Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'R. Jones' _publ_contact_author_address ; Department of Chemistry University of Texas at Austin Austin Texas 78712-116 UNITED STATES OF AMERICA ; _publ_contact_author_email RAJONES@MAIL.UTEXAS.EDU _publ_section_title ; Syntheses, Structures and Luminescent Properties of New Lanthanide-Based Coordination Polymers Based on 1,4-Benzenedicarboxylate (BDC) ; loop_ _publ_author_name 'R. Jones' 'Rachel Pen-Jen Lai' 'Joseph H. Rivers' 'Xiaoping Yang.' data_complex-1 _database_code_depnum_ccdc_archive 'CCDC 644754' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H88 Eu4 O40' _chemical_formula_weight 2105.18 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 11.716(2) _cell_length_b 13.693(3) _cell_length_c 13.800(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.44(3) _cell_angle_gamma 90.00 _cell_volume 2183.8(8) _cell_formula_units_Z 1 _cell_measurement_temperature 153(1) _cell_measurement_reflns_used CCD _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 2.917 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.5192 _exptl_absorpt_correction_T_max 0.7066 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(1) _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 CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8600 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.52 _reflns_number_total 4975 _reflns_number_gt 3827 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _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^)+(0.0354P)^2^+4.5648P] 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 SHELXL _refine_ls_extinction_coef 0.0030(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(7) _refine_ls_number_reflns 4975 _refine_ls_number_parameters 262 _refine_ls_number_restraints 177 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.1031 _refine_ls_wR_factor_gt 0.0947 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.074 _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 Eu1 Eu 0.386479(12) 0.959839(10) 0.086584(9) 0.01153(4) Uani 1 1 d U . . O1 O 0.27793(18) 1.10144(16) 0.02019(15) 0.0217(6) Uani 1 1 d U . . O2 O 0.43638(17) 1.09368(15) -0.04572(14) 0.0175(5) Uani 1 1 d U . . O3 O 0.02876(19) 1.42840(17) -0.33863(15) 0.0233(6) Uani 1 1 d U . . O4 O 0.17499(18) 1.40527(16) -0.42245(14) 0.0189(5) Uani 1 1 d U . . O5 O 0.44027(19) 0.89779(16) 0.25165(14) 0.0203(6) Uani 1 1 d U . . O6 O 0.33337(19) 1.02971(16) 0.24880(15) 0.0207(6) Uani 1 1 d U . . C1 C 0.3352(3) 1.1280(2) -0.0439(2) 0.0172(7) Uani 1 1 d U . . C2 C 0.2842(3) 1.2001(2) -0.1210(2) 0.0177(7) Uani 1 1 d U . . C3 C 0.1798(3) 1.2457(3) -0.1136(2) 0.0301(9) Uani 1 1 d U . . H3A H 0.1445 1.2345 -0.0590 0.036 Uiso 1 1 calc R . . C4 C 0.1286(3) 1.3073(3) -0.1871(2) 0.0303(9) Uani 1 1 d U . . H4A H 0.0582 1.3367 -0.1822 0.036 Uiso 1 1 calc R . . C5 C 0.1811(3) 1.3258(2) -0.2686(2) 0.0190(8) Uani 1 1 d U . . C6 C 0.2860(3) 1.2815(3) -0.2747(2) 0.0248(8) Uani 1 1 d U . . H6A H 0.3220 1.2941 -0.3287 0.030 Uiso 1 1 calc R . . C7 C 0.3383(3) 1.2188(3) -0.2018(2) 0.0270(9) Uani 1 1 d U . . H7A H 0.4087 1.1895 -0.2068 0.032 Uiso 1 1 calc R . . C8 C 0.1238(3) 1.3922(2) -0.3498(2) 0.0182(8) Uani 1 1 d U . . C9 C 0.4041(3) 0.9700(2) 0.2949(2) 0.0168(7) Uani 1 1 d U . . C10 C 0.4521(3) 0.9853(2) 0.4019(2) 0.0183(8) Uani 1 1 d U . . C11 C 0.5418(3) 0.9262(3) 0.4469(2) 0.0271(9) Uani 1 1 d U . . H11A H 0.5701 0.8766 0.4114 0.032 Uiso 1 1 calc R . . C12 C 0.5889(3) 0.9409(3) 0.5441(2) 0.0280(9) Uani 1 1 d U . . H12A H 0.6488 0.9010 0.5737 0.034 Uiso 1 1 calc R . . O1W O 0.1867(2) 0.92111(19) 0.10522(17) 0.0295(6) Uani 1 1 d U . . H1M H 0.1686 0.9785 0.1106 0.035 Uiso 1 1 calc R . . C1W C 0.1004(4) 0.8735(4) 0.0376(4) 0.0684(15) Uani 1 1 d U . . H1X H 0.0303 0.8693 0.0649 0.103 Uiso 1 1 calc R . . H1Y H 0.1262 0.8090 0.0247 0.103 Uiso 1 1 calc R . . H1Z H 0.0863 0.9100 -0.0226 0.103 Uiso 1 1 calc R . . O2W O 0.3694(2) 0.77889(17) 0.08905(15) 0.0264(6) Uani 1 1 d U . . H2W H 0.3506 0.7534 0.1379 0.032 Uiso 1 1 calc R . . C2W C 0.3961(4) 0.7057(3) 0.0246(3) 0.0464(12) Uani 1 1 d U . . H2X H 0.3779 0.6428 0.0487 0.070 Uiso 1 1 calc R . . H2Y H 0.4771 0.7084 0.0205 0.070 Uiso 1 1 calc R . . H2Z H 0.3516 0.7160 -0.0395 0.070 Uiso 1 1 calc R . . O3W O 0.6891(2) 1.3233(2) -0.24037(17) 0.0802(11) Uani 1 1 d DU . . H3Z H 0.7227 1.3749 -0.2246 0.096 Uiso 1 1 calc R . . C3W C 0.5929(3) 1.3412(4) -0.3189(2) 0.0654(15) Uani 1 1 d DU . . H3M H 0.5725 1.4091 -0.3196 0.098 Uiso 1 1 calc R . . H3O H 0.5277 1.3025 -0.3083 0.098 Uiso 1 1 calc R . . H3L H 0.6148 1.3238 -0.3807 0.098 Uiso 1 1 calc R . . O4W O 0.1409(6) 0.8527(5) 0.26703(15) 0.081(2) Uani 0.50 1 d PDU . . H4I H 0.2016 0.8701 0.2501 0.121 Uiso 0.50 1 calc PR . . C4W C 0.1588(11) 0.8393(8) 0.37216(18) 0.098(3) Uani 0.50 1 d PDU . . H4U H 0.2290 0.8034 0.3923 0.147 Uiso 0.50 1 calc PR . . H4V H 0.0948 0.8037 0.3901 0.147 Uiso 0.50 1 calc PR . . H4T H 0.1644 0.9018 0.4040 0.147 Uiso 0.50 1 calc PR . . O4W' O 0.3404(2) 1.5294(6) -0.1882(5) 0.180(4) Uani 0.50 1 d PDU . . H4G H 0.2922 1.4940 -0.1690 0.270 Uiso 0.50 1 calc PR . . C4W' C 0.4545(3) 1.5048(8) -0.1364(7) 0.115(4) Uani 0.50 1 d PDU . . H4F H 0.5042 1.5608 -0.1347 0.138 Uiso 0.50 1 calc PR . . H4X H 0.4859 1.4522 -0.1698 0.138 Uiso 0.50 1 calc PR . . H4Y H 0.4492 1.4852 -0.0706 0.138 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01344(7) 0.01325(7) 0.00718(6) 0.00005(6) -0.00044(5) -0.00085(6) O1 0.0233(10) 0.0251(12) 0.0184(10) 0.0094(9) 0.0083(9) 0.0079(10) O2 0.0175(10) 0.0184(11) 0.0160(10) 0.0016(8) 0.0007(8) 0.0029(9) O3 0.0215(11) 0.0307(12) 0.0175(10) 0.0095(10) 0.0023(9) 0.0115(10) O4 0.0212(10) 0.0257(12) 0.0095(9) 0.0046(9) 0.0016(8) 0.0062(9) O5 0.0299(11) 0.0197(11) 0.0106(9) -0.0005(8) 0.0016(9) 0.0040(10) O6 0.0208(10) 0.0251(11) 0.0145(10) 0.0031(9) -0.0023(9) 0.0056(10) C1 0.0185(14) 0.0177(14) 0.0141(13) 0.0017(12) -0.0014(12) 0.0035(13) C2 0.0167(14) 0.0207(15) 0.0146(13) 0.0039(12) -0.0004(11) 0.0060(13) C3 0.0278(16) 0.043(2) 0.0221(15) 0.0139(15) 0.0115(13) 0.0126(16) C4 0.0264(16) 0.041(2) 0.0250(16) 0.0117(15) 0.0095(13) 0.0164(16) C5 0.0209(15) 0.0231(15) 0.0122(13) 0.0045(12) 0.0002(12) 0.0071(13) C6 0.0257(16) 0.0354(18) 0.0147(13) 0.0106(13) 0.0073(12) 0.0108(15) C7 0.0228(16) 0.0390(19) 0.0203(15) 0.0114(14) 0.0063(13) 0.0122(15) C8 0.0214(15) 0.0194(15) 0.0128(13) -0.0006(12) 0.0002(12) 0.0035(13) C9 0.0182(14) 0.0209(15) 0.0121(12) 0.0037(12) 0.0050(11) -0.0017(13) C10 0.0195(14) 0.0239(16) 0.0116(13) -0.0007(12) 0.0027(12) 0.0011(13) C11 0.0350(18) 0.0334(17) 0.0127(14) -0.0067(13) 0.0035(13) 0.0125(15) C12 0.0285(17) 0.0340(19) 0.0188(15) -0.0007(14) -0.0039(14) 0.0140(15) O1W 0.0260(12) 0.0299(12) 0.0326(12) -0.0060(11) 0.0045(10) -0.0078(11) C1W 0.041(2) 0.101(3) 0.064(3) -0.034(3) 0.009(2) -0.026(2) O2W 0.0412(13) 0.0188(11) 0.0195(10) 0.0008(9) 0.0057(10) -0.0050(10) C2W 0.073(3) 0.0246(18) 0.042(2) -0.0018(17) 0.011(2) -0.002(2) O3W 0.100(2) 0.081(2) 0.0477(16) 0.0334(15) -0.0247(16) -0.0631(17) C3W 0.065(3) 0.079(3) 0.048(2) 0.019(2) -0.001(2) -0.027(2) O4W 0.077(3) 0.116(4) 0.051(3) 0.027(3) 0.017(3) -0.058(3) C4W 0.090(5) 0.108(6) 0.102(5) 0.045(5) 0.032(4) -0.012(5) O4W' 0.181(6) 0.163(6) 0.192(7) -0.025(5) 0.015(5) -0.009(5) C4W' 0.123(6) 0.096(6) 0.123(6) 0.004(5) 0.014(5) 0.018(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O2 2.355(2) 3_675 ? Eu1 O3 2.371(2) 4_686 ? Eu1 O4 2.382(2) 2_544 ? Eu1 O1 2.415(2) . ? Eu1 O5 2.416(2) . ? Eu1 O1W 2.454(2) . ? Eu1 O2W 2.486(2) . ? Eu1 O6 2.602(2) . ? Eu1 O2 2.717(2) . ? Eu1 C9 2.851(3) . ? Eu1 C1 2.923(3) . ? Eu1 Eu1 4.0101(10) 3_675 ? O1 C1 1.248(4) . ? O2 C1 1.279(4) . ? O2 Eu1 2.355(2) 3_675 ? O3 C8 1.251(4) . ? O3 Eu1 2.371(2) 4_585 ? O4 C8 1.263(4) . ? O4 Eu1 2.382(2) 2_554 ? O5 C9 1.263(4) . ? O6 C9 1.260(4) . ? C1 C2 1.503(4) . ? C2 C3 1.391(5) . ? C2 C7 1.395(5) . ? C3 C4 1.378(5) . ? C3 H3A 0.9300 . ? C4 C5 1.392(5) . ? C4 H4A 0.9300 . ? C5 C6 1.385(5) . ? C5 C8 1.512(4) . ? C6 C7 1.387(4) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C9 C10 1.506(4) . ? C10 C12 1.387(5) 3_676 ? C10 C11 1.390(5) . ? C11 C12 1.379(4) . ? C11 H11A 0.9300 . ? C12 C10 1.387(5) 3_676 ? C12 H12A 0.9300 . ? O1W C1W 1.417(5) . ? O1W H1M 0.8200 . ? C1W H1X 0.9600 . ? C1W H1Y 0.9600 . ? C1W H1Z 0.9600 . ? O2W