16 Gd2 O8 150.38(18) . . ? O3 Gd2 O8 104.8(2) . . ? O12 Gd2 O2 85.38(15) . . ? O16 Gd2 O2 129.90(15) . . ? O3 Gd2 O2 65.35(15) . . ? O8 Gd2 O2 79.68(17) . . ? O12 Gd2 O9 131.72(16) . . ? O16 Gd2 O9 80.25(19) . . ? O3 Gd2 O9 82.75(16) . . ? O8 Gd2 O9 77.7(2) . . ? O2 Gd2 O9 134.18(17) . . ? O12 Gd2 O10 81.13(16) . . ? O16 Gd2 O10 75.70(18) . . ? O3 Gd2 O10 133.08(16) . . ? O8 Gd2 O10 75.07(19) . . ? O2 Gd2 O10 151.99(17) . . ? O9 Gd2 O10 50.85(17) . . ? O12 Gd2 O1 69.61(14) . . ? O16 Gd2 O1 67.96(14) . . ? O3 Gd2 O1 81.20(14) . . ? O8 Gd2 O1 137.97(18) . . ? O2 Gd2 O1 64.98(13) . . ? O9 Gd2 O1 143.70(17) . . ? O10 Gd2 O1 130.67(15) . . ? O12 Gd2 N2 106.46(17) . . ? O16 Gd2 N2 75.36(19) . . ? O3 Gd2 N2 107.88(17) . . ? O8 Gd2 N2 76.2(2) . . ? O2 Gd2 N2 152.22(18) . . ? O9 Gd2 N2 25.56(18) . . ? O10 Gd2 N2 25.35(18) . . ? O1 Gd2 N2 142.52(17) . . ? O1 Cu1 O1 180.000(1) . 2_566 ? O1 Cu1 O2 90.29(17) . 2_566 ? O1 Cu1 O2 89.71(17) 2_566 2_566 ? O1 Cu1 O2 89.71(17) . . ? O1 Cu1 O2 90.29(17) 2_566 . ? O2 Cu1 O2 180.00(19) 2_566 . ? O1 Cu1 Gd1 53.62(12) . 2_566 ? O1 Cu1 Gd1 126.38(12) 2_566 2_566 ? O2 Cu1 Gd1 49.69(12) 2_566 2_566 ? O2 Cu1 Gd1 130.31(12) . 2_566 ? O1 Cu1 Gd2 124.15(12) . 2_566 ? O1 Cu1 Gd2 55.85(12) 2_566 2_566 ? O2 Cu1 Gd2 47.20(12) 2_566 2_566 ? O2 Cu1 Gd2 132.80(12) . 2_566 ? Gd1 Cu1 Gd2 70.54(3) 2_566 2_566 ? O15 Cu2 O16 172.4(2) . . ? O15 Cu2 O1 92.77(19) . . ? O16 Cu2 O1 94.11(19) . . ? O15 Cu2 N4 87.0(2) . . ? O16 Cu2 N4 86.3(2) . . ? O1 Cu2 N4 177.5(2) . . ? O15 Cu2 Gd1 41.76(14) . 2_566 ? O16 Cu2 Gd1 144.85(15) . 2_566 ? O1 Cu2 Gd1 51.04(12) . 2_566 ? N4 Cu2 Gd1 128.75(16) . 2_566 ? O14 Cu3 O12 164.0(2) . . ? O14 Cu3 O1 92.48(18) . . ? O12 Cu3 O1 95.75(18) . . ? O14 Cu3 N3 87.1(2) . . ? O12 Cu3 N3 85.6(2) . . ? O1 Cu3 N3 176.1(2) . . ? O14 Cu3 Gd1 41.90(14) . 2_566 ? O12 Cu3 Gd1 145.98(14) . 2_566 ? O1 Cu3 Gd1 50.95(12) . 2_566 ? N3 Cu3 Gd1 128.09(15) . 2_566 ? Cu2 O1 Cu3 107.05(19) . . ? Cu2 O1 Cu1 123.9(2) . . ? Cu3 O1 Cu1 128.9(2) . . ? Cu2 O1 Gd1 92.99(16) . 2_566 ? Cu3 O1 Gd1 92.85(15) . 2_566 ? Cu1 O1 Gd1 88.20(14) . 2_566 ? Cu2 O1 Gd2 90.23(15) . . ? Cu3 O1 Gd2 89.02(15) . . ? Cu1 O1 Gd2 87.56(14) . . ? Gd1 O1 Gd2 175.63(17) 2_566 . ? C1 O2 Cu1 117.0(4) . . ? C1 O2 Gd1 123.6(4) . . ? Cu1 O2 Gd1 91.80(16) . . ? C1 O2 Gd2 121.0(3) . . ? Cu1 O2 Gd2 96.11(18) . . ? Gd1 O2 Gd2 100.70(15) . . ? C2 O3 Gd1 123.5(4) . . ? C2 O3 Gd2 122.6(4) . . ? Gd1 O3 Gd2 108.21(19) . . ? N1 O4 Gd1 96.6(3) . . ? N1 O5 Gd1 95.2(3) . . ? C3 O7 Gd1 143.5(5) . . ? C3 O8 Gd2 127.7(5) . . ? N2 O9 Gd2 95.6(4) . . ? N2 O10 Gd2 95.8(4) . . ? C8 O12 Cu3 114.7(4) . . ? C8 O12 Gd2 139.6(4) . . ? Cu3 O12 Gd2 105.4(2) . . ? C11 O13 H13 109.5 . . ? C13 O14 Cu3 112.3(4) . . ? C13 O14 Gd1 141.7(4) . 2_566 ? Cu3 O14 Gd1 103.67(19) . 2_566 ? C15 O15 Cu2 112.5(4) . . ? C15 O15 Gd1 143.5(4) . 2_566 ? Cu2 O15 Gd1 103.9(2) . 