Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Duk-Young Jung' _publ_contact_author_address ; Department of Chemistry Sungkyunkwan University Chunchun-dong 300 Suwon city Gyunggi-do 440-746 SOUTH KOREA ; _publ_contact_author_email DYJUNG@SKKU.EDU _publ_section_title ; Two-dimensional carboxylate bridged network of europium(III)-transition metal(II) glutarate compounds ; loop_ _publ_author_name 'Duk-Young Jung.' 'YooJin Kim.' 'YunJu Park.' data_{[Eu2Mn(4H2O)][O2C(CH2)3CO2]4}(2H2O) _database_code_depnum_ccdc_archive 'CCDC 259941' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((Eu2Mn(4H2O))(O2C(CH2)3CO2)4)(2H2O) _chemical_melting_point ? _chemical_formula_moiety C20H36Eu2MnO22 _chemical_formula_sum 'C20 H36 Eu2 Mn O22' _chemical_formula_weight 987.35 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' Mn Mn 0.3368 0.7283 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.839(2) _cell_length_b 9.0555(14) _cell_length_c 10.5957(16) _cell_angle_alpha 105.960(11) _cell_angle_beta 98.053(17) _cell_angle_gamma 109.828(15) _cell_volume 741.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour PINK _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 471 _exptl_absorpt_coefficient_mu 4.693 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 2666 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2487 _reflns_number_gt 2197 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0616P)^2^+4.2493P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2487 _refine_ls_number_parameters 204 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1155 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _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 Eu1 Eu 0.23519(5) 0.61237(5) 0.12624(4) 0.02454(17) Uani 1 1 d . . . Mn1 Mn 0.5000 1.0000 0.5000 0.0329(4) Uani 1 2 d S . . O1 O 0.2412(11) 0.9690(13) 0.4410(10) 0.089(4) Uani 1 1 d . . . O2 O 0.3734(12) 0.4193(11) 0.1307(9) 0.063(2) Uani 1 1 d . . . O3 O 0.2435(7) 0.8466(7) 0.0374(6) 0.0337(14) Uani 1 1 d . . . O4 O 0.4704(7) 0.8763(7) 0.2840(6) 0.0328(13) Uani 1 1 d . . . O5 O 0.5225(7) 0.7417(7) 0.1024(6) 0.0353(14) Uani 1 1 d . . . O6 O 0.0146(9) 0.6238(8) -0.0544(7) 0.0502(19) Uani 1 1 d . . . O7 O 0.0518(8) 0.7187(9) 0.2354(7) 0.0441(16) Uani 1 1 d . . . O8 O 0.2322(10) 0.4662(9) -0.1027(7) 0.0525(19) Uani 1 1 d . . . O9 O 0.4206(9) 0.7570(8) 0.5311(6) 0.0470(17) Uani 1 1 d . . . O10 O 0.2512(9) 0.5684(9) 0.3364(7) 0.0471(17) Uani 1 1 d . . . C1 C 0.1045(10) 0.7706(10) -0.0467(8) 0.0263(17) Uani 1 1 d . A . C2 C 0.0363(10) 0.8422(11) -0.1411(9) 0.0295(18) Uani 1 1 d . . . H2A H -0.0563 0.8642 -0.1135 0.035 Uiso 1 1 calc R A . H2B H -0.0068 0.7591 -0.2319 0.035 Uiso 1 1 calc R . . C3 C 0.1627(11) 1.0040(11) -0.1466(10) 0.0319(18) Uani 1 1 d . A . H3A H 0.1039 1.0557 -0.1922 0.038 Uiso 1 1 calc R . . H3B H 0.2197 1.0813 -0.0547 0.038 Uiso 1 1 calc R . . C5 C 0.5609(10) 0.8716(10) 0.2007(8) 0.0263(17) Uani 1 1 d . . . C4 C 0.2898(11) 0.9732(11) -0.2203(9) 0.037(2) Uani 1 1 d . . . H4A H 0.3276 0.8973 -0.1894 0.044 Uiso 1 1 calc R A . H4B H 0.2358 0.9182 -0.3167 0.044 Uiso 1 1 calc R . . C6A C 0.083(2) 0.817(2) 0.3777(19) 0.023(5) Uiso 0.399(17) 1 d P A 1 C7A C -0.073(3) 0.772(3) 0.430(2) 0.027(5) Uiso 0.399(17) 1 d P . 1 C8A C 0.116(3) 0.395(3) 0.546(2) 0.029(5) Uiso 0.399(17) 1 d P . 1 C6B C -0.1106(18) 0.6353(18) 0.2142(14) 0.028(3) Uiso 0.601(17) 1 d P . 2 C7B C -0.177(2) 0.672(2) 0.3368(17) 0.042(4) Uiso 0.601(17) 1 d P . 2 C8B C 0.210(2) 0.487(2) 0.6191(18) 0.046(4) Uiso 0.601(17) 1 d P . 2 C9 C 0.2968(14) 0.4690(14) 0.5144(10) 0.045(2) Uani 1 1 d . . . C10 C 0.3275(12) 0.6120(11) 0.4571(9) 0.036(2) Uani 1 1 d . A . OW O 0.3496(9) 0.1716(8) 0.2357(7) 0.0467(17) 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 0.0214(2) 0.0192(2) 0.0268(2) 0.00878(16) 0.00192(15) 0.00179(16) Mn1 0.0449(11) 0.0304(10) 0.0201(8) 0.0053(7) 0.0032(8) 0.0157(9) O1 0.045(5) 0.106(8) 0.070(6) -0.040(5) -0.017(4) 0.044(5) O2 0.094(7) 0.066(5) 0.085(6) 0.055(5) 0.059(5) 0.059(5) O3 0.023(3) 0.026(3) 0.041(3) 0.015(3) -0.007(3) 0.000(2) O4 0.028(3) 0.030(3) 0.028(3) 0.004(2) 0.008(2) 0.001(3) O5 0.026(3) 0.030(3) 0.040(3) 0.007(3) 0.013(3) 0.002(3) O6 0.041(4) 0.032(4) 0.052(4) 0.025(3) -0.018(3) -0.013(3) O7 0.032(3) 0.057(4) 0.056(4) 0.028(4) 0.022(3) 0.022(3) O8 0.060(5) 0.038(4) 0.034(4) 0.008(3) 0.000(3) -0.002(3) O9 0.062(5) 0.034(4) 0.033(3) 0.007(3) -0.008(3) 0.015(3) O10 0.058(5) 0.044(4) 0.033(3) 0.014(3) 0.003(3) 0.015(3) C1 0.024(4) 0.024(4) 0.029(4) 0.011(3) 0.010(3) 0.005(3) C2 0.016(4) 0.031(4) 0.042(5) 0.019(4) 0.006(3) 0.004(3) C3 0.027(4) 0.025(4) 0.049(5) 0.017(4) 0.014(4) 0.011(4) C5 0.024(4) 0.025(4) 0.029(4) 0.009(3) 0.006(3) 0.008(3) C4 0.034(5) 0.025(4) 0.040(5) 0.008(4) 0.012(4) 0.000(4) C9 0.050(6) 0.051(6) 0.040(5) 0.021(5) 0.009(4) 0.024(5) C10 0.042(5) 0.033(5) 0.029(4) 0.007(4) 0.004(4) 0.015(4) OW 0.045(4) 0.036(4) 0.052(4) 0.015(3) -0.007(3) 0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O6 2.336(6) 2_565 ? Eu1 O10 2.361(6) . ? Eu1 O8 2.414(7) . ? Eu1 O7 2.421(6) . ? Eu1 O2 2.456(7) . ? Eu1 O5 2.492(6) . ? Eu1 O4 2.507(6) . ? Eu1 O3 2.530(6) . ? Eu1 O6 2.584(6) . ? Eu1 C5 2.860(8) . ? Eu1 C1 2.953(8) . ? Eu1 Eu1 4.0907(15) 2_565 ? Mn1 O1 2.184(8) 2_676 ? Mn1 O1 2.184(8) . ? Mn1 O4 2.187(6) 2_676 ? Mn1 O4 2.187(6) . ? Mn1 O9 2.205(7) 2_676 ? Mn1 O9 2.205(7) . ? O1 C6A 1.49(2) . ? O3 C1 1.249(10) . ? O4 C5 1.273(10) . ? O5 C5 1.241(10) . ? O6 C1 1.269(10) . ? O6 Eu1 2.336(6) 2_565 ? O7 C6B 1.328(16) . ? O7 C6A 1.46(2) . ? O8 C6B 1.331(16) 2_565 ? O9 C10 1.239(11) . ? O10 C10 1.243(11) . ? C1 C2 1.496(11) . ? C2 C3 1.534(11) . ? C3 C4 1.513(12) . ? C5 C4 1.505(12) 2_675 ? C4 C5 1.505(11) 2_675 ? C6A C7A 1.53(3) . ? C7A C8A 1.54(3) 2_566 ? C8A C7A 1.54(3) 2_566 ? C8A C9 1.63(2) . ? C6B O8 1.331(16) 2_565 ? C6B C7B 1.50(2) . ? C7B C8B 1.58(2) 2_566 ? C8B C9 1.44(2) . ? C8B C7B 1.58(2) 2_566 ? C9 C10 1.537(14) . ? 