C2W 1.410(5) . ? O2W H2W 0.8200 . ? C2W H2X 0.9600 . ? C2W H2Y 0.9600 . ? C2W H2Z 0.9600 . ? O3W C3W 1.450(2) . ? O3W H3Z 0.8200 . ? C3W H3M 0.9600 . ? C3W H3O 0.9600 . ? C3W H3L 0.9600 . ? O4W C4W 1.443(2) . ? O4W H4I 0.8200 . ? C4W H4U 0.9600 . ? C4W H4V 0.9600 . ? C4W H4T 0.9600 . ? O4W' C4W' 1.448(3) . ? O4W' H4G 0.8200 . ? C4W' H4F 0.9600 . ? C4W' H4X 0.9600 . ? C4W' H4Y 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 O2 Eu1 O3 73.79(8) 3_675 4_686 ? O2 Eu1 O4 79.37(7) 3_675 2_544 ? O3 Eu1 O4 134.25(8) 4_686 2_544 ? O2 Eu1 O1 126.07(7) 3_675 . ? O3 Eu1 O1 86.32(8) 4_686 . ? O4 Eu1 O1 80.38(7) 2_544 . ? O2 Eu1 O5 90.72(8) 3_675 . ? O3 Eu1 O5 76.14(8) 4_686 . ? O4 Eu1 O5 141.06(7) 2_544 . ? O1 Eu1 O5 132.81(7) . . ? O2 Eu1 O1W 148.31(8) 3_675 . ? O3 Eu1 O1W 135.10(8) 4_686 . ? O4 Eu1 O1W 83.51(8) 2_544 . ? O1 Eu1 O1W 76.19(8) . . ? O5 Eu1 O1W 86.04(8) . . ? O2 Eu1 O2W 76.67(8) 3_675 . ? O3 Eu1 O2W 133.61(8) 4_686 . ? O4 Eu1 O2W 71.81(7) 2_544 . ? O1 Eu1 O2W 140.04(7) . . ? O5 Eu1 O2W 69.26(7) . . ? O1W Eu1 O2W 72.71(8) . . ? O2 Eu1 O6 131.67(7) 3_675 . ? O3 Eu1 O6 68.81(8) 4_686 . ? O4 Eu1 O6 148.86(7) 2_544 . ? O1 Eu1 O6 81.13(7) . . ? O5 Eu1 O6 51.71(7) . . ? O1W Eu1 O6 67.82(8) . . ? O2W Eu1 O6 108.87(7) . . ? O2 Eu1 O2 75.75(8) 3_675 . ? O3 Eu1 O2 69.13(7) 4_686 . ? O4 Eu1 O2 68.74(7) 2_544 . ? O1 Eu1 O2 50.33(7) . . ? O5 Eu1 O2 144.99(7) . . ? O1W Eu1 O2 122.01(7) . . ? O2W Eu1 O2 135.07(7) . . ? O6 Eu1 O2 115.99(7) . . ? O2 Eu1 C9 109.61(8) 3_675 . ? O3 Eu1 C9 66.43(8) 4_686 . ? O4 Eu1 C9 159.18(8) 2_544 . ? O1 Eu1 C9 106.85(8) . . ? O5 Eu1 C9 26.11(8) . . ? O1W Eu1 C9 79.49(9) . . ? O2W Eu1 C9 91.57(8) . . ? O6 Eu1 C9 26.20(8) . . ? O2 Eu1 C9 131.03(8) . . ? O2 Eu1 C1 101.41(8) 3_675 . ? O3 Eu1 C1 79.55(8) 4_686 . ? O4 Eu1 C1 70.23(8) 2_544 . ? O1 Eu1 C1 24.77(8) . . ? O5 Eu1 C1 148.54(8) . . ? O1W Eu1 C1 97.55(9) . . ? O2W Eu1 C1 141.64(8) . . ? O6 Eu1 C1 100.73(8) . . ? O2 Eu1 C1 25.88(8) . . ? C9 Eu1 C1 123.78(9) . . ? O2 Eu1 Eu1 41.05(5) 3_675 3_675 ? O3 Eu1 Eu1 66.09(6) 4_686 3_675 ? O4 Eu1 Eu1 69.27(5) 2_544 3_675 ? O1 Eu1 Eu1 85.02(5) . 3_675 ? O5 Eu1 Eu1 124.22(6) . 3_675 ? O1W Eu1 Eu1 149.20(6) . 3_675 ? O2W Eu1 Eu1 110.14(6) . 3_675 ? O6 Eu1 Eu1 133.43(5) . 3_675 ? O2 Eu1 Eu1 34.69(4) . 3_675 ? C9 Eu1 Eu1 129.93(6) . 3_675 ? C1 Eu1 Eu1 60.43(6) . 3_675 ? C1 O1 Eu1 101.04(19) . . ? C1 O2 Eu1 167.15(19) . 3_675 ? C1 O2 Eu1 86.09(17) . . ? Eu1 O2 Eu1 104.25(7) 3_675 . ? C8 O3 Eu1 141.1(2) . 4_585 ? C8 O4 Eu1 133.67(19) . 2_554 ? C9 O5 Eu1 96.55(17) . . ? C9 O6 Eu1 88.00(18) . . ? O1 C1 O2 121.0(3) . . ? O1 C1 C2 119.7(3) . . ? O2 C1 C2 119.3(3) . . ? O1 C1 Eu1 54.18(15) . . ? O2 C1 Eu1 68.02(16) . . ? C2 C1 Eu1 166.3(2) . . ? C3 C2 C7 119.8(3) . . ? C3 C2 C1 119.7(3) . . ? C7 C2 C1 120.5(3) . . ? C4 C3 C2 120.1(3) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C3 C4 C5 120.6(3) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C6 C5 C4 118.9(3) . . ? C6 C5 C8 120.6(3) . . ? C4 C5 C8 120.5(3) . . ? C5 C6 C7 121.2(3) . . ? C5 C6 H6A 119.4 . . ? C7 C6 H6A 119.4 . . ? C6 C7 C2 119.3(3) . . ? C6 C7 H7A 120.4 . . ? C2 C7 H7A 120.4 . . ? O3 C8 O4 126.2(3) . . ? O3 C8 C5 116.3(3) . . ? O4 C8 C5 117.5(3) . . ? O6 C9 O5 120.9(3) . . ? O6 C9 C10 120.9(3) . . ? O5 C9 C10 118.2(3) . . ? O6 C9 Eu1 65.80(16) . . ? O5 C9 Eu1 57.34(14) . . ? C10 C9 Eu1 161.6(2) . . ? C12 C10 C11 119.1(3) 3_676 . ? C12 C10 C9 121.5(3) 3_676 . ? C11 C10 C9 119.3(3) . . ? C12 C11 C10 120.1(3) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C11 C12 C10 120.7(3) . 3_676 ? C11 C12 H12A 119.6 . . ? C10 C12 H12A 119.6 3_676 . ? C1W O1W Eu1 128.3(3) . . ? C1W O1W H1M 109.5 . . ? Eu1 O1W H1M 93.8 . . ? O1W C1W H1X 109.5 . . ? O1W C1W H1Y 109.5 . . ? H1X C1W H1Y 109.5 . . ? O1W C1W H1Z 109.5 . . ? H1X C1W H1Z 109.5 . . ? H1Y C1W H1Z 109.5 . . ? C2W O2W Eu1 132.3(2) . . ? C2W O2W H2W 109.5 . . ? Eu1 O2W H2W 117.9 . . ? O2W C2W H2X 109.5 . . ? O2W C2W H2Y 109.5 . . ? H2X C2W H2Y 109.5 . . ? O2W C2W H2Z 109.5 . . ? H2X C2W H2Z 109.5 . . ? H2Y C2W H2Z 109.5 . . ? C3W O3W H3Z 109.5 . . ? O3W C3W H3M 109.5 . . ? O3W C3W H3O 109.5 . . ? H3M C3W H3O 109.5 . . ? O3W C3W H3L 109.5 . . ? H3M C3W H3L 109.5 . . ? H3O C3W H3L 109.5 . . ? C4W O4W H4I 109.5 . . ? O4W C4W H4U 109.5 . . ? O4W C4W H4V 109.5 . . ? H4U C4W H4V 109.5 . . ? O4W C4W H4T 109.5 . . ? H4U C4W H4T 109.5 . . ? H4V C4W H4T 109.5 . . ? C4W' O4W' H4G 109.5 . . ? O4W' C4W' H4F 109.5 . . ? O4W' C4W' H4X 109.5 . . ? H4F C4W' H4X 109.5 . . ? O4W' C4W' H4Y 109.5 . . ? H4F C4W' H4Y 109.5 . . ? H4X C4W' H4Y 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.453 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.181 # Attachment 'Complex-2(final).CIF' data_complex-2 _database_code_depnum_ccdc_archive 'CCDC 644755' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H24.50 Cl Eu O9.25' _chemical_formula_weight 516.24 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' 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 11.573(2) _cell_length_b 16.726(3) _cell_length_c 12.162(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.55(3) _cell_angle_gamma 90.00 _cell_volume 2204.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 153(1) _cell_measurement_reflns_used CCD _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1026 _exptl_absorpt_coefficient_mu 3.002 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.5361 _exptl_absorpt_correction_T_max 0.6922 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(1) _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 CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7098 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_sigmaI/netI 0.1341 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3879 _reflns_number_gt 2261 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _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^)+(0.0354P)^2^+4.5648P] 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 SHELXL _refine_ls_extinction_coef 0.0052(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.21(6) _refine_ls_number_reflns 3879 _refine_ls_number_parameters 223 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.1201 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1813 _refine_ls_wR_factor_gt 0.1483 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.020 _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 Eu1 Eu 0.37384(5) 0.02497(3) 0.08089(5) 0.0255(2) Uani 1 1 d U . . Cl1 Cl 0.0152(3) -0.1572(2) 0.0522(3) 0.0502(9) Uani 1 1 d U . . O1 O 0.4634(7) -0.1166(5) -0.1238(7) 0.032(2) Uani 1 1 d U . . O2 O 0.3457(7) -0.1010(4) -0.0150(6) 0.030(2) Uani 1 1 d U . . O3 O 0.0056(7) -0.4375(5) -0.2756(7) 0.032(2) Uani 1 1 d U . . O4 O 0.1040(7) -0.4472(4) -0.4024(7) 0.032(2) Uani 1 1 d U . . C1 C 0.3774(11) -0.1367(7) -0.0888(10) 0.027(3) Uani 1 1 d U . . C2 C 0.3035(11) -0.2091(7) -0.1460(10) 0.027(3) Uani 1 1 d U . . C3 C 0.3379(11) -0.2527(7) -0.2271(10) 0.033(3) Uani 1 1 d U . . H3A H 0.4057 -0.2371 -0.2461 0.039 Uiso 1 1 calc R . . C4 C 0.2689(11) -0.3205(7) -0.2802(10) 0.031(3) Uani 1 1 d U . . H4A H 0.2921 -0.3502 -0.3337 0.037 Uiso 1 1 calc R . . C5 C 0.1660(10) -0.3436(6) -0.2532(10) 0.026(3) Uani 1 1 d U . . C6 C 0.1337(11) -0.2998(7) -0.1679(10) 0.031(3) Uani 1 1 d U . . H6A H 0.0677 -0.3159 -0.1464 0.037 Uiso 1 1 calc R . . C7 C 0.2019(11) -0.2329(7) -0.1175(10) 0.034(3) Uani 1 1 d U . . H7A H 0.1796 -0.2031 -0.0635 0.041 Uiso 1 1 calc R . . C8 C 0.0840(12) -0.4147(7) -0.3133(11) 0.035(3) Uani 1 1 d U . . O1W O 0.2653(7) 0.1544(4) 0.0685(7) 0.035(2) Uani 1 1 d U . . H1W H 0.1965 0.1520 0.0177 0.041 Uiso 1 1 calc R . . C1W C 0.3125(18) 0.2358(11) 0.0749(16) 0.092(6) Uani 1 1 d U . . H1WA H 0.2477 0.2730 0.0700 0.138 Uiso 1 1 calc R . . H1WB H 0.3413 0.2448 0.0109 0.138 Uiso 1 1 calc R . . H1WC H 0.3794 0.2431 0.1480 0.138 Uiso 1 1 calc R . . O2W O 0.4139(8) 0.0806(5) 0.2832(7) 0.040(2) Uani 1 1 d U . . H2W H 0.3796 0.1242 0.2767 0.048 Uiso 1 1 calc R . . C2W C 0.5257(14) 0.0822(10) 0.3808(12) 0.062(4) Uani 1 1 d U . . H2WA H 0.5118 0.1070 0.4463 0.093 Uiso 1 1 calc R . . H2WB H 0.5864 0.1122 0.3609 0.093 Uiso 1 1 calc R . . H2WC H 0.5547 0.0286 0.4013 0.093 Uiso 1 1 calc R . . O3W O 0.2316(8) -0.0370(5) 0.1673(7) 0.040(2) Uani 1 1 d U . . H3W H 0.2027 0.0084 0.1571 0.048 Uiso 1 1 calc R . . C3W C 