Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Ruiz-Perez, Catalina' 'Anderson, Kirsty M.' 'Bocanegra, Eduardo H.' 'Hernandez-Molina, Maria' 'Julve, M.' 'Lloret, F.' 'Lopez, Trinidad' 'Lorenzo-Luis, Pablo A.' 'Martin, Inocencio R.' 'Orpen, A.' _publ_contact_author_name 'Prof Catalina Ruiz-Perez' _publ_contact_author_address ; Laboratorio de Rayos X y Materiales Moleculares, Departamento de Física Fundamen Universidad de La Laguna Avda Astrofísico Francisco Sánchez La Laguna Tenerife E-38204 SPAIN ; _publ_contact_author_email 'CARUIZ@ULL.ES' _publ_section_title ; A phase transition in the three-dimensional compound [Eu2(mal)3(H2O)6] (H2mal = malonic acid) ; data_compound1 _database_code_CSD 181893 #COMPOUND AT 293K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H18 Eu2 O18' _chemical_formula_weight 718.15 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 I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 11.094(6) _cell_length_b 12.246(4) _cell_length_c 13.581(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.00(3) _cell_angle_gamma 90.00 _cell_volume 1842.5(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 6.838 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1681 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0041 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1625 _reflns_number_gt 1624 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+30.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00176(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1625 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 1.361 _refine_ls_restrained_S_all 1.361 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.004 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 0.59645(3) 0.85151(3) 0.21684(2) 0.0123(2) Uani 1 1 d . . . O1 O 0.3906(5) 0.8559(4) 0.1653(5) 0.0257(13) Uani 1 1 d . . . O2 O 0.5190(5) 0.6677(4) 0.2262(4) 0.0197(11) Uani 1 1 d . . . O3 O 0.4171(5) 0.5157(4) 0.2007(4) 0.0307(13) Uani 1 1 d . . . O4 O 0.2002(5) 0.8162(5) 0.1280(5) 0.0298(13) Uani 1 1 d . . . O5 O 0.6098(4) 0.7581(5) 0.0515(3) 0.0218(11) Uani 1 1 d . . . O6 O 0.7518(4) 0.7093(4) 0.1597(3) 0.0172(10) Uani 1 1 d . . . C1 C 0.3086(6) 0.7885(6) 0.1396(5) 0.0173(14) Uani 1 1 d . . . C2 C 0.3409(7) 0.6717(6) 0.1197(6) 0.0234(16) Uani 1 1 d . . . H2A H 0.2670 0.6293 0.1190 0.028 Uiso 1 1 calc R . . H2B H 0.3703 0.6683 0.0538 0.028 Uiso 1 1 calc R . . C3 C 0.4314(6) 0.6159(6) 0.1876(5) 0.0179(14) Uani 1 1 d . . . C4 C 0.7001(6) 0.7009(6) 0.0750(5) 0.0155(14) Uani 1 1 d . . . C5 