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 O6 Eu1 O10 84.0(2) 2_565 . ? O6 Eu1 O8 77.0(3) 2_565 . ? O10 Eu1 O8 137.7(3) . . ? O6 Eu1 O7 77.2(3) 2_565 . ? O10 Eu1 O7 72.5(2) . . ? O8 Eu1 O7 136.5(3) . . ? O6 Eu1 O2 86.1(3) 2_565 . ? O10 Eu1 O2 70.7(3) . . ? O8 Eu1 O2 70.6(3) . . ? O7 Eu1 O2 140.9(2) . . ? O6 Eu1 O5 147.5(3) 2_565 . ? O10 Eu1 O5 109.0(2) . . ? O8 Eu1 O5 73.6(2) . . ? O7 Eu1 O5 134.7(2) . . ? O2 Eu1 O5 71.4(3) . . ? O6 Eu1 O4 158.6(2) 2_565 . ? O10 Eu1 O4 77.6(2) . . ? O8 Eu1 O4 124.2(2) . . ? O7 Eu1 O4 86.8(2) . . ? O2 Eu1 O4 97.9(3) . . ? O5 Eu1 O4 51.63(19) . . ? O6 Eu1 O3 117.6(2) 2_565 . ? O10 Eu1 O3 137.8(2) . . ? O8 Eu1 O3 84.2(2) . . ? O7 Eu1 O3 77.5(2) . . ? O2 Eu1 O3 140.8(2) . . ? O5 Eu1 O3 73.0(2) . . ? O4 Eu1 O3 71.68(19) . . ? O6 Eu1 O6 67.6(2) 2_565 . ? O10 Eu1 O6 137.2(3) . . ? O8 Eu1 O6 67.5(3) . . ? O7 Eu1 O6 70.4(3) . . ? O2 Eu1 O6 134.3(3) . . ? O5 Eu1 O6 112.1(2) . . ? O4 Eu1 O6 120.3(2) . . ? O3 Eu1 O6 50.21(19) . . ? O6 Eu1 C5 172.4(3) 2_565 . ? O10 Eu1 C5 96.4(2) . . ? O8 Eu1 C5 97.9(2) . . ? O7 Eu1 C5 110.2(2) . . ? O2 Eu1 C5 86.9(3) . . ? O5 Eu1 C5 25.6(2) . . ? O4 Eu1 C5 26.4(2) . . ? O3 Eu1 C5 66.9(2) . . ? O6 Eu1 C5 115.9(2) . . ? O6 Eu1 C1 92.9(2) 2_565 . ? O10 Eu1 C1 145.1(2) . . ? O8 Eu1 C1 74.0(2) . . ? O7 Eu1 C1 72.9(2) . . ? O2 Eu1 C1 143.9(2) . . ? O5 Eu1 C1 92.1(2) . . ? O4 Eu1 C1 95.9(2) . . ? O3 Eu1 C1 24.8(2) . . ? O6 Eu1 C1 25.4(2) . . ? C5 Eu1 C1 91.0(2) . . ? O6 Eu1 Eu1 35.74(16) 2_565 2_565 ? O10 Eu1 Eu1 113.80(19) . 2_565 ? O8 Eu1 Eu1 68.3(2) . 2_565 ? O7 Eu1 Eu1 70.27(18) . 2_565 ? O2 Eu1 Eu1 113.7(2) . 2_565 ? O5 Eu1 Eu1 136.03(15) . 2_565 ? O4 Eu1 Eu1 148.30(15) . 2_565 ? O3 Eu1 Eu1 81.94(13) . 2_565 ? O6 Eu1 Eu1 31.88(14) . 2_565 ? C5 Eu1 Eu1 147.36(16) . 2_565 ? C1 Eu1 Eu1 57.21(15) . 2_565 ? O1 Mn1 O1 180.000(1) 2_676 . ? O1 Mn1 O4 86.1(3) 2_676 2_676 ? O1 Mn1 O4 93.9(3) . 2_676 ? O1 Mn1 O4 93.9(3) 2_676 . ? O1 Mn1 O4 86.1(3) . . ? O4 Mn1 O4 180.000(1) 2_676 . ? O1 Mn1 O9 90.8(4) 2_676 2_676 ? O1 Mn1 O9 89.2(4) . 2_676 ? O4 Mn1 O9 90.8(2) 2_676 2_676 ? O4 Mn1 O9 89.2(2) . 2_676 ? O1 Mn1 O9 89.2(4) 2_676 . ? O1 Mn1 O9 90.8(4) . . ? O4 Mn1 O9 89.2(2) 2_676 . ? O4 Mn1 O9 90.8(2) . . ? O9 Mn1 O9 180.000(1) 2_676 . ? C6A O1 Mn1 132.1(10) . . ? C1 O3 Eu1 96.9(5) . . ? C5 O4 Mn1 138.5(5) . . ? C5 O4 Eu1 92.4(5) . . ? Mn1 O4 Eu1 127.0(3) . . ? C5 O5 Eu1 94.0(5) . . ? C1 O6 Eu1 153.4(6) . 2_565 ? C1 O6 Eu1 93.8(5) . . ? Eu1 O6 Eu1 112.4(2) 2_565 . ? C6B O7 C6A 96.6(10) . . ? C6B O7 Eu1 125.7(7) . . ? C6A O7 Eu1 128.1(8) . . ? C6B O8 Eu1 133.4(8) 2_565 . ? C10 O9 Mn1 133.7(6) . . ? C10 O10 Eu1 149.2(7) . . ? O3 C1 O6 119.1(8) . . ? O3 C1 C2 123.7(7) . . ? O6 C1 C2 117.2(7) . . ? O3 C1 Eu1 58.3(4) . . ? O6 C1 Eu1 60.8(4) . . ? C2 C1 Eu1 176.8(6) . . ? C1 C2 C3 114.6(7) . . ? C4 C3 C2 112.3(7) . . ? O5 C5 O4 120.0(7) . . ? O5 C5 C4 120.8(7) . 2_675 ? O4 C5 C4 119.1(7) . 2_675 ? O5 C5 Eu1 60.4(4) . . ? O4 C5 Eu1 61.1(4) . . ? C4 C5 Eu1 165.7(6) 2_675 . ? C5 C4 C3 114.6(7) 2_675 . ? O7 C6A O1 117.8(13) . . ? O7 C6A C7A 112.6(15) . . ? O1 C6A C7A 127.8(15) . . ? C6A C7A C8A 111.7(16) . 2_566 ? C7A C8A C9 115.1(15) 2_566 . ? O7 C6B O8 133.0(12) . 2_565 ? O7 C6B C7B 115.1(12) . . ? O8 C6B C7B 111.7(12) 2_565 . ? C6B C7B C8B 104.9(13) . 2_566 ? C9 C8B C7B 106.9(13) . 2_566 ? C8B C9 C10 111.8(10) . . ? C8B C9 C8A 37.0(10) . . ? C10 C9 C8A 116.5(11) . . ? O9 C10 O10 125.6(9) . . ? O9 C10 C9 119.8(8) . . ? O10 C10 C9 114.6(8) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 1.208 _refine_diff_density_min -1.456 _refine_diff_density_rms 0.204 data_{[Eu2Fe(4H2O)][O2C(CH2)3CO2]4}(2H2O) _database_code_depnum_ccdc_archive 'CCDC 259942' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((Eu2Fe(4H2O))(O2C(CH2)3CO2)4)(2H2O) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H36 Eu2 Fe O22' _chemical_formula_weight 988.26 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' Fe Fe 0.3463 0.8444 '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 10.3466(17) _cell_length_b 11.726(2) _cell_length_c 12.6124(19) _cell_angle_alpha 74.512(12) _cell_angle_beta 84.358(11) _cell_angle_gamma 81.316(13) _cell_volume 1455.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.62 _cell_measurement_theta_max 12.38 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 4.845 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.0086 _exptl_absorpt_correction_T_max 0.0318 _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 'Siemens P4' _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 5374 _diffrn_reflns_av_R_equivalents 0.0126 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5067 _reflns_number_gt 4731 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0639P)^2^+3.3098P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5067 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.1003 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.36617(2) 0.246645(19) 0.865169(18) 0.02589(11) Uani 1 1 d . . . Eu2 Eu 0.15034(2) 0.246714(19) 0.619876(18) 0.02554(11) Uani 1 1 d . . . Fe1 Fe 0.0000 0.0000 0.5000 0.0286(2) Uani 1 2 d S . . Fe2 Fe 0.5000 0.5000 1.0000 0.0300(2) Uani 1 2 d S . . O1 O 0.2607(4) 0.4465(3) 0.7828(3) 0.0360(8) Uani 1 1 d . . . O2 O 0.5312(3) 0.3490(3) 0.9350(3) 0.0330(8) Uani 1 1 d . . . O3 O 0.5864(3) 0.1641(3) 0.9284(3) 0.0364(8) Uani 1 1 d . . . O4 O 0.3309(4) 0.0833(4) 1.0296(3) 0.0475(10) Uani 1 1 d . . . O5 O 0.5286(3) 0.3238(4) 0.7115(3) 0.0366(8) Uani 1 1 d . . . O6 O 0.4045(4) 0.0609(3) 0.8142(3) 0.0384(8) Uani 1 1 d . . . O7 O 0.3570(3) 0.2758(3) 0.6566(3) 0.0342(8) Uani 1 1 d . . . O8 O 0.1597(3) 0.2201(3) 0.8295(3) 0.0334(8) Uani 1 1 d . . . O9 O 0.2542(4) 0.3234(4) 1.0061(3) 0.0448(9) Uani 1 1 d . . . O10 O 0.1712(4) 0.4076(3) 0.4532(3) 0.0456(10) Uani 1 1 d . . . O11 O 0.2743(4) 0.1666(3) 0.4792(3) 0.0399(8) Uani 1 1 d . . . O12 O -0.0154(3) 0.1742(4) 0.7779(3) 0.0372(8) Uani 1 1 d . . . O13 O 0.1108(4) 0.4296(3) 0.6701(3) 0.0399(9) Uani 1 1 d . . . O14 O -0.0191(3) 0.1573(3) 0.5523(3) 0.0331(8) Uani 1 1 d . . . O15 O -0.0737(3) 0.3403(3) 0.5647(3) 0.0359(8) Uani 1 1 d . . . O16 O 0.2509(4) 0.0479(3) 0.7066(3) 0.0345(8) Uani 1 1 d . . . O17 O 0.0935(4) -0.0889(3) 0.6530(3) 0.0435(9) Uani 1 1 d . . . O18 O 0.1772(4) 0.0450(4) 0.4148(3) 0.0414(9) Uani 1 1 d . . . O19 O 0.3924(5) 0.5848(3) 0.8555(4) 0.0494(10) Uani 1 1 d . . . O20 O 0.3326(4) 0.4342(4) 1.0948(3) 0.0435(9) Uani 1 1 d . . . C1 C -0.1069(5) 0.2472(4) 0.5509(4) 0.0289(10) Uani 1 1 d . . . C2 C -0.2464(5) 0.2362(5) 0.5403(5) 0.0397(12) Uani 1 1 d . . . H2A H -0.2820 0.1936 0.6114 0.048 Uiso 1 1 calc R . . H2B H -0.2491 0.1881 0.4890 0.048 Uiso 1 1 calc R . . C3 C 0.6662(5) 0.3532(5) 0.5016(4) 0.0335(11) Uani 1 1 d . . . H3A H 0.6877 0.3874 0.4241 0.040 Uiso 1 1 calc R . . H3B H 0.6829 0.4087 0.5421 0.040 Uiso 1 1 calc R . . C4 C 0.5221(5) 0.3375(5) 0.5179(4) 0.0331(11) Uani 1 1 d . . . H4A H 0.4723 0.4097 0.4763 0.040 Uiso 1 1 calc R . . H4B H 0.5091 0.2728 0.4873 0.040 Uiso 1 1 calc R . . C5 C 0.4678(5) 0.3117(4) 0.6346(4) 0.0280(10) Uani 1 1 d . . . C6 C 0.3511(5) 0.0057(5) 0.7633(4) 0.0304(10) Uani 1 1 d . . . C7 C 0.4075(5) -0.1228(4) 0.7689(4) 0.0341(11) Uani 1 1 d . . . H7A H 0.4539 -0.1552 0.8359 0.041 Uiso 1 1 calc R . . H7B H 