Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Jean-Pierre Costes' _publ_contact_author_address ; Laboratoire de Chimie de Coordinati 205, route de Narbonne Toulouse Cedex 04 31077 FRANCE ; _publ_contact_author_email COSTES@LCC-TOULOUSE.FR _publ_contact_author_phone '(33) 0561333152' _publ_contact_author_fax '(33) 0561553003' _publ_section_title ; The First Example of a Hetero-Tetranuclear [(VO)Gd]2 Complex: Synthesis, Crystal Structure and Magnetic Properties of [VOLGd(hfa)2CH3OH ]2*2CH3OH*2(CH3)2CO ; loop_ _publ_author_name 'Jean-Pierre Costes' 'Juan-Modesto Clemente Juan' 'Sergiu Shova' 'Nicolas Suet' data_VOGd _database_code_depnum_ccdc_archive 'CCDC 270841' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[LVOGd(hfa)2(CH3OH)]2((CH3)2CO)2(CH3OH)2' _chemical_formula_sum 'C33 H33 F12 Gd N2 O11 V' _chemical_formula_weight 1069.80 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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 'P c c n' _symmetry_space_group_name_Hall '-P 2ab 2ac' _symmetry_Int_Tables_number 56 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 28.631(6) _cell_length_b 16.612(3) _cell_length_c 17.346(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8250(3) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2850 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 26.0 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4224 _exptl_absorpt_coefficient_mu 1.931 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.751 _exptl_absorpt_correction_T_max 0.794 _exptl_absorpt_process_details 'R. H. Blessing, Acta Cryst., 1995, a51, 33' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type omega-Phi _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 59127 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8103 _reflns_number_gt 5921 _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 for Windows (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^)+(0.0274P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8103 _refine_ls_number_parameters 612 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0664 _refine_ls_wR_factor_gt 0.0587 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.100 _refine_ls_shift/su_mean 0.010 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 0.126871(6) 0.453356(10) 0.067833(10) 0.02183(6) Uani 1 1 d . . . V1 V 0.02168(2) 0.37366(4) 0.14080(3) 