0.2501(16) -0.0610(10) 0.2809(13) 0.068(5) Uani 1 1 d U . . H3WA H 0.1749 -0.0831 0.2845 0.102 Uiso 1 1 calc R . . H3WB H 0.2744 -0.0159 0.3327 0.102 Uiso 1 1 calc R . . H3WC H 0.3138 -0.1009 0.3044 0.102 Uiso 1 1 calc R . . O4W O 0.1550(7) 0.0178(5) -0.0607(7) 0.038(2) Uani 1 1 d U . . H4W H 0.1056 0.0494 -0.0505 0.045 Uiso 1 1 calc R . . C4W C 0.1013(13) -0.0195(8) -0.1732(12) 0.051(4) Uani 1 1 d U . . H4WA H 0.0135 -0.0115 -0.2016 0.076 Uiso 1 1 calc R . . H4WB H 0.1189 -0.0757 -0.1661 0.076 Uiso 1 1 calc R . . H4WC H 0.1353 0.0037 -0.2273 0.076 Uiso 1 1 calc R . . O5W O 0.3011(12) 0.2087(8) 0.3344(12) 0.113(5) Uani 1 1 d U . . H5WD H 0.3436 0.2337 0.3925 0.136 Uiso 1 1 calc R . . C5W C 0.1745(17) 0.2301(12) 0.3061(15) 0.093(6) Uani 1 1 d U . . H5WC H 0.1361 0.2356 0.2226 0.139 Uiso 1 1 calc R . . H5WB H 0.1693 0.2800 0.3432 0.139 Uiso 1 1 calc R . . H5WA H 0.1331 0.1892 0.3336 0.139 Uiso 1 1 calc R . . O6W O 0.0000 0.0000 -0.5000 0.19(3) Uani 0.50 2 d SPU . . H6WA H -0.0416 -0.0005 -0.5731 0.234 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0242(4) 0.0195(4) 0.0288(4) -0.0011(3) 0.0043(3) -0.0002(3) Cl1 0.0316(19) 0.048(2) 0.070(2) -0.0108(19) 0.0162(17) 0.0014(17) O1 0.026(4) 0.030(4) 0.038(4) -0.006(4) 0.009(4) -0.006(4) O2 0.034(4) 0.030(4) 0.022(4) -0.010(3) 0.006(4) 0.001(4) O3 0.031(4) 0.028(4) 0.038(4) 0.002(4) 0.013(4) -0.008(4) O4 0.033(5) 0.025(4) 0.033(4) -0.004(4) 0.005(4) 0.003(4) C1 0.022(6) 0.027(6) 0.031(6) -0.004(5) 0.008(5) 0.005(5) C2 0.025(6) 0.029(6) 0.029(6) -0.002(5) 0.011(5) 0.002(5) C3 0.029(6) 0.037(6) 0.034(6) -0.006(5) 0.012(5) -0.003(5) C4 0.038(6) 0.025(6) 0.033(6) -0.011(5) 0.015(5) -0.001(5) C5 0.022(6) 0.023(5) 0.030(6) -0.002(5) 0.004(5) 0.001(5) C6 0.034(6) 0.026(6) 0.031(6) -0.004(5) 0.009(5) -0.001(5) C7 0.032(6) 0.033(6) 0.035(6) -0.004(5) 0.011(5) 0.001(5) C8 0.035(6) 0.022(6) 0.036(6) -0.003(5) -0.001(5) 0.001(5) O1W 0.031(5) 0.024(4) 0.041(4) -0.005(4) 0.004(4) -0.001(4) C1W 0.094(9) 0.086(9) 0.093(9) -0.011(8) 0.029(8) 0.004(8) O2W 0.045(5) 0.041(5) 0.032(4) -0.002(4) 0.011(4) 0.003(4) C2W 0.065(8) 0.066(8) 0.047(7) 0.002(6) 0.009(6) 0.007(7) O3W 0.044(5) 0.039(5) 0.040(5) 0.010(4) 0.017(4) 0.003(4) C3W 0.076(9) 0.071(8) 0.058(8) 0.000(7) 0.023(7) -0.003(7) O4W 0.031(5) 0.032(5) 0.041(5) -0.006(4) 0.002(4) 0.000(4) C4W 0.043(7) 0.042(7) 0.055(7) -0.011(6) 0.002(6) 0.005(6) O5W 0.089(8) 0.104(8) 0.122(8) -0.056(7) 0.007(6) 0.016(6) C5W 0.081(9) 0.102(10) 0.092(9) -0.025(8) 0.028(7) 0.017(8) O6W 0.20(3) 0.21(3) 0.18(3) -0.010(10) 0.072(13) -0.006(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O4 2.321(8) 2_554 ? Eu1 O1 2.341(8) 3_655 ? Eu1 O2 2.375(7) . ? Eu1 O3 2.376(8) 4_656 ? Eu1 O3W 2.471(8) . ? Eu1 O1W 2.481(8) . ? Eu1 O4W 2.516(8) . ? Eu1 O2W 2.517(8) . ? Eu1 O4 2.907(8) 4_656 ? Eu1 C8 2.963(12) 4_656 ? Eu1 Eu1 4.1388(15) 3_655 ? O1 C1 1.258(13) . ? O1 Eu1 2.341(8) 3_655 ? O2 C1 1.235(13) . ? O3 C8 1.213(14) . ? O3 Eu1 2.376(8) 4 ? O4 C8 1.304(14) . ? O4 Eu1 2.321(8) 2_544 ? O4 Eu1 2.907(8) 4 ? C1 C2 1.506(16) . ? C2 C3 1.392(16) . ? C2 C7 1.395(16) . ? C3 C4 1.407(16) . ? C3 H3A 0.9300 . ? C4 C5 1.396(16) . ? C4 H4A 0.9300 . ? C5 C6 1.424(16) . ? C5 C8 1.537(16) . ? C6 C7 1.382(16) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 Eu1 2.963(12) 4 ? O1W C1W 1.458(19) . ? O1W H1W 0.8200 . ? C1W H1WA 0.9600 . ? C1W H1WB 0.9600 . ? C1W H1WC 0.9600 . ? O2W C2W 1.416(15) . ? O2W H2W 0.8200 . ? C2W H2WA 0.9600 . ? C2W H2WB 0.9600 . ? C2W H2WC 0.9600 . ? O3W C3W 1.381(16) . ? O3W H3W 0.8200 . ? C3W H3WA 0.9600 . ? C3W H3WB 0.9600 . ? C3W H3WC 0.9600 . ? O4W C4W 1.432(14) . ? O4W H4W 0.8200 . ? C4W H4WA 0.9600 . ? C4W H4WB 0.9600 . ? C4W H4WC 0.9600 . ? O5W C5W 1.43(2) . ? O5W H5WD 0.8200 . ? C5W H5WC 0.9600 . ? C5W H5WB 0.9600 . ? C5W H5WA 0.9600 . ? O6W H6WA 0.8500 . ? 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 Eu1 O1 74.5(3) 2_554 3_655 ? O4 Eu1 O2 76.1(3) 2_554 . ? O1 Eu1 O2 130.7(3) 3_655 . ? O4 Eu1 O3 123.9(3) 2_554 4_656 ? O1 Eu1 O3 88.9(3) 3_655 4_656 ? O2 Eu1 O3 75.9(3) . 4_656 ? O4 Eu1 O3W 142.3(3) 2_554 . ? O1 Eu1 O3W 141.6(3) 3_655 . ? O2 Eu1 O3W 80.8(3) . . ? O3 Eu1 O3W 77.3(3) 4_656 . ? O4 Eu1 O1W 89.3(3) 2_554 . ? O1 Eu1 O1W 78.0(3) 3_655 . ? O2 Eu1 O1W 139.9(3) . . ? O3 Eu1 O1W 139.7(3) 4_656 . ? O3W Eu1 O1W 89.6(3) . . ? O4 Eu1 O4W 77.6(3) 2_554 . ? O1 Eu1 O4W 136.2(3) 3_655 . ? O2 Eu1 O4W 72.0(3) . . ? O3 Eu1 O4W 134.9(3) 4_656 . ? O3W Eu1 O4W 67.1(3) . . ? O1W Eu1 O4W 68.5(3) . . ? O4 Eu1 O2W 142.9(3) 2_554 . ? O1 Eu1 O2W 71.5(3) 3_655 . ? O2 Eu1 O2W 139.0(3) . . ? O3 Eu1 O2W 70.0(3) 4_656 . ? O3W Eu1 O2W 70.2(3) . . ? O1W Eu1 O2W 69.7(3) . . ? O4W Eu1 O2W 118.9(3) . . ? O4 Eu1 O4 75.9(3) 2_554 4_656 ? O1 Eu1 O4 68.4(2) 3_655 4_656 ? O2 Eu1 O4 66.5(2) . 4_656 ? O3 Eu1 O4 48.5(2) 4_656 4_656 ? O3W Eu1 O4 120.9(3) . 4_656 ? O1W Eu1 O4 145.8(2) . 4_656 ? O4W Eu1 O4 134.7(2) . 4_656 ? O2W Eu1 O4 104.3(2) . 4_656 ? O4 Eu1 C8 100.8(3) 2_554 4_656 ? O1 Eu1 C8 80.7(3) 3_655 4_656 ? O2 Eu1 C8 67.1(3) . 4_656 ? O3 Eu1 C8 23.1(3) 4_656 4_656 ? O3W Eu1 C8 97.0(3) . 4_656 ? O1W Eu1 C8 153.0(3) . 4_656 ? O4W Eu1 C8 138.0(3) . 4_656 ? O2W Eu1 C8 87.9(3) . 4_656 ? O4 Eu1 C8 25.7(3) 4_656 4_656 ? O4 Eu1 Eu1 42.9(2) 2_554 3_655 ? O1 Eu1 Eu1 65.91(19) 3_655 3_655 ? O2 Eu1 Eu1 65.50(19) . 3_655 ? O3 Eu1 Eu1 81.21(19) 4_656 3_655 ? O3W Eu1 Eu1 143.6(2) . 3_655 ? O1W Eu1 Eu1 125.01(19) . 3_655 ? O4W Eu1 Eu1 111.93(19) . 3_655 ? O2W Eu1 Eu1 128.38(19) . 3_655 ? O4 Eu1 Eu1 32.94(16) 4_656 3_655 ? C8 Eu1 Eu1 58.2(3) 4_656 3_655 ? C1 O1 Eu1 140.3(7) . 3_655 ? C1 O2 Eu1 139.5(8) . . ? C8 O3 Eu1 106.7(7) . 4 ? C8 O4 Eu1 166.3(7) . 2_544 ? C8 O4 Eu1 79.6(7) . 4 ? Eu1 O4 Eu1 104.1(3) 2_544 4 ? O2 C1 O1 126.1(11) . . ? O2 C1 C2 117.3(11) . . ? O1 C1 C2 116.5(10) . . ? C3 C2 C7 120.2(11) . . ? C3 C2 C1 119.4(10) . . ? C7 C2 C1 120.4(10) . . ? C2 C3 C4 119.3(11) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C5 C4 C3 120.6(10) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? C4 C5 C6 119.6(10) . . ? C4 C5 C8 122.6(10) . . ? C6 C5 C8 117.9(11) . . ? C7 C6 C5 119.0(11) . . ? C7 C6 H6A 120.5 . . ? C5 C6 H6A 120.5 . . ? C6 C7 C2 121.4(12) . . ? C6 C7 H7A 119.3 . . ? C2 C7 H7A 119.3 . . ? O3 C8 O4 123.9(11) . . ? O3 C8 C5 118.9(11) . . ? O4 C8 C5 117.2(11) . . ? O3 C8 Eu1 50.2(6) . 4 ? O4 C8 Eu1 74.8(6) . 4 ? C5 C8 Eu1 164.7(8) . 4 ? C1W O1W Eu1 129.7(9) . . ? C1W O1W H1W 109.5 . . ? Eu1 O1W H1W 109.9 . . ? O1W C1W H1WA 109.5 . . ? O1W C1W H1WB 109.5 . . ? H1WA C1W H1WB 109.5 . . ? O1W C1W H1WC 109.5 . . ? H1WA C1W H1WC 109.5 . . ? H1WB C1W H1WC 109.5 . . ? C2W O2W Eu1 128.8(8) . . ? C2W O2W H2W 109.5 . . ? Eu1 O2W H2W 108.4 . . ? O2W C2W H2WA 109.5 . . ? O2W C2W H2WB 109.5 . . ? H2WA C2W H2WB 109.5 . . ? O2W C2W H2WC 109.5 . . ? H2WA C2W H2WC 109.5 . . ? H2WB C2W H2WC 109.5 . . ? C3W O3W Eu1 130.9(9) . . ? C3W O3W H3W 109.5 . . ? Eu1 O3W H3W 81.1 . . ? O3W C3W H3WA 109.5 . . ? O3W C3W H3WB 109.5 . . ? H3WA C3W H3WB 109.5 . . ? O3W C3W H3WC 109.5 . . ? H3WA C3W H3WC 109.5 . . ? H3WB C3W H3WC 109.5 . . ? C4W O4W Eu1 132.1(8) . . ? C4W O4W H4W 109.5 . . ? Eu1 O4W H4W 117.0 . . ? O4W C4W H4WA 109.5 . . ? O4W C4W H4WB 109.5 . . ? H4WA C4W H4WB 109.5 . . ? O4W C4W H4WC 109.5 . . ? H4WA C4W H4WC 109.5 . . ? H4WB C4W H4WC 109.5 . . ? C5W O5W H5WD 109.5 . . ? O5W C5W H5WC 109.5 . . ? O5W C5W H5WB 109.5 . . ? H5WC C5W H5WB 109.5 . . ? O5W C5W H5WA 109.5 . . ? H5WC C5W H5WA 109.5 . . ? H5WB C5W H5WA 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.044 _refine_diff_density_min -0.985 _refine_diff_density_rms 0.218 # Attachment 'Complex-3(final).CIF' data_complex-3 _database_code_depnum_ccdc_archive 'CCDC 644756' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H24.50 Cl Gd O9.25' _chemical_formula_weight 521.53 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 11.518(2) _cell_length_b 16.889(3) _cell_length_c 12.161(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.59(3) _cell_angle_gamma 90.00 _cell_volume 2199.