0.3361 -0.1690 0.7731 0.041 Uiso 1 1 calc R . . C8 C 0.5000(7) -0.1364(5) 0.6713(6) 0.0582(16) Uani 1 1 d . . . H8A H 0.5325 -0.2203 0.6808 0.070 Uiso 1 1 calc R . . H8B H 0.4515 -0.1102 0.6052 0.070 Uiso 1 1 calc R . . C9 C 0.3891(6) 0.0700(6) 0.3444(7) 0.0634(19) Uani 1 1 d . . . H9A H 0.4219 -0.0139 0.3709 0.076 Uiso 1 1 calc R . . H9B H 0.3565 0.0805 0.2724 0.076 Uiso 1 1 calc R . . C10 C 0.2727(5) 0.0974(4) 0.4208(4) 0.0341(11) Uani 1 1 d . . . C11 C 0.0456(4) 0.1888(4) 0.8529(4) 0.0276(10) Uani 1 1 d . . . C12 C -0.0090(5) 0.1715(5) 0.9696(4) 0.0350(11) Uani 1 1 d . . . H12A H 0.0044 0.2396 0.9952 0.042 Uiso 1 1 calc R . . H12B H 0.0403 0.1014 1.0148 0.042 Uiso 1 1 calc R . . C13 C -0.1532(5) 0.1568(5) 0.9876(4) 0.0347(11) Uani 1 1 d . . . H13A H -0.1702 0.0981 0.9510 0.042 Uiso 1 1 calc R . . H13B H -0.1744 0.1269 1.0658 0.042 Uiso 1 1 calc R . . C14 C 0.7592(5) 0.2722(5) 0.9443(5) 0.0381(12) Uani 1 1 d . . . H14A H 0.7631 0.3247 0.9914 0.046 Uiso 1 1 calc R . . H14B H 0.7935 0.3107 0.8712 0.046 Uiso 1 1 calc R . . C15 C 0.6195(5) 0.2593(4) 0.9379(4) 0.0288(10) Uani 1 1 d . . . C16 C 0.2544(5) 0.3666(4) 1.0845(4) 0.0340(11) Uani 1 1 d . . . C17 C 0.1468(5) 0.3379(5) 1.1748(4) 0.0417(12) Uani 1 1 d . . . H17A H 0.1060 0.2724 1.1652 0.050 Uiso 1 1 calc R . . H17B H 0.1853 0.3123 1.2458 0.050 Uiso 1 1 calc R . . C18 C 0.0456(7) 0.4418(6) 1.1740(5) 0.0558(16) Uani 1 1 d . . . H18A H 0.0168 0.4753 1.0998 0.067 Uiso 1 1 calc R . . H18B H 0.0832 0.5027 1.1954 0.067 Uiso 1 1 calc R . . C19 C 0.0735(6) 0.5937(5) 0.7465(5) 0.0441(13) Uani 1 1 d . . . H19A H 0.0442 0.6432 0.6762 0.053 Uiso 1 1 calc R . . H19B H 0.1249 0.6385 0.7770 0.053 Uiso 1 1 calc R . . C20 C 0.1548(5) 0.4810(5) 0.7312(4) 0.0361(11) Uani 1 1 d . . . OW1 O 0.3671(4) 0.4656(4) 0.2920(3) 0.0483(10) Uani 1 1 d . . . OW2 O 0.1356(4) 0.0289(4) 0.2081(3) 0.0484(10) 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 0.02351(15) 0.02783(16) 0.02739(16) -0.00748(11) -0.00205(10) -0.00562(10) Eu2 0.02294(15) 0.02734(16) 0.02790(16) -0.00862(11) -0.00126(10) -0.00551(10) Fe1 0.0258(5) 0.0300(5) 0.0331(5) -0.0135(4) -0.0002(4) -0.0046(4) Fe2 0.0324(5) 0.0289(5) 0.0314(5) -0.0121(4) 0.0015(4) -0.0069(4) O1 0.0345(19) 0.0304(19) 0.042(2) -0.0082(16) -0.0046(16) -0.0033(15) O2 0.0308(18) 0.0321(18) 0.0395(19) -0.0157(15) -0.0027(15) -0.0025(15) O3 0.0322(18) 0.0284(18) 0.049(2) -0.0084(16) -0.0094(16) -0.0024(15) O4 0.053(2) 0.035(2) 0.043(2) 0.0044(17) 0.0071(18) -0.0032(18) O5 0.0300(18) 0.053(2) 0.0316(18) -0.0148(17) 0.0004(15) -0.0155(16) O6 0.037(2) 0.0346(19) 0.047(2) -0.0158(16) -0.0087(17) -0.0031(16) O7 0.0247(17) 0.044(2) 0.0374(19) -0.0132(16) -0.0002(14) -0.0116(15) O8 0.0232(17) 0.041(2) 0.0378(19) -0.0124(16) 0.0001(14) -0.0073(15) O9 0.042(2) 0.059(2) 0.042(2) -0.0266(19) 0.0052(17) -0.0159(18) O10 0.057(3) 0.035(2) 0.036(2) -0.0008(16) 0.0089(18) -0.0042(18) O11 0.041(2) 0.045(2) 0.039(2) -0.0189(17) 0.0047(16) -0.0116(17) O12 0.0303(18) 0.055(2) 0.0315(18) -0.0153(17) 0.0003(15) -0.0158(17) O13 0.043(2) 0.037(2) 0.045(2) -0.0176(17) -0.0048(17) -0.0069(16) O14 0.0294(18) 0.0332(19) 0.0409(19) -0.0165(15) -0.0037(15) -0.0035(15) O15 0.0277(18) 0.0304(18) 0.050(2) -0.0113(16) -0.0064(16) -0.0024(14) O16 0.0349(19) 0.0292(18) 0.041(2) -0.0101(15) -0.0051(16) -0.0051(15) O17 0.051(2) 0.039(2) 0.044(2) -0.0111(17) -0.0143(18) -0.0071(18) O18 0.036(2) 0.047(2) 0.047(2) -0.0219(18) 0.0074(17) -0.0131(17) O19 0.068(3) 0.032(2) 0.050(2) -0.0084(17) -0.024(2) -0.0036(19) O20 0.045(2) 0.049(2) 0.043(2) -0.0213(18) 0.0109(17) -0.0203(18) C1 0.028(2) 0.032(3) 0.027(2) -0.0098(19) 0.0020(19) -0.004(2) C2 0.025(3) 0.035(3) 0.062(4) -0.019(3) -0.004(2) -0.003(2) C3 0.027(2) 0.040(3) 0.030(2) -0.004(2) -0.0009(19) -0.005(2) C4 0.028(3) 0.041(3) 0.029(2) -0.007(2) -0.0030(19) -0.006(2) C5 0.025(2) 0.028(2) 0.031(2) -0.0074(19) -0.0022(19) -0.0029(18) C6 0.025(2) 0.035(3) 0.030(2) -0.009(2) 0.0051(19) -0.005(2) C7 0.030(2) 0.031(3) 0.042(3) -0.011(2) 0.005(2) -0.008(2) C8 0.063(4) 0.044(3) 0.064(4) -0.014(3) 0.012(3) -0.004(3) C9 0.052(4) 0.060(4) 0.089(5) -0.040(4) 0.031(3) -0.023(3) C10 0.034(3) 0.032(3) 0.034(3) -0.006(2) 0.002(2) -0.006(2) C11 0.022(2) 0.029(2) 0.031(2) -0.0060(19) -0.0007(19) -0.0034(18) C12 0.024(2) 0.050(3) 0.029(2) -0.008(2) 0.0004(19) -0.003(2) C13 0.025(2) 0.043(3) 0.032(2) -0.004(2) 0.0006(19) -0.005(2) C14 0.026(3) 0.034(3) 0.056(3) -0.015(2) -0.001(2) -0.005(2) C15 0.028(2) 0.031(3) 0.027(2) -0.0073(19) 0.0007(19) -0.005(2) C16 0.035(3) 0.034(3) 0.033(3) -0.012(2) 0.004(2) -0.006(2) C17 0.044(3) 0.042(3) 0.038(3) -0.012(2) 0.012(2) -0.012(2) C18 0.065(4) 0.047(3) 0.046(3) -0.005(3) 0.010(3) 0.002(3) C19 0.040(3) 0.042(3) 0.051(3) -0.016(3) -0.001(3) -0.002(2) C20 0.034(3) 0.038(3) 0.035(3) -0.009(2) 0.004(2) -0.008(2) OW1 0.057(3) 0.054(2) 0.036(2) -0.0093(18) 0.0010(18) -0.021(2) OW2 0.055(3) 0.054(3) 0.038(2) -0.0118(18) 0.0036(18) -0.018(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 O8 2.309(3) . ? Eu1 O9 2.334(4) . ? Eu1 O6 2.399(4) . ? Eu1 O1 2.431(4) . ? Eu1 O4 2.458(4) . ? Eu1 O3 2.459(3) . ? Eu1 O5 2.506(4) . ? Eu1 O7 2.571(4) . ? Eu1 O2 2.571(3) . ? Eu1 C15 2.897(5) . ? Eu1 C5 2.933(5) . ? Eu1 Eu2 3.9893(6) . ? Eu2 O7 2.324(3) . ? Eu2 O13 2.362(4) . ? Eu2 O11 2.398(4) . ? Eu2 O16 2.418(4) . ? Eu2 O10 2.437(4) . ? Eu2 O15 2.490(3) . ? Eu2 O14 2.495(3) . ? Eu2 O12 2.549(4) . ? Eu2 O8 2.587(4) . ? Eu2 C1 2.880(5) . ? Eu2 C11 2.967(5) . ? Fe1 O14 2.095(3) . ? Fe1 O14 2.095(3) 2_556 ? Fe1 O18 2.097(4) . ? Fe1 O18 2.097(4) 2_556 ? Fe1 O17 2.176(4) . ? Fe1 O17 2.176(4) 2_556 ? Fe2 O2 2.112(3) . ? Fe2 O2 2.112(3) 2_667 ? Fe2 O20 2.128(4) 2_667 ? Fe2 O20 2.128(4) . ? Fe2 O19 2.156(4) 2_667 ? Fe2 O19 2.156(4) . ? O1 C20 1.286(6) . ? O2 C15 1.280(6) . ? O3 C15 1.253(6) . ? O5 C5 1.256(6) . ? O6 C6 1.239(6) . ? O7 C5 1.261(6) . ? O8 C11 1.272(6) . ? O9 C16 1.225(6) . ? O11 C10 1.236(6) . ? O12 C11 1.249(6) . ? O13 C20 1.251(6) . ? O14 C1 1.281(6) . ? O15 C1 1.252(6) . ? O16 C6 1.277(6) . ? O18 C10 1.257(6) . ? O20 C16 1.252(6) . ? C1 C2 1.490(7) . ? C2 C3 1.514(7) 1_455 ? C3 C2 1.514(7) 1_655 ? C3 C4 1.517(7) . ? C4 C5 1.491(7) . ? C6 C7 1.516(7) . ? C7 C8 1.512(8) . ? C8 C9 1.450(9) 2_656 ? C9 C8 1.450(9) 2_656 ? C9 C10 1.517(8) . ? C11 C12 1.497(7) . ? C12 C13 1.515(7) . ? C13 C14 1.511(7) 1_455 ? C14 C15 1.488(7) . ? C14 C13 1.511(7) 1_655 ? C16 C17 1.520(7) . ? C17 C18 1.480(8) . ? C18 C19 1.544(8) 2_567 ? C19 C20 1.503(8) . ? C19 C18 1.544(8) 2_567 ? 