Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' # Attachment 'CiffileB716098D.cif' _journal_coden_Cambridge 0222 _publ_contact_author ; Dr Jean-Pierre Costes Laboratoire de Chimie de Coordination du CNRS 205 Route de Narbonne 31077 Toulouse Cedex 4 France ; _publ_contact_author_phone '(33) 0561333152' _publ_contact_author_fax '(33) 0561553003' _publ_contact_author_email costes@lcc-toulouse.fr _publ_requested_coeditor_name ? #_publ_referenced_number ' ' _publ_section_title ; Tetranuclear [Cu-Ln]2 Single Molecule Magnets: Synthsis, ... ; loop_ _publ_author_name _publ_author_address J.-P.Costes ; Laboratoire de Chimie de Coordination du CNRS 205 Route de Narbonne 31077 Toulouse Cedex 4 France ; S.Shova ; Department of Chemistry Moldova State University A. Mateevici str. 60 2009 Chisinau Moldova ; W.Wernsdorfer ; Institut N\'eel et UJF BP 166 38042 Grenoble Cedex 9 France ; _publ_contact_author_name 'Dr Jean-Pierre Costes' data_[LCuDy(hfa)2(dmf)2]2 _database_code_depnum_ccdc_archive 'CCDC 611028' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H33 Cu Dy F12 N4 O9' _chemical_formula_sum 'C34 H33 Cu Dy F12 N4 O9' _chemical_formula_weight 1095.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.193(3) _cell_length_b 16.971(3) _cell_length_c 17.553(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.67(3) _cell_angle_gamma 90.00 _cell_volume 4090.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 3890 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 30.1 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 2.443 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5727 _exptl_absorpt_correction_T_max 0.7354 _exptl_absorpt_process_details 'c.f. r.h. blessing, acta cryst. (1995), a51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Oxford Difraction, XCALIBUR' _diffrn_measurement_method omega-phi _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28585 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8028 _reflns_number_gt 6602 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0677P)^2^+11.5000P] 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 8028 _refine_ls_number_parameters 581 _refine_ls_number_restraints 94 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1226 _refine_ls_wR_factor_gt 0.1172 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.021508(17) 0.612326(13) 0.697922(13) 0.01999(10) Uani 1 1 d . . . Cu1 Cu 0.11142(4) 0.64677(4) 0.54538(3) 0.02037(15) Uani 1 1 d . . . F1 F -0.0691(9) 0.9345(7) 0.7636(7) 0.0717(17) Uiso 0.490(11) 1 d P A 1 F2 F 0.0132(8) 0.9144(7) 0.6814(8) 0.0717(17) Uiso 0.490(11) 1 d P A 1 F3 F -0.1307(10) 0.8754(7) 0.6471(7) 0.0717(17) Uiso 0.490(11) 1 d P A 1 