Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Kwang-hwa Lii' _publ_contact_author_address ; Department of Chemistry National Central University Chungli 320 TAIWAN ; _publ_contact_author_email LIIKH@CC.NCU.EDU.TW _publ_section_title ; Synthesis, crystal structure, magnetic and luminescence properties of KEuGe2O6: A europium cyclogermanate containing infinite chains of edge-sharing Eu-O polyhedra ; loop_ _publ_author_name 'Kwang-hwa Lii' 'Bor-Chen Chang' 'Pei-Lin Chen' 'Pei-Yun Chiang' ; Han-Ching Yeh ; data_07oc11m _database_code_depnum_ccdc_archive 'CCDC 665615' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Eu Ge2 K O6' _chemical_formula_weight 432.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 8.6908(4) _cell_length_b 10.8647(6) _cell_length_c 19.2607(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.8610(10) _cell_angle_gamma 90.00 _cell_volume 1773.03(16) _cell_formula_units_Z 12 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3801 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description lamellar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 4.858 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 21.255 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.41654 _exptl_absorpt_correction_T_max 0.96204 _exptl_absorpt_process_details 'SADABS program' _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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6466 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.31 _reflns_number_total 2215 _reflns_number_gt 1996 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _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^)+(0.0167P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2215 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0399 _refine_ls_wR_factor_gt 0.0391 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _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 K1 K 0.18077(11) 0.89456(9) 0.07533(5) 0.0205(2) Uani 1 1 d . . . K2 K -0.5000 0.89388(12) 0.2500 0.0148(3) Uani 1 2 d S . . Eu1 Eu 0.0000 0.85447(2) 0.2500 0.00836(7) Uani 1 2 d S . . Eu2 Eu -0.32477(2) 0.793489(17) 0.080933(10) 0.00796(6) Uani 1 1 d . . . Ge1 Ge 0.23257(5) 0.13232(4) 0.25774(2) 0.00826(9) Uani 1 1 d . . . Ge2 Ge 0.02380(4) 0.58869(4) 0.09471(2) 0.00829(9) Uani 1 1 d . . . Ge3 Ge 0.11611(5) 0.07952(4) 0.39213(2) 0.00843(9) Uani 1 1 d . . . O1 O 0.1922(3) -0.0127(2) 0.22392(15) 0.0122(6) Uani 1 1 d . . . O2 O 0.2508(3) 0.2495(2) 0.19998(14) 0.0100(5) Uani 1 1 d . . . O3 O 0.1054(3) 0.1728(2) 0.31529(14) 0.0116(6) Uani 1 1 d . . . O4 