0.02110(14) Uani 1 1 d . . . F1 F 0.1257(13) 0.6548(9) 0.2852(16) 0.158(14) Uani 0.55(3) 1 d P A 1 F2 F 0.1332(9) 0.7211(9) 0.1858(12) 0.122(6) Uani 0.55(3) 1 d P A 1 F3 F 0.1885(5) 0.7119(13) 0.2610(15) 0.123(11) Uani 0.55(3) 1 d P A 1 F4* F 0.1811(11) 0.7308(12) 0.2217(18) 0.137(11) Uani 0.45(3) 1 d P A 2 F5* F 0.1623(10) 0.6507(11) 0.3122(7) 0.103(6) Uani 0.45(3) 1 d P A 2 F6* F 0.1127(6) 0.6871(18) 0.233(2) 0.119(14) Uani 0.45(3) 1 d P A 2 F4 F 0.30943(10) 0.5495(2) 0.1671(2) 0.1059(13) Uani 1 1 d . A 3 F5 F 0.29558(10) 0.4268(2) 0.1526(2) 0.1052(13) Uani 1 1 d . A 3 F6 F 0.29549(10) 0.5035(3) 0.0578(2) 0.1154(14) Uani 1 1 d . A 3 F7 F 0.1868(6) 0.6949(6) -0.0746(12) 0.127(8) Uani 0.58(3) 1 d P B 1 F8 F 0.2316(8) 0.6447(6) -0.1479(9) 0.114(7) Uani 0.58(3) 1 d P B 1 F9 F 0.2492(10) 0.6506(14) -0.0278(19) 0.204(17) Uani 0.58(3) 1 d P B 1 F1* F 0.2614(7) 0.6261(14) -0.096(2) 0.153(12) Uani 0.42(3) 1 d P B 2 F2* F 0.2248(14) 0.6789(15) -0.0191(14) 0.146(14) Uani 0.42(3) 1 d P B 2 F3* F 0.1972(14) 0.681(2) -0.119(3) 0.30(2) Uani 0.42(3) 1 d P B 2 F11 F 0.20169(16) 0.2802(2) -0.1143(2) 0.1272(16) Uani 1 1 d . B . F12 F 0.16251(12) 0.3348(2) -0.2011(2) 0.0942(11) Uani 1 1 d . B . F13 F 0.23473(11) 0.3595(2) -0.19123(18) 0.0967(11) Uani 1 1 d . B . N1 N -0.03204(9) 0.42165(16) 0.08296(15) 0.0195(7) Uani 1 1 d . . . N2 N -0.01099(10) 0.43672(17) 0.22705(16) 0.0240(7) Uani 1 1 d . . . O1 O 0.05800(8) 0.36937(13) 0.04599(12) 0.0206(5) Uani 1 1 d . . . O2 O 0.08051(8) 0.41475(15) 0.18000(13) 0.0255(6) Uani 1 1 d . . . O3 O 0.01290(9) 0.28191(14) 0.16439(13) 0.0307(6) Uani 1 1 d . . . O4 O -0.06952(8) 0.46434(14) -0.02510(13) 0.0246(6) Uani 1 1 d . . . O5 O 0.15159(10) 0.31997(16) 0.10451(17) 0.0385(7) Uani 1 1 d D . . O6 O 0.16717(9) 0.55734(15) -0.00467(15) 0.0352(7) Uani 1 1 d . . . O7 O 0.15578(9) 0.39826(16) -0.04601(14) 0.0343(7) Uani 1 1 d . . . O8 O 0.13522(8) 0.55976(15) 0.15775(14) 0.0312(6) Uani 1 1 d . . . O9 O 0.20656(8) 0.45914(16) 0.10706(15) 0.0335(6) Uani 1 1 d . . . O10 O -0.06427(17) 0.0726(3) -0.0570(2) 0.0982(15) Uani 1 1 d . . . O11 O 0.09596(13) 0.19804(18) 0.1417(2) 0.0535(9) Uani 1 1 d . . . C1 C 0.03792(12) 0.3489(2) -0.02215(19) 0.0207(8) Uani 1 1 d . . . C2 C 0.06388(13) 0.3021(2) -0.0739(2) 0.0267(8) Uani 1 1 d . . . H2 H 0.0937 0.2849 -0.0604 0.032 Uiso 1 1 calc R . . C3 C 0.04557(14) 0.2812(2) -0.1449(2) 0.0344(10) Uani 