F4* F -0.0871(8) 0.8903(6) 0.6393(6) 0.064(3) Uani 0.510(11) 1 d PU A 2 F5* F 0.0225(8) 0.9332(6) 0.7294(7) 0.073(3) Uani 0.510(11) 1 d PU A 2 F6* F -0.1219(7) 0.9164(5) 0.7464(5) 0.048(2) Uani 0.510(11) 1 d PU A 2 F5 F 0.1020(3) 0.6758(3) 0.9850(2) 0.0542(11) Uani 1 1 d . A . F4 F -0.0501(4) 0.6519(3) 0.9549(3) 0.0666(13) Uani 1 1 d . A . F6 F 0.0023(3) 0.7686(2) 0.9850(2) 0.0523(10) Uani 1 1 d . A . F7 F -0.1001(6) 0.3771(4) 0.8330(4) 0.0798(12) Uani 0.76 1 d PDU B 1 F8 F -0.1837(5) 0.4483(4) 0.8955(4) 0.0724(11) Uani 0.76 1 d PDU B 1 F9 F -0.0338(5) 0.4541(5) 0.9189(4) 0.0767(12) Uani 0.76 1 d PDU B 1 F1* F -0.0396(14) 0.3931(11) 0.8693(14) 0.0717(17) Uiso 0.24 1 d PD B 2 F2* F -0.0735(16) 0.4766(13) 0.9332(10) 0.0717(17) Uiso 0.24 1 d PD B 2 F3* F -0.1926(13) 0.4071(13) 0.8581(14) 0.0717(17) Uiso 0.24 1 d PD B 2 F10 F -0.2960(9) 0.7273(9) 0.6620(9) 0.146(7) Uani 0.64 1 d P B 1 F11 F -0.3432(6) 0.6748(6) 0.7553(4) 0.076(3) Uani 0.64 1 d P B 1 F12 F -0.3670(8) 0.6181(7) 0.6400(10) 0.136(7) Uani 0.64 1 d P B 1 F7* F -0.3684(12) 0.6323(10) 0.7345(11) 0.0717(17) Uiso 0.36 1 d P B 2 F8* F -0.2884(13) 0.7324(11) 0.7088(10) 0.0717(17) Uiso 0.36 1 d P B 2 F9* F -0.3477(15) 0.6530(13) 0.6307(12) 0.0717(17) Uiso 0.36 1 d P B 2 O1 O -0.0175(2) 0.6499(2) 0.56172(19) 0.0199(7) Uani 1 1 d . . . O2 O 0.1554(2) 0.6633(2) 0.65911(19) 0.0218(7) Uani 1 1 d . . . O3 O -0.0167(3) 0.4982(2) 0.3684(2) 0.0262(8) Uani 1 1 d . . . O4 O -0.0024(3) 0.7553(2) 0.6980(2) 0.0289(8) Uani 1 1 d . . . O5 O 0.0383(3) 0.6580(2) 0.8277(2) 0.0326(9) Uani 1 1 d . . . O6 O -0.0422(3) 0.5145(2) 0.7733(2) 0.0306(8) Uani 1 1 d . . . O7 O -0.1439(3) 0.6366(2) 0.6884(2) 0.0328(9) Uani 1 1 d . . . O8 O 0.0941(3) 0.7824(3) 0.5024(3) 0.0423(11) Uani 1 1 d . . . O9 O 0.1580(3) 0.5456(2) 0.7806(2) 0.0272(8) Uani 1 1 d . . . N1 N 0.0765(3) 0.5880(2) 0.4486(2) 0.0207(9) Uani 1 1 d . . . N2 N 0.2438(3) 0.6409(3) 0.5330(2) 0.0233(9) Uani 1 1 d . . . N3 N -0.0197(6) 0.8734(5) 0.4529(5) 0.0737(14) Uani 1 1 d U . . N4 N 0.2122(4) 0.4516(3) 0.8725(3) 0.0337(11) Uani 1 1 d . . . C1 C -0.0980(4) 0.6312(3) 0.5052(3) 0.0217(10) Uani 1 1 d . . . C2 C -0.1871(4) 0.6613(3) 0.5114(3) 0.0285(12) Uani 1 1 d . . . H1 H -0.1884 0.6966 0.5517 0.034 Uiso 1 1 d R . . C3 C -0.2724(4) 0.6398(4) 0.4598(3) 0.0350(13) Uani 1 1 d . . . H2 H -0.3308 0.6604 0.4658 0.042 Uiso 1 1 d R . . C4 C -0.2734(4) 0.5875(4) 0.3983(3) 0.0340(13) Uani 1 1 d . . . H3 H -0.3318 0.5720 0.3641 0.041 Uiso 1 1 d R . . C5 C -0.1855(4) 0.5596(3) 0.3892(3) 0.0272(12) Uani 1 1 d . . . H4 H -0.1857 0.5248 0.3482 0.033 Uiso 1 1 d R . . C6 C -0.0967(4) 0.5820(3) 0.4396(3) 0.0213(10) Uani 1 1 d . . . C7 C -0.0078(4) 0.5535(3) 0.4190(3) 