O 0.4253(3) 0.1553(3) 0.31784(14) 0.0124(6) Uani 1 1 d . . . O5 O -0.0022(3) 0.4333(2) 0.10408(15) 0.0125(6) Uani 1 1 d . . . O6 O -0.1327(3) 0.6692(2) 0.04345(14) 0.0105(6) Uani 1 1 d . . . O7 O 0.1905(3) 0.6131(3) 0.05623(15) 0.0142(6) Uani 1 1 d . . . O8 O -0.0174(3) 0.1272(2) 0.43988(15) 0.0121(6) Uani 1 1 d . . . O9 O 0.1093(3) -0.0758(2) 0.37116(14) 0.0110(6) 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 K1 0.0163(5) 0.0254(5) 0.0194(5) -0.0011(4) 0.0030(4) 0.0008(4) K2 0.0149(6) 0.0154(6) 0.0140(6) 0.000 0.0029(5) 0.000 Eu1 0.00750(13) 0.00914(13) 0.00793(14) 0.000 0.00062(10) 0.000 Eu2 0.00793(9) 0.00880(10) 0.00700(10) -0.00009(7) 0.00132(7) -0.00018(7) Ge1 0.00885(19) 0.0085(2) 0.0070(2) 0.00082(15) 0.00081(15) -0.00129(15) Ge2 0.00791(19) 0.0097(2) 0.0067(2) -0.00008(15) 0.00033(15) 0.00167(15) Ge3 0.00831(19) 0.0090(2) 0.0082(2) -0.00003(15) 0.00224(15) 0.00124(15) O1 0.0152(14) 0.0071(13) 0.0147(15) -0.0017(11) 0.0039(11) -0.0030(11) O2 0.0114(13) 0.0101(13) 0.0069(13) 0.0029(10) -0.0010(10) -0.0009(10) O3 0.0126(13) 0.0108(14) 0.0109(14) 0.0040(11) 0.0019(11) 0.0018(11) O4 0.0104(13) 0.0178(15) 0.0072(14) 0.0039(11) -0.0018(11) -0.0026(11) O5 0.0111(13) 0.0093(14) 0.0165(15) 0.0001(11) 0.0020(11) 0.0007(11) O6 0.0090(13) 0.0150(14) 0.0061(14) -0.0001(11) -0.0013(10) 0.0047(11) O7 0.0100(14) 0.0234(16) 0.0090(14) 0.0025(12) 0.0014(11) 0.0011(11) O8 0.0113(13) 0.0133(14) 0.0129(15) 0.0021(11) 0.0052(11) 0.0039(11) O9 0.0116(13) 0.0085(14) 0.0125(14) -0.0015(11) 0.0021(11) 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 K1 O5 2.720(3) 3 ? K1 O8 2.798(3) 6_565 ? K1 O8 2.882(3) 2_565 ? K1 O9 2.946(3) 2_565 ? K1 O7 2.990(3) 7_565 ? K1 O1 3.015(3) 1_565 ? K1 O7 3.084(3) . ? K1 Ge3 3.4363(10) 2_565 ? K1 Ge3 3.4587(11) 6_565 ? K1 Ge2 3.6028(10) 3 ? K1 Ge2 3.6428(11) . ? K1 Ge3 3.8382(11) 4 ? K2 O3 2.771(3) 4_455 ? K2 O3 2.771(3) 3_455 ? K2 O1 2.800(3) 2_565 ? K2 O1 2.800(3) 1_465 ? K2 O5 2.839(3) 3_455 ? K2 O5 2.839(3) 4_455 ? K2 O2 3.012(3) 3_455 ? K2 O2 3.012(3) 4_455 ? K2 O4 3.252(3) 2_565 ? K2 O4 3.252(3) 1_465 ? K2 Ge1 3.4712(11) 4_455 ? K2 Ge1 3.4712(11) 3_455 ? Eu1 O1 2.345(3) 1_565 ? Eu1 O1 2.345(3) 2_565 ? Eu1 O9 2.436(3) 2_565 ? Eu1 O9 2.436(3) 1_565 ? Eu1 O2 2.448(3) 3_455 ? Eu1 O2 2.448(3) 4 ? Eu1 O4 2.681(3) 4 ? Eu1 O4 2.681(3) 3_455 ? Eu1 Ge1 3.3770(4) 3_455 ? Eu1 Ge1 3.3770(5) 4 ? Eu1 Ge1 3.6174(5) 1_565 ? Eu1 Ge1 3.6174(5) 2_565 ? Eu2 O8 2.250(3) 4_455 ? Eu2 O5 2.278(3) 3_455 ? Eu2 O2 2.291(3) 3_455 ? Eu2 O9 2.368(3) 2_565 ? Eu2 O6 2.376(3) 7_465 ? Eu2 O6 2.381(3) . ? Eu2 Ge2 3.4992(5) 