C 0.7500 0.6256(8) 0.0000 0.017(2) Uani 1 2 d S . . H5A H 0.6875 0.5801 -0.0294 0.021 Uiso 0.50 1 d PR . . H5B H 0.8125 0.5801 0.0294 0.021 Uiso 0.50 1 d PR . . O1W O 0.7919(5) 0.9364(5) 0.1809(5) 0.0367(15) Uani 1 1 d . . . O2W O 0.5745(7) 0.9941(5) 0.0855(5) 0.0484(19) Uani 1 1 d . . . O3W O 0.4921(5) 0.8201(5) 0.3745(4) 0.0259(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0122(3) 0.0124(3) 0.0121(3) -0.00034(11) 0.00064(14) 0.00009(11) O1 0.020(3) 0.017(3) 0.039(3) 0.000(2) -0.004(2) 0.000(2) O2 0.019(3) 0.019(2) 0.022(3) 0.003(2) 0.002(2) 0.001(2) O3 0.041(3) 0.017(3) 0.034(3) 0.004(2) -0.003(3) -0.005(2) O4 0.015(3) 0.025(3) 0.048(4) -0.006(3) -0.002(2) 0.005(2) O5 0.021(3) 0.035(3) 0.009(2) 0.002(2) 0.0016(19) 0.008(2) O6 0.016(2) 0.028(3) 0.007(2) 0.0003(19) 0.0010(18) 0.002(2) C1 0.012(3) 0.025(4) 0.015(3) 0.001(3) 0.005(3) -0.002(3) C2 0.019(4) 0.021(4) 0.031(4) -0.002(3) -0.002(3) -0.003(3) C3 0.019(3) 0.017(3) 0.017(3) -0.001(3) 0.006(3) -0.001(3) C4 0.018(3) 0.019(3) 0.010(3) 0.000(3) 0.006(3) -0.006(3) C5 0.022(5) 0.017(5) 0.013(5) 0.000 0.005(4) 0.000 O1W 0.027(3) 0.022(3) 0.060(4) 0.015(3) -0.005(3) -0.010(2) O2W 0.061(4) 0.032(3) 0.049(4) 0.019(3) -0.030(3) -0.018(3) O3W 0.023(3) 0.037(3) 0.018(3) -0.004(2) 0.007(2) -0.009(2) _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 2.310(5) 4 ? Eu1 O1 2.353(6) . ? Eu1 O2 2.415(5) . ? Eu1 O6 2.430(5) 7_665 ? Eu1 O1W 2.476(6) . ? Eu1 O2W 2.499(6) . ? Eu1 O3W 2.517(5) . ? Eu1 O5 2.532(5) . ? Eu1 O6 2.597(5) . ? Eu1 C4 2.944(7) . ? Eu1 Eu1 4.2753(9) 7_665 ? O1 C1 1.265(9) . ? O2 C3 1.253(9) . ? O3 C3 1.252(9) . ? O3 Eu1 2.310(5) 4_545 ? O4 C1 1.251(9) . ? O5 C4 1.250(9) . ? O6 C4 1.262(8) . ? O6 Eu1 2.430(5) 7_665 ? C1 C2 1.503(11) . ? C2 C3 1.492(11) . ? C4 C5 1.501(9) . ? C5 C4 1.501(9) 2_655 ? 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 O1 92.2(2) 4 . ? O3 Eu1 O2 138.9(2) 4 . ? O1 Eu1 O2 72.23(17) . . ? O3 Eu1 O6 89.58(19) 4 7_665 ? O1 Eu1 O6 146.99(18) . 7_665 ? O2 Eu1 O6 85.03(17) . 7_665 ? O3 Eu1 O1W 79.1(2) 4 . ? O1 Eu1 O1W 141.0(2) . . ? O2 Eu1 O1W 135.99(19) . . ? O6 Eu1 O1W 71.50(18) 7_665 . ? O3 Eu1 O2W 74.4(2) 4 . ? O1 Eu1 O2W 73.4(2) . . ? O2 Eu1 O2W 131.87(19) . . ? O6 Eu1 O2W 138.14(19) 7_665 . ? O1W Eu1 O2W 67.6(2) . . ? O3 Eu1 O3W 71.1(2) 4 . ? O1 Eu1 O3W 77.0(2) . . ? O2 Eu1 O3W 68.39(18) . . ? O6 Eu1 O3W 72.47(17) 7_665 . ? O1W Eu1 O3W 132.7(2) . . ? O2W Eu1 O3W 133.0(2) . . ? O3 Eu1 O5 146.28(19) 4 . ? O1 Eu1 O5 81.21(19) . . ? O2 Eu1 O5 70.30(18) . . ? O6 Eu1 O5 113.77(16) 7_665 . ? O1W Eu1 