0.0211(10) Uani 1 1 d . . . C8 C 0.1617(4) 0.5571(3) 0.4261(3) 0.0269(11) Uani 1 1 d . . . H5 H 0.1467 0.5508 0.3693 0.032 Uiso 1 1 d R . . H6 H 0.1787 0.5059 0.4501 0.032 Uiso 1 1 d R . . C9 C 0.2477(4) 0.6140(3) 0.4530(3) 0.0272(12) Uani 1 1 d . . . C10 C 0.3411(4) 0.5699(4) 0.4522(4) 0.0377(14) Uani 1 1 d . . . H7 H 0.3953 0.6056 0.4658 0.057 Uiso 1 1 d R . . H8 H 0.3361 0.5489 0.4005 0.057 Uiso 1 1 d R . . H9 H 0.3509 0.5277 0.4897 0.057 Uiso 1 1 d R . . C11 C 0.2331(5) 0.6864(4) 0.4000(3) 0.0374(14) Uani 1 1 d . . . H10 H 0.1727 0.7115 0.4006 0.056 Uiso 1 1 d R . . H11 H 0.2318 0.6708 0.3472 0.056 Uiso 1 1 d R . . H12 H 0.2858 0.7227 0.4189 0.056 Uiso 1 1 d R . . C12 C 0.3188(4) 0.6643(3) 0.5832(3) 0.0299(12) Uani 1 1 d . . . H13 H 0.3775 0.6623 0.5690 0.036 Uiso 1 1 d R . . C13 C 0.3217(4) 0.6943(3) 0.6617(3) 0.0284(12) Uani 1 1 d . . . C14 C 0.4100(4) 0.7281(4) 0.7049(4) 0.0413(15) Uani 1 1 d . . . H14 H 0.4624 0.7302 0.6822 0.050 Uiso 1 1 d R . . C15 C 0.4209(5) 0.7581(4) 0.7788(4) 0.0453(16) Uani 1 1 d . . . H15 H 0.4793 0.7811 0.8058 0.054 Uiso 1 1 d R . . C16 C 0.3427(5) 0.7532(3) 0.8133(3) 0.0360(14) Uani 1 1 d . . . H16 H 0.3497 0.7722 0.8641 0.043 Uiso 1 1 d R . . C17 C 0.2555(4) 0.7211(3) 0.7731(3) 0.0278(12) Uani 1 1 d . . . H17 H 0.2047 0.7183 0.7977 0.033 Uiso 1 1 d R . . C18 C 0.2415(4) 0.6919(3) 0.6966(3) 0.0229(11) Uani 1 1 d . . . C19 C -0.0241(4) 0.8008(3) 0.7462(3) 0.0308(12) Uani 1 1 d . A . C20 C -0.0552(5) 0.8835(4) 0.7138(4) 0.0412(15) Uani 1 1 d . . . C21 C -0.0211(4) 0.7881(3) 0.8250(3) 0.0317(13) Uani 1 1 d . . . H18 H -0.0411 0.8275 0.8542 0.038 Uiso 1 1 d R A . C22 C 0.0113(4) 0.7168(3) 0.8595(3) 0.0273(12) Uani 1 1 d . A . C23 C 0.0165(5) 0.7034(3) 0.9468(3) 0.0345(13) Uani 1 1 d . . . C24 C -0.1163(7) 0.5091(5) 0.7976(5) 0.0669(11) Uani 1 1 d U B . C25 C -0.1124(6) 0.4466(5) 0.8595(5) 0.0697(10) Uani 1 1 d DU . . C26 C -0.2012(5) 0.5542(4) 0.7759(4) 0.0427(16) Uani 1 1 d . . . H19 H -0.2534 0.5438 0.7974 0.051 Uiso 1 1 d R B . C27 C -0.2074(5) 0.6145(4) 0.7214(4) 0.0353(14) Uani 1 1 d . B . C28 C -0.3035(6) 0.6587(6) 0.6978(5) 0.057(2) Uani 1 1 d . . . C29 C 0.0162(5) 0.8139(3) 0.4998(4) 0.0433(16) Uani 1 1 d . . . H20 H -0.0198 0.7950 0.5334 0.052 Uiso 1 1 d R . . C30 C 0.0310(7) 0.9028(6) 0.3967(6) 0.0757(15) Uani 1 1 d U . . H21 H 0.0908 0.8743 0.4021 0.114 Uiso 1 1 d R . . H22 H 0.0450 0.9577 0.4068 0.114 Uiso 1 1 d R . . H23 H -0.0093 0.8963 0.3442 0.114 Uiso 1 1 d R . . C31 C -0.1155(7) 0.9016(6) 0.4507(6) 0.0770(15) Uani 1 1 d U . . H24 H -0.1369 0.8804 0.4942 0.115 Uiso 1 1 d R . . H25 H -0.1602 0.8864 0.4021 0.115 Uiso 1 1 d R . . H26 H -0.1132 0.9581 0.4544 0.115 Uiso 1 1 d R . . C32 