1 1 d . . . H3 H 0.0630 0.2498 -0.1787 0.041 Uiso 1 1 calc R . . C4 C 0.00111(15) 0.3068(2) -0.1659(2) 0.0400(11) Uani 1 1 d . . . H4 H -0.0114 0.2924 -0.2134 0.048 Uiso 1 1 calc R . . C5 C -0.02399(13) 0.3535(2) -0.1159(2) 0.0301(9) Uani 1 1 d . . . H5 H -0.0534 0.3717 -0.1307 0.036 Uiso 1 1 calc R . . C6 C -0.00698(12) 0.3747(2) -0.04348(18) 0.0198(8) Uani 1 1 d . . . C7 C -0.03773(12) 0.4231(2) 0.0072(2) 0.0218(8) Uani 1 1 d . . . C8 C -0.06505(12) 0.4705(2) 0.12770(19) 0.0245(9) Uani 1 1 d . . . H8A H -0.0966 0.4613 0.1091 0.029 Uiso 1 1 calc R . . H8B H -0.0578 0.5271 0.1210 0.029 Uiso 1 1 calc R . . C9 C -0.06217(12) 0.4486(2) 0.2128(2) 0.0244(8) Uani 1 1 d . . . C10 C -0.08429(14) 0.5150(2) 0.2605(2) 0.0354(10) Uani 1 1 d . . . H10A H -0.0850 0.4992 0.3137 0.053 Uiso 1 1 calc R . . H10B H -0.1156 0.5245 0.2427 0.053 Uiso 1 1 calc R . . H10C H -0.0663 0.5634 0.2552 0.053 Uiso 1 1 calc R . . C11 C -0.08619(13) 0.3677(2) 0.2288(2) 0.0340(10) Uani 1 1 d . . . H11A H -0.0752 0.3282 0.1926 0.051 Uiso 1 1 calc R . . H11B H -0.1194 0.3738 0.2235 0.051 Uiso 1 1 calc R . . H11C H -0.0790 0.3504 0.2803 0.051 Uiso 1 1 calc R . . C12 C 0.00810(13) 0.4597(2) 0.2898(2) 0.0295(9) Uani 1 1 d . . . H12 H -0.0110 0.4841 0.3263 0.035 Uiso 1 1 calc R . . C13 C 0.05683(13) 0.4509(2) 0.3087(2) 0.0285(9) Uani 1 1 d . . . C14 C 0.07083(15) 0.4669(3) 0.3851(2) 0.0427(11) Uani 1 1 d . . . H14 H 0.0486 0.4830 0.4210 0.051 Uiso 1 1 calc R . . C15 C 0.11657(16) 0.4593(3) 0.4075(2) 0.0515(13) Uani 1 1 d . . . H15 H 0.1252 0.4710 0.4579 0.062 Uiso 1 1 calc R . . C16 C 0.14943(16) 0.4344(3) 0.3551(2) 0.0497(13) Uani 1 1 d . . . H16 H 0.1803 0.4282 0.3705 0.060 Uiso 1 1 calc R . . C17 C 0.13708(14) 0.4183(3) 0.2799(2) 0.0393(11) Uani 1 1 d . . . H17 H 0.1597 0.4012 0.2452 0.047 Uiso 1 1 calc R . . C18 C 0.09112(14) 0.4275(2) 0.2552(2) 0.0303(10) Uani 1 1 d . . . C19 C 0.16879(15) 0.5969(2) 0.1860(2) 0.0377(10) Uani 1 1 d . A . C20 C 0.1547(2) 0.6692(4) 0.2358(4) 0.0684(17) Uani 1 1 d . . . C21 C 0.21584(15) 0.5792(3) 0.1784(3) 0.0449(12) Uani 1 1 d . . . H21 H 0.2378 0.6131 0.2009 0.054 Uiso 1 1 calc R A . C22 C 0.23093(14) 0.5127(2) 0.1385(2) 0.0342(10) Uani 1 1 d . A . C23 C 0.28310(16) 0.4986(3) 0.1291(3) 0.0534(13) Uani 1 1 d . . . C24 C 0.19374(14) 0.5560(3) -0.0600(3) 0.0409(11) Uani 1 1 d . B . C25 C 0.2175(3) 0.6375(4) -0.0787(5) 0.0727(17) Uani 