O5 85.6(2) . . ? O2W Eu1 O5 72.0(2) . . ? O3W Eu1 O5 137.42(18) . . ? O3 Eu1 O6 142.13(19) 4 . ? O1 Eu1 O6 125.11(17) . . ? O2 Eu1 O6 68.55(17) . . ? O6 Eu1 O6 63.52(17) 7_665 . ? O1W Eu1 O6 67.71(18) . . ? O2W Eu1 O6 107.3(2) . . ? O3W Eu1 O6 119.59(17) . . ? O5 Eu1 O6 50.31(15) . . ? O3 Eu1 C4 154.2(2) 4 . ? O1 Eu1 C4 103.05(19) . . ? O2 Eu1 C4 66.59(18) . . ? O6 Eu1 C4 88.81(17) 7_665 . ? O1W Eu1 C4 76.0(2) . . ? O2W Eu1 C4 89.9(2) . . ? O3W Eu1 C4 132.35(19) . . ? O5 Eu1 C4 24.97(18) . . ? O6 Eu1 C4 25.35(17) . . ? O3 Eu1 Eu1 118.38(15) 4 7_665 ? O1 Eu1 Eu1 145.69(12) . 7_665 ? O2 Eu1 Eu1 74.26(13) . 7_665 ? O6 Eu1 Eu1 32.94(11) 7_665 7_665 ? O1W Eu1 Eu1 65.75(14) . 7_665 ? O2W Eu1 Eu1 127.12(19) . 7_665 ? O3W Eu1 Eu1 97.40(14) . 7_665 ? O5 Eu1 Eu1 80.86(11) . 7_665 ? O6 Eu1 Eu1 30.59(10) . 7_665 ? C4 Eu1 Eu1 55.89(14) . 7_665 ? C1 O1 Eu1 137.8(5) . . ? C3 O2 Eu1 136.1(5) . . ? C3 O3 Eu1 159.2(5) . 4_545 ? C4 O5 Eu1 96.3(4) . . ? C4 O6 Eu1 150.3(5) . 7_665 ? C4 O6 Eu1 92.9(4) . . ? Eu1 O6 Eu1 116.48(17) 7_665 . ? O4 C1 O1 122.0(7) . . ? O4 C1 C2 118.2(6) . . ? O1 C1 C2 119.7(6) . . ? C3 C2 C1 118.9(6) . . ? O3 C3 O2 122.6(7) . . ? O3 C3 C2 116.8(7) . . ? O2 C3 C2 120.6(7) . . ? O5 C4 O6 120.5(6) . . ? O5 C4 C5 119.3(5) . . ? O6 C4 C5 120.2(6) . . ? O5 C4 Eu1 58.7(3) . . ? O6 C4 Eu1 61.8(3) . . ? C5 C4 Eu1 178.0(4) . . ? C4 C5 C4 104.2(8) . 2_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.220 _refine_diff_density_min -1.100 _refine_diff_density_rms 0.213 data_compound2 _database_code_CSD 181894 #COMPOUND AT 173k _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H18 Eu2 O18' _chemical_formula_weight 718.15 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 Ia loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z' 'x+1/2, y+1/2, z+1/2' 'x+1, -y+1/2, z+1/2' _cell_length_a 11.0504(12) _cell_length_b 12.2959(16) _cell_length_c 13.467(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.915(16) _cell_angle_gamma 90.00 _cell_volume 1828.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 145 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 6.890 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.213550 _exptl_absorpt_correction_T_max 0.355024 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD area detector' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 4749 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2940 _reflns_number_gt 2741 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0138P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00172(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 