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 O8 Eu1 O9 83.83(13) . . ? O8 Eu1 O6 77.07(13) . . ? O9 Eu1 O6 138.23(14) . . ? O8 Eu1 O1 75.18(13) . . ? O9 Eu1 O1 71.94(14) . . ? O6 Eu1 O1 135.20(13) . . ? O8 Eu1 O4 82.75(14) . . ? O9 Eu1 O4 70.05(15) . . ? O6 Eu1 O4 70.93(14) . . ? O1 Eu1 O4 137.62(13) . . ? O8 Eu1 O3 150.49(12) . . ? O9 Eu1 O3 105.92(14) . . ? O6 Eu1 O3 77.48(12) . . ? O1 Eu1 O3 134.21(12) . . ? O4 Eu1 O3 75.01(14) . . ? O8 Eu1 O5 121.07(12) . . ? O9 Eu1 O5 133.53(13) . . ? O6 Eu1 O5 87.77(13) . . ? O1 Eu1 O5 77.52(13) . . ? O4 Eu1 O5 144.18(14) . . ? O3 Eu1 O5 72.38(12) . . ? O8 Eu1 O7 71.22(12) . . ? O9 Eu1 O7 138.87(14) . . ? O6 Eu1 O7 67.72(13) . . ? O1 Eu1 O7 70.37(12) . . ? O4 Eu1 O7 134.85(13) . . ? O3 Eu1 O7 111.93(12) . . ? O5 Eu1 O7 50.56(11) . . ? O8 Eu1 O2 154.66(12) . . ? O9 Eu1 O2 73.84(12) . . ? O6 Eu1 O2 127.87(12) . . ? O1 Eu1 O2 86.44(12) . . ? O4 Eu1 O2 100.25(14) . . ? O3 Eu1 O2 51.26(11) . . ? O5 Eu1 O2 70.06(11) . . ? O7 Eu1 O2 119.08(11) . . ? O8 Eu1 C15 172.56(13) . . ? O9 Eu1 C15 92.53(13) . . ? O6 Eu1 C15 101.76(13) . . ? O1 Eu1 C15 109.90(13) . . ? O4 Eu1 C15 89.92(14) . . ? O3 Eu1 C15 25.40(13) . . ? O5 Eu1 C15 65.99(12) . . ? O7 Eu1 C15 115.33(13) . . ? O2 Eu1 C15 26.21(13) . . ? O8 Eu1 C5 96.41(13) . . ? O9 Eu1 C5 143.66(14) . . ? O6 Eu1 C5 75.95(13) . . ? O1 Eu1 C5 73.04(13) . . ? O4 Eu1 C5 146.21(14) . . ? O3 Eu1 C5 91.65(13) . . ? O5 Eu1 C5 25.17(12) . . ? O7 Eu1 C5 25.42(12) . . ? O2 Eu1 C5 94.67(12) . . ? C15 Eu1 C5 90.37(13) . . ? O8 Eu1 Eu2 37.82(9) . . ? O9 Eu1 Eu2 115.42(10) . . ? O6 Eu1 Eu2 67.52(9) . . ? O1 Eu1 Eu2 68.92(9) . . ? O4 Eu1 Eu2 112.27(11) . . ? O3 Eu1 Eu2 138.10(9) . . ? O5 Eu1 Eu2 83.66(8) . . ? O7 Eu1 Eu2 33.40(7) . . ? O2 Eu1 Eu2 147.45(8) . . ? C15 Eu1 Eu2 148.55(9) . . ? C5 Eu1 Eu2 58.69(9) . . ? O7 Eu2 O13 76.76(13) . . ? O7 Eu2 O11 82.05(13) . . ? O13 Eu2 O11 138.07(14) . . ? O7 Eu2 O16 76.35(13) . . ? O13 Eu2 O16 134.47(13) . . ? O11 Eu2 O16 72.20(13) . . ? O7 Eu2 O10 86.33(14) . . ? O13 Eu2 O10 71.84(14) . . ? O11 Eu2 O10 71.05(14) . . ? O16 Eu2 O10 141.09(13) . . ? O7 Eu2 O15 146.89(12) . . ? O13 Eu2 O15 73.05(12) . . ? O11 Eu2 O15 112.19(13) . . ? O16 Eu2 O15 135.72(12) . . ? O10 Eu2 O15 71.70(14) . . ? O7 Eu2 O14 158.51(12) . . ? O13 Eu2 O14 124.21(13) . . ? O11 Eu2 O14 78.39(12) . . ? O16 Eu2 O14 89.17(12) . . ? O10 Eu2 O14 95.61(14) . . ? O15 Eu2 O14 51.81(11) . . ? O7 Eu2 O12 120.20(12) . . ? O13 Eu2 O12 85.72(13) . . ? O11 Eu2 O12 136.07(13) . . ? O16 Eu2 O12 77.09(13) . . ? O10 Eu2 O12 140.60(13) . . ? O15 Eu2 O12 70.93(12) . . ? O14 Eu2 O12 70.43(12) . . ? O7 Eu2 O8 70.69(12) . . ? O13 Eu2 O8 67.13(13) . . ? O11 Eu2 O8 137.09(12) . . ? O16 Eu2 O8 69.59(12) . . ? O10 Eu2 O8 136.37(13) . . ? O15 Eu2 O8 108.61(12) . . ? O14 Eu2 O8 119.31(12) . . ? O12 Eu2 O8 49.95(11) . . ? O7 Eu2 C1 171.02(14) . . ? O13 Eu2 C1 97.93(13) . . ? O11 Eu2 C1 97.70(13) . . ? O16 Eu2 C1 112.20(13) . . ? O10 Eu2 C1 85.12(15) . . ? O15 Eu2 C1 25.67(13) . . ? O14 Eu2 C1 26.35(13) . . ? O12 Eu2 C1 65.95(12) . . ? O8 Eu2 C1 114.22(12) . . ? O7 Eu2 C11 95.92(12) . . ? O13 Eu2 C11 74.07(13) . . ? O11 Eu2 C11 144.58(13) . . ? O16 Eu2 C11 72.98(13) . . ? O10 Eu2 C11 144.33(13) . . ? O15 Eu2 C11 88.67(13) . . ? O14 Eu2 C11 94.86(12) . . ? O12 Eu2 C11 24.71(12) . . ? O8 Eu2 C11 25.31(12) . . ? C1 Eu2 C11 89.46(13) . . ? O7 Eu2 Eu1 37.51(9) . . ? O13 Eu2 Eu1 67.85(9) . . ? O11 Eu2 Eu1 112.86(9) . . ? O16 Eu2 Eu1 68.38(8) . . ? O10 Eu2 Eu1 115.74(11) . . ? O15 Eu2 Eu1 134.07(9) . . ? O14 Eu2 Eu1 148.55(9) . . ? O12 Eu2 Eu1 82.87(8) . . ? O8 Eu2 Eu1 33.18(7) . . ? C1 Eu2 Eu1 146.97(9) . . ? C11 Eu2 Eu1 58.42(9) . . ? O14 Fe1 O14 180.0 . 2_556 ? O14 Fe1 O18 88.68(14) . . ? O14 Fe1 O18 91.32(14) 2_556 . ? O14 Fe1 O18 91.32(14) . 2_556 ? O14 Fe1 O18 88.68(14) 2_556 2_556 ? O18 Fe1 O18 180.00(11) . 2_556 ? O14 Fe1 O17 86.83(14) . . ? O14 Fe1 O17 93.17(14) 2_556 . ? O18 Fe1 O17 93.06(16) . . ? O18 Fe1 O17 86.94(16) 2_556 . ? O14 Fe1 O17 93.17(14) . 2_556 ? O14 Fe1 O17 86.83(14) 2_556 2_556 ? O18 Fe1 O17 86.94(16) . 2_556 ? O18 Fe1 O17 93.06(16) 2_556 2_556 ? O17 Fe1 O17 180.00(13) . 2_556 ? O2 Fe2 O2 180.000(1) . 2_667 ? O2 Fe2 O20 90.44(14) . 2_667 ? O2 Fe2 O20 89.56(14) 2_667 2_667 ? O2 Fe2 O20 89.56(14) . . ? O2 Fe2 O20 90.44(14) 2_667 . ? O20 Fe2 O20 180.000(1) 2_667 . ? O2 Fe2 O19 94.97(15) . 2_667 ? O2 Fe2 O19 85.03(15) 2_667 2_667 ? O20 Fe2 O19 93.43(18) 2_667 2_667 ? O20 Fe2 O19 86.57(17) . 2_667 ? O2 Fe2 O19 85.03(15) . . ? O2 Fe2 O19 94.97(15) 2_667 . ? O20 Fe2 O19 86.57(17) 2_667 . ? O20 Fe2 O19 93.43(18) . . ? O19 Fe2 O19 180.000(1) 2_667 . ? C20 O1 Eu1 130.4(3) . . ? C15 O2 Fe2 136.9(3) . . ? C15 O2 Eu1 91.3(3) . . ? Fe2 O2 Eu1 129.88(15) . . ? C15 O3 Eu1 97.3(3) . . ? C5 O5 Eu1 96.8(3) . . ? C6 O6 Eu1 138.9(3) . . ? C5 O7 Eu2 156.3(3) . . ? C5 O7 Eu1 93.6(3) . . ? Eu2 O7 Eu1 109.09(13) . . ? C11 O8 Eu1 156.1(3) . . ? C11 O8 Eu2 94.3(3) . . ? Eu1 O8 Eu2 109.00(13) . . ? C16 O9 Eu1 150.4(4) . . ? C10 O11 Eu2 143.2(3) . . ? C11 O12 Eu2 96.7(3) . . ? C20 O13 Eu2 139.4(4) . . ? C1 O14 Fe1 136.5(3) . . ? C1 O14 Eu2 93.8(3) . . ? Fe1 O14 Eu2 129.25(16) . . ? C1 O15 Eu2 94.8(3) . . ? C6 O16 Eu2 134.5(3) . . ? C10 O18 Fe1 140.9(3) . . ? C16 O20 Fe2 134.3(3) . . ? O15 C1 O14 118.6(4) . . ? O15 C1 C2 121.7(4) . . ? O14 C1 C2 119.6(4) . . ? O15 C1 Eu2 59.5(3) . . ? O14 C1 Eu2 59.8(2) . . ? C2 C1 Eu2 167.9(4) . . ? C1 C2 C3 115.2(4) . 1_455 ? C2 C3 C4 112.1(4) 1_655 . ? C5 C4 C3 115.2(4) . . ? O5 C5 O7 119.0(4) . . ? O5 C5 C4 122.5(4) . . ? O7 C5 C4 118.5(4) . . ? O5 C5 Eu1 58.1(2) . . ? O7 C5 Eu1 61.0(3) . . ? C4 C5 Eu1 176.8(3) . . ? O6 C6 O16 125.3(5) . . ? O6 C6 C7 117.9(4) . . ? O16 C6 C7 116.8(4) . . ? C8 C7 C6 113.3(4) . . ? C9 C8 C7 114.2(5) 2_656 . ? C8 C9 C10 119.8(5) 2_656 . ? O11 C10 O18 125.4(5) . . ? O11 C10 C9 121.9(5) . . ? O18 C10 C9 112.7(5) . . ? O12 C11 O8 118.8(4) . . ? O12 C11 C12 123.1(4) . . ? O8 C11 C12 118.1(4) . . ? O12 C11 Eu2 58.6(2) . . ? O8 C11 Eu2 60.4(2) . . ? C12 C11 Eu2 174.8(4) . . ? C11 C12 C13 115.1(4) . . ? C14 C13 C12 112.6(4) 1_455 . ? C15 C14 C13 115.0(4) . 1_655 ? O3 C15 O2 118.6(4) . . ? O3 C15 C14 121.5(4) . . ? O2 C15 C14 119.8(4) . . ? O3 C15 Eu1 57.3(2) . . ? O2 C15 Eu1 62.5(2) . . ? C14 C15 Eu1 165.2(4) . . ? O9 C16 O20 125.9(5) . . ? O9 C16 C17 116.3(5) . . ? O20 C16 C17 117.8(4) . . ? C18 C17 C16 112.2(5) . . ? C17 C18 C19 111.5(5) . 2_567 ? C20 C19 C18 107.9(5) . 