1 1 d . . . C26 C 0.20442(15) 0.4907(3) -0.1082(3) 0.0482(12) Uani 1 1 d . . . H26 H 0.2257 0.4976 -0.1482 0.058 Uiso 1 1 calc R B . C27 C 0.18414(15) 0.4176(3) -0.0974(2) 0.0385(11) Uani 1 1 d . B . C28 C 0.19625(19) 0.3479(3) -0.1519(3) 0.0596(14) Uani 1 1 d . . . C29 C 0.19477(16) 0.2786(3) 0.0961(3) 0.0718(17) Uani 1 1 d . . . H29A H 0.1927 0.2417 0.0536 0.108 Uiso 1 1 calc R . . H29B H 0.2015 0.2493 0.1425 0.108 Uiso 1 1 calc R . . H29C H 0.2193 0.3168 0.0864 0.108 Uiso 1 1 calc R . . C30 C -0.0721(2) 0.1328(4) -0.0219(3) 0.0675(16) Uani 1 1 d . . . C31 C -0.1159(3) 0.1765(5) -0.0274(5) 0.133(3) Uani 1 1 d . . . H31A H -0.1097 0.2325 -0.0361 0.200 Uiso 1 1 calc R . . H31B H -0.1331 0.1703 0.0197 0.200 Uiso 1 1 calc R . . H31C H -0.1339 0.1554 -0.0695 0.200 Uiso 1 1 calc R . . C32 C -0.0379(3) 0.1670(4) 0.0305(5) 0.159(4) Uani 1 1 d . . . H32A H -0.0184 0.1250 0.0504 0.238 Uiso 1 1 calc R . . H32B H -0.0537 0.1933 0.0723 0.238 Uiso 1 1 calc R . . H32C H -0.0191 0.2055 0.0033 0.238 Uiso 1 1 calc R . . C33 C 0.09323(18) 0.1461(3) 0.0770(3) 0.0653(14) Uani 1 1 d . . . H33A H 0.1242 0.1324 0.0603 0.098 Uiso 1 1 calc R . . H33B H 0.0770 0.1728 0.0359 0.098 Uiso 1 1 calc R . . H33C H 0.0767 0.0980 0.0910 0.098 Uiso 1 1 calc R . . H5O H 0.1304(11) 0.288(2) 0.121(2) 0.052(14) Uiso 1 1 d D . . H11O H 0.0680(15) 0.212(3) 0.153(3) 0.056(16) 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 Gd1 0.01981(9) 0.02280(10) 0.02290(10) 0.00029(9) -0.00023(9) 0.00319(8) V1 0.0236(3) 0.0211(3) 0.0187(3) 0.0026(3) 0.0007(3) 0.0021(3) F1 0.23(3) 0.126(11) 0.120(16) -0.077(12) 0.099(19) -0.004(16) F2 0.157(13) 0.064(6) 0.145(12) -0.041(8) -0.048(11) 0.058(7) F3 0.080(8) 0.125(16) 0.164(19) -0.113(15) -0.053(11) 0.018(9) F4* 0.21(3) 0.056(8) 0.140(18) -0.051(10) 0.023(14) -0.043(11) F5* 0.138(14) 0.114(10) 0.057(7) -0.036(6) -0.017(8) 0.047(10) F6* 0.072(11) 0.12(2) 0.17(2) -0.125(18) -0.069(15) 0.056(12) F4 0.0346(17) 0.114(3) 0.169(4) -0.056(3) -0.027(2) -0.0049(17) F5 0.0427(18) 0.084(2) 0.189(4) 0.031(3) -0.007(2) 0.0263(17) F6 0.0393(18) 0.227(5) 0.079(3) 0.010(3) 0.0139(17) 0.001(2) F7 0.160(13) 0.038(5) 0.183(17) 0.033(7) 0.099(13) 0.014(5) F8 0.165(17) 0.086(6) 0.092(8) 0.029(5) 0.079(9) -0.030(8) F9 0.19(2) 0.126(18) 0.29(3) 0.092(18) -0.17(2) -0.119(17) F1* 0.075(10) 0.149(14) 0.23(3) 0.029(19) 0.034(16) -0.063(9) F2* 0.25(4) 0.079(13) 