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 153(1) _cell_measurement_reflns_used CCD _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1030 _exptl_absorpt_coefficient_mu 3.172 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.5782 _exptl_absorpt_correction_T_max 0.7053 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(1) _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 CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8889 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5023 _reflns_number_gt 3619 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _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^)+(0.0726P)^2^+7.9662P] 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 shelxl _refine_ls_extinction_coef 0.0036(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.10(8) _refine_ls_number_reflns 5023 _refine_ls_number_parameters 223 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1449 _refine_ls_wR_factor_gt 0.1311 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.072 _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 1.37305(3) -0.024450(17) 1.08166(3) 0.02019(13) Uani 1 1 d U . . Cl1 Cl 1.01644(17) 0.15848(12) 1.0513(2) 0.0434(5) Uani 1 1 d U . . O1 O 1.4595(4) 0.1120(3) 0.8723(4) 0.0302(11) Uani 1 1 d U . . O2 O 1.3421(4) 0.0985(3) 0.9818(4) 0.0260(11) Uani 1 1 d U . . O3 O 1.1101(5) 0.4434(3) 0.5977(4) 0.0307(11) Uani 1 1 d U . . O4 O 1.0102(5) 0.4369(3) 0.7211(4) 0.0313(11) Uani 1 1 d U . . C1 C 1.3737(6) 0.1330(4) 0.9077(6) 0.0242(15) Uani 1 1 d U . . C2 C 1.3030(6) 0.2068(4) 0.8509(6) 0.0229(14) Uani 1 1 d U . . C3 C 1.3365(7) 0.2499(4) 0.7690(6) 0.0288(16) Uani 1 1 d U . . H3A H 1.4038 0.2337 0.7496 0.035 Uiso 1 1 calc R . . C4 C 1.2692(7) 0.3169(4) 0.7167(6) 0.0293(16) Uani 1 1 d U . . H4A H 1.2918 0.3455 0.6624 0.035 Uiso 1 1 calc R . . C5 C 1.1683(6) 0.3418(4) 0.7446(6) 0.0248(15) Uani 1 1 d U . . C6 C 1.1357(6) 0.2996(4) 0.8272(6) 0.0270(15) Uani 1 1 d U . . H6A H 1.0697 0.3169 0.8477 0.032 Uiso 1 1 calc R . . C7 C 1.2010(6) 0.2319(4) 0.8790(6) 0.0276(15) Uani 1 1 d U . . H7A H 1.1773 0.2031 0.9324 0.033 Uiso 1 1 calc R . . C8 C 1.0910(6) 0.4119(4) 0.6839(6) 0.0256(15) Uani 1 1 d U . . O1W O 1.2661(5) -0.1517(3) 1.0730(5) 0.0314(12) Uani 1 1 d U . . H1W H 1.1911 -0.1536 1.0604 0.038 Uiso 1 1 calc R . . C1W C 1.3148(9) -0.2308(5) 1.0810(9) 0.053(2) Uani 1 1 d U . . H1WA H 1.2500 -0.2682 1.0746 0.080 Uiso 1 1 calc R . . H1WB H 1.3823 -0.2375 1.1556 0.080 Uiso 1 1 calc R . . H1WC H 1.3447 -0.2394 1.0179 0.080 Uiso 1 1 calc R . . O2W O 1.2337(5) 0.0367(3) 1.1680(5) 0.0361(13) Uani 1 1 d U . . H2W H 1.1805 0.0655 1.1220 0.043 Uiso 1 1 calc R . . C2W C 1.2564(9) 0.0608(6) 1.2846(8) 0.051(2) Uani 1 1 d U . . H2WA H 1.1818 0.0836 1.2889 0.077 Uiso 1 1 calc R . . H2WB H 1.3222 0.0994 1.3084 0.077 Uiso 1 1 calc R . . H2WC H 1.2806 0.0158 1.3363 0.077 Uiso 1 1 calc R . . O3W O 1.4180(5) -0.0779(3) 1.2852(4) 0.0345(12) Uani 1 1 d U . . H3W H 1.3827 -0.1204 1.2828 0.041 Uiso 1 1 calc R . . C3W C 1.5312(8) -0.0766(6) 1.3841(7) 0.049(2) Uani 1 1 d U . . H3WA H 1.5204 -0.1040 1.4488 0.074 Uiso 1 1 calc R . . H3WB H 1.5549 -0.0227 1.4066 0.074 Uiso 1 1 calc R . . H3WC H 1.5954 -0.1021 1.3643 0.074 Uiso 1 1 calc R . . O4W O 1.1510(5) -0.0181(3) 0.9397(5) 0.0348(13) Uani 1 1 d U . . H4W H 1.1060 -0.0538 0.9467 0.042 Uiso 1 1 calc R . . C4W C 1.0955(8) 0.0168(5) 0.8240(7) 0.044(2) Uani 1 1 d U . . H4WA H 1.0069 0.0086 0.7946 0.066 Uiso 1 1 calc R . . H4WB H 1.1299 -0.0074 0.7714 0.066 Uiso 1 1 calc R . . H4WC H 1.1128 0.0726 0.8290 0.066 Uiso 1 1 calc R . . O5W O 1.3038(7) -0.1989(5) 1.3469(8) 0.085(3) Uani 1 1 d U . . H5WE H 1.3413 -0.2160 1.4138 0.101 Uiso 1 1 calc R . . C5W C 1.1784(10) -0.2242(8) 1.3072(11) 0.077(3) Uani 1 1 d U . . H5WC H 1.1277 -0.1891 1.2464 0.116 Uiso 1 1 calc R . . H5WB H 1.1499 -0.2238 1.3720 0.116 Uiso 1 1 calc R . . H5WA H 1.1723 -0.2769 1.2760 0.116 Uiso 1 1 calc R . . O6W O 1.0000 0.0000 0.5000 0.048(4) Uani 0.50 2 d SPU . . H6WA H 0.9775 0.0251 0.4371 0.057 Uiso 0.50 1 d PR . . 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 0.01813(18) 0.01582(18) 0.0238(2) 0.00046(13) 0.00441(13) 0.00014(13) Cl1 0.0241(9) 0.0414(11) 0.0637(14) 0.0092(10) 0.0151(9) -0.0005(8) O1 0.026(2) 0.027(3) 0.038(3) 0.008(2) 0.012(2) 0.006(2) O2 0.026(2) 0.022(2) 0.028(3) 0.009(2) 0.007(2) 0.002(2) O3 0.032(3) 0.024(2) 0.030(3) 0.004(2) 0.005(2) -0.004(2) O4 0.030(3) 0.030(3) 0.034(3) 0.001(2) 0.012(2) 0.007(2) C1 0.021(3) 0.024(3) 0.023(3) -0.002(3) 0.004(3) -0.002(3) C2 0.022(3) 0.022(3) 0.025(3) 0.002(3) 0.008(3) -0.002(3) C3 0.027(3) 0.029(4) 0.032(4) 0.002(3) 0.014(3) 0.003(3) C4 0.031(4) 0.030(4) 0.028(4) 0.009(3) 0.011(3) 0.003(3) C5 0.021(3) 0.022(3) 0.030(4) 0.003(3) 0.009(3) 0.002(3) C6 0.025(3) 0.025(3) 0.029(4) 0.003(3) 0.009(3) 0.006(3) C7 0.029(4) 0.021(3) 0.035(4) 0.005(3) 0.013(3) 0.000(3) C8 0.023(3) 0.022(3) 0.027(4) 0.000(3) 0.003(3) -0.001(3) O1W 0.027(3) 0.022(2) 0.043(3) 0.003(2) 0.010(2) -0.003(2) C1W 0.054(5) 0.035(5) 0.064(6) 0.002(4) 0.015(5) -0.007(4) O2W 0.029(3) 0.045(3) 0.032(3) -0.001(2) 0.009(2) 0.010(2) C2W 0.053(5) 0.058(6) 0.043(5) -0.006(5) 0.017(4) 0.016(5) O3W 0.037(3) 0.033(3) 0.031(3) 0.004(2) 0.009(2) 0.000(2) C3W 0.048(5) 0.053(5) 0.033(4) 0.005(4) -0.002(4) 0.003(4) O4W 0.027(3) 0.029(3) 0.040(3) 0.005(2) 0.004(2) -0.004(2) C4W 0.038(4) 0.041(5) 0.036(5) 0.007(4) -0.005(4) -0.007(4) O5W 0.071(5) 0.070(5) 0.097(6) 0.047(5) 0.013(4) -0.003(4) C5W 0.056(6) 0.089(9) 0.079(8) 0.025(7) 0.018(6) -0.006(6) O6W 0.033(8) 0.071(11) 0.038(9) 0.039(9) 0.011(7) 0.025(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 O3 2.324(5) 2_746 ? Gd1 O1 2.329(5) 3_857 ? Gd1 O4 2.364(5) 4_666 ? Gd1 O2 2.366(4) . ? Gd1 O2W 2.447(5) . ? Gd1 O1W 2.460(5) . ? Gd1 O3W 2.503(5) . ? Gd1 O4W 2.507(5) . ? Gd1 C8 3.028(7) 4_666 ? O1 C1 1.265(8) . ? O1 Gd1 2.329(5) 3_857 ? O2 C1 1.234(8) . ? O3 C8 1.265(9) . ? O3 Gd1 2.324(5) 2_756 ? O4 C8 1.249(9) . ? O4 Gd1 2.364(5) 4_565 ? C1 C2 1.511(9) . ? C2 C3 1.399(10) . ? C2 C7 1.404(10) . ? C3 C4 1.386(10) . ? C3 H3A 0.9300 . ? C4 C5 1.391(10) . ? C4 H4A 0.9300 . ? C5 C6 1.391(10) . ? C5 C8 1.502(9) . ? C6 C7 1.385(9) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 Gd1 3.028(7) 4_565 ? O1W C1W 1.439(10) . ? O1W H1W 0.8200 . ? C1W H1WA 0.9600 . ? C1W H1WB 0.9600 . ? C1W H1WC 0.9600 . ? O2W C2W 1.404(10) . ? O2W H2W 0.8200 . ? C2W H2WA 0.9600 . ? C2W H2WB 0.9600 . ? C2W H2WC 0.9600 . ? O3W C3W 1.412(9) . ? O3W H3W 0.8200 . ? C3W H3WA 0.9600 . ? C3W H3WB 0.9600 . ? C3W H3WC 0.9600 . ? O4W C4W 1.440(9) . ? O4W H4W 0.8200 . ? C4W H4WA 0.9600 . ? C4W H4WB 0.9600 . ? C4W H4WC 0.9600 . ? O5W C5W 1.410(12) . ? O5W H5WE 0.8200 . ? C5W H5WC 0.9600 . ? C5W H5WB 0.9600 . ? C5W H5WA 0.9600 . ? O6W H6WA 0.8283 . ? 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 Gd1 O1 74.34(18) 2_746 3_857 ? O3 Gd1 O4 123.71(18) 2_746 4_666 ? O1 Gd1 O4 87.07(18) 3_857 4_666 ? O3 Gd1 O2 76.82(17) 2_746 . ? O1 Gd1 O2 129.48(17) 3_857 . ? O4 Gd1 O2 75.74(17) 4_666 . ? O3 Gd1 O2W 142.74(17) 2_746 . ? O1 Gd1 O2W 141.32(18) 3_857 . ? O4 Gd1 O2W 78.37(18) 4_666 . ? O2 Gd1 O2W 81.42(18) . . ? O3 Gd1 O1W 88.25(18) 2_746 . ? O1 Gd1 O1W 79.24(16) 3_857 . ? O4 Gd1 O1W 140.29(17) 4_666 . ? O2 Gd1 O1W 140.03(16) . . ? O2W Gd1 O1W 89.42(18) . . ? O3 Gd1 O3W 141.77(17) 2_746 . ? O1 Gd1 O3W 71.42(17) 3_857 . ? O4 Gd1 O3W 71.08(17) 4_666 . ? O2 Gd1 O3W 139.59(17) . . ? O2W Gd1 O3W 69.98(17) . . ? O1W Gd1 O3W 69.23(17) . . ? O3 Gd1 O4W 77.27(18) 2_746 . ? O1 Gd1 O4W 137.52(17) 3_857 . ? O4 Gd1 O4W 135.29(17) 4_666 . ? O2 Gd1 O4W 71.71(16) . . ? O2W Gd1 O4W 67.28(18) . . ? O1W Gd1 O4W 68.88(16) . . ? O3W Gd1 O4W 118.94(17) . . ? O3 Gd1 C8 100.90(19) 2_746 4_666 ? O1 Gd1 C8 79.14(18) 3_857 4_666 ? O4 Gd1 C8 22.80(18) 4_666 4_666 ? O2 Gd1 C8 66.74(17) . 4_666 ? O2W Gd1 C8 97.71(19) . 4_666 ? O1W Gd1 C8 153.22(17) . 4_666 ? O3W Gd1 C8 88.96(18) . 4_666 ? O4W Gd1 C8 137.54(17) . 4_666 ? C1 O1 Gd1 141.0(5) . 3_857 ? C1 O2 Gd1 139.4(5) . . ? C8 O3 Gd1 167.4(5) . 2_756 ? C8 O4 Gd1 110.0(4) . 4_565 ? O2 C1 O1 126.4(6) . . ? O2 C1 C2 117.9(6) . . ? O1 C1 C2 115.7(6) . . ? C3 C2 C7 119.4(6) . . ? C3 C2 C1 120.8(6) . . ? C7 C2 C1 119.8(6) . . ? C4 C3 C2 119.8(7) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C3 C4 C5 120.7(7) . . ? C3 C4 H4A 119.6 . . ? C5 C4 H4A 119.6 . . ? C4 C5 C6 119.6(6) . . ? C4 C5 C8 121.0(6) . . ? C6 C5 C8 119.4(6) . . ? C7 C6 C5 120.3(7) . . ? C7 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? C6 C7 C2 120.1(7) . . ? C6 C7 H7A 119.9 . . ? C2 C7 H7A 119.9 . . ? O4 C8 O3 122.6(6) . . ? O4 C8 C5 118.3(6) . . ? O3 C8 C5 119.2(6) . . ? O4 C8 Gd1 47.2(3) . 4_565 ? O3 C8 Gd1 76.5(4) . 