2_567 ? O13 C20 O1 126.7(5) . . ? O13 C20 C19 116.0(5) . . ? O1 C20 C19 117.3(5) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.457 _refine_diff_density_min -2.424 _refine_diff_density_rms 0.180 data_{[Eu2Co(4H2O)][O2C(CH2)3CO2]4}(2H2O) _database_code_depnum_ccdc_archive 'CCDC 259943' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((Eu2Co(4H2O))(O2C(CH2)3CO2)4)(2H2O) _chemical_melting_point ? _chemical_formula_moiety C20H36CoEu2O22 _chemical_formula_sum 'C20 H36 Co Eu2 O22' _chemical_formula_weight 991.34 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' Co Co 0.3494 0.9721 '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 10.4024(15) _cell_length_b 11.750(2) _cell_length_c 12.679(2) _cell_angle_alpha 74.606(13) _cell_angle_beta 84.189(9) _cell_angle_gamma 81.296(11) _cell_volume 1473.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 4.93 _cell_measurement_theta_max 12.51 _exptl_crystal_description BLOCK _exptl_crystal_colour BLUE _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 946 _exptl_absorpt_coefficient_mu 4.854 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.0060 _exptl_absorpt_correction_T_max 0.0340 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% ? _diffrn_reflns_number 5450 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5142 _reflns_number_gt 4637 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.1531P)^2^+1.6038P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5142 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.1811 _refine_ls_wR_factor_gt 0.1739 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Eu1 Eu 0.36619(3) 0.24662(3) 0.86499(3) 0.02659(19) Uani 1 1 d . . . Eu2 Eu 0.15026(3) 0.24639(3) 0.62064(3) 0.02618(19) Uani 1 1 d . . . Co1 Co 0.0000 0.0000 0.5000 0.0285(3) Uani 1 2 d S . . Co2 Co 0.5000 0.5000 1.0000 0.0288(3) Uani 1 2 d S . . O1 O 0.2613(5) 0.4471(5) 0.7816(5) 0.0363(12) Uani 1 1 d . . . O2 O 0.5308(4) 0.3490(5) 0.9358(4) 0.0321(11) Uani 1 1 d . . . O3 O 0.5856(5) 0.1636(4) 0.9280(5) 0.0388(12) Uani 1 1 d . . . O4 O 0.3299(6) 0.0842(5) 1.0305(5) 0.0477(14) Uani 1 1 d . . . O5 O 0.5292(5) 0.3232(5) 0.7113(4) 0.0375(12) Uani 1 1 d . . . O6 O 0.4041(5) 0.0605(5) 0.8153(5) 0.0387(12) Uani 1 1 d . . . O7 O 0.3584(5) 0.2741(5) 0.6570(4) 0.0323(11) Uani 1 1 d . . . O8 O 0.1575(5) 0.2209(5) 0.8303(4) 0.0324(11) Uani 1 1 d . . . O9 O 0.2535(6) 0.3265(6) 1.0052(5) 0.0479(14) Uani 1 1 d . . . O10 O 0.1726(6) 0.4075(5) 0.4536(5) 0.0444(14) Uani 1 1 d . . . O11 O 0.2742(5) 0.1635(5) 0.4793(5) 0.0401(12) Uani 1 1 d . . . O12 O -0.0157(5) 0.1741(5) 0.7796(4) 0.0374(12) Uani 1 1 d . . . O13 O 0.1124(5) 0.4288(5) 0.6701(5) 0.0390(12) Uani 1 1 d . . . O14 O -0.0183(4) 0.1556(5) 0.5523(4) 0.0312(11) Uani 1 1 d . . . O15 O -0.0725(5) 0.3398(5) 0.5663(5) 0.0396(13) Uani 1 1 d . . . O16 O 0.2506(5) 0.0470(5) 0.7075(5) 0.0363(12) Uani 1 1 d . . . O17 O 0.0952(5) -0.0879(5) 0.6484(5) 0.0415(13) Uani 1 1 d . . . O18 O 0.1746(5) 0.0426(5) 0.4156(5) 0.0406(12) Uani 1 1 d . . . O19 O 0.3931(6) 0.5836(5) 0.8589(5) 0.0426(13) Uani 1 1 d . . . O20 O 0.3347(5) 0.4367(5) 1.0935(5) 0.0432(13) Uani 1 1 d . . . C1 C -0.1059(7) 0.2461(6) 0.5520(6) 0.0296(15) Uani 1 1 d . . . C2 C -0.2467(7) 0.2361(8) 0.5414(8) 0.0404(18) Uani 1 1 d . . . H2A H -0.2498 0.1870 0.4914 0.048 Uiso 1 1 calc R . . H2B H -0.2831 0.1954 0.6124 0.048 Uiso 1 1 calc R . . C3 C -0.3317(7) 0.3527(7) 0.5012(6) 0.0338(15) Uani 1 1 d . . . H3A H -0.3095 0.3852 0.4239 0.041 Uiso 1 1 calc R . . H3B H -0.3151 0.4089 0.5406 0.041 Uiso 1 1 calc R . . C4 C 0.5241(6) 0.3374(7) 0.5175(6) 0.0332(15) Uani 1 1 d . . . H4A H 0.4750 0.4096 0.4764 0.040 Uiso 1 1 calc R . . H4B H 0.5111 0.2732 0.4865 0.040 Uiso 1 1 calc R . . C5 C 0.4688(6) 0.3110(6) 0.6345(5) 0.0270(14) Uani 1 1 d . . . C6 C 0.3513(6) 0.0048(7) 0.7635(6) 0.0308(15) Uani 1 1 d . . . C7 C 0.4082(7) -0.1239(6) 0.7669(6) 0.0328(15) Uani 1 1 d . . . H7A H 0.4543 -0.1575 0.8332 0.039 Uiso 1 1 calc R . . H7B H 0.3375 -0.1701 0.7700 0.039 Uiso 1 1 calc R . . C8 C 0.5003(6) 0.1344(5) 0.3302(5) 0.0503(19) Uani 1 1 d . . . H8A H 0.5479 0.1039 0.3961 0.060 Uiso 1 1 calc R . . H8B H 0.4702 0.2180 0.3243 0.060 Uiso 1 1 calc R . . C9 C 0.3865(6) 0.0708(5) 0.3421(5) 0.057(2) Uani 1 1 d R . . H9A H 0.4174 -0.0137 0.3641 0.068 Uiso 1 1 d R . . H9B H 0.3540 0.0866 0.2699 0.068 Uiso 1 1 d R . . C10 C 0.2703(7) 0.0949(6) 0.4205(6) 0.0328(15) Uani 1 1 d . . . C11 C 0.0454(6) 0.1889(6) 0.8533(6) 0.0281(14) Uani 1 1 d . . . C12 C -0.0100(7) 0.1721(8) 0.9712(6) 0.0363(16) Uani 1 1 d . . . H12A H 0.0028 0.2404 0.9963 0.044 Uiso 1 1 calc R . . H12B H 0.0389 0.1024 1.0164 0.044 Uiso 1 1 calc R . . C13 C 0.8448(7) 0.1570(7) 0.9885(6) 0.0367(16) Uani 1 1 d . . . H13A H 0.8283 0.0982 0.9521 0.044 Uiso 1 1 calc R . . H13B H 0.8226 0.1276 1.0663 0.044 Uiso 1 1 calc R . . C14 C 0.7583(7) 0.2734(8) 0.9443(8) 0.0412(19) Uani 1 1 d . . . H14A H 0.7620 0.3262 0.9907 0.049 Uiso 1 1 calc R . . H14B H 0.7931 0.3109 0.8715 0.049 Uiso 1 1 calc R . . C15 C 0.6172(7) 0.2597(7) 0.9379(6) 0.0312(15) Uani 1 1 d . . . C16 C 0.2557(7) 0.3693(6) 1.0836(6) 0.0340(15) Uani 1 1 d . . . C17 C 0.1509(7) 0.3386(7) 1.1760(6) 0.0422(16) Uani 1 1 d . . . H17A H 0.1113 0.2721 1.1678 0.051 Uiso 1 1 calc R . . H17B H 0.1906 0.3146 1.2458 0.051 Uiso 1 1 calc R . . C18 C 0.0469(9) 0.4432(7) 1.1755(7) 0.054(2) Uani 1 1 d . . . H18A H 0.0197 0.4775 1.1015 0.065 Uiso 1 1 calc R . . H18B H 0.0827 0.5037 1.1985 0.065 Uiso 1 1 calc R . . C19 C 0.0734(7) 0.5943(7) 0.7469(7) 0.0414(18) Uani 1 1 d . . . H19A H 0.0456 0.6442 0.6768 0.050 Uiso 1 1 calc R . . H19B H 0.1231 0.6387 0.7789 0.050 Uiso 1 1 calc R . . C20 C 0.1551(7) 0.4828(7) 0.7316(6) 0.0345(16) Uani 1 1 d . . . OW1 O 0.3694(6) 0.4654(5) 0.2927(5) 0.0460(14) Uani 1 1 d . . . OW2 O 0.1330(6) 0.0294(6) 0.2073(5) 0.0467(14) 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 0.0260(3) 0.0287(3) 0.0262(3) -0.00770(18) -0.00281(17) -0.00483(17) Eu2 0.0253(3) 0.0285(3) 0.0261(3) -0.00839(18) -0.00205(17) -0.00480(17) Co1 0.0270(7) 0.0306(8) 0.0306(8) -0.0123(6) -0.0014(6) -0.0044(6) Co2 0.0301(7) 0.0303(8) 0.0282(7) -0.0108(6) -0.0005(6) -0.0052(6) O1 0.033(3) 0.034(3) 0.042(3) -0.009(2) -0.003(2) -0.003(2) O2 0.031(3) 0.031(3) 0.039(3) -0.020(2) -0.004(2) 0.001(2) O3 0.035(3) 0.027(3) 0.054(3) -0.008(2) -0.010(2) -0.002(2) O4 0.051(3) 0.036(3) 0.043(3) 0.006(2) 0.006(3) -0.002(2) O5 0.033(3) 0.055(4) 0.028(3) -0.014(2) -0.003(2) -0.012(2) O6 0.035(3) 0.037(3) 0.047(3) -0.015(2) -0.010(2) -0.001(2) O7 0.030(3) 0.040(3) 0.035(3) -0.021(2) 0.001(2) -0.009(2) O8 0.028(2) 0.040(3) 0.034(3) -0.017(2) 0.003(2) -0.010(2) O9 0.053(3) 0.059(4) 0.041(3) -0.028(3) 0.006(3) -0.015(3) O10 0.054(3) 0.032(3) 0.039(3) 0.000(2) 0.009(3) -0.004(2) O11 0.043(3) 0.045(3) 0.037(3) -0.016(2) 0.003(2) -0.012(2) O12 0.033(3) 0.057(4) 