C 0.1591(4) 0.5136(3) 0.8443(3) 0.0318(12) Uani 1 1 d . . . H27 H 0.1195 0.5346 0.8741 0.038 Uiso 1 1 d R . . C33 C 0.2731(6) 0.4150(5) 0.8285(4) 0.060(2) Uani 1 1 d . . . H28 H 0.2364 0.3752 0.7948 0.089 Uiso 1 1 d R . . H29 H 0.3286 0.3914 0.8640 0.089 Uiso 1 1 d R . . H30 H 0.2946 0.4540 0.7970 0.089 Uiso 1 1 d R . . C34 C 0.2043(6) 0.4138(5) 0.9450(5) 0.059(2) Uani 1 1 d . . . H31 H 0.1695 0.4477 0.9723 0.088 Uiso 1 1 d R . . H32 H 0.2682 0.4037 0.9780 0.088 Uiso 1 1 d R . . H33 H 0.1697 0.3650 0.9325 0.088 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02446(15) 0.01890(14) 0.01688(14) -0.00049(9) 0.00570(10) 0.00091(9) Cu1 0.0219(3) 0.0218(3) 0.0172(3) -0.0016(2) 0.0047(2) -0.0020(2) F4* 0.066(3) 0.064(3) 0.063(3) 0.0011(10) 0.0158(12) 0.0014(10) F5* 0.073(3) 0.071(3) 0.074(3) 0.0018(10) 0.0167(13) -0.0010(10) F6* 0.048(3) 0.048(3) 0.049(3) 0.0007(10) 0.0134(12) 0.0028(10) F5 0.062(3) 0.071(3) 0.0258(18) 0.0063(18) 0.0038(18) 0.024(2) F4 0.083(3) 0.076(3) 0.048(2) 0.002(2) 0.030(2) -0.031(3) F6 0.081(3) 0.053(2) 0.0278(19) -0.0064(17) 0.0219(19) 0.014(2) F7 0.097(3) 0.071(2) 0.075(3) 0.028(2) 0.029(2) -0.005(2) F8 0.081(3) 0.078(3) 0.064(2) 0.035(2) 0.0277(19) -0.009(2) F9 0.080(3) 0.080(3) 0.070(2) 0.034(2) 0.020(2) -0.008(2) F10 0.115(8) 0.161(11) 0.202(13) 0.139(11) 0.115(10) 0.114(9) F11 0.049(4) 0.121(7) 0.062(5) -0.016(5) 0.025(4) 0.046(5) F12 0.054(6) 0.109(9) 0.192(13) -0.056(9) -0.070(7) 0.038(6) O1 0.0217(18) 0.0214(18) 0.0168(16) -0.0006(14) 0.0049(14) 0.0006(14) O2 0.0225(18) 0.0245(18) 0.0170(17) -0.0025(14) 0.0025(14) -0.0019(14) O3 0.030(2) 0.0217(18) 0.0259(19) -0.0063(15) 0.0047(16) -0.0012(15) O4 0.040(2) 0.025(2) 0.0232(19) -0.0016(15) 0.0113(17) 0.0022(16) O5 0.049(3) 0.024(2) 0.0226(19) -0.0017(16) 0.0057(18) 0.0077(17) O6 0.032(2) 0.033(2) 0.028(2) 0.0040(17) 0.0108(17) -0.0025(17) O7 0.029(2) 0.040(2) 0.031(2) 0.0085(18) 0.0104(18) 0.0050(17) O8 0.047(3) 0.032(2) 0.046(3) 0.0076(19) 0.008(2) -0.002(2) O9 0.028(2) 0.028(2) 0.0236(19) 0.0045(15) 0.0018(16) 0.0003(15) N1 0.023(2) 0.019(2) 0.020(2) -0.0033(17) 0.0061(18) -0.0040(17) N2 0.026(2) 0.022(2) 0.023(2) -0.0012(18) 0.0093(19) -0.0043(18) N3 0.0766(18) 0.0704(19) 0.0719(19) 0.0006(15) 0.0148(13) 0.0025(13) N4 0.038(3) 0.031(3) 0.028(2) 0.008(2) 0.001(2) 0.005(2) C1 0.026(3) 0.022(2) 0.016(2) 0.0075(19) 0.003(2) 0.000(2) C2 0.032(3) 0.031(3) 0.020(3) 0.001(2) 0.003(2) 0.009(2) C3 0.025(3) 0.048(4) 0.032(3) 0.002(3) 0.006(2) 0.008(3) C4 0.021(3) 0.047(3) 0.029(3) 0.001(3) -0.004(2) 0.000(2) C5 0.031(3) 0.024(3) 0.023(3) 0.001(2) 0.001(2) 0.000(2) C6 0.028(3) 0.016(2) 0.018(2) 0.0041(19) 0.003(2) 0.001(2) C7 0.031(3) 0.017(2) 0.015(2) 0.0043(19) 