0.48(3) _refine_ls_number_reflns 2940 _refine_ls_number_parameters 300 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0204 _refine_ls_R_factor_gt 0.0190 _refine_ls_wR_factor_ref 0.0414 _refine_ls_wR_factor_gt 0.0411 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.958 _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 1.23186(2) 0.14560(3) 0.355556(19) 0.00877(17) Uani 1 1 d . . . O1W O 1.0313(11) 0.0670(6) 0.3971(8) 0.019(2) Uani 1 1 d D . . H1 H 0.970(5) 0.087(5) 0.346(4) 0.023 Uiso 1 1 d D . . H2 H 1.008(6) -0.001(3) 0.427(4) 0.023 Uiso 1 1 d D . . O2W O 1.3419(10) 0.1736(7) 0.1947(8) 0.0172(19) Uani 1 1 d DU . . H3 H 1.291(5) 0.195(5) 0.137(4) 0.021 Uiso 1 1 d D . . H4 H 1.403(4) 0.232(4) 0.206(4) 0.021 Uiso 1 1 d D . . O3W O 1.2520(9) 0.0072(7) 0.4818(6) 0.020(2) Uani 1 1 d D . . H5 H 1.177(3) 0.002(6) 0.518(4) 0.023 Uiso 1 1 d D . . H6 H 1.321(3) -0.013(5) 0.524(4) 0.023 Uiso 1 1 d D . . O1 O 1.4363(13) 0.1448(5) 0.4046(10) 0.017(3) Uani 1 1 d . . . O2 O 1.6303(9) 0.1864(7) 0.4425(8) 0.020(2) Uani 1 1 d . . . O3 O 1.3106(10) 0.3264(8) 0.3361(8) 0.012(2) Uani 1 1 d . . . O4 O 1.4127(9) 0.4836(6) 0.3547(7) 0.020(2) Uani 1 1 d . . . O5 O 1.0803(9) 0.2924(6) 0.4089(7) 0.0131(19) Uani 1 1 d . . . O6 O 1.2218(10) 0.2499(6) 0.5179(7) 0.016(2) Uani 1 1 d . . . C1 C 1.5215(13) 0.2134(9) 0.4285(10) 0.013(3) Uani 1 1 d . . . C2 C 1.4902(12) 0.3282(10) 0.4424(9) 0.013(2) Uani 1 1 d . . . H2A H 1.5654 0.3712 0.4371 0.016 Uiso 1 1 calc R . . H2B H 1.4628 0.3368 0.5112 0.016 Uiso 1 1 calc R . . C3 C 1.3964(13) 0.3784(10) 0.3744(10) 0.013(3) Uani 1 1 d . . . C4 C 1.1326(12) 0.3045(7) 0.4939(9) 0.008(2) Uani 1 1 d U . . Eu2 Eu 0.92749(2) 0.34957(3) 0.283923(18) 0.00927(18) Uani 1 1 d . . . O11W O 0.9219(8) 0.4857(6) 0.1356(6) 0.0143(18) Uani 1 1 d D . . H11 H 0.959(5) 0.555(3) 0.157(4) 0.017 Uiso 1 1 d D . . H12 H 0.974(5) 0.452(4) 0.086(4) 0.017 Uiso 1 1 d D . . O12W O 1.1239(10) 0.4297(6) 0.2435(8) 0.020(3) Uani 1 1 d D . . H13 H 1.201(4) 0.397(5) 0.261(5) 0.024 Uiso 1 1 d D . . H14 H 1.131(6) 0.5090(17) 0.250(5) 0.024 Uiso 1 1 d D . . O13W O 0.8217(9) 0.3242(7) 0.4439(7) 0.0149(17) Uani 1 1 d D . . H15 H 0.806(5) 0.387(3) 0.487(4) 0.018 Uiso 1 1 d D . . H16 H 0.881(5) 0.278(4) 0.479(4) 0.018 Uiso 1 1 d D . . O11 O 0.8432(10) 0.1678(7) 0.2945(8) 0.011(2) Uani 1 1 d . . . O12 O 0.7378(8) 0.0192(6) 0.2698(6) 0.0146(17) Uani 1 1 d . . . O13 O 0.7182(12) 0.3589(5) 0.2301(10) 0.015(3) Uani 1 1 d . . . O14 O 0.5295(8) 0.3221(7) 0.1939(7) 