0.026(3) -0.011(2) -0.002(2) -0.017(2) O13 0.044(3) 0.037(3) 0.038(3) -0.012(2) -0.008(2) -0.005(2) O14 0.027(2) 0.033(3) 0.038(3) -0.018(2) -0.007(2) 0.000(2) O15 0.031(2) 0.031(3) 0.059(4) -0.013(2) -0.009(2) -0.002(2) O16 0.037(3) 0.031(3) 0.042(3) -0.012(2) -0.006(2) -0.001(2) O17 0.049(3) 0.039(3) 0.038(3) -0.009(2) -0.013(2) -0.006(2) O18 0.038(3) 0.047(3) 0.041(3) -0.020(2) 0.010(2) -0.012(2) O19 0.053(3) 0.035(3) 0.040(3) -0.007(2) -0.016(3) -0.005(2) O20 0.048(3) 0.047(3) 0.040(3) -0.020(3) 0.011(2) -0.018(3) C1 0.030(4) 0.028(3) 0.031(4) -0.008(3) 0.003(3) -0.005(3) C2 0.027(4) 0.044(4) 0.055(5) -0.022(4) -0.005(3) -0.001(3) C3 0.030(3) 0.035(4) 0.034(4) -0.004(3) 0.002(3) -0.007(3) C4 0.029(3) 0.043(4) 0.028(4) -0.009(3) -0.005(3) -0.005(3) C5 0.031(3) 0.029(3) 0.021(3) -0.009(3) -0.001(3) -0.002(3) C6 0.023(3) 0.037(4) 0.034(4) -0.015(3) 0.003(3) -0.003(3) C7 0.029(3) 0.028(3) 0.042(4) -0.014(3) 0.004(3) -0.001(3) C8 0.052(5) 0.045(4) 0.050(5) -0.009(4) -0.003(4) 0.001(3) C9 0.053(5) 0.057(5) 0.067(6) -0.031(4) 0.023(4) -0.019(4) C10 0.035(3) 0.036(4) 0.025(3) -0.006(3) 0.004(3) -0.004(3) C11 0.028(3) 0.030(3) 0.028(3) -0.012(3) 0.002(3) -0.005(3) C12 0.026(3) 0.061(5) 0.023(3) -0.014(3) -0.002(3) -0.004(3) C13 0.032(4) 0.050(4) 0.027(4) -0.008(3) 0.002(3) -0.006(3) C14 0.027(4) 0.042(4) 0.056(5) -0.014(4) -0.006(3) -0.005(3) C15 0.026(3) 0.035(4) 0.031(4) -0.006(3) 0.001(3) -0.007(3) C16 0.036(3) 0.036(4) 0.031(4) -0.013(3) 0.004(3) -0.008(3) C17 0.044(4) 0.042(4) 0.038(4) -0.012(3) 0.008(3) -0.003(3) C18 0.066(5) 0.047(5) 0.039(5) -0.001(4) 0.005(4) 0.003(4) C19 0.035(4) 0.042(4) 0.046(5) -0.013(4) -0.002(3) 0.000(3) C20 0.032(4) 0.037(4) 0.039(4) -0.015(3) 0.000(3) -0.008(3) OW1 0.057(3) 0.051(4) 0.033(3) -0.012(3) 0.002(3) -0.021(3) OW2 0.056(3) 0.051(4) 0.035(3) -0.011(3) 0.002(3) -0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O8 2.337(5) . ? Eu1 O9 2.355(6) . ? Eu1 O6 2.399(5) . ? Eu1 O1 2.448(6) . ? Eu1 O3 2.466(5) . ? Eu1 O4 2.474(6) . ? Eu1 O5 2.519(5) . ? Eu1 O7 2.579(5) . ? Eu1 O2 2.587(5) . ? Eu1 C15 2.895(7) . ? Eu1 C5 2.948(7) . ? Eu1 Eu2 4.0074(7) . ? Eu2 O7 2.345(5) . ? Eu2 O13 2.357(5) . ? Eu2 O11 2.429(5) . ? Eu2 O16 2.432(5) . ? Eu2 O10 2.455(6) . ? Eu2 O15 2.490(5) . ? Eu2 O14 2.516(4) . ? Eu2 O12 2.567(5) . ? Eu2 O8 2.602(5) . ? Eu2 C1 2.886(7) . ? Eu2 C11 2.977(7) . ? Co1 O18 2.072(5) 2_556 ? Co1 O18 2.072(5) . ? Co1 O14 2.081(5) . ? Co1 O14 2.081(5) 2_556 ? Co1 O17 2.150(5) . ? Co1 O17 2.150(5) 2_556 ? Co2 O20 2.103(5) 2_667 ? Co2 O20 2.103(5) . ? Co2 O2 2.110(5) 2_667 ? Co2 O2 2.110(5) . ? Co2 O19 2.131(5) . ? Co2 O19 2.131(5) 2_667 ? O1 C20 1.288(9) . ? O2 C15 1.271(9) . ? O3 C15 1.262(9) . ? O5 C5 1.260(8) . ? O6 C6 1.254(9) . ? O7 C5 1.268(8) . ? O8 C11 1.262(8) . ? O9 C16 1.232(9) . ? O11 C10 1.241(9) . ? O12 C11 1.245(8) . ? O13 C20 1.275(9) . ? O14 C1 1.291(9) . ? O15 C1 1.265(9) . ? O16 C6 1.285(9) . ? O18 C10 1.262(9) . ? O20 C16 1.261(9) . ? C1 C2 1.509(10) . ? C2 C3 1.507(11) . ? C3 C4 1.525(9) 1_455 ? C4 C5 1.506(9) . ? C4 C3 1.525(9) 1_655 ? C6 C7 1.529(9) . ? C7 C8 1.499(9) 2_656 ? C8 C9 1.4679 . ? C8 C7 1.499(9) 2_656 ? C9 C10 1.528(9) . ? C11 C12 1.519(9) . ? C12 C13 1.534(9) 1_455 ? C13 C14 1.522(11) . ? C13 C12 1.534(9) 1_655 ? C14 C15 1.513(10) . ? C16 C17 1.525(10) . ? C17 C18 1.508(11) . ? C18 C19 1.555(11) 2_567 ? C19 C20 1.496(10) . ? C19 C18 1.555(11) 2_567 ? 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 O8 Eu1 O9 83.39(19) . . ? O8 Eu1 O6 77.53(17) . . ? O9 Eu1 O6 138.5(2) . . ? O8 Eu1 O1 74.92(18) . . ? O9 Eu1 O1 71.7(2) . . ? O6 Eu1 O1 135.19(19) . . ? O8 Eu1 O3 150.66(18) . . ? O9 Eu1 O3 106.2(2) . . ? O6 Eu1 O3 77.31(17) . . ? O1 Eu1 O3 134.31(17) . . ? O8 Eu1 O4 82.8(2) . . ? O9 Eu1 O4 70.2(2) . . ? O6 Eu1 O4 71.1(2) . . ? O1 Eu1 O4 137.53(19) . . ? O3 Eu1 O4 75.0(2) . . ? O8 Eu1 O5 121.37(17) . . ? O9 Eu1 O5 133.1(2) . . ? O6 Eu1 O5 87.95(19) . . ? O1 Eu1 O5 77.35(19) . . ? O3 Eu1 O5 72.41(18) . . ? O4 Eu1 O5 144.37(19) . . ? O8 Eu1 O7 71.67(17) . . ? O9 Eu1 O7 138.8(2) . . ? O6 Eu1 O7 67.69(18) . . ? O1 Eu1 O7 70.42(18) . . ? O3 Eu1 O7 111.68(18) . . ? O4 Eu1 O7 135.06(19) . . ? O5 Eu1 O7 50.51(16) . . ? O8 Eu1 O2 154.03(17) . . ? O9 Eu1 O2 73.39(18) . . ? O6 Eu1 O2 127.92(16) . . ? O1 Eu1 O2 86.64(17) . . ? O3 Eu1 O2 51.37(16) . . ? O4 Eu1 O2 99.7(2) . . ? O5 Eu1 O2 70.41(17) . . ? O7 Eu1 O2 119.46(16) . . ? O8 Eu1 C15 172.2(2) . . ? O9 Eu1 C15 92.3(2) . . ? O6 Eu1 C15 101.94(19) . . ? O1 Eu1 C15 109.84(19) . . ? O3 Eu1 C15 25.67(19) . . ? O4 Eu1 C15 89.7(2) . . ? O5 Eu1 C15 66.19(19) . . ? O7 Eu1 C15 115.45(19) . . ? O2 Eu1 C15 26.05(19) . . ? O8 Eu1 C5 96.80(18) . . ? O9 Eu1 C5 143.1(2) . . ? O6 Eu1 C5 76.21(19) . . ? O1 Eu1 C5 72.81(18) . . ? O3 Eu1 C5 91.62(19) . . ? O4 Eu1 C5 146.6(2) . . ? O5 Eu1 C5 25.12(17) . . ? O7 Eu1 C5 25.41(17) . . ? O2 Eu1 C5 94.97(17) . . ? C15 Eu1 C5 90.54(19) . . ? O8 Eu1 Eu2 38.05(13) . . ? O9 Eu1 Eu2 115.11(15) . . ? O6 Eu1 Eu2 67.78(13) . . ? O1 Eu1 Eu2 68.69(13) . . ? O3 Eu1 Eu2 138.19(13) . . ? O4 Eu1 Eu2 112.50(16) . . ? O5 Eu1 Eu2 83.78(11) . . ? O7 Eu1 Eu2 33.62(11) . . ? O2 Eu1 Eu2 147.79(12) . . ? C15 Eu1 Eu2 148.94(15) . . ? C5 Eu1 Eu2 58.87(13) . . ? O7 Eu2 O13 76.91(18) . . ? O7 Eu2 O11 82.05(17) . . ? O13 Eu2 O11 138.28(19) . . ? O7 Eu2 O16 75.92(18) . . ? O13 Eu2 O16 134.34(19) . . ? O11 Eu2 O16 71.98(19) . . ? O7 Eu2 O10 86.3(2) . . ? O13 Eu2 O10 71.8(2) . . ? O11 Eu2 O10 71.3(2) . . ? O16 Eu2 O10 140.9(2) . . ? O7 Eu2 O15 147.33(18) . . ? O13 Eu2 O15 73.28(17) . . ? O11 Eu2 O15 112.16(19) . . ? O16 Eu2 O15 135.73(18) . . ? O10 Eu2 O15 72.0(2) . . ? O7 Eu2 O14 157.62(17) . . ? O13 Eu2 O14 124.91(18) . . ? O11 Eu2 O14 77.56(17) . . ? O16 Eu2 O14 88.99(17) . . ? O10 Eu2 O14 95.68(19) . . ? O15 Eu2 O14 52.20(16) . . ? O7 Eu2 O12 120.07(17) . . ? O13 Eu2 O12 85.92(19) . . ? O11 Eu2 O12 135.67(18) . . ? O16 Eu2 O12 77.01(19) . . ? O10 Eu2 O12 140.91(19) . . ? O15 Eu2 O12 71.00(18) . . ? O14 Eu2 O12 70.94(17) . . ? O7 Eu2 O8 71.12(17) . . ? O13 Eu2 O8 66.96(18) . . ? O11 Eu2 O8 137.42(18) . . ? O16 Eu2 O8 69.83(18) . . ? O10 Eu2 O8 136.28(19) . . ? O15 Eu2 O8 108.13(18) . . ? O14 Eu2 O8 119.37(16) . . ? O12 Eu2 O8 49.49(15) . . ? O7 Eu2 C1 171.4(2) . . ? O13 Eu2 C1 98.44(19) . . ? O11 Eu2 C1 97.25(19) . . ? O16 Eu2 C1 112.06(19) . . ? O10 Eu2 C1 85.4(2) . . ? O15 Eu2 C1 25.91(19) . . ? O14 Eu2 C1 26.52(18) . . ? O12 Eu2 C1 66.16(18) . . ? O8 Eu2 C1 113.95(19) . . ? O7 Eu2 C11 95.99(18) . . ? O13 Eu2 C11 74.29(19) . . ? O11 Eu2 C11 144.19(19) . . ? O16 Eu2 C11 72.88(19) . . ? O10 Eu2 C11 144.50(19) . . ? O15 Eu2 C11 88.63(19) . . ? O14 Eu2 C11 95.18(17) . . ? O12 Eu2 C11 24.54(17) . . ? O8 Eu2 C11 24.99(17) . . ? C1 Eu2 C11 89.55(19) . . ? O7 Eu2 Eu1 37.52(13) . . ? O13 Eu2 Eu1 67.75(13) . . ? O11 Eu2 Eu1 112.93(13) . . ? O16 Eu2 Eu1 68.28(13) . . ? O10 Eu2 Eu1 115.56(15) . . ? O15 Eu2 Eu1 134.10(13) . . ? O14 Eu2 Eu1 148.71(13) . . ? O12 Eu2 Eu1 82.77(11) . . ? O8 Eu2 Eu1 33.60(10) . . ? C1 Eu2 Eu1 147.18(14) . . ? C11 Eu2 Eu1 58.50(12) . . ? O18 Co1 O18 180.00(15) 2_556 . ? O18 Co1 O14 90.8(2) 2_556 . ? O18 Co1 O14 89.2(2) . . ? O18 Co1 O14 89.2(2) 2_556 2_556 ? O18 Co1 O14 90.8(2) . 