0.006(2) 0.001(2) C8 0.032(3) 0.027(3) 0.025(3) -0.006(2) 0.012(2) -0.003(2) C9 0.029(3) 0.031(3) 0.026(3) 0.002(2) 0.014(2) -0.003(2) C10 0.031(3) 0.045(4) 0.041(3) -0.004(3) 0.017(3) -0.002(3) C11 0.047(4) 0.041(3) 0.028(3) 0.005(3) 0.016(3) -0.005(3) C12 0.023(3) 0.035(3) 0.032(3) -0.004(2) 0.008(2) -0.005(2) C13 0.026(3) 0.030(3) 0.027(3) -0.003(2) 0.001(2) -0.001(2) C14 0.026(3) 0.054(4) 0.040(4) -0.007(3) 0.002(3) -0.005(3) C15 0.034(4) 0.051(4) 0.042(4) -0.011(3) -0.006(3) -0.010(3) C16 0.042(4) 0.032(3) 0.027(3) -0.008(2) -0.003(3) -0.005(3) C17 0.031(3) 0.026(3) 0.024(3) -0.004(2) 0.005(2) 0.000(2) C18 0.027(3) 0.016(2) 0.022(2) 0.0014(19) -0.001(2) -0.001(2) C19 0.032(3) 0.028(3) 0.032(3) 0.000(2) 0.007(2) 0.004(2) C20 0.055(4) 0.036(3) 0.034(3) 0.003(3) 0.014(3) 0.015(3) C21 0.042(3) 0.027(3) 0.028(3) -0.002(2) 0.012(3) 0.007(2) C22 0.029(3) 0.033(3) 0.021(3) -0.003(2) 0.009(2) 0.002(2) C23 0.047(4) 0.032(3) 0.028(3) 0.000(2) 0.015(3) -0.001(3) C24 0.076(3) 0.070(2) 0.061(2) 0.028(2) 0.0276(19) -0.008(2) C25 0.079(2) 0.071(2) 0.063(2) 0.0294(19) 0.0262(18) -0.008(2) C26 0.031(3) 0.060(4) 0.041(4) 0.011(3) 0.015(3) -0.003(3) C27 0.031(3) 0.045(4) 0.030(3) -0.002(3) 0.007(3) 0.006(3) C28 0.042(4) 0.086(6) 0.045(4) 0.006(4) 0.016(3) 0.012(4) C29 0.058(4) 0.024(3) 0.038(3) 0.001(3) -0.006(3) 0.003(3) C30 0.0768(17) 0.0740(18) 0.0748(17) 0.0007(10) 0.0165(10) 0.0003(10) C31 0.0773(17) 0.0762(18) 0.0764(17) -0.0009(10) 0.0173(10) 0.0021(10) C32 0.029(3) 0.033(3) 0.032(3) 0.004(2) 0.005(2) 0.004(2) C33 0.072(5) 0.059(5) 0.046(4) -0.002(4) 0.011(4) 0.032(4) C34 0.062(5) 0.061(5) 0.051(4) 0.030(4) 0.009(4) 0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O3 2.200(3) 3_566 ? Dy1 O2 2.340(4) . ? Dy1 O7 2.347(4) . ? Dy1 O5 2.360(4) . ? Dy1 O9 2.391(4) . ? Dy1 O1 2.400(3) . ? Dy1 O6 2.436(4) . ? Dy1 O4 2.451(4) . ? Dy1 Cu1 3.2969(10) . ? Cu1 O1 1.923(3) . ? Cu1 N1 1.923(4) . ? Cu1 N2 1.948(4) . ? Cu1 O2 1.955(3) . ? Cu1 O8 2.416(4) . ? F1 C20 1.281(12) . ? F2 C20 1.349(13) . ? F3 C20 1.380(13) . ? F4* C20 1.276(12) . ? F5* C20 1.360(13) . ? F6* C20 1.346(11) . ? F5 C23 1.315(7) . ? F4 C23 1.322(7) . ? F6 C23 1.335(7) . ? F7 C25 1.295(9) . ? F8 C25 1.322(9) . ? F9 C25 1.326(9) . ? F1* C25 1.353(14) . ? F2* C25 1.371(14) . ? F3* C25 1.315(14) . ? F10 C28 1.340(14) . ? F11 C28 1.303(10) . ? F12 C28 1.362(13) . ? F7* C28 1.329(18) . ? F8* C28 1.275(19) . ? F9* C28 1.19(2) . ? O1 C1 1.348(6) . ? O2 C18 1.326(6) . ? O3 C7 1.277(6) . ? O3 Dy1 2.200(3) 3_566 ? O4 C19 1.241(7) . ? O5 C22 1.249(6) . ? O6 C24 1.234(9) . ? O7 C27 1.246(7) . ? O8 C29 1.220(8) . ? O9 C32 1.241(7) . ? N1 C7 1.315(7) . ? N1 C8 1.461(7) . ? N2 C12 1.262(7) . ? N2 