0.107(15) 0.025(9) 0.025(18) -0.091(18) F3* 0.21(3) 0.24(3) 0.43(5) 0.29(3) -0.20(3) -0.15(2) F11 0.200(5) 0.088(3) 0.093(3) -0.002(2) 0.055(3) 0.073(3) F12 0.078(2) 0.112(3) 0.092(3) -0.059(2) 0.002(2) 0.009(2) F13 0.066(2) 0.136(3) 0.088(2) -0.039(2) 0.0402(18) 0.007(2) N1 0.0205(16) 0.0195(15) 0.0183(17) 0.0018(12) 0.0041(13) 0.0007(12) N2 0.0261(17) 0.0257(18) 0.0200(17) 0.0027(13) 0.0023(14) -0.0013(13) O1 0.0228(13) 0.0222(13) 0.0169(13) 0.0003(10) 0.0003(10) 0.0044(11) O2 0.0252(14) 0.0338(15) 0.0175(14) 0.0003(11) -0.0023(11) 0.0020(12) O3 0.0400(16) 0.0245(14) 0.0274(15) 0.0064(11) 0.0047(12) 0.0001(12) O4 0.0255(14) 0.0266(15) 0.0218(14) 0.0022(11) -0.0017(11) 0.0081(11) O5 0.0259(16) 0.0283(17) 0.061(2) 0.0090(15) 0.0025(15) 0.0102(13) O6 0.0312(15) 0.0387(17) 0.0356(16) 0.0041(13) 0.0042(13) -0.0070(13) O7 0.0301(16) 0.0399(17) 0.0329(16) -0.0053(13) 0.0079(13) 0.0025(13) O8 0.0300(16) 0.0339(16) 0.0296(15) -0.0060(12) -0.0047(12) 0.0035(12) O9 0.0238(14) 0.0359(16) 0.0408(16) -0.0055(14) -0.0025(12) 0.0043(13) O10 0.140(4) 0.104(4) 0.050(3) -0.011(2) 0.018(3) -0.006(3) O11 0.053(2) 0.0338(19) 0.074(3) 0.0072(17) 0.009(2) 0.0097(17) C1 0.028(2) 0.0154(19) 0.019(2) 0.0021(15) 0.0003(16) -0.0048(16) C2 0.027(2) 0.024(2) 0.029(2) -0.0021(18) 0.0022(18) 0.0044(16) C3 0.036(2) 0.034(2) 0.033(2) -0.0148(19) 0.010(2) -0.0007(19) C4 0.045(3) 0.046(3) 0.029(2) -0.015(2) -0.008(2) 0.002(2) C5 0.027(2) 0.035(2) 0.029(2) -0.0042(18) -0.0039(18) 0.0007(18) C6 0.025(2) 0.0185(19) 0.0164(18) 0.0010(14) 0.0021(15) -0.0007(15) C7 0.020(2) 0.0189(19) 0.027(2) 0.0022(16) -0.0007(17) -0.0061(16) C8 0.024(2) 0.028(2) 0.021(2) 0.0022(16) 0.0031(16) 0.0076(16) C9 0.0244(19) 0.027(2) 0.022(2) -0.0003(17) 0.0058(16) -0.0007(17) C10 0.033(2) 0.040(2) 0.032(2) -0.0070(19) 0.0077(19) 0.005(2) C11 0.031(2) 0.040(2) 0.032(2) 0.0074(19) 0.0072(18) -0.0014(19) C12 0.036(2) 0.032(2) 0.020(2) 0.0006(18) 0.0062(17) -0.0001(19) C13 0.031(2) 0.033(2) 0.021(2) 0.0034(18) -0.0024(17) -0.0008(19) C14 0.044(3) 0.060(3) 0.023(2) -0.006(2) 0.001(2) 0.000(2) C15 0.053(3) 0.077(4) 0.024(2) -0.004(2) -0.014(2) -0.003(3) C16 0.039(3) 0.078(4) 0.033(3) 0.006(2) -0.015(2) 0.003(2) C17 0.035(3) 0.056(3) 0.027(2) 0.004(2) -0.0051(19) 0.001(2) C18 0.036(2) 0.034(2) 0.020(2) 0.0035(17) -0.0071(18) -0.0015(18) C19 0.043(3) 0.035(3) 0.036(3) -0.007(2) -0.010(2) 0.006(2) C20 