2_556 ? O14 Co1 O14 180.0 . 2_556 ? O18 Co1 O17 87.9(2) 2_556 . ? O18 Co1 O17 92.1(2) . . ? O14 Co1 O17 87.0(2) . . ? O14 Co1 O17 93.0(2) 2_556 . ? O18 Co1 O17 92.1(2) 2_556 2_556 ? O18 Co1 O17 87.9(2) . 2_556 ? O14 Co1 O17 93.0(2) . 2_556 ? O14 Co1 O17 87.0(2) 2_556 2_556 ? O17 Co1 O17 180.00(19) . 2_556 ? O20 Co2 O20 180.000(1) 2_667 . ? O20 Co2 O2 89.8(2) 2_667 2_667 ? O20 Co2 O2 90.2(2) . 2_667 ? O20 Co2 O2 90.2(2) 2_667 . ? O20 Co2 O2 89.8(2) . . ? O2 Co2 O2 180.000(1) 2_667 . ? O20 Co2 O19 87.0(2) 2_667 . ? O20 Co2 O19 93.0(2) . . ? O2 Co2 O19 94.7(2) 2_667 . ? O2 Co2 O19 85.3(2) . . ? O20 Co2 O19 93.0(2) 2_667 2_667 ? O20 Co2 O19 87.0(2) . 2_667 ? O2 Co2 O19 85.3(2) 2_667 2_667 ? O2 Co2 O19 94.7(2) . 2_667 ? O19 Co2 O19 180.000(1) . 2_667 ? C20 O1 Eu1 131.1(5) . . ? C15 O2 Co2 137.5(5) . . ? C15 O2 Eu1 90.6(4) . . ? Co2 O2 Eu1 130.1(2) . . ? C15 O3 Eu1 96.5(4) . . ? C5 O5 Eu1 96.8(4) . . ? C6 O6 Eu1 139.1(5) . . ? C5 O7 Eu2 156.0(5) . . ? C5 O7 Eu1 93.8(4) . . ? Eu2 O7 Eu1 108.85(19) . . ? C11 O8 Eu1 156.4(5) . . ? C11 O8 Eu2 94.4(4) . . ? Eu1 O8 Eu2 108.35(18) . . ? C16 O9 Eu1 149.5(5) . . ? C10 O11 Eu2 142.8(5) . . ? C11 O12 Eu2 96.5(4) . . ? C20 O13 Eu2 140.8(5) . . ? C1 O14 Co1 136.8(4) . . ? C1 O14 Eu2 93.0(4) . . ? Co1 O14 Eu2 129.8(2) . . ? C1 O15 Eu2 94.8(4) . . ? C6 O16 Eu2 134.5(5) . . ? C10 O18 Co1 141.0(5) . . ? C16 O20 Co2 134.3(5) . . ? O15 C1 O14 119.0(6) . . ? O15 C1 C2 121.2(6) . . ? O14 C1 C2 119.7(6) . . ? O15 C1 Eu2 59.3(4) . . ? O14 C1 Eu2 60.5(3) . . ? C2 C1 Eu2 168.0(5) . . ? C3 C2 C1 115.3(6) . . ? C2 C3 C4 111.6(6) . 1_455 ? C5 C4 C3 115.4(6) . 1_655 ? O5 C5 O7 118.8(6) . . ? O5 C5 C4 122.2(6) . . ? O7 C5 C4 119.0(6) . . ? O5 C5 Eu1 58.0(4) . . ? O7 C5 Eu1 60.8(4) . . ? C4 C5 Eu1 177.1(5) . . ? O6 C6 O16 125.0(7) . . ? O6 C6 C7 118.6(6) . . ? O16 C6 C7 116.4(6) . . ? C8 C7 C6 112.8(6) 2_656 . ? C9 C8 C7 114.3(4) . 2_656 ? C8 C9 C10 120.3(4) . . ? O11 C10 O18 125.9(7) . . ? O11 C10 C9 120.3(6) . . ? O18 C10 C9 113.8(6) . . ? O12 C11 O8 119.4(6) . . ? O12 C11 C12 122.8(6) . . ? O8 C11 C12 117.8(6) . . ? O12 C11 Eu2 59.0(4) . . ? O8 C11 Eu2 60.6(4) . . ? C12 C11 Eu2 174.6(5) . . ? C11 C12 C13 114.7(6) . 1_455 ? C14 C13 C12 112.0(6) . 1_655 ? C15 C14 C13 114.3(7) . . ? O3 C15 O2 119.9(6) . . ? O3 C15 C14 121.0(7) . . ? O2 C15 C14 119.0(7) . . ? O3 C15 Eu1 57.8(4) . . ? O2 C15 Eu1 63.4(3) . . ? C14 C15 Eu1 165.0(6) . . ? O9 C16 O20 126.2(7) . . ? O9 C16 C17 116.2(6) . . ? O20 C16 C17 117.7(6) . . ? C18 C17 C16 111.4(6) . . ? C17 C18 C19 111.5(6) . 2_567 ? C20 C19 C18 107.4(7) . 2_567 ? O13 C20 O1 124.6(7) . . ? O13 C20 C19 116.7(7) . . ? O1 C20 C19 118.8(7) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 3.023 _refine_diff_density_min -5.166 _refine_diff_density_rms 0.389 data_[Eu2Ni(4H2O)[O2C(CH2)3CO2]4](2H2O) _database_code_depnum_ccdc_archive 'CCDC 259944' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common (Eu2Ni(4H2O)(O2C(CH2)CO2)4)(2H2O) _chemical_melting_point C20H36Eu2NiO22 _chemical_formula_moiety ? _chemical_formula_sum 'C20 H36 Eu2 Ni O22' _chemical_formula_weight 991.12 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' Ni Ni 0.3393 1.1124 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.899(2) _cell_length_b 9.210(2) _cell_length_c 10.087(3) _cell_angle_alpha 106.055(5) _cell_angle_beta 97.118(4) _cell_angle_gamma 110.197(4) _cell_volume 723.2(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3550 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 28.46 _exptl_crystal_description prism _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 486 _exptl_absorpt_coefficient_mu 5.025 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6843 _exptl_absorpt_correction_T_max 0.7726 _exptl_absorpt_process_details 'Bruker SADABS' _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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4549 _diffrn_reflns_av_R_equivalents 0.0144 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.47 _reflns_number_total 3264 _reflns_number_gt 2991 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0433P)^2^+0.6006P] 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 0.0000(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3264 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 3.809 _refine_ls_shift/su_mean 0.017 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 0.22979(2) 0.10646(2) 0.122976(19) 0.02125(8) Uani 1 1 d . . . Ni1 Ni 0.5000 0.5000 0.5000 0.01925(14) Uani 1 2 d S . . O1 O 0.2612(4) 0.4858(5) 0.4446(4) 0.0308(7) Uani 1 1 d . . . O2 O 0.3640(5) -0.0824(4) 0.1291(4) 0.0382(8) Uani 1 1 d . . . O3 O 0.2399(3) 0.3466(3) 0.0420(3) 0.0292(6) Uani 1 1 d . . . O4 O 0.4648(3) 0.3661(3) 0.2883(3) 0.0239(5) Uani 1 1 d . . . O5 O 0.5101(3) 0.2398(3) 0.0907(3) 0.0304(6) Uani 1 1 d . . . O6 O 0.0141(3) 0.1267(3) -0.0608(3) 0.0283(6) Uani 1 1 d . . . O7 O 0.0446(3) 0.2046(3) 0.2412(3) 0.0294(6) Uani 1 1 d . . . O8 O 0.2155(3) -0.0422(4) -0.1169(3) 0.0331(6) Uani 1 1 d . . . O9 O 0.4195(4) 0.2832(3) 0.5399(3) 0.0337(7) Uani 1 1 d . . . O10 O 0.2510(4) 0.0712(4) 0.3499(3) 0.0388(7) Uani 1 1 d . . . O1W O 0.3345(5) 0.6614(4) 0.2418(4) 0.0393(8) Uani 1 1 d . . . C1 C 0.1035(4) 0.2724(4) -0.0478(4) 0.0219(7) Uani 1 1 d . . . C2 C 0.0422(5) 0.3512(5) -0.1411(4) 0.0272(8) Uani 1 1 d . . . H2A H -0.0496 0.3726 -0.1106 0.033 Uiso 1 1 calc R . . H2B H 0.0000 0.2732 -0.2376 0.033 Uiso 1 1 calc R . . C3 C 0.1683(5) 0.5111(5) -0.1432(4) 0.0281(8) Uani 1 1 d . . . H3A H 0.1121 0.5635 -0.1900 0.034 Uiso 1 1 calc R . . H3B H 0.2225 0.5851 -0.0462 0.034 Uiso 1 1 calc R . . C4 C 0.7029(5) 0.5177(5) 0.2198(5) 0.0329(9) Uani 1 1 d . . . H4A H 0.7543 0.5711 0.3208 0.040 Uiso 1 1 calc R . . H4B H 0.6666 0.5929 0.1877 0.040 Uiso 1 1 calc R . . C5 C 0.5541(4) 0.3653(4) 0.1987(4) 0.0218(7) Uani 1 1 d . . . C6 C -0.1114(5) 0.1459(4) 0.2276(4) 0.0235(7) Uani 1 1 d . . . C7 C -0.1718(6) 0.2070(6) 0.3556(5) 0.0357(9) Uani 1 1 d . . . H7A H -0.1068 0.3244 0.4000 0.043 Uiso 1 1 calc R . . H7B