C9 1.491(7) . ? N3 C29 1.320(9) . ? N3 C31 1.433(12) . ? N3 C30 1.449(12) . ? N4 C32 1.315(7) . ? N4 C33 1.438(9) . ? N4 C34 1.455(8) . ? C1 C2 1.395(8) . ? C1 C6 1.426(7) . ? C2 C3 1.365(8) . ? C2 H1 0.9300 . ? C3 C4 1.394(9) . ? C3 H2 0.9300 . ? C4 C5 1.382(8) . ? C4 H3 0.9300 . ? C5 C6 1.396(7) . ? C5 H4 0.9300 . ? C6 C7 1.480(7) . ? C8 C9 1.534(7) . ? C8 H5 0.9700 . ? C8 H6 0.9700 . ? C9 C11 1.523(8) . ? C9 C10 1.527(8) . ? C10 H7 0.9600 . ? C10 H8 0.9600 . ? C10 H9 0.9600 . ? C11 H10 0.9600 . ? C11 H11 0.9600 . ? C11 H12 0.9600 . ? C12 C13 1.460(8) . ? C12 H13 0.9300 . ? C13 C14 1.412(8) . ? C13 C18 1.422(8) . ? C14 C15 1.365(9) . ? C14 H14 0.9300 . ? C15 C16 1.395(9) . ? C15 H15 0.9300 . ? C16 C17 1.372(8) . ? C16 H16 0.9300 . ? C17 C18 1.398(7) . ? C17 H17 0.9300 . ? C19 C21 1.389(8) . ? C19 C20 1.537(8) . ? C21 C22 1.380(8) . ? C21 H18 0.9300 . ? C22 C23 1.532(8) . ? C24 C26 1.396(11) . ? C24 C25 1.509(10) . ? C26 C27 1.388(9) . ? C26 H19 0.9300 . ? C27 C28 1.519(9) . ? C29 H20 0.9300 . ? C30 H21 0.9600 . ? C30 H22 0.9600 . ? C30 H23 0.9600 . ? C31 H24 0.9600 . ? C31 H25 0.9600 . ? C31 H26 0.9600 . ? C32 H27 0.9300 . ? C33 H28 0.9600 . ? C33 H29 0.9600 . ? C33 H30 0.9600 . ? C34 H31 0.9600 . ? C34 H32 0.9600 . ? C34 H33 0.9600 . ? 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 O3 Dy1 O2 94.59(13) 3_566 . ? O3 Dy1 O7 102.46(14) 3_566 . ? O2 Dy1 O7 141.76(13) . . ? O3 Dy1 O5 140.60(13) 3_566 . ? O2 Dy1 O5 105.58(13) . . ? O7 Dy1 O5 82.26(15) . . ? O3 Dy1 O9 80.14(13) 3_566 . ? O2 Dy1 O9 76.06(12) . . ? O7 Dy1 O9 140.19(13) . . ? O5 Dy1 O9 72.66(13) . . ? O3 Dy1 O1 74.44(12) 3_566 . ? O2 Dy1 O1 67.11(12) . . ? O7 Dy1 O1 84.75(13) . . ? O5 Dy1 O1 144.61(12) . . ? O9 Dy1 O1 132.65(12) . . ? O3 Dy1 O6 74.93(13) 3_566 . ? O2 Dy1 O6 148.28(13) . . ? O7 Dy1 O6 69.87(14) . . ? O5 Dy1 O6 70.13(14) . . ? O9 Dy1 O6 72.71(13) . . ? O1 Dy1 O6 134.35(13) . . ? O3 Dy1 O4 149.23(13) 3_566 . ? O2 Dy1 O4 75.92(12) . . ? O7 Dy1 O4 71.94(14) . . ? O5 Dy1 O4 69.77(12) . . ? O9 Dy1 O4 124.04(13) . . ? O1 Dy1 O4 74.92(11) . . ? O6 Dy1 O4 127.18(13) . . ? O3 Dy1 Cu1 71.84(10) 3_566 . ? O2 Dy1 Cu1 35.74(8) . . ? O7 Dy1 Cu1 119.80(10) . . ? O5 Dy1 Cu1 139.48(10) . . ? O9 Dy1 Cu1 98.98(9) . . ? O1 Dy1 Cu1 35.19(8) . . ? O6 Dy1 Cu1 146.68(9) . . ? O4 Dy1 Cu1 84.65(8) . . ? O1 Cu1 N1 95.98(16) . . ? O1 Cu1 N2 177.49(17) . . ? N1 Cu1 N2 85.13(18) . . ? O1 Cu1 O2 85.02(15) . . ? N1 Cu1 O2 156.96(17) . . ? N2 Cu1 O2 93.08(17) . . ? O1 Cu1 O8 89.70(15) . . ? N1 Cu1 O8 103.61(17) . . ? N2 Cu1 O8 92.22(17) . . ? O2 Cu1 O8 99.41(15) . . ? O1 Cu1 Dy1 46.00(10) . . ? N1 Cu1 Dy1 123.99(13) . . ? N2 Cu1 Dy1 131.59(13) . . ? O2 Cu1 Dy1 44.36(10) . . ? O8 Cu1 Dy1 113.16(12) . . ? C1 O1 Cu1 123.0(3) . . ? C1 O1 Dy1 127.5(3) . . ? Cu1 O1 Dy1 98.81(14) . . ? C18 O2 Cu1 125.1(3) . . ? C18 O2 Dy1 134.9(3) . . ? Cu1 O2 Dy1 99.89(14) . . ? C7 O3 Dy1 168.3(3) . 