4_565 ? C5 C8 Gd1 161.6(5) . 4_565 ? C1W O1W Gd1 129.1(5) . . ? C1W O1W H1W 109.5 . . ? Gd1 O1W H1W 121.3 . . ? O1W C1W H1WA 109.5 . . ? O1W C1W H1WB 109.5 . . ? H1WA C1W H1WB 109.5 . . ? O1W C1W H1WC 109.5 . . ? H1WA C1W H1WC 109.5 . . ? H1WB C1W H1WC 109.5 . . ? C2W O2W Gd1 130.4(5) . . ? C2W O2W H2W 109.5 . . ? Gd1 O2W H2W 113.6 . . ? O2W C2W H2WA 109.5 . . ? O2W C2W H2WB 109.5 . . ? H2WA C2W H2WB 109.5 . . ? O2W C2W H2WC 109.5 . . ? H2WA C2W H2WC 109.5 . . ? H2WB C2W H2WC 109.5 . . ? C3W O3W Gd1 128.9(5) . . ? C3W O3W H3W 109.5 . . ? Gd1 O3W H3W 111.2 . . ? O3W C3W H3WA 109.5 . . ? O3W C3W H3WB 109.5 . . ? H3WA C3W H3WB 109.5 . . ? O3W C3W H3WC 109.5 . . ? H3WA C3W H3WC 109.5 . . ? H3WB C3W H3WC 109.5 . . ? C4W O4W Gd1 131.6(5) . . ? C4W O4W H4W 109.5 . . ? Gd1 O4W H4W 114.9 . . ? O4W C4W H4WA 109.5 . . ? O4W C4W H4WB 109.5 . . ? H4WA C4W H4WB 109.5 . . ? O4W C4W H4WC 109.5 . . ? H4WA C4W H4WC 109.5 . . ? H4WB C4W H4WC 109.5 . . ? C5W O5W H5WE 109.5 . . ? O5W C5W H5WC 109.5 . . ? O5W C5W H5WB 109.5 . . ? H5WC C5W H5WB 109.5 . . ? O5W C5W H5WA 109.5 . . ? H5WC C5W H5WA 109.5 . . ? H5WB C5W H5WA 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.842 _refine_diff_density_min -1.006 _refine_diff_density_rms 0.206 # Attachment 'Complex-4(final).CIF' data_complex-4 _database_code_depnum_ccdc_archive 'CCDC 644757' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H24.50 Cl O9.25 Tb' _chemical_formula_weight 523.20 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' 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 11.451(2) _cell_length_b 16.845(3) _cell_length_c 12.168(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.12(3) _cell_angle_gamma 90.00 _cell_volume 2189.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 153(1) _cell_measurement_reflns_used CCD _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1034 _exptl_absorpt_coefficient_mu 3.388 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.5022 _exptl_absorpt_correction_T_max 0.6780 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(1) _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 CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7311 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.0925 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3850 _reflns_number_gt 2590 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _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^)+(0.0831P)^2^+1.0736P] 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 shelxl _refine_ls_extinction_coef 0.0035(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.10(8) _refine_ls_number_reflns 3850 _refine_ls_number_parameters 223 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1495 _refine_ls_wR_factor_gt 0.1339 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.103 _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 Tb1 Tb 0.37193(2) 0.023740(14) 0.08203(2) 0.02343(6) Uani 1 1 d U . . Cl1 Cl 0.01633(13) -0.16037(9) 0.05186(14) 0.0435(4) Uani 1 1 d U . . O1 O 0.4610(3) -0.1095(2) -0.1283(3) 0.0286(10) Uani 1 1 d U . . O2 O 0.3432(3) -0.0982(2) -0.0168(3) 0.0282(10) Uani 1 1 d U . . O3 O 0.0106(3) -0.4367(2) -0.2810(3) 0.0287(10) Uani 1 1 d U . . O4 O 0.1148(3) -0.4419(2) -0.4031(3) 0.0306(10) Uani 1 1 d U . . C1 C 0.3738(4) -0.1322(3) -0.0939(4) 0.0245(14) Uani 1 1 d U . . C2 C 0.3041(5) -0.2061(3) -0.1484(4) 0.0256(14) Uani 1 1 d U . . C3 C 0.3380(5) -0.2491(3) -0.2313(4) 0.0315(15) Uani 1 1 d U . . H3A H 0.4060 -0.2326 -0.2501 0.038 Uiso 1 1 calc R . . C4 C 0.2710(5) -0.3157(3) -0.2853(4) 0.0297(14) Uani 1 1 d U . . H4A H 0.2941 -0.3436 -0.3403 0.036 Uiso 1 1 calc R . . C5 C 0.1681(4) -0.3415(3) -0.2573(4) 0.0258(14) Uani 1 1 d U . . C6 C 0.1373(5) -0.2992(3) -0.1736(4) 0.0269(14) Uani 1 1 d U . . H6A H 0.0717 -0.3169 -0.1519 0.032 Uiso 1 1 calc R . . C7 C 0.2016(4) -0.2313(3) -0.1216(4) 0.0274(14) Uani 1 1 d U . . H7A H 0.1764 -0.2025 -0.0687 0.033 Uiso 1 1 calc R . . C8 C 0.0932(5) -0.4110(3) -0.3174(4) 0.0285(15) Uani 1 1 d U . . O1W O 0.2664(3) 0.1512(2) 0.0750(3) 0.0347(11) Uani 1 1 d U . . H1W H 0.1967 0.1498 0.0232 0.042 Uiso 1 1 calc R . . C1W C 0.3169(8) 0.2296(5) 0.0822(7) 0.086(3) Uani 1 1 d U . . H1WA H 0.2530 0.2678 0.0773 0.104 Uiso 1 1 calc R . . H1WB H 0.3460 0.2377 0.0183 0.104 Uiso 1 1 calc R . . H1WC H 0.3854 0.2358 0.1557 0.104 Uiso 1 1 calc R . . O2W O 0.4167(3) 0.0756(2) 0.2851(3) 0.0332(10) Uani 1 1 d U . . H2W H 0.3819 0.1189 0.2780 0.040 Uiso 1 1 calc R . . C2W C 0.5301(6) 0.0775(4) 0.3831(5) 0.0475(18) Uani 1 1 d U . . H2WA H 0.5163 0.1023 0.4485 0.057 Uiso 1 1 calc R . . H2WB H 0.5913 0.1072 0.3634 0.057 Uiso 1 1 calc R . . H2WC H 0.5597 0.0243 0.4041 0.057 Uiso 1 1 calc R . . O3W O 0.2341(3) -0.0400(2) 0.1678(3) 0.0371(11) Uani 1 1 d U . . H3W H 0.2055 0.0051 0.1601 0.045 Uiso 1 1 calc R . . C3W C 0.2597(6) -0.0660(5) 0.2840(5) 0.058(2) Uani 1 1 d U . . H3WA H 0.1853 -0.0885 0.2903 0.070 Uiso 1 1 calc R . . H3WB H 0.2867 -0.0217 0.3370 0.070 Uiso 1 1 calc R . . H3WC H 0.3245 -0.1054 0.3041 0.070 Uiso 1 1 calc R . . O4W O 0.1491(3) 0.0172(2) -0.0565(3) 0.0347(11) Uani 1 1 d U . . H4W H 0.0993 0.0488 -0.0465 0.042 Uiso 1 1 calc R . . C4W C 0.0968(6) -0.0159(4) -0.1733(5) 0.0463(18) Uani 1 1 d U . . H4WA H 0.0077 -0.0084 -0.2036 0.056 Uiso 1 1 calc R . . H4WB H 0.1153 -0.0716 -0.1703 0.056 Uiso 1 1 calc R . . H4WC H 0.1325 0.0102 -0.2239 0.056 Uiso 1 1 calc R . . O5W O 0.3049(5) 0.2002(4) 0.3415(6) 0.109(2) Uani 1 1 d U . . H5WD H 0.3468 0.2259 0.3995 0.131 Uiso 1 1 calc R . . C5W C 0.1776(7) 0.2208(5) 0.3095(7) 0.080(2) Uani 1 1 d U . . H5WC H 0.1405 0.2260 0.2255 0.096 Uiso 1 1 calc R . . H5WB H 0.1709 0.2704 0.3458 0.096 Uiso 1 1 calc R . . H5WA H 0.1348 0.1802 0.3356 0.096 Uiso 1 1 calc R . . O6W O 0.0000 0.0000 -0.5000 0.053(3) Uani 0.50 2 d SPU . . H6W H -0.0190 0.0493 -0.4569 0.063 Uiso 0.50 1 d PR . . 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 0.02354(10) 0.01756(11) 0.02847(11) -0.00091(12) 0.00849(8) 0.00022(12) Cl1 0.0294(6) 0.0405(8) 0.0615(8) -0.0079(7) 0.0175(6) 0.0014(6) O1 0.0265(16) 0.0251(18) 0.0339(16) -0.0057(15) 0.0103(13) -0.0013(15) O2 0.0283(16) 0.0226(18) 0.0295(16) -0.0080(15) 0.0052(13) -0.0037(15) O3 0.0320(16) 0.0277(18) 0.0275(15) -0.0041(15) 0.0123(12) -0.0079(16) O4 0.0306(17) 0.0263(17) 0.0314(16) -0.0073(15) 0.0072(13) 0.0030(16) C1 0.023(2) 0.021(2) 0.025(2) 0.006(2) 0.0035(18) 0.000(2) C2 0.024(2) 0.022(2) 0.027(2) 0.003(2) 0.0045(18) 0.003(2) C3 0.031(2) 0.031(3) 0.035(2) -0.004(2) 0.0159(18) -0.003(2) C4 0.032(2) 0.029(3) 0.028(2) -0.007(2) 0.0109(18) -0.001(2) C5 0.022(2) 0.021(2) 0.032(2) 0.001(2) 0.0063(18) -0.001(2) C6 0.027(2) 0.028(3) 0.026(2) -0.001(2) 0.0091(17) -0.006(2) C7 0.028(2) 0.024(2) 0.030(2) -0.007(2) 0.0101(18) 0.003(2) C8 0.027(2) 0.023(3) 0.030(2) -0.005(2) 0.0048(19) 0.002(2) O1W 0.0274(17) 0.0267(19) 0.0467(19) -0.0003(17) 0.0092(14) 0.0005(16) C1W 0.089(4) 0.074(4) 0.092(4) 0.000(4) 0.028(3) 0.003(4) O2W 0.0345(17) 0.0290(19) 0.0371(17) 0.0014(16) 0.0139(13) 0.0060(16) C2W 0.046(3) 0.052(3) 0.037(3) -0.008(3) 0.007(2) 0.002(3) O3W 0.0374(17) 0.036(2) 0.0400(17) 0.0086(16) 0.0159(14) 0.0019(16) C3W 0.059(3) 0.063(4) 0.057(3) 0.001(3) 0.026(2) -0.013(3) O4W 0.0323(17) 0.0278(18) 0.0411(18) -0.0096(16) 0.0098(14) 0.0091(16) C4W 0.046(3) 0.041(3) 0.039(3) -0.004(3) -0.002(2) -0.001(3) O5W 0.086(3) 0.093(3) 0.130(4) -0.052(3) 0.017(3) 0.015(3) C5W 0.079(4) 0.084(4) 0.078(4) -0.010(3) 0.028(3) 0.017(3) O6W 0.056(5) 0.060(5) 0.041(4) -0.008(4) 0.017(3) -0.014(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 Tb1 O1 2.299(3) 3_655 ? Tb1 O4 2.310(4) 2_554 ? Tb1 O2 2.343(3) . ? Tb1 O3 2.354(3) 4_656 ? Tb1 O3W 2.433(4) . ? Tb1 O1W 2.451(4) . ? Tb1 O2W 2.494(3) . ? Tb1 O4W 2.503(3) . ? O1 C1 1.273(7) . ? O1 Tb1 2.299(3) 3_655 ? O2 C1 1.252(7) . ? O3 C8 1.256(7) . ? O3 Tb1 2.354(3) 4 ? O4 C8 1.267(7) . ? O4 Tb1 2.310(4) 2_544 ? C1 C2 1.500(7) . ? C2 C7 1.392(8) . ? C2 C3 1.405(8) . ? C3 C4 1.384(7) . ? C3 H3A 0.9300 . ? C4 C5 1.408(8) . ? C4 H4A 0.9300 . ? C5 C6 1.389(8) . ? C5 C8 1.479(7) . ? C6 C7 1.384(7) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? O1W C1W 1.431(9) . ? O1W H1W 0.8200 . ? C1W H1WA 0.9600 . ? C1W H1WB 0.9600 . ? C1W H1WC 0.9600 . ? O2W C2W 1.412(6) . ? O2W H2W 0.8200 . ? C2W H2WA 0.9600 . ? C2W H2WB 0.9600 . ? C2W H2WC 0.9600 . ? O3W C3W 1.406(7) . ? O3W H3W 0.8200 . ? C3W H3WA 0.9600 . ? C3W H3WB 0.9600 . ? C3W H3WC 0.9600 . ? O4W C4W 1.441(6) . ? O4W H4W 0.8200 . ? C4W H4WA 0.9600 . ? C4W H4WB 0.9600 . ? C4W H4WC 0.9600 . ? O5W C5W 1.409(10) . ? O5W H5WD 0.8200 . ? C5W H5WC 0.9600 . ? C5W H5WB 0.9600 . ? C5W H5WA 0.9600 . ? O6W H6W 1.0461 . ? 