H -0.2849 0.1924 0.3227 0.043 Uiso 1 1 calc R . . C8 C -0.1676(8) 0.1306(8) 0.4669(6) 0.0556(14) Uani 1 1 d . . . H8A H -0.0578 0.1340 0.4951 0.067 Uiso 1 1 calc R . . H8B H -0.1917 0.1929 0.5499 0.067 Uiso 1 1 calc R . . C9 C -0.2841(11) -0.0350(9) 0.4165(8) 0.093(3) Uani 1 1 d . . . H9A H -0.2485 -0.0967 0.3415 0.111 Uiso 1 1 calc R . . H9B H -0.3882 -0.0364 0.3726 0.111 Uiso 1 1 calc R . . C10 C 0.3209(5) 0.1342(5) 0.4767(5) 0.0360(10) Uani 1 1 d . . . H101 H 0.208(9) 0.417(9) 0.410(7) 0.05(2) Uiso 1 1 d . . . H102 H 0.266(10) 0.559(11) 0.428(8) 0.09(3) Uiso 1 1 d . . . H103 H 0.381(8) -0.106(8) 0.192(7) 0.05(2) Uiso 1 1 d . . . H104 H 0.403(11) -0.125(11) 0.073(9) 0.10(3) Uiso 1 1 d . . . H105 H 0.317(7) 0.582(7) 0.183(6) 0.034(14) Uiso 1 1 d . . . H106 H 0.430(9) 0.682(8) 0.298(7) 0.06(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01547(11) 0.01671(11) 0.02533(12) 0.00273(7) 0.00239(7) 0.00353(7) Ni1 0.0187(3) 0.0177(3) 0.0180(3) 0.0058(2) 0.0033(2) 0.0040(2) O1 0.0240(15) 0.0294(17) 0.0321(16) 0.0031(15) 0.0036(12) 0.0096(14) O2 0.048(2) 0.0381(18) 0.048(2) 0.0223(16) 0.0230(17) 0.0297(16) O3 0.0227(13) 0.0230(13) 0.0343(15) 0.0114(12) -0.0036(11) 0.0027(11) O4 0.0206(12) 0.0250(13) 0.0189(12) 0.0046(10) 0.0052(10) 0.0030(10) O5 0.0229(13) 0.0256(14) 0.0335(15) 0.0006(12) 0.0096(11) 0.0054(11) O6 0.0233(13) 0.0219(13) 0.0313(14) 0.0063(11) 0.0025(11) 0.0030(11) O7 0.0210(13) 0.0272(14) 0.0307(15) 0.0003(12) 0.0059(11) 0.0063(11) O8 0.0237(14) 0.0312(15) 0.0344(16) 0.0013(13) 0.0033(12) 0.0084(12) O9 0.0416(17) 0.0229(14) 0.0269(14) 0.0105(12) -0.0007(12) 0.0031(12) O10 0.0377(17) 0.0318(16) 0.0311(16) 0.0029(13) -0.0003(13) 0.0047(13) O1W 0.045(2) 0.0301(17) 0.0368(18) 0.0065(15) -0.0041(15) 0.0171(15) C1 0.0186(16) 0.0217(17) 0.0257(18) 0.0085(14) 0.0064(13) 0.0078(13) C2 0.0171(16) 0.031(2) 0.031(2) 0.0144(16) 0.0033(14) 0.0043(15) C3 0.0239(18) 0.030(2) 0.035(2) 0.0164(17) 0.0096(16) 0.0107(16) C4 0.028(2) 0.028(2) 0.032(2) 0.0050(17) 0.0140(16) -0.0004(16) C5 0.0173(16) 0.0226(17) 0.0226(17) 0.0079(14) 0.0020(13) 0.0056(13) C6 0.0246(18) 0.0185(17) 0.0279(19) 0.0074(15) 0.0061(15) 0.0097(14) C7 0.032(2) 0.049(3) 0.035(2) 0.021(2) 0.0157(18) 0.018(2) C8 0.061(4) 0.057(3) 0.054(3) 0.027(3) 0.015(3) 0.023(3) C9 0.105(6) 0.051(4) 0.079(5) 0.027(4) -0.038(4) -0.003(4) C10 0.033(2) 0.0232(19) 0.041(2) 0.0129(18) -0.0073(18) 0.0026(17) _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 O6 2.327(3) 2 ? Eu1 O8 2.391(3) . ? Eu1 O10 2.393(3) . ? Eu1 O7 2.424(3) . ? Eu1 O2 2.435(3) . ? Eu1 O5 2.478(3) . ? Eu1 O4 2.520(3) . ? Eu1 O3 2.539(3) . ? Eu1 O6 2.591(3) . ? Eu1 C5 2.879(4) . ? Eu1 C1 2.954(4) . ? Eu1 Eu1 3.9978(9) 2 ? Ni1 O9 2.047(3) . ? Ni1 O9 2.047(3) 2_666 ? Ni1 O4 2.071(3) 2_666 ? Ni1 O4 2.071(3) . ? Ni1 O1 2.078(3) . ? Ni1 O1 2.078(3) 2_666 ? O3 C1 1.254(4) . ? O4 C5 1.276(5) . ? O5 C5 1.249(5) . ? O6 C1 1.261(5) . ? O6 Eu1 2.327(3) 2 ? O7 C6 1.278(5) . ? O8 C6 1.249(5) 2 ? O9 C10 1.267(5) . ? O10 C10 1.226(5) . ? C1 C2 1.495(5) . ? C2 C3 1.519(5) . ? C3 C4 1.516(6) 2_665 ? C4 C5 1.500(5) . ? C4 C3 1.516(6) 2_665 ? C6 O8 1.249(5) 2 ? C6 C7 1.500(6) . ? C7 C8 1.484(7) . ? C8 C9 1.417(9) . ? C9 C10 1.590(8) 2_556 ? C10 C9 1.590(8) 2_556 ? 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 O6 Eu1 O8 76.72(10) 2 . ? O6 Eu1 O10 82.96(10) 2 . ? O8 Eu1 O10 138.73(11) . . ? O6 Eu1 O7 75.61(10) 2 . ? O8 Eu1 O7 134.64(9) . . ? O10 Eu1 O7 71.34(11) . . ? O6 Eu1 O2 84.62(12) 2 . ? O8 Eu1 O2 72.13(12) . . ? O10 Eu1 O2 70.49(13) . . ? O7 Eu1 O2 138.70(12) . . ? O6 Eu1 O5 149.15(10) 2 . ? O8 Eu1 O5 75.71(9) . . ? O10 Eu1 O5 109.49(11) . . ? O7 Eu1 O5 134.72(9) . . ? O2 Eu1 O5 73.99(11) . . ? O6 Eu1 O4 156.10(9) 2 . ? O8 Eu1 O4 126.66(9) . . ? O10 Eu1 O4 75.41(10) . . ? O7 Eu1 O4 87.77(9) . . ? O2 Eu1 O4 97.40(11) . . ? O5 Eu1 O4 51.57(9) . . ? O6 Eu1 O3 120.76(9) 2 . ? O8 Eu1 O3 87.53(10) . . ? O10 Eu1 O3 133.53(10) . . ? O7 Eu1 O3 76.84(10) . . ? O2 Eu1 O3 143.32(11) . . ? O5 Eu1 O3 71.51(10) . . ? O4 Eu1 O3 70.32(9) . . ? O6 Eu1 O6 71.35(11) 2 . ? O8 Eu1 O6 67.27(10) . . ? O10 Eu1 O6 137.77(11) . . ? O7 Eu1 O6 70.15(10) . . ? O2 Eu1 O6 136.36(12) . . ? O5 Eu1 O6 109.66(10) . . ? O4 Eu1 O6 119.29(9) . . ? O3 Eu1 O6 50.13(8) . . ? O6 Eu1 C5 172.25(10) 2 . ? O8 Eu1 C5 100.45(10) . . ? O10 Eu1 C5 94.90(10) . . ? O7 Eu1 C5 110.84(10) . . ? O2 Eu1 C5 87.64(12) . . ? O5 Eu1 C5 25.59(10) . . ? O4 Eu1 C5 26.27(9) . . ? O3 Eu1 C5 65.91(9) . . ? O6 Eu1 C5 114.47(10) . . ? O6 Eu1 C1 96.34(10) 2 . ? O8 Eu1 C1 75.56(10) . . ? O10 Eu1 C1 142.93(11) . . ? O7 Eu1 C1 72.62(10) . . ? O2 Eu1 C1 146.54(12) . . ? O5 Eu1 C1 89.96(10) . . ? O4 Eu1 C1 94.87(10) . . ? O3 Eu1 C1 24.95(9) . . ? O6 Eu1 C1 25.21(9) . . ? C5 Eu1 C1 89.85(10) . . ? O6 Eu1 Eu1 37.88(7) 2 2 ? O8 Eu1 Eu1 67.41(7) . 2 ? O10 Eu1 Eu1 114.12(8) . 2 ? O7 Eu1 Eu1 68.61(7) . 2 ? O2 Eu1 Eu1 114.48(9) . 2 ? O5 Eu1 Eu1 135.87(7) . 2 ? O4 Eu1 Eu1 148.12(6) . 2 ? O3 Eu1 Eu1 83.24(6) . 2 ? O6 Eu1 Eu1 33.46(6) . 2 ? C5 Eu1 Eu1 147.68(7) . 2 ? C1 Eu1 Eu1 58.53(7) . 2 ? O9 Ni1 O9 179.999(2) . 2_666 ? O9 Ni1 O4 91.22(11) . 2_666 ? O9 Ni1 O4 88.78(11) 2_666 2_666 ? O9 Ni1 O4 88.78(11) . . ? O9 Ni1 O4 91.22(11) 2_666 . ? O4 Ni1 O4 180.0 2_666 . ? O9 Ni1 O1 92.35(15) . . ? O9 Ni1 O1 87.65(15) 2_666 . ? O4 Ni1 O1 93.32(12) 2_666 . ? O4 Ni1 O1 86.68(12) . . ? O9 Ni1 O1 87.65(15) . 2_666 ? O9 Ni1 O1 92.35(15) 2_666 2_666 ? O4 Ni1 O1 86.68(12) 2_666 2_666 ? O4 Ni1 O1 93.32(12) . 2_666 ? O1 Ni1 O1 180.0(2) . 2_666 ? C1 O3 Eu1 96.4(2) . . ? C5 O4 Ni1 135.7(2) . . ? C5 O4 Eu1 92.8(2) . . ? Ni1 O4 Eu1 130.92(12) . . ? C5 O5 Eu1 95.5(2) . . ? C1 O6 Eu1 156.4(2) . 2 ? C1 O6 Eu1 93.7(2) . . ? Eu1 O6 Eu1 108.65(11) 2 . ? C6 O7 Eu1 134.0(2) . . ? C6 O8 Eu1 140.1(3) 2 . ? C10 O9 Ni1 138.9(3) . . ? C10 O10 Eu1 146.0(3) . . ? O3 C1 O6 119.7(3) . . ? O3 C1 C2 122.0(3) . . ? O6 C1 C2 118.3(3) . . ? O3 C1 Eu1 58.68(19) . . ? O6 C1 Eu1 61.08(19) . . ? C2 C1 Eu1 176.8(3) . . ? C1 C2 C3 115.8(3) . . ? C4 C3 C2 111.8(3) 2_665 . ? C5 C4 C3 115.0(4) . 2_665 ? O5 C5 O4 118.9(3) . . ? O5 C5 C4 121.3(3) . . ? O4 C5 C4 119.6(3) . . ? O5 C5 Eu1 58.96(19) . . ? O4 C5 Eu1 60.94(18) . . ? C4 C5 Eu1 166.7(3) . . ? O8 C6 O7 124.9(4) 2 . ? O8 C6 C7 118.4(4) 2 . ? O7 C6 C7 116.7(3) . . ? C8 C7 C6 117.9(4) . . ? C9 C8 C7 111.0(5) . . ? C8 C9 C10 120.1(5) . 2_556 ? O10 C10 O9 125.9(4) . . ? O10 C10 C9 121.8(4) . 2_556 ? O9 C10 C9 112.2(4) . 2_556 ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 28.47 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 2.033 _refine_diff_density_min -0.916 _refine_diff_density_rms 0.130