3_566 ? C19 O4 Dy1 132.4(4) . . ? C22 O5 Dy1 136.6(3) . . ? C24 O6 Dy1 134.8(5) . . ? C27 O7 Dy1 137.9(4) . . ? C29 O8 Cu1 116.7(4) . . ? C32 O9 Dy1 125.3(4) . . ? C7 N1 C8 117.8(4) . . ? C7 N1 Cu1 125.8(3) . . ? C8 N1 Cu1 112.3(3) . . ? C12 N2 C9 121.9(5) . . ? C12 N2 Cu1 125.0(4) . . ? C9 N2 Cu1 112.8(3) . . ? C29 N3 C31 119.1(8) . . ? C29 N3 C30 120.5(8) . . ? C31 N3 C30 119.8(8) . . ? C32 N4 C33 120.6(5) . . ? C32 N4 C34 121.1(6) . . ? C33 N4 C34 118.0(6) . . ? O1 C1 C2 118.2(5) . . ? O1 C1 C6 123.4(5) . . ? C2 C1 C6 118.3(5) . . ? C3 C2 C1 121.3(5) . . ? C3 C2 H1 119.5 . . ? C1 C2 H1 119.2 . . ? C2 C3 C4 121.2(5) . . ? C2 C3 H2 119.3 . . ? C4 C3 H2 119.5 . . ? C5 C4 C3 118.4(5) . . ? C5 C4 H3 120.8 . . ? C3 C4 H3 120.8 . . ? C4 C5 C6 121.9(5) . . ? C4 C5 H4 118.8 . . ? C6 C5 H4 119.3 . . ? C5 C6 C1 118.5(5) . . ? C5 C6 C7 116.4(5) . . ? C1 C6 C7 125.1(5) . . ? O3 C7 N1 121.5(5) . . ? O3 C7 C6 118.0(5) . . ? N1 C7 C6 120.3(4) . . ? N1 C8 C9 109.8(4) . . ? N1 C8 H5 109.7 . . ? C9 C8 H5 109.7 . . ? N1 C8 H6 109.6 . . ? C9 C8 H6 109.9 . . ? H5 C8 H6 108.2 . . ? N2 C9 C11 107.3(4) . . ? N2 C9 C10 113.5(5) . . ? C11 C9 C10 111.9(5) . . ? N2 C9 C8 105.5(4) . . ? C11 C9 C8 110.2(5) . . ? C10 C9 C8 108.3(5) . . ? C9 C10 H7 109.3 . . ? C9 C10 H8 109.6 . . ? H7 C10 H8 109.5 . . ? C9 C10 H9 109.5 . . ? H7 C10 H9 109.5 . . ? H8 C10 H9 109.5 . . ? C9 C11 H10 109.5 . . ? C9 C11 H11 109.4 . . ? H10 C11 H11 109.5 . . ? C9 C11 H12 109.4 . . ? H10 C11 H12 109.5 . . ? H11 C11 H12 109.5 . . ? N2 C12 C13 125.9(5) . . ? N2 C12 H13 117.1 . . ? C13 C12 H13 117.0 . . ? C14 C13 C18 118.6(5) . . ? C14 C13 C12 117.2(5) . . ? C18 C13 C12 124.2(5) . . ? C15 C14 C13 122.2(6) . . ? C15 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? C14 C15 C16 118.6(6) . . ? C14 C15 H15 120.9 . . ? C16 C15 H15 120.6 . . ? C17 C16 C15 121.0(5) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 121.6(6) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.3 . . ? O2 C18 C17 119.7(5) . . ? O2 C18 C13 122.3(5) . . ? C17 C18 C13 118.0(5) . . ? O4 C19 C21 129.2(5) . . ? O4 C19 C20 114.4(5) . . ? C21 C19 C20 116.3(5) . . ? F4* C20 F1 124.2(8) . . ? F4* C20 F6* 107.0(8) . . ? F1 C20 F6* 35.2(5) . . ? F4* C20 F2 68.9(7) . . ? F1 C20 F2 106.1(9) . . ? F6* C20 F2 132.6(8) . . ? F4* C20 F5* 102.1(8) . . ? F1 C20 F5* 72.6(8) . . ? F6* C20 F5* 106.3(8) . . ? F2 C20 F5* 37.8(6) . . ? F4* C20 F3 30.8(6) . . ? F1 C20 F3 115.2(9) . . ? F6* C20 F3 85.6(8) . . ? F2 C20 F3 