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 O1 Tb1 O4 75.03(12) 3_655 2_554 ? O1 Tb1 O2 128.85(13) 3_655 . ? O4 Tb1 O2 77.35(12) 2_554 . ? O1 Tb1 O3 85.91(12) 3_655 4_656 ? O4 Tb1 O3 124.50(13) 2_554 4_656 ? O2 Tb1 O3 75.58(11) . 4_656 ? O1 Tb1 O3W 141.55(12) 3_655 . ? O4 Tb1 O3W 142.01(11) 2_554 . ? O2 Tb1 O3W 80.81(13) . . ? O3 Tb1 O3W 78.33(12) 4_656 . ? O1 Tb1 O1W 79.31(12) 3_655 . ? O4 Tb1 O1W 86.94(13) 2_554 . ? O2 Tb1 O1W 140.73(11) . . ? O3 Tb1 O1W 140.27(12) 4_656 . ? O3W Tb1 O1W 90.78(13) . . ? O1 Tb1 O2W 71.43(13) 3_655 . ? O4 Tb1 O2W 141.82(12) 2_554 . ? O2 Tb1 O2W 139.15(12) . . ? O3 Tb1 O2W 70.84(12) 4_656 . ? O3W Tb1 O2W 70.30(12) . . ? O1W Tb1 O2W 69.51(12) . . ? O1 Tb1 O4W 138.49(12) 3_655 . ? O4 Tb1 O4W 76.92(12) 2_554 . ? O2 Tb1 O4W 72.26(11) . . ? O3 Tb1 O4W 135.50(12) 4_656 . ? O3W Tb1 O4W 66.93(12) . . ? O1W Tb1 O4W 69.18(11) . . ? O2W Tb1 O4W 118.56(12) . . ? C1 O1 Tb1 142.2(3) . 3_655 ? C1 O2 Tb1 139.4(3) . . ? C8 O3 Tb1 111.5(3) . 4 ? C8 O4 Tb1 167.8(3) . 2_544 ? O2 C1 O1 125.0(4) . . ? O2 C1 C2 117.6(5) . . ? O1 C1 C2 117.4(5) . . ? C7 C2 C3 119.0(5) . . ? C7 C2 C1 120.6(5) . . ? C3 C2 C1 120.3(5) . . ? C4 C3 C2 120.6(5) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C3 C4 C5 120.3(5) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? C6 C5 C4 118.4(5) . . ? C6 C5 C8 120.9(5) . . ? C4 C5 C8 120.7(5) . . ? C7 C6 C5 121.7(5) . . ? C7 C6 H6A 119.2 . . ? C5 C6 H6A 119.2 . . ? C6 C7 C2 120.0(5) . . ? C6 C7 H7A 120.0 . . ? C2 C7 H7A 120.0 . . ? O3 C8 O4 122.9(5) . . ? O3 C8 C5 118.3(5) . . ? O4 C8 C5 118.8(5) . . ? C1W O1W Tb1 128.5(4) . . ? C1W O1W H1W 109.5 . . ? Tb1 O1W H1W 109.4 . . ? O1W C1W H1WA 109.5 . . ? O1W C1W H1WB 109.5 . . ? H1WA C1W H1WB 109.5 . . ? O1W C1W H1WC 109.5 . . ? H1WA C1W H1WC 109.5 . . ? H1WB C1W H1WC 109.5 . . ? C2W O2W Tb1 130.0(4) . . ? C2W O2W H2W 109.5 . . ? Tb1 O2W H2W 106.7 . . ? O2W C2W H2WA 109.5 . . ? O2W C2W H2WB 109.5 . . ? H2WA C2W H2WB 109.5 . . ? O2W C2W H2WC 109.5 . . ? H2WA C2W H2WC 109.5 . . ? H2WB C2W H2WC 109.5 . . ? C3W O3W Tb1 129.5(3) . . ? C3W O3W H3W 109.5 . . ? Tb1 O3W H3W 80.6 . . ? O3W C3W H3WA 109.5 . . ? O3W C3W H3WB 109.5 . . ? H3WA C3W H3WB 109.5 . . ? O3W C3W H3WC 109.5 . . ? H3WA C3W H3WC 109.5 . . ? H3WB C3W H3WC 109.5 . . ? C4W O4W Tb1 129.9(3) . . ? C4W O4W H4W 109.5 . . ? Tb1 O4W H4W 117.8 . . ? O4W C4W H4WA 109.5 . . ? O4W C4W H4WB 109.5 . . ? H4WA C4W H4WB 109.5 . . ? O4W C4W H4WC 109.5 . . ? H4WA C4W H4WC 109.5 . . ? H4WB C4W H4WC 109.5 . . ? C5W O5W H5WD 109.5 . . ? O5W C5W H5WC 109.5 . . ? O5W C5W H5WB 109.5 . . ? H5WC C5W H5WB 109.5 . . ? O5W C5W H5WA 109.5 . . ? H5WC C5W H5WA 109.5 . . ? H5WB C5W H5WA 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.881 _refine_diff_density_min -0.919 _refine_diff_density_rms 0.199 # Attachment 'Complex-5(final).CIF' data_complex-5 _database_code_depnum_ccdc_archive 'CCDC 644758' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H17 Eu N2 O10' _chemical_formula_weight 501.24 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' Eu Eu -0.1578 3.6682 '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 10.017(2) _cell_length_b 10.550(2) _cell_length_c 11.273(2) _cell_angle_alpha 93.13(3) _cell_angle_beta 104.24(3) _cell_angle_gamma 117.94(3) _cell_volume 999.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 153(1) _cell_measurement_reflns_used CCD _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 3.183 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.5892 _exptl_absorpt_correction_T_max 0.7021 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(1) _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 CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7375 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0840 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4449 _reflns_number_gt 3593 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _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^)+(0.0354P)^2^+4.5648P] 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 SHELXL _refine_ls_extinction_coef 0.0077(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.15(5) _refine_ls_number_reflns 4449 _refine_ls_number_parameters 235 _refine_ls_number_restraints 158 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1478 _refine_ls_wR_factor_gt 0.1387 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.117 _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 Eu1 Eu 0.73517(5) 0.62317(5) -0.94435(4) 0.01573(15) Uani 1 1 d U . . O1 O 0.3784(8) 0.4570(7) -0.8383(6) 0.0239(14) Uani 1 1 d U . . O2 O 0.6434(7) 0.5585(7) -0.7723(6) 0.0233(14) Uani 1 1 d U . . O3 O 0.4849(7) 0.3434(6) -1.0047(6) 0.0194(13) Uani 1 1 d U . . O4 O 0.7325(7) 0.3959(7) -0.9707(6) 0.0250(15) Uani 1 1 d U . . O5 O 0.8575(8) 0.8416(7) -1.0461(7) 0.0279(15) Uani 1 1 d U . . O6 O 0.9513(8) 0.6961(7) -1.0461(7) 0.0301(16) Uani 1 1 d U . . O7 O 1.0032(9) 0.8576(7) -1.1654(7) 0.0321(17) Uani 1 1 d U . . N1 N 0.9392(9) 0.7997(8) -1.0873(7) 0.0207(17) Uani 1 1 d U . . C1 C 0.5075(11) 0.5057(10) -0.7536(9) 0.023(2) Uani 1 1 d U . . C2 C 0.5053(11) 0.5035(10) -0.6221(8) 0.0214(19) Uani 1 1 d U . . C3 C 0.3624(12) 0.4523(11) -0.5967(9) 0.027(2) Uani 1 1 d U . . H3A H 0.2693 0.4194 -0.6622 0.032 Uiso 1 1 calc R . . C4 C 0.6442(12) 0.5507(11) -0.5230(9) 0.027(2) Uani 1 1 d U . . H4A H 0.7411 0.5841 -0.5385 0.032 Uiso 1 1 calc R . . C5 C 0.5896(11) 0.3036(9) -0.9914(8) 0.0182(18) Uani 1 1 d U . . C6 C 0.5407(11) 0.1452(9) -0.9982(9) 0.0196(19) Uani 1 1 d U . . C7 C 0.3936(12) 0.0463(10) -0.9898(10) 0.027(2) Uani 1 1 d U . . H7A H 0.3223 0.0769 -0.9825 0.032 Uiso 1 1 calc R . . C8 C 0.3530(12) -0.0997(10) -0.9925(10) 0.028(2) Uani 1 1 d U . . H8A H 0.2535 -0.1669 -0.9879 0.034 Uiso 1 1 calc R . . O1W O 0.8523(8) 0.8583(7) -0.8000(6) 0.0296(16) Uani 1 1 d U . . H1W H 0.9085 0.9317 -0.8234 0.036 Uiso 1 1 calc R . . C1W C 0.8294(19) 0.9008(14) -0.6869(13) 0.061(4) Uani 1 1 d U . . H1WA H 0.8987 1.0042 -0.6562 0.091 Uiso 1 1 calc R . . H1WB H 0.8531 0.8487 -0.6254 0.091 Uiso 1 1 calc R . . H1WC H 0.7211 0.8780 -0.7033 0.091 Uiso 1 1 calc R . . O2W O 0.9748(8) 0.6593(8) -0.7900(6) 0.0324(17) Uani 1 1 d U . . H2W H 0.9927 0.6913 -0.7165 0.039 Uiso 1 1 calc R . . C2W C 1.0827(14) 0.6079(14) -0.7995(12) 0.044(3) Uani 1 1 d U . . H2WA H 1.1666 0.6426 -0.7219 0.066 Uiso 1 1 calc R . . H2WB H 1.1269 0.6440 -0.8651 0.066 Uiso 1 1 calc R . . H2WC H 1.0264 0.5028 -0.8180 0.066 Uiso 1 1 calc R . . N1W N 1.056(3) 0.704(3) -0.527(2) 0.161(9) Uani 1 1 d DU . . C5W C 1.117(2) 0.702(2) -0.4208(16) 0.080(5) Uani 1 1 d DU . . C4W C 1.221(3) 0.714(3) -0.307(2) 0.128(8) Uani 1 1 d DU . . H4WA H 1.1638 0.6838 -0.2475 0.192 Uiso 1 1 calc R . . H4WB H 1.3051 0.8133 -0.2776 0.192 Uiso 1 1 calc R . . H4WC H 1.2641 0.6516 -0.3188 0.192 Uiso 1 1 calc R . . O3W O 1.798(4) 1.076(4) -0.384(3) 0.130(11) Uani 0.50 1 d PU . . H3WY H 1.7706 1.1496 -0.4035 0.195 Uiso 0.50 1 d PR . . H3WX H 1.8534 1.0652 -0.4387 0.195 Uiso 0.50 1 d PR . . O3W' O 1.653(5) 0.922(5) -0.380(4) 0.177(16) Uani 0.50 1 d PU . . H3WO H 1.5787 0.9418 -0.3541 0.266 Uiso 0.50 1 d PR . . H3WN H 1.6811 0.8649 -0.3268 0.266 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0174(2) 0.0143(2) 0.0164(2) 0.00495(15) 0.00684(16) 0.00754(17) O1 0.025(3) 0.026(3) 0.014(3) 0.003(3) 0.008(3) 0.007(3) O2 0.020(3) 0.031(3) 0.018(3) 0.007(3) 0.008(3) 0.011(3) O3 0.020(3) 0.019(3) 0.024(3) 0.006(2) 0.007(3) 0.014(3) O4 0.021(3) 0.016(3) 0.036(4) 0.006(3) 0.007(3) 0.009(3) O5 0.031(4) 0.023(3) 0.037(4) 0.006(3) 0.021(3) 0.014(3) O6 0.027(3) 0.031(3) 0.041(4) 0.019(3) 0.017(3) 0.016(3) O7 0.036(4) 0.029(3) 0.035(4) 0.011(3) 0.025(3) 0.012(3) N1 0.018(4) 0.018(4) 0.021(4) 0.006(3) 0.011(3) 0.003(3) C1 0.024(5) 0.021(4) 0.022(4) 0.005(3) 0.012(4) 0.007(4) C2 0.023(4) 0.022(4) 0.014(4) 0.006(3) 0.006(3) 0.007(3) C3 0.022(4) 0.037(5) 0.018(4) 0.006(4) 0.007(4) 0.011(4) C4 0.023(4) 0.032(5) 0.023(4) 0.007(4) 0.013(4) 0.008(4) C5 0.022(4) 