0.015(2) Uani 1 1 d . . . O15 O 1.0814(9) 0.2022(6) 0.2300(7) 0.0118(19) Uani 1 1 d . . . O16 O 0.9410(9) 0.2537(6) 0.1196(7) 0.015(2) Uani 1 1 d . . . C11 C 0.7555(12) 0.1141(9) 0.2585(9) 0.011(3) Uani 1 1 d . . . C12 C 0.6693(13) 0.1722(10) 0.1837(10) 0.011(2) Uani 1 1 d U . . H12A H 0.5927 0.1304 0.1793 0.013 Uiso 1 1 calc R . . H12B H 0.7057 0.1687 0.1176 0.013 Uiso 1 1 calc R . . C13 C 0.6369(13) 0.2945(8) 0.2051(9) 0.008(3) Uani 1 1 d . . . C14 C 1.0321(12) 0.1940(8) 0.1460(10) 0.013(3) Uani 1 1 d U . . C15 C 1.0810(16) 0.1178(4) 0.0674(12) 0.0117(11) Uani 1 1 d U . . H15A H 1.1443 0.0691 0.0961 0.014 Uiso 1 1 calc R . . H15B H 1.0154 0.0732 0.0363 0.014 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0082(4) 0.0081(3) 0.0100(4) 0.0000(2) -0.0001(3) -0.0002(2) O1W 0.013(6) 0.019(4) 0.026(6) 0.000(3) -0.006(5) -0.005(3) O2W 0.017(2) 0.017(2) 0.017(2) -0.0005(10) 0.0009(10) 0.0001(10) O3W 0.022(4) 0.022(4) 0.014(4) 0.009(3) -0.010(3) -0.005(3) O1 0.021(7) 0.003(5) 0.025(7) -0.002(3) -0.005(5) -0.002(3) O2 0.016(6) 0.012(4) 0.034(6) -0.012(4) 0.002(4) 0.002(4) O3 0.010(5) 0.013(3) 0.013(4) -0.005(3) -0.003(4) 0.002(4) O4 0.033(5) 0.005(3) 0.021(4) 0.002(3) -0.002(3) -0.005(3) O5 0.016(5) 0.015(4) 0.008(5) 0.001(3) -0.003(4) -0.002(3) O6 0.023(7) 0.016(4) 0.008(5) -0.001(3) -0.003(4) 0.006(3) C1 0.009(8) 0.022(5) 0.009(6) 0.005(4) 0.001(5) -0.003(5) C2 0.006(4) 0.018(4) 0.015(5) -0.004(3) 0.001(3) -0.003(3) C3 0.016(7) 0.011(4) 0.011(6) 0.005(4) 0.011(5) 0.005(5) C4 0.008(3) 0.008(3) 0.008(3) 0.0002(10) 0.0008(10) -0.0013(10) Eu2 0.0090(4) 0.0085(3) 0.0103(4) -0.0002(2) -0.0003(3) 0.0004(2) O11W 0.010(3) 0.014(3) 0.019(4) 0.002(3) 0.003(3) -0.004(2) O12W 0.016(6) 0.008(4) 0.035(7) 0.014(3) -0.003(5) 0.000(3) O13W 0.014(3) 0.021(3) 0.010(3) -0.007(2) 0.001(2) -0.005(2) O11 0.006(5) 0.013(4) 0.015(5) 0.007(3) 0.001(4) -0.003(3) O12 0.019(4) 0.015(3) 0.011(4) 0.002(3) -0.001(3) 0.000(3) O13 0.009(6) 0.020(5) 0.015(6) 0.002(3) 0.001(5) 0.005(3) O14 0.007(5) 0.013(4) 0.023(5) 0.007(3) -0.006(4) -0.001(3) O15 0.008(5) 0.015(4) 0.012(5) -0.003(3) 0.002(4) 0.000(3) O16 0.010(6) 0.019(4) 0.014(5) -0.001(3) 0.003(4) 0.005(3) C11 0.015(7) 0.007(5) 0.011(6) -0.008(4) 0.004(5) -0.006(5) C12 0.011(3) 0.011(2) 0.011(3) -0.0005(10) -0.0001(10) 0.0005(10) C13 0.016(8) 0.004(4) 0.003(6) 0.000(4) 0.000(5) -0.002(4) C14 0.013(3) 0.013(3) 0.013(3) 0.0005(10) 0.0011(10) -0.0011(10) C15 0.0112(13) 0.0115(13) 0.0125(13) -0.0003(10) 0.0001(9) 0.0002(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 O1 