2_566 ? C17 O16 Cu2 113.3(4) . . ? C17 O16 Gd2 140.2(4) . . ? Cu2 O16 Gd2 106.6(2) . . ? C19 O17 H17 109.5 . . ? C3S O1S C2S 115.3(14) . . ? C5S O2S H2S 109.5 . . ? O6 N1 O5 122.2(5) . . ? O6 N1 O4 120.2(5) . . ? O5 N1 O4 117.5(5) . . ? O6 N1 Gd1 173.8(5) . . ? O5 N1 Gd1 59.9(3) . . ? O4 N1 Gd1 57.9(3) . . ? O11 N2 O10 121.1(6) . . ? O11 N2 O9 121.5(7) . . ? O10 N2 O9 117.4(6) . . ? O11 N2 Gd2 176.3(7) . . ? O10 N2 Gd2 58.9(3) . . ? O9 N2 Gd2 58.8(3) . . ? C10 N3 C9 113.2(5) . . ? C10 N3 C12 112.1(5) . . ? C9 N3 C12 112.5(6) . . ? C10 N3 Cu3 110.9(4) . . ? C9 N3 Cu3 103.8(4) . . ? C12 N3 Cu3 103.6(4) . . ? C18 N4 C14 114.7(6) . . ? C18 N4 C16 111.4(6) . . ? C14 N4 C16 114.2(6) . . ? C18 N4 Cu2 109.9(5) . . ? C14 N4 Cu2 104.0(4) . . ? C16 N4 Cu2 101.4(4) . . ? O2 C1 H1A 109.5 . . ? O2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O3 C2 H2A 109.5 . . ? O3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O8 C3 O7 124.4(7) . . ? O8 C3 C4 120.6(7) . . ? O7 C3 C4 115.0(7) . . ? C5 C4 C7 110.4(10) . . ? C5 C4 C3 111.2(7) . . ? C7 C4 C3 108.9(8) . . ? C5 C4 C6 110.5(9) . . ? C7 C4 C6 107.5(10) . . ? C3 C4 C6 108.2(7) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? O12 C8 C9 108.5(5) . . ? O12 C8 H8A 110.0 . . ? C9 C8 H8A 110.0 . . ? O12 C8 H8B 110.0 . . ? C9 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? N3 C9 C8 109.7(6) . . ? N3 C9 H9A 109.7 . . ? C8 C9 H9A 109.7 . . ? N3 C9 H9B 109.7 . . ? C8 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? N3 C10 C11 114.0(5) . . ? N3 C10 H10A 108.8 . . ? C11 C10 H10A 108.8 . . ? N3 C10 H10B 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.6 . . ? O13 C11 C10 112.6(6) . . ? O13 C11 H11A 109.1 . . ? C10 C11 H11A 109.1 . . ? O13 C11 H11B 109.1 . . ? C10 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? N3 C12 C13 108.8(6) . . ? N3 C12 H12A 109.9 . . ? C13 C12 H12A 109.9 . . ? N3 C12 H12B 109.9 . . ? C13 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? O14 C13 C12 109.2(5) . . ? O14 C13 H13A 109.8 . . ? C12 C13 H13A 109.8 . . ? O14 C13 H13B 109.8 . . ? C12 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? N4 C14 C15 107.8(6) . . ? N4 C14 H14A 110.2 . . ? C15 C14 H14A 110.2 . . ? N4 C14 H14B 110.2 . . ? C15 C14 H14B 110.2 . . ? H14A C14 H14B 108.5 . . ? O15 C15 C14 108.8(6) . . ? O15 C15 H15A 109.9 . . ? C14 C15 H15A 109.9 . . ? O15 C15 H15B 109.9 . . ? C14 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? N4 C16 C17 108.6(6) . . ? N4 C16 H16A 110.0 . . ? C17 C16 H16A 110.0 . . ? N4 C16 H16B 110.0 . . ? C17 C16 H16B 110.0 . . ? H16A C16 H16B 108.4 . . ? O16 C17 C16 109.9(5) . . ? O16 C17 H17A 109.7 . . ? C16 C17 H17A 109.7 . . ? O16 C17 H17B 109.7 . . ? C16 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? N4 C18 C19 116.2(7) . . ? N4 C18 H18A 108.2 . . ? C19 C18 H18A 108.2 . . ? N4 C18 H18B 108.2 . . ? C19 C18 H18B 108.2 . . ? H18A C18 H18B 107.4 . . ? O17 C19 C18 109.5(6) . . ? O17 C19 H19A 109.8 . . ? C18 C19 H19A 109.8 . . ? O17 C19 H19B 109.8 . . ? C18 C19 H19B 109.8 . . ? H19A C19 H19B 108.2 . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C1S C2S O1S 114(2) . . ? C1S C2S H2S1 108.8 . . ? O1S C2S H2S1 108.8 . . ? C1S C2S H2S2 108.8 . . ? O1S C2S H2S2 108.8 . . ? H2S1 C2S H2S2 107.7 . . ? O1S C3S C4S 114.8(13) . . ? O1S C3S H3S1 108.6 . . ? C4S C3S H3S1 108.6 . . ? O1S C3S H3S2 108.6 . . ? C4S C3S H3S2 108.6 . . ? H3S1 C3S H3S2 107.6 . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? O2S C5S H5S1 109.5 . . ? O2S C5S H5S2 109.5 . . ? H5S1 C5S H5S2 109.5 . . ? O2S C5S H5S3 109.5 . . ? H5S1 C5S H5S3 109.5 . . ? H5S2 C5S H5S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 1.095 _refine_diff_density_min -1.331 _refine_diff_density_rms 0.153