0.014(4) 0.018(4) 0.006(3) 0.007(3) 0.008(3) C6 0.022(4) 0.015(4) 0.023(4) 0.005(3) 0.005(3) 0.011(3) C7 0.027(5) 0.021(4) 0.042(5) 0.006(4) 0.017(4) 0.016(4) C8 0.024(4) 0.021(4) 0.042(5) 0.007(4) 0.014(4) 0.011(4) O1W 0.040(4) 0.019(3) 0.025(3) 0.002(3) 0.014(3) 0.009(3) C1W 0.085(8) 0.042(6) 0.049(6) 0.004(5) 0.033(6) 0.022(6) O2W 0.032(4) 0.045(4) 0.021(3) -0.003(3) 0.001(3) 0.024(3) C2W 0.040(6) 0.053(6) 0.047(6) 0.007(5) 0.009(5) 0.031(5) N1W 0.159(12) 0.170(12) 0.153(12) 0.039(9) 0.046(9) 0.080(9) C5W 0.085(9) 0.084(8) 0.064(8) 0.018(7) 0.012(7) 0.040(7) C4W 0.130(11) 0.128(11) 0.125(12) 0.022(8) 0.017(8) 0.074(9) O3W 0.134(14) 0.126(13) 0.124(14) 0.024(9) 0.033(9) 0.063(10) O3W' 0.187(18) 0.167(18) 0.179(18) 0.039(10) 0.064(11) 0.084(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O3 2.332(6) 2_663 ? Eu1 O2 2.346(6) . ? Eu1 O1 2.348(6) 2_663 ? Eu1 O4 2.387(6) . ? Eu1 O2W 2.440(7) . ? Eu1 O1W 2.464(6) . ? Eu1 O6 2.520(7) . ? Eu1 O5 2.542(7) . ? Eu1 O3 2.732(6) . ? Eu1 C5 2.931(8) . ? Eu1 N1 2.936(7) . ? Eu1 Eu1 3.973(2) 2_663 ? O1 C1 1.251(11) . ? O1 Eu1 2.348(6) 2_663 ? O2 C1 1.285(11) . ? O3 C5 1.281(10) . ? O3 Eu1 2.332(6) 2_663 ? O4 C5 1.247(11) . ? O5 N1 1.259(10) . ? O6 N1 1.256(10) . ? O7 N1 1.237(10) . ? C1 C2 1.489(12) . ? C2 C3 1.384(13) . ? C2 C4 1.399(13) . ? C3 C4 1.369(13) 2_664 ? C3 H3A 0.9300 . ? C4 C3 1.369(13) 2_664 ? C4 H4A 0.9300 . ? C5 C6 1.497(12) . ? C6 C7 1.381(13) . ? C6 C8 1.380(13) 2_653 ? C7 C8 1.393(13) . ? C7 H7A 0.9300 . ? C8 C6 1.380(13) 2_653 ? C8 H8A 0.9300 . ? O1W C1W 1.434(14) . ? O1W H1W 0.8200 . ? C1W H1WA 0.9600 . ? C1W H1WB 0.9600 . ? C1W H1WC 0.9600 . ? O2W C2W 1.440(13) . ? O2W H2W 0.8200 . ? C2W H2WA 0.9600 . ? C2W H2WB 0.9600 . ? C2W H2WC 0.9600 . ? N1W C5W 1.20(2) . ? C5W C4W 1.39(2) . ? C4W H4WA 0.9600 . ? C4W H4WB 0.9600 . ? C4W H4WC 0.9600 . ? O3W O3W' 1.61(5) . ? O3W H3WY 0.9602 . ? O3W H3WX 0.9599 . ? O3W' H3WO 0.9594 . ? O3W' H3WN 0.9606 . ? 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 Eu1 O2 79.7(2) 2_663 . ? O3 Eu1 O1 74.5(2) 2_663 2_663 ? O2 Eu1 O1 134.6(2) . 2_663 ? O3 Eu1 O4 126.6(2) 2_663 . ? O2 Eu1 O4 87.6(2) . . ? O1 Eu1 O4 79.1(2) 2_663 . ? O3 Eu1 O2W 149.4(2) 2_663 . ? O2 Eu1 O2W 78.8(2) . . ? O1 Eu1 O2W 135.7(2) 2_663 . ? O4 Eu1 O2W 73.8(2) . . ? O3 Eu1 O1W 81.8(2) 2_663 . ? O2 Eu1 O1W 75.6(2) . . ? O1 Eu1 O1W 134.6(2) 2_663 . ? O4 Eu1 O1W 144.1(2) . . ? O2W Eu1 O1W 72.0(2) . . ? O3 Eu1 O6 128.7(2) 2_663 . ? O2 Eu1 O6 150.2(2) . . ? O1 Eu1 O6 70.3(2) 2_663 . ? O4 Eu1 O6 81.5(2) . . ? O2W Eu1 O6 71.6(2) . . ? O1W Eu1 O6 97.5(2) . . ? O3 Eu1 O5 84.2(2) 2_663 . ? O2 Eu1 O5 141.5(2) . . ? O1 Eu1 O5 71.9(2) 2_663 . ? O4 Eu1 O5 129.3(2) . . ? O2W Eu1 O5 99.6(2) . . ? O1W Eu1 O5 67.6(2) . . ? O6 Eu1 O5 50.1(2) . . ? O3 Eu1 O3 76.9(2) 2_663 . ? O2 Eu1 O3 69.4(2) . . ? O1 Eu1 O3 68.8(2) 2_663 . ? O4 Eu1 O3 50.29(19) . . ? O2W Eu1 O3 114.7(2) . . ? O1W Eu1 O3 141.6(2) . . ? O6 Eu1 O3 120.8(2) . . ? O5 Eu1 O3 139.6(2) . . ? O3 Eu1 C5 102.7(2) 2_663 . ? O2 Eu1 C5 76.5(2) . . ? O1 Eu1 C5 73.7(2) 2_663 . ? O4 Eu1 C5 24.5(2) . . ? O2W Eu1 C5 93.1(2) . . ? O1W Eu1 C5 150.4(2) . . ? O6 Eu1 C5 101.8(2) . . ? O5 Eu1 C5 141.5(2) . . ? O3 Eu1 C5 25.8(2) . . ? O3 Eu1 N1 105.5(2) 2_663 . ? O2 Eu1 N1 158.6(2) . . ? O1 Eu1 N1 66.0(2) 2_663 . ? O4 Eu1 N1 104.6(2) . . ? O2W Eu1 N1 87.7(2) . . ? O1W Eu1 N1 84.5(2) . . ? O6 Eu1 N1 25.2(2) . . ? O5 Eu1 N1 25.3(2) . . ? O3 Eu1 N1 131.8(2) . . ? C5 Eu1 N1 121.2(2) . . ? O3 Eu1 Eu1 42.06(15) 2_663 2_663 ? O2 Eu1 Eu1 69.68(16) . 2_663 ? O1 Eu1 Eu1 66.08(16) 2_663 2_663 ? O4 Eu1 Eu1 84.90(16) . 2_663 ? O2W Eu1 Eu1 142.48(18) . 2_663 ? O1W Eu1 Eu1 117.12(17) . 2_663 ? O6 Eu1 Eu1 135.95(17) . 2_663 ? O5 Eu1 Eu1 117.71(16) . 2_663 ? O3 Eu1 Eu1 34.88(12) . 2_663 ? C5 Eu1 Eu1 60.65(18) . 2_663 ? N1 Eu1 Eu1 128.01(15) . 2_663 ? C1 O1 Eu1 141.5(6) . 2_663 ? C1 O2 Eu1 134.9(6) . . ? C5 O3 Eu1 169.7(6) . 2_663 ? C5 O3 Eu1 85.8(5) . . ? Eu1 O3 Eu1 103.1(2) 2_663 . ? C5 O4 Eu1 103.0(5) . . ? N1 O5 Eu1 95.1(5) . . ? N1 O6 Eu1 96.3(5) . . ? O7 N1 O6 121.9(8) . . ? O7 N1 O5 121.2(8) . . ? O6 N1 O5 116.9(7) . . ? O7 N1 Eu1 168.9(6) . . ? O6 N1 Eu1 58.5(4) . . ? O5 N1 Eu1 59.6(4) . . ? O1 C1 O2 124.2(8) . . ? O1 C1 C2 118.5(8) . . ? O2 C1 C2 117.3(8) . . ? C3 C2 C4 118.9(8) . . ? C3 C2 C1 119.5(8) . . ? C4 C2 C1 121.7(8) . . ? C4 C3 C2 121.2(9) 2_664 . ? C4 C3 H3A 119.4 2_664 . ? C2 C3 H3A 119.4 . . ? C3 C4 C2 120.0(9) 2_664 . ? C3 C4 H4A 120.0 2_664 . ? C2 C4 H4A 120.0 . . ? O4 C5 O3 120.7(8) . . ? O4 C5 C6 119.5(8) . . ? O3 C5 C6 119.7(8) . . ? O4 C5 Eu1 52.5(4) . . ? O3 C5 Eu1 68.4(4) . . ? C6 C5 Eu1 170.0(6) . . ? C7 C6 C8 120.1(8) . 2_653 ? C7 C6 C5 120.6(8) . . ? C8 C6 C5 119.2(8) 2_653 . ? C6 C7 C8 119.5(9) . . ? C6 C7 H7A 120.3 . . ? C8 C7 H7A 120.3 . . ? C6 C8 C7 120.4(9) 2_653 . ? C6 C8 H8A 119.8 2_653 . ? C7 C8 H8A 119.8 . . ? C1W O1W Eu1 133.9(7) . . ? C1W O1W H1W 109.5 . . ? Eu1 O1W H1W 116.1 . . ? O1W C1W H1WA 109.5 . . ? O1W C1W H1WB 109.5 . . ? H1WA C1W H1WB 109.5 . . ? O1W C1W H1WC 109.5 . . ? H1WA C1W H1WC 109.5 . . ? H1WB C1W H1WC 109.5 . . ? C2W O2W Eu1 130.3(6) . . ? C2W O2W H2W 109.5 . . ? Eu1 O2W H2W 119.1 . . ? O2W C2W H2WA 109.5 . . ? O2W C2W H2WB 109.5 . . ? H2WA C2W H2WB 109.5 . . ? O2W C2W H2WC 109.5 . . ? H2WA C2W H2WC 109.5 . . ? H2WB C2W H2WC 109.5 . . ? N1W C5W C4W 166(3) . . ? C5W C4W H4WA 109.5 . . ? C5W C4W H4WB 109.5 . . ? H4WA C4W H4WB 109.5 . . ? C5W C4W H4WC 109.5 . . ? H4WA C4W H4WC 109.5 . . ? H4WB C4W H4WC 109.5 . . ? O3W' O3W H3WY 114.7 . . ? O3W' O3W H3WX 112.3 . . ? H3WY O3W H3WX 109.4 . . ? O3W O3W' H3WO 107.9 . . ? O3W O3W' H3WN 115.3 . . ? H3WO O3W' H3WN 109.4 . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.986 _refine_diff_density_min -1.026 _refine_diff_density_rms 0.143 # Attachment 'Complex-6(final).CIF' data_complex-6 _database_code_depnum_ccdc_archive 'CCDC 644759' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H17 Gd N2 O10' _chemical_formula_weight 506.53 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' 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 10.019(2) _cell_length_b 10.545(2) _cell_length_c 11.263(2) _cell_angle_alpha 93.07(3) _cell_angle_beta 104.27(3) _cell_angle_gamma 118.08(3) _cell_volume 997.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 153(1) _cell_measurement_reflns_used CCD _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 494 _exptl_absorpt_coefficient_mu 3.372 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.5122 _exptl_absorpt_correction_T_max 0.6893 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(1) _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 CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5675 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3415 _reflns_number_gt 2990 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _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^)+(0.0460P)^2^+2.7786P] 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 Shelxl _refine_ls_extinction_coef 0.0032(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(3) _refine_ls_number_reflns 3415 _refine_ls_number_parameters 235 _refine_ls_number_restraints 158 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.162 _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 0.73540(4) 0.62372(3) -0.94408(3) 0.02214(14) Uani 1 1 d U . . O1 O 0.3777(6) 0.4562(5) -0.8386(4) 0.0289(11) Uani 1 1 d U . . O2 O 0.6447(6) 0.5577(5) -0.7725(4) 0.0291(11) Uani 1 1 d U . . O3 O 0.4839(6) 0.3425(5) -1.0054(4) 0.0268(11) Uani 1 1 d U . . O4 O 0.7324(6) 0.3967(5) -0.9698(5) 0.0313(11) Uani 1 1 d U . . O5 O 0.8565(6) 0.8412(5) -1.0468(5) 0.0334(12) Uani 1 1 d U . . O6 O 0.9510(6) 0.6956(6) -1.0461(5) 0.0359(12) Uani 1 1 d U . . O7 O 1.0030(6) 0.8570(5) -1.1657(5) 0.0365(13) Uani 1 1 d U . . N1 N 0.9383(7) 0.7991(6) -1.0881(6) 0.0298(14) Uani 1 1 d U . . C1 C 0.5107(9) 0.5064(8) -0.7538(6) 0.0282(16) Uani 1 1 d U . . C2 C 0.5055(8) 0.5025(8) -0.6228(6) 0.0269(15) Uani 1 1 d U . . C3 C 0.3624(9) 0.4523(8) -0.5975(7) 0.0347(17) Uani 1 1 d U . . H3A H 0.2695 0.4202 -0.6631 0.042 Uiso 1 1 calc R . . C4 C 0.6450(9) 0.5510(8) -0.5241(7) 0.0336(17) Uani 1 1 d U . . H4A H 0.7420 0.5852 -0.5396 0.040 Uiso 1 1 calc R . . C5 C 0.5883(9) 0.3047(8) -0.9921(6) 0.0278(16) Uani 1 1 d U . . C6 C 0.5388(9) 0.1454(8) -0.9982(7) 0.0285(16) Uani 1 1 d