99.7(8) . . ? F5* C20 F3 130.4(8) . . ? F4* C20 C19 117.1(7) . . ? F1 C20 C19 116.4(7) . . ? F6* C20 C19 112.9(6) . . ? F2 C20 C19 109.9(7) . . ? F5* C20 C19 110.5(7) . . ? F3 C20 C19 108.2(7) . . ? C22 C21 C19 119.8(5) . . ? C22 C21 H18 120.2 . . ? C19 C21 H18 120.1 . . ? O5 C22 C21 127.5(5) . . ? O5 C22 C23 112.8(5) . . ? C21 C22 C23 119.7(5) . . ? F5 C23 F4 107.6(5) . . ? F5 C23 F6 106.0(5) . . ? F4 C23 F6 106.9(5) . . ? F5 C23 C22 111.6(5) . . ? F4 C23 C22 110.5(5) . . ? F6 C23 C22 113.8(5) . . ? O6 C24 C26 128.0(7) . . ? O6 C24 C25 115.0(8) . . ? C26 C24 C25 117.0(7) . . ? F7 C25 F3* 74.0(12) . . ? F7 C25 F8 112.4(7) . . ? F3* C25 F8 42.0(10) . . ? F7 C25 F9 101.9(8) . . ? F3* C25 F9 128.0(12) . . ? F8 C25 F9 102.4(7) . . ? F7 C25 F1* 42.9(10) . . ? F3* C25 F1* 106.9(15) . . ? F8 C25 F1* 127.3(12) . . ? F9 C25 F1* 60.1(11) . . ? F7 C25 F2* 128.3(12) . . ? F3* C25 F2* 110.3(15) . . ? F8 C25 F2* 73.4(11) . . ? F9 C25 F2* 33.3(9) . . ? F1* C25 F2* 91.0(15) . . ? F7 C25 C24 111.4(7) . . ? F3* C25 C24 118.1(12) . . ? F8 C25 C24 115.8(7) . . ? F9 C25 C24 111.6(7) . . ? F1* C25 C24 116.8(12) . . ? F2* C25 C24 110.5(12) . . ? C27 C26 C24 119.5(6) . . ? C27 C26 H19 120.2 . . ? C24 C26 H19 120.3 . . ? O7 C27 C26 127.9(6) . . ? O7 C27 C28 115.5(6) . . ? C26 C27 C28 116.6(6) . . ? F9* C28 F8* 104.8(14) . . ? F9* C28 F11 124.1(12) . . ? F8* C28 F11 76.5(10) . . ? F9* C28 F7* 101.3(14) . . ? F8* C28 F7* 111.6(12) . . ? F11 C28 F7* 37.5(7) . . ? F9* C28 F10 72.0(11) . . ? F8* C28 F10 35.7(9) . . ? F11 C28 F10 106.4(10) . . ? F7* C28 F10 131.8(11) . . ? F9* C28 F12 30.4(11) . . ? F8* C28 F12 131.5(11) . . ? F11 C28 F12 110.4(10) . . ? F7* C28 F12 77.3(11) . . ? F10 C28 F12 101.9(12) . . ? F9* C28 C27 116.2(12) . . ? F8* C28 C27 109.8(10) . . ? F11 C28 C27 115.3(7) . . ? F7* C28 C27 112.8(10) . . ? F10 C28 C27 112.6(7) . . ? F12 C28 C27 109.4(7) . . ? O8 C29 N3 124.1(8) . . ? O8 C29 H20 117.6 . . ? N3 C29 H20 118.2 . . ? N3 C30 H21 109.8 . . ? N3 C30 H22 108.9 . . ? H21 C30 H22 109.5 . . ? N3 C30 H23 109.7 . . ? H21 C30 H23 109.5 . . ? H22 C30 H23 109.5 . . ? N3 C31 H24 110.0 . . ? N3 C31 H25 110.0 . . ? H24 C31 H25 109.5 . . ? N3 C31 H26 108.4 . . ? H24 C31 H26 109.5 . . ? H25 C31 H26 109.5 . . ? O9 C32 N4 124.4(6) . . ? O9 C32 H27 117.8 . . ? N4 C32 H27 117.8 . . ? N4 C33 H28 109.2 . . ? N4 C33 H29 109.7 . . ? H28 C33 H29 109.5 . . ? N4 C33 H30 109.5 . . ? H28 C33 H30 109.5 . . ? H29 C33 H30 109.5 . . ? N4 C34 H31 109.6 . . ? N4 C34 H32 109.6 . . ? H31 C34 H32 109.5 . . ? N4 C34 H33 109.2 . . ? H31 C34 H33 109.5 . . ? H32 C34 H33 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.141 _refine_diff_density_min -1.979 _refine_diff_density_rms 0.141