2.332(14) . ? Eu1 O12 2.334(7) 2 ? Eu1 O3 2.405(10) . ? Eu1 O3W 2.411(8) . ? Eu1 O15 2.433(10) . ? Eu1 O1W 2.498(11) . ? Eu1 O6 2.541(9) . ? Eu1 O2W 2.544(11) . ? Eu1 O5 2.580(9) . ? Eu1 C4 2.938(11) . ? Eu1 Eu2 4.2797(5) . ? O1 C1 1.297(17) . ? O2 C1 1.255(17) . ? O3 C3 1.241(17) . ? O4 C3 1.334(15) . ? O4 Eu2 2.270(7) 2_565 ? O5 C4 1.274(15) . ? O5 Eu2 2.448(9) . ? O6 C4 1.227(15) . ? C1 C2 1.466(16) . ? C2 C3 1.493(19) . ? C4 C15 1.502(17) 4_455 ? Eu2 O4 2.270(7) 2_465 ? Eu2 O13 2.403(14) . ? Eu2 O11 2.427(9) . ? Eu2 O12W 2.461(11) . ? Eu2 O13W 2.505(10) . ? Eu2 O16 2.516(9) . ? Eu2 O15 2.606(8) . ? Eu2 O11W 2.606(8) . ? Eu2 C14 2.930(12) . ? O11 C11 1.257(16) . ? O12 C11 1.194(15) . ? O12 Eu1 2.334(7) 2_455 ? O13 C13 1.236(16) . ? O14 C13 1.239(16) . ? O15 C14 1.244(16) . ? O16 C14 1.286(15) . ? C11 C12 1.538(19) . ? C12 C13 1.574(16) . ? C14 C15 1.527(18) . ? C15 C4 1.502(17) 4_454 ? 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 Eu1 O12 95.4(3) . 2 ? O1 Eu1 O3 71.6(3) . . ? O12 Eu1 O3 137.1(3) 2 . ? O1 Eu1 O3W 74.5(3) . . ? O12 Eu1 O3W 74.5(3) 2 . ? O3 Eu1 O3W 134.8(3) . . ? O1 Eu1 O15 146.2(4) . . ? O12 Eu1 O15 86.2(3) 2 . ? O3 Eu1 O15 84.3(3) . . ? O3W Eu1 O15 137.5(3) . . ? O1 Eu1 O1W 142.5(4) . . ? O12 Eu1 O1W 79.3(3) 2 . ? O3 Eu1 O1W 135.1(3) . . ? O3W Eu1 O1W 68.3(3) . . ? O15 Eu1 O1W 71.1(3) . . ? O1 Eu1 O6 80.1(4) . . ? O12 Eu1 O6 150.1(3) 2 . ? O3 Eu1 O6 69.7(3) . . ? O3W Eu1 O6 75.8(3) . . ? O15 Eu1 O6 113.9(3) . . ? O1W Eu1 O6 86.4(3) . . ? O1 Eu1 O2W 75.8(4) . . ? O12 Eu1 O2W 71.0(3) 2 . ? O3 Eu1 O2W 66.2(3) . . ? O3W Eu1 O2W 131.4(3) . . ? O15 Eu1 O2W 72.8(4) . . ? O1W Eu1 O2W 134.1(3) . . ? O6 Eu1 O2W 134.5(3) . . ? O1 Eu1 O5 123.7(3) . . ? O12 Eu1 O5 140.7(3) 2 . ? O3 Eu1 O5 67.9(3) . . ? O3W Eu1 O5 110.0(3) . . ? O15 Eu1 O5 63.8(2) . . ? O1W Eu1 O5 67.6(3) . . ? O6 Eu1 O5 50.2(3) . . ? O2W Eu1 O5 118.4(3) . . ? O1 Eu1 C4 101.6(4) . . ? O12 Eu1 C4 155.3(3) 2 . ? O3 Eu1 C4 66.3(3) . . ? O3W Eu1 C4 92.8(3) . . ? O15 Eu1 C4 89.4(3) . . ? O1W Eu1 C4 76.2(3) . . ? O6 Eu1 C4 24.5(3) . . ? O2W Eu1 C4 130.5(3) . . ? O5 Eu1 C4 25.7(3) . . ? O1 Eu1 Eu2 144.35(14) . . ? O12 Eu1 Eu2 115.6(2) 2 . ? O3 Eu1 Eu2 73.6(3) . . ? O3W Eu1 Eu2 128.7(2) . . ? O15 Eu1 Eu2 33.1(2) . . ? O1W Eu1 Eu2 65.2(2) . . ? O6 Eu1 Eu2 80.9(2) . . ? O2W Eu1 Eu2 97.1(2) . . ? O5 Eu1 Eu2 30.7(2) . . ? C4 Eu1 Eu2 56.4(2) . . ? C1 O1 Eu1 139.1(8) . . ? C3 O3 Eu1 134.8(9) . . ? C3 O4 Eu2 166.4(9) . 