U . . C7 C 0.3934(9) 0.0448(8) -0.9893(7) 0.0329(17) Uani 1 1 d U . . H7A H 0.3214 0.0742 -0.9810 0.039 Uiso 1 1 calc R . . C8 C 0.3540(9) -0.0995(8) -0.9927(8) 0.0363(18) Uani 1 1 d U . . H8A H 0.2542 -0.1674 -0.9889 0.044 Uiso 1 1 calc R . . O1W O 0.8513(7) 0.8577(5) -0.8000(5) 0.0382(13) Uani 1 1 d U . . H1W H 0.9077 0.9315 -0.8231 0.046 Uiso 1 1 calc R . . C1W C 0.8240(15) 0.8998(11) -0.6876(10) 0.073(3) Uani 1 1 d U . . H1WA H 0.8931 1.0033 -0.6563 0.110 Uiso 1 1 calc R . . H1WB H 0.8456 0.8473 -0.6256 0.110 Uiso 1 1 calc R . . H1WC H 0.7153 0.8768 -0.7066 0.110 Uiso 1 1 calc R . . O2W O 0.9755(6) 0.6625(6) -0.7902(5) 0.0401(13) Uani 1 1 d U . . H2W H 0.9936 0.6945 -0.7166 0.048 Uiso 1 1 calc R . . C2W C 1.0829(11) 0.6091(11) -0.8000(9) 0.054(2) Uani 1 1 d U . . H2WA H 1.1671 0.6437 -0.7224 0.082 Uiso 1 1 calc R . . H2WB H 1.1271 0.6446 -0.8659 0.082 Uiso 1 1 calc R . . H2WC H 1.0255 0.5039 -0.8182 0.082 Uiso 1 1 calc R . . N1W N 1.054(2) 0.707(2) -0.5361(14) 0.192(8) Uani 1 1 d DU . . C5W C 1.1088(18) 0.6978(17) -0.4224(13) 0.102(4) Uani 1 1 d DU . . C4W C 1.226(2) 0.714(2) -0.3103(15) 0.153(7) Uani 1 1 d DU . . H4WA H 1.1781 0.6860 -0.2452 0.229 Uiso 1 1 calc R . . H4WB H 1.3103 0.8145 -0.2849 0.229 Uiso 1 1 calc R . . H4WC H 1.2691 0.6526 -0.3259 0.229 Uiso 1 1 calc R . . O3W O 1.800(3) 1.081(3) -0.387(2) 0.135(8) Uani 0.50 1 d PU . . H3WY H 1.7721 1.1548 -0.4074 0.203 Uiso 0.50 1 d PR . . H3WX H 1.8549 1.0704 -0.4425 0.203 Uiso 0.50 1 d PR . . O3W' O 1.659(4) 0.928(4) -0.366(3) 0.200(13) Uani 0.50 1 d PU . . H3WO H 1.5849 0.9479 -0.3399 0.299 Uiso 0.50 1 d PR . . H3WN H 1.6873 0.8711 -0.3126 0.299 Uiso 0.50 1 d PR . . 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 0.0252(2) 0.0200(2) 0.0237(2) 0.00702(14) 0.01141(15) 0.01114(15) O1 0.027(3) 0.031(3) 0.030(3) 0.009(2) 0.016(2) 0.012(2) O2 0.028(3) 0.030(3) 0.025(3) 0.009(2) 0.013(2) 0.009(2) O3 0.032(3) 0.025(2) 0.032(3) 0.008(2) 0.013(2) 0.019(2) O4 0.032(3) 0.020(2) 0.042(3) 0.008(2) 0.013(2) 0.013(2) O5 0.039(3) 0.026(3) 0.043(3) 0.012(2) 0.024(3) 0.017(2) O6 0.032(3) 0.037(3) 0.049(3) 0.023(3) 0.020(2) 0.019(2) O7 0.044(3) 0.031(3) 0.039(3) 0.015(2) 0.029(3) 0.014(2) N1 0.030(3) 0.027(3) 0.034(3) 0.010(3) 0.016(3) 0.011(3) C1 0.030(4) 0.026(4) 0.024(4) 0.005(3) 0.009(3) 0.009(3) C2 0.026(4) 0.026(3) 0.026(3) 0.009(3) 0.014(3) 0.008(3) C3 0.030(4) 0.042(4) 0.028(4) 0.006(3) 0.010(3) 0.015(3) C4 0.031(4) 0.040(4) 0.025(4) 0.005(3) 0.014(3) 0.012(3) C5 0.033(4) 0.028(4) 0.025(3) 0.007(3) 0.012(3) 0.016(3) C6 0.030(4) 0.025(4) 0.034(4) 0.010(3) 0.012(3) 0.016(3) C7 0.029(4) 0.026(4) 0.050(4) 0.011(3) 0.019(3) 0.016(3) C8 0.028(4) 0.029(4) 0.060(5) 0.016(3) 0.020(4) 0.017(3) O1W 0.050(3) 0.026(3) 0.036(3) 0.007(2) 0.021(3) 0.013(2) C1W 0.103(7) 0.051(5) 0.059(6) 0.007(4) 0.042(5) 0.026(5) O2W 0.036(3) 0.052(3) 0.032(3) 0.001(2) 0.006(2) 0.025(3) C2W 0.046(5) 0.060(5) 0.064(5) 0.014(4) 0.013(4) 0.035(4) N1W 0.195(11) 0.199(11) 0.178(11) 0.042(8) 0.066(8) 0.091(8) C5W 0.109(8) 0.099(8) 0.093(8) 0.011(6) 0.024(6) 0.052(6) C4W 0.153(11) 0.156(11) 0.146(11) 0.021(8) 0.017(8) 0.088(8) O3W 0.140(11) 0.126(11) 0.130(11) 0.032(8) 0.025(8) 0.066(9) O3W' 0.211(16) 0.179(15) 0.202(16) 0.050(10) 0.067(10) 0.089(10) _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 O3 2.328(5) 2_663 ? Gd1 O2 2.336(4) . ? Gd1 O1 2.345(5) 2_663 ? Gd1 O4 2.381(4) . ? Gd1 O2W 2.429(5) . ? Gd1 O1W 2.452(5) . ? Gd1 O6 2.517(5) . ? Gd1 O5 2.535(5) . ? Gd1 O3 2.740(5) . ? Gd1 C5 2.920(7) . ? Gd1 N1 2.932(6) . ? Gd1 Gd1 3.972(2) 2_663 ? O1 C1 1.274(9) . ? O1 Gd1 2.345(5) 2_663 ? O2 C1 1.268(8) . ? O3 C5 1.263(8) . ? O3 Gd1 2.328(5) 2_663 ? O4 C5 1.251(9) . ? O5 N1 1.263(7) . ? O6 N1 1.260(7) . ? O7 N1 1.233(7) . ? C1 C2 1.492(9) . ? C2 C3 1.386(10) . ? C2 C4 1.396(10) . ? C3 C4 1.391(10) 2_664 ? C3 H3A 0.9300 . ? C4 C3 1.391(10) 2_664 ? C4 H4A 0.9300 . ? C5 C6 1.503(10) . ? C6 C7 1.373(10) . ? C6 C8 1.392(10) 2_653 ? C7 C8 1.376(10) . ? C7 H7A 0.9300 . ? C8 C6 1.392(10) 2_653 ? C8 H8A 0.9300 . ? O1W C1W 1.449(11) . ? O1W H1W 0.8200 . ? C1W H1WA 0.9600 . ? C1W H1WB 0.9600 . ? C1W H1WC 0.9600 . ? O2W C2W 1.451(10) . ? O2W H2W 0.8200 . ? C2W H2WA 0.9600 . ? C2W H2WB 0.9600 . ? C2W H2WC 0.9600 . ? N1W C5W 1.292(5) . ? C5W C4W 1.437(5) . ? C4W H4WA 0.9600 . ? C4W H4WB 0.9600 . ? C4W H4WC 0.9600 . ? O3W O3W' 1.65(4) . ? O3W H3WY 0.9600 . ? O3W H3WX 0.9600 . ? O3W' H3WO 0.9599 . ? O3W' H3WN 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 Gd1 O2 80.02(17) 2_663 . ? O3 Gd1 O1 74.76(16) 2_663 2_663 ? O2 Gd1 O1 134.77(17) . 2_663 ? O3 Gd1 O4 126.81(17) 2_663 . ? O2 Gd1 O4 87.04(17) . . ? O1 Gd1 O4 79.19(17) 2_663 . ? O3 Gd1 O2W 149.07(17) 2_663 . ? O2 Gd1 O2W 78.77(18) . . ? O1 Gd1 O2W 135.62(17) 2_663 . ? O4 Gd1 O2W 74.19(18) . . ? O3 Gd1 O1W 81.46(18) 2_663 . ? O2 Gd1 O1W 75.73(17) . . ? O1 Gd1 O1W 134.63(17) 2_663 . ? O4 Gd1 O1W 144.06(18) . . ? O2W Gd1 O1W 71.66(19) . . ? O3 Gd1 O6 128.83(16) 2_663 . ? O2 Gd1 O6 149.87(18) . . ? O1 Gd1 O6 70.01(17) 2_663 . ? O4 Gd1 O6 81.30(17) . . ? O2W Gd1 O6 71.35(18) . . ? O1W Gd1 O6 97.96(18) . . ? O3 Gd1 O5 84.03(16) 2_663 . ? O2 Gd1 O5 142.10(16) . . ? O1 Gd1 O5 71.50(17) 2_663 . ? O4 Gd1 O5 129.34(16) . . ? O2W Gd1 O5 99.33(18) . . ? O1W Gd1 O5 68.00(16) . . ? O6 Gd1 O5 50.35(15) . . ? O3 Gd1 O3 77.12(16) 2_663 . ? O2 Gd1 O3 69.41(16) . . ? O1 Gd1 O3 68.73(15) 2_663 . ? O4 Gd1 O3 50.21(15) . . ? O2W Gd1 O3 115.37(17) . . ? O1W Gd1 O3 141.56(15) . . ? O6 Gd1 O3 120.33(16) . . ? O5 Gd1 O3 139.17(16) . . ? O3 Gd1 C5 102.55(19) 2_663 . ? O2 Gd1 C5 76.24(18) . . ? O1 Gd1 C5 73.49(18) 2_663 . ? O4 Gd1 C5 24.72(18) . . ? O2W Gd1 C5 94.0(2) . . ? O1W Gd1 C5 150.49(18) . . ? O6 Gd1 C5 101.63(18) . . ? O5 Gd1 C5 141.16(17) . . ? O3 Gd1 C5 25.53(17) . . ? O3 Gd1 N1 105.46(16) 2_663 . ? O2 Gd1 N1 159.05(18) . . ? O1 Gd1 N1 65.55(17) 2_663 . ? O4 Gd1 N1 104.50(17) . . ? O2W Gd1 N1 87.52(18) . . ? O1W Gd1 N1 85.00(17) . . ? O6 Gd1 N1 25.30(16) . . ? O5 Gd1 N1 25.40(16) . . ? O3 Gd1 N1 131.34(16) . . ? C5 Gd1 N1 120.90(18) . . ? O3 Gd1 Gd1 42.27(12) 2_663 2_663 ? O2 Gd1 Gd1 69.86(13) . 2_663 ? O1 Gd1 Gd1 66.15(12) 2_663 2_663 ? O4 Gd1 Gd1 84.82(13) . 2_663 ? O2W Gd1 Gd1 142.98(13) . 2_663 ? O1W Gd1 Gd1 116.96(13) . 2_663 ? O6 Gd1 Gd1 135.72(13) . 2_663 ? O5 Gd1 Gd1 117.46(13) . 2_663 ? O3 Gd1 Gd1 34.85(9) . 2_663 ? C5 Gd1 Gd1 60.32(15) . 2_663 ? N1 Gd1 Gd1 127.73(13) . 2_663 ? C1 O1 Gd1 140.3(4) . 2_663 ? C1 O2 Gd1 134.7(5) . . ? C5 O3 Gd1 170.3(5) . 2_663 ? C5 O3 Gd1 85.2(4) . . ? Gd1 O3 Gd1 102.88(16) 2_663 . ? C5 O4 Gd1 102.5(4) . . ? N1 O5 Gd1 95.2(4) . . ? N1 O6 Gd1 96.1(4) . . ? O7 N1 O6 121.7(6) . . ? O7 N1 O5 121.5(6) . . ? O6 N1 O5 116.8(5) . . ? O7 N1 Gd1 169.4(5) . . ? O6 N1 Gd1 58.6(3) . . ? O5 N1 Gd1 59.4(3) . . ? O2 C1 O1 125.3(6) . . ? O2 C1 C2 118.3(6) . . ? O1 C1 C2 116.4(6) . . ? C3 C2 C4 119.2(7) . . ? C3 C2 C1 120.3(7) . . ? C4 C2 C1 120.4(6) . . ? C2 C3 C4 121.3(7) . 2_664 ? C2 C3 H3A 119.4 . . ? C4 C3 H3A 119.4 2_664 . ? C3 C4 C2 119.5(7) 2_664 . ? C3 C4 H4A 120.3 2_664 . ? C2 C4 H4A 120.3 . . ? O4 C5 O3 121.8(6) . . ? O4 C5 C6 119.1(6) . . ? O3 C5 C6 119.0(6) . . ? O4 C5 Gd1 52.7(3) . . ? O3 C5 Gd1 69.3(4) . . ? C6 C5 Gd1 169.6(5) . . ? C7 C6 C8 118.9(6) . 2_653 ? C7 C6 C5 121.9(6) . . ? C8 C6 C5 119.1(7) 2_653 . ? C6 C7 C8 120.1(7) . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C7 C8 C6 121.1(7) . 2_653 ? C7 C8 H8A 119.5 . . ? C6 C8 H8A 119.5 2_653 . ? C1W O1W Gd1 133.5(5) . . ? C1W O1W H1W 109.5 . . ? Gd1 O1W H1W 116.2 . . ? O1W C1W H1WA 109.5 . . ? O1W C1W H1WB 109.5 . . ? H1WA C1W H1WB 109.5 . . ? O1W C1W H1WC 109.5 . . ? H1WA C1W H1WC 109.5 . . ? H1WB C1W H1WC 109.5 . . ? C2W O2W Gd1 129.8(5) . . ? C2W O2W H2W 109.5 . . ? Gd1 O2W H2W 119.3 . . ? O2W C2W H2WA 109.5 . . ? O2W C2W H2WB 109.5 . . ? H2WA C2W H2WB 109.5 . . ? O2W C2W H2WC 109.5 . . ? H2WA C2W H2WC 109.5 . . ? H2WB C2W H2WC 109.5 . . ? N1W C5W C4W 157(2) . . ? C5W C4W H4WA 109.5 . . ? C5W C4W H4WB 109.5 . . ? H4WA C4W H4WB 109.5 . . ? C5W C4W H4WC 109.5 . . ? H4WA C4W H4WC 109.5 . . ? H4WB C4W H4WC 109.5 . . ? O3W' O3W H3WY 116.2 . . ? O3W' O3W H3WX 116.4 . . ? H3WY O3W H3WX 109.5 . . ? O3W O3W' H3WO 109.5 . . ? O3W O3W' H3WN 119.7 . . ? H3WO O3W' H3WN 109.5 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.885 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.155