0.058(4) 0.061(4) 0.086(5) -0.036(4) -0.029(4) 0.015(3) C21 0.035(3) 0.043(3) 0.057(3) -0.014(2) -0.020(2) -0.002(2) C22 0.028(2) 0.037(2) 0.037(2) 0.003(2) -0.010(2) 0.003(2) C23 0.034(3) 0.064(4) 0.062(4) -0.008(3) -0.011(3) -0.003(3) C24 0.030(2) 0.049(3) 0.044(3) 0.017(2) -0.004(2) -0.005(2) C25 0.075(5) 0.068(5) 0.075(5) 0.012(4) 0.019(4) -0.025(4) C26 0.041(3) 0.063(3) 0.041(3) 0.003(2) 0.019(2) -0.001(3) C27 0.032(2) 0.052(3) 0.031(2) -0.003(2) 0.003(2) 0.011(2) C28 0.061(4) 0.073(4) 0.045(3) -0.003(3) 0.016(3) 0.023(3) C29 0.042(3) 0.046(3) 0.127(5) 0.010(3) 0.008(3) 0.023(2) C30 0.088(5) 0.075(4) 0.040(3) 0.006(3) 0.008(3) -0.025(4) C31 0.110(7) 0.132(7) 0.157(8) -0.023(6) 0.011(6) 0.002(5) C32 0.197(9) 0.106(6) 0.174(8) 0.034(6) -0.110(7) -0.085(6) C33 0.075(4) 0.055(3) 0.065(4) 0.012(3) -0.001(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O4 2.262(2) 5_565 ? Gd1 O7 2.329(2) . ? Gd1 O8 2.369(2) . ? Gd1 O9 2.383(2) . ? Gd1 O5 2.411(3) . ? Gd1 O6 2.428(3) . ? Gd1 O2 2.441(2) . ? Gd1 O1 2.445(2) . ? Gd1 V1 3.5251(8) . ? V1 O3 1.598(2) . ? V1 O2 1.941(2) . ? V1 O1 1.947(2) . ? V1 N1 2.002(3) . ? V1 N2 2.052(3) . ? F1 C20 1.218(13) . ? F2 C20 1.369(15) . ? F3 C20 1.277(16) . ? F4* C20 1.29(2) . ? F5* C20 1.378(16) . ? F6* C20 1.239(14) . ? F4 C23 1.310(5) . ? F5 C23 1.309(5) . ? F6 C23 1.291(6) . ? F7 C25 1.299(15) . ? F8 C25 1.273(12) . ? F9 C25 1.286(19) . ? F1* C25 1.309(18) . ? F2* C25 1.26(2) . ? F3* C25 1.169(18) . ? F11 C28 1.310(6) . ? F12 C28 1.306(6) . ? F13 C28 1.310(5) . ? N1 C7 1.324(4) . ? N1 C8 1.468(4) . ? N2 C12 1.277(4) . ? N2 C9 1.499(4) . ? O1 C1 1.358(4) . ? O2 C18 1.356(4) . ? O4 C7 1.269(4) . ? O4 Gd1 2.262(2) 5_565 ? O5 C29 1.422(5) . ? O6 C24 1.225(5) . ? O7 C27 1.248(5) . ? O8 C19 1.243(4) . ? O9 C22 1.256(4) . ? O10 C30 1.193(6) . ? O11 C33 1.417(5) . ? C1 C2 1.401(5) . ? C1 C6 1.405(5) . ? C2 C3 1.382(5) . ? C3 C4 1.391(5) . ? C4 C5 1.368(5) . ? C5 C6 1.392(5) . ? C6 C7 1.482(5) . ? C8 C9 1.523(5) . ? C9 C10 1.517(5) . ? C9 C11 1.535(5) . ? C12 C13 1.441(5) . ? C13 C18 1.406(5) . ? C13 C14 1.409(5) . ? C14 C15 1.372(6) . ? C15 C16 1.372(6) . ? C16 C17 1.378(5) . ? C17 C18 1.392(5) . ? C19 C21 1.385(6) . ? C19 C20 1.531(6) . ? C21 C22 1.372(5) . ? C22 C23 1.521(6) . ? C24 C26 1.403(6) . ? C24 C25 1.549(7) . ? C26 C27 1.360(6) . ? C27 C28 1.535(6) . ? C30 C32 1.450(7) . ? C30 C31 1.452(8) . ? 