2_565 ? C4 O5 Eu2 150.0(7) . . ? C4 O5 Eu1 93.0(7) . . ? Eu2 O5 Eu1 116.7(4) . . ? C4 O6 Eu1 96.2(8) . . ? O2 C1 O1 123.3(11) . . ? O2 C1 C2 117.7(11) . . ? O1 C1 C2 119.0(12) . . ? C1 C2 C3 118.8(12) . . ? O3 C3 O4 121.5(13) . . ? O3 C3 C2 123.2(11) . . ? O4 C3 C2 115.3(12) . . ? O6 C4 O5 120.6(11) . . ? O6 C4 C15 119.6(12) . 4_455 ? O5 C4 C15 119.7(12) . 4_455 ? O6 C4 Eu1 59.3(6) . . ? O5 C4 Eu1 61.3(6) . . ? C15 C4 Eu1 177.8(8) 4_455 . ? O4 Eu2 O13 90.1(3) 2_465 . ? O4 Eu2 O11 140.7(3) 2_465 . ? O13 Eu2 O11 72.2(3) . . ? O4 Eu2 O5 91.7(3) 2_465 . ? O13 Eu2 O5 148.9(4) . . ? O11 Eu2 O5 87.3(3) . . ? O4 Eu2 O12W 78.9(3) 2_465 . ? O13 Eu2 O12W 139.6(3) . . ? O11 Eu2 O12W 136.4(3) . . ? O5 Eu2 O12W 71.0(3) . . ? O4 Eu2 O13W 73.1(3) 2_465 . ? O13 Eu2 O13W 78.1(4) . . ? O11 Eu2 O13W 69.1(3) . . ? O5 Eu2 O13W 72.8(4) . . ? O12W Eu2 O13W 132.9(3) . . ? O4 Eu2 O16 143.1(3) 2_465 . ? O13 Eu2 O16 80.9(3) . . ? O11 Eu2 O16 69.8(3) . . ? O5 Eu2 O16 114.2(3) . . ? O12W Eu2 O16 85.1(3) . . ? O13W Eu2 O16 137.8(3) . . ? O4 Eu2 O15 143.4(3) 2_465 . ? O13 Eu2 O15 125.4(3) . . ? O11 Eu2 O15 68.4(3) . . ? O5 Eu2 O15 63.2(2) . . ? O12W Eu2 O15 68.1(3) . . ? O13W Eu2 O15 118.7(3) . . ? O16 Eu2 O15 51.0(3) . . ? O4 Eu2 O11W 75.0(3) 2_465 . ? O13 Eu2 O11W 74.9(3) . . ? O11 Eu2 O11W 129.6(3) . . ? O5 Eu2 O11W 135.2(3) . . ? O12W Eu2 O11W 64.6(3) . . ? O13W Eu2 O11W 137.7(3) . . ? O16 Eu2 O11W 68.1(2) . . ? O15 Eu2 O11W 103.4(3) . . ? O4 Eu2 C14 153.0(3) 2_465 . ? O13 Eu2 C14 103.6(4) . . ? O11 Eu2 C14 66.2(3) . . ? O5 Eu2 C14 88.3(3) . . ? O12W Eu2 C14 75.6(3) . . ? O13W Eu2 C14 132.0(3) . . ? O16 Eu2 C14 25.9(3) . . ? O15 Eu2 C14 25.1(3) . . ? O11W Eu2 C14 86.1(3) . . ? O4 Eu2 Eu1 120.1(3) 2_465 . ? O13 Eu2 Eu1 146.82(16) . . ? O11 Eu2 Eu1 75.4(3) . . ? O5 Eu2 Eu1 32.6(2) . . ? O12W Eu2 Eu1 65.9(2) . . ? O13W Eu2 Eu1 96.8(2) . . ? O16 Eu2 Eu1 81.6(2) . . ? O15 Eu2 Eu1 30.6(2) . . ? O11W Eu2 Eu1 123.2(2) . . ? C14 Eu2 Eu1 55.7(3) . . ? C11 O11 Eu2 138.9(9) . . ? C11 O12 Eu1 156.8(9) . 2_455 ? C13 O13 Eu2 137.3(7) . . ? C14 O15 Eu1 151.4(8) . . ? C14 O15 Eu2 92.2(7) . . ? Eu1 O15 Eu2 116.3(4) . . ? C14 O16 Eu2 95.3(8) . . ? O12 C11 O11 126.2(14) . . ? O12 C11 C12 115.9(12) . . ? O11 C11 C12 117.5(11) . . ? C11 C12 C13 117.6(11) . . ? O13 C13 O14 122.8(10) . . ? O13 C13 C12 119.6(12) . . ? O14 C13 C12 117.5(10) . . ? O15 C14 O16 121.4(11) . . ? O15 C14 C15 121.7(12) . . ? O16 C14 C15 116.8(12) . . ? O15 C14 Eu2 62.7(6) . . ? O16 C14 Eu2 58.8(6) . . ? C15 C14 Eu2 175.4(9) . . ? C4 C15 C14 102.5(4) 4_454 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.806 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.114