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 O4 Gd1 O7 102.57(9) 5_565 . ? O4 Gd1 O8 80.68(8) 5_565 . ? O7 Gd1 O8 144.65(9) . . ? O4 Gd1 O9 139.86(9) 5_565 . ? O7 Gd1 O9 85.28(9) . . ? O8 Gd1 O9 71.66(8) . . ? O4 Gd1 O5 148.76(9) 5_565 . ? O7 Gd1 O5 76.01(10) . . ? O8 Gd1 O5 118.83(9) . . ? O9 Gd1 O5 71.38(9) . . ? O4 Gd1 O6 75.24(9) 5_565 . ? O7 Gd1 O6 70.82(9) . . ? O8 Gd1 O6 76.25(9) . . ? O9 Gd1 O6 70.38(9) . . ? O5 Gd1 O6 130.60(9) . . ? O4 Gd1 O2 91.45(8) 5_565 . ? O7 Gd1 O2 139.99(9) . . ? O8 Gd1 O2 74.11(8) . . ? O9 Gd1 O2 107.67(8) . . ? O5 Gd1 O2 73.01(9) . . ? O6 Gd1 O2 149.10(9) . . ? O4 Gd1 O1 73.06(8) 5_565 . ? O7 Gd1 O1 86.04(8) . . ? O8 Gd1 O1 127.52(8) . . ? O9 Gd1 O1 147.09(8) . . ? O5 Gd1 O1 75.72(9) . . ? O6 Gd1 O1 135.14(8) . . ? O2 Gd1 O1 62.30(7) . . ? O4 Gd1 V1 74.00(6) 5_565 . ? O7 Gd1 V1 117.43(7) . . ? O8 Gd1 V1 97.47(6) . . ? O9 Gd1 V1 136.94(6) . . ? O5 Gd1 V1 79.10(7) . . ? O6 Gd1 V1 149.21(6) . . ? O2 Gd1 V1 31.85(5) . . ? O1 Gd1 V1 32.04(5) . . ? O3 V1 O2 112.47(12) . . ? O3 V1 O1 105.39(11) . . ? O2 V1 O1 81.09(10) . . ? O3 V1 N1 112.79(12) . . ? O2 V1 N1 134.63(11) . . ? O1 V1 N1 90.09(10) . . ? O3 V1 N2 103.21(12) . . ? O2 V1 N2 87.74(11) . . ? O1 V1 N2 151.40(11) . . ? N1 V1 N2 79.16(11) . . ? O3 V1 Gd1 125.77(9) . . ? O2 V1 Gd1 41.58(7) . . ? O1 V1 Gd1 41.77(7) . . ? N1 V1 Gd1 109.08(8) . . ? N2 V1 Gd1 117.36(8) . . ? C7 N1 C8 115.8(3) . . ? C7 N1 V1 126.8(2) . . ? C8 N1 V1 116.7(2) . . ? C12 N2 C9 121.3(3) . . ? C12 N2 V1 125.4(3) . . ? C9 N2 V1 113.1(2) . . ? C1 O1 V1 121.2(2) . . ? C1 O1 Gd1 128.26(19) . . ? V1 O1 Gd1 106.20(10) . . ? C18 O2 V1 125.9(2) . . ? C18 O2 Gd1 127.2(2) . . ? V1 O2 Gd1 106.57(10) . . ? C7 O4 Gd1 172.4(2) . 5_565 ? C29 O5 Gd1 132.2(3) . . ? C24 O6 Gd1 133.5(3) . . ? C27 O7 Gd1 137.4(3) . . ? C19 O8 Gd1 135.1(2) . . ? C22 O9 Gd1 133.2(2) . . ? O1 C1 C2 118.2(3) . . ? O1 C1 C6 122.7(3) . . ? C2 C1 C6 119.1(3) . . ? C3 C2 C1 120.6(3) . . ? C2 C3 C4 120.2(4) . . ? C5 C4 C3 119.2(4) . . ? C4 C5 C6 122.1(4) . . ? C5 C6 C1 118.7(3) . . ? C5 C6 C7 117.7(3) . . ? C1 C6 C7 123.6(3) . . ? O4 C7 N1 122.5(3) . . ? O4 C7 C6 117.2(3) . . ? N1 C7 C6 120.4(3) . . ? N1 C8 C9 110.2(3) . . ? N2 C9 C10 114.5(3) . . ? N2 C9 C8 104.1(3) . . ? C10 C9 C8 109.4(3) . . ? N2 C9 C11 107.0(3) . . ? C10 C9 C11 110.6(3) . . ? C8 C9 C11 111.1(3) . . ? N2 C12 C13 125.3(3) . . ? C18 C13 C14 118.3(3) . . ? C18 C13 C12 123.6(3) . . ? C14 C13 C12 118.1(3) . . ? C15 C14 C13 121.4(4) . . ? C16 C15 C14 119.6(4) . . ? C15 C16 C17 120.6(4) . . ? C16 C17 C18 120.8(4) . . ? O2 C18 C17 119.4(3) . . ? O2 C18 C13 121.5(3) . . ? C17 C18 C13 119.1(3) . . ? O8 C19 C21 127.5(4) . . ? O8 C19 C20 114.1(4) . . ? C21 C19 C20 118.4(4) . . ? F1 C20 F6* 53.7(10) . . ? F1 C20 F3 112.6(13) . . ? F6* C20 F3 127.7(10) . . ? F1 C20 F4* 133.2(11) . . ? F6* C20 F4* 111.6(15) . . ? F3 C20 F4* 35.2(12) . . ? F1 C20 F2 105.1(13) . . ? F6* C20 F2 52.4(12) . . ? F3 C20 F2 102.0(12) . . ? F4* C20 F2 69.3(13) . . ? F1 C20 F5* 52.2(14) . . ? F6* C20 F5* 103.9(16) . . ? F3 C20 F5* 71.1(10) . . ? F4* C20 F5* 105.4(12) . . ? F2 C20 F5* 145.1(9) . . ? F1 C20 C19 115.0(7) . . ? F6* C20 C19 115.1(7) . . ? F3 C20 C19 115.4(9) . . ? F4* C20 C19 111.1(11) . . ? F2 C20 C19 104.8(8) . . ? F5* C20 C19 109.0(7) . . ? C22 C21 C19 121.7(4) . . ? O9 C22 C21 127.9(4) . . ? O9 C22 C23 113.0(4) . . ? C21 C22 C23 119.2(4) . . ? F6 C23 F4 106.4(5) . . ? F6 C23 F5 106.3(5) . . ? F4 C23 F5 106.0(4) . . ? F6 C23 C22 111.3(4) . . ? F4 C23 C22 114.3(4) . . ? F5 C23 C22 112.0(4) . . ? O6 C24 C26 128.1(4) . . ? O6 C24 C25 114.8(5) . . ? C26 C24 C25 117.1(5) . . ? F3* C25 F2* 104(3) . . ? F3* C25 F8 62(3) . . ? F2* C25 F8 131.9(11) . . ? F3* C25 F9 131.2(18) . . ? F2* C25 F9 39.3(18) . . ? F8 C25 F9 113.9(14) . . ? F3* C25 F7 40(3) . . ? F2* C25 F7 70.6(16) . . ? F8 C25 F7 101.4(11) . . ? F9 C25 F7 108.5(17) . . ? F3* C25 F1* 115(2) . . ? F2* C25 F1* 96.4(18) . . ? F8 C25 F1* 59.0(11) . . ? F9 C25 F1* 60.4(12) . . ? F7 C25 F1* 140.3(11) . . ? F3* C25 C24 117.0(11) . . ? F2* C25 C24 112.3(9) . . ? F8 C25 C24 114.8(8) . . ? F9 C25 C24 108.4(10) . . ? F7 C25 C24 109.5(7) . . ? F1* C25 C24 110.1(11) . . ? C27 C26 C24 121.0(4) . . ? O7 C27 C26 127.3(4) . . ? O7 C27 C28 113.2(4) . . ? C26 C27 C28 119.5(4) . . ? F12 C28 F11 105.7(5) . . ? F12 C28 F13 107.9(4) . . ? F11 C28 F13 106.6(4) . . ? F12 C28 C27 111.1(4) . . ? F11 C28 C27 111.6(4) . . ? F13 C28 C27 113.5(5) . . ? O10 C30 C32 121.5(7) . . ? O10 C30 C31 123.1(6) . . ? C32 C30 C31 115.4(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5O O11 0.855(10) 1.825(16) 2.656(4) 163(4) . O11 H11O O3 0.86(4) 1.97(5) 2.784(4) 158(4) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.284 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.078