3_455 ? Eu2 Ge3 3.5593(4) 4_455 ? Eu2 Ge3 3.5772(5) 2_565 ? Eu2 Ge2 3.6702(5) 7_465 ? Eu2 Eu2 3.7558(4) 7_465 ? Ge1 O1 1.711(3) . ? Ge1 O2 1.721(3) . ? Ge1 O3 1.786(3) . ? Ge1 O4 1.829(3) . ? Ge1 Eu1 3.3770(4) 3_545 ? Ge1 K2 3.4712(11) 3_545 ? Ge1 K2 3.5056(10) 1_645 ? Ge1 Eu1 3.6174(5) 1_545 ? Ge2 O5 1.718(3) . ? Ge2 O6 1.730(3) . ? Ge2 O7 1.787(3) . ? Ge2 O4 1.796(3) 4 ? Ge2 Eu2 3.4992(5) 3_545 ? Ge2 K1 3.6028(10) 3_445 ? Ge2 Eu2 3.6702(5) 7_465 ? Ge2 K2 3.7073(8) 3_545 ? Ge3 O8 1.713(3) . ? Ge3 O9 1.733(3) . ? Ge3 O3 1.779(3) . ? Ge3 O7 1.790(3) 4_545 ? Ge3 K1 3.4363(10) 2_545 ? Ge3 K1 3.4587(11) 6_566 ? Ge3 Eu2 3.5593(4) 4_445 ? Ge3 Eu2 3.5772(5) 2_545 ? Ge3 Eu1 3.6416(5) 1_545 ? Ge3 K1 3.8382(11) 4_545 ? O1 Eu1 2.345(3) 1_545 ? O1 K2 2.800(3) 1_645 ? O1 K1 3.015(3) 1_545 ? O2 Eu2 2.291(3) 3_545 ? O2 Eu1 2.448(3) 3_545 ? O2 K2 3.012(3) 3_545 ? O3 K2 2.771(3) 3_545 ? O4 Ge2 1.796(3) 4_545 ? O4 Eu1 2.681(3) 3_545 ? O4 K2 3.252(3) 1_645 ? O5 Eu2 2.278(3) 3_545 ? O5 K1 2.720(3) 3_445 ? O5 K2 2.839(3) 3_545 ? O6 Eu2 2.376(3) 7_465 ? O7 Ge3 1.790(3) 4 ? O7 K1 2.990(3) 7_565 ? O8 Eu2 2.250(3) 4_445 ? O8 K1 2.798(3) 6_566 ? O8 K1 2.882(3) 2_545 ? O9 Eu2 2.368(3) 2_545 ? O9 Eu1 2.436(3) 1_545 ? O9 K1 2.946(3) 2_545 ? 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 O5 K1 O8 126.04(9) 3 6_565 ? O5 K1 O8 109.80(8) 3 2_565 ? O8 K1 O8 78.01(9) 6_565 2_565 ? O5 K1 O9 144.98(9) 3 2_565 ? O8 K1 O9 86.47(8) 6_565 2_565 ? O8 K1 O9 59.94(8) 2_565 2_565 ? O5 K1 O7 67.88(8) 3 7_565 ? O8 K1 O7 58.42(8) 6_565 7_565 ? O8 K1 O7 101.94(8) 2_565 7_565 ? O9 K1 O7 144.13(8) 2_565 7_565 ? O5 K1 O1 86.40(8) 3 1_565 ? O8 K1 O1 142.82(8) 6_565 1_565 ? O8 K1 O1 73.42(8) 2_565 1_565 ? O9 K1 O1 58.75(7) 2_565 1_565 ? O7 K1 O1 150.95(8) 7_565 1_565 ? O5 K1 O7 97.16(8) 3 . ? O8 K1 O7 80.35(8) 6_565 . ? O8 K1 O7 152.08(8) 2_565 . ? O9 K1 O7 101.44(8) 2_565 . ? O7 K1 O7 81.15(8) 7_565 . ? O1 K1 O7 116.66(8) 1_565 . ? O5 K1 Ge3 129.80(7) 3 2_565 ? O8 K1 Ge3 83.58(6) 6_565 2_565 ? O8 K1 Ge3 29.85(5) 2_565 2_565 ? O9 K1 Ge3 30.29(5) 2_565 2_565 ? O7 K1 Ge3 127.48(6) 7_565 2_565 ? O1 K1 Ge3 59.92(5) 1_565 2_565 ? O7 K1 Ge3 130.04(6) . 2_565 ? O5 K1 Ge3 97.02(6) 3 6_565 ? O8 K1 Ge3 29.44(5) 6_565 6_565 ? O8 K1 Ge3 81.97(6) 2_565 6_565 ? O9 K1 Ge3 113.00(6) 2_565 6_565 ? O7 K1 Ge3 31.16(5) 7_565 6_565 ? O1 K1 Ge3 154.79(6) 1_565 6_565 ? O7 K1 Ge3 87.80(6) . 6_565 ? Ge3 K1 Ge3 100.39(3) 2_565 6_565 ? O5 K1 Ge2 27.23(6) 3 3 ? O8 K1 Ge2 118.00(6) 6_565 3 ? O8 K1 Ge2 82.80(6) 2_565 3 ? O9 K1 Ge2 130.74(6) 2_565 3 ? O7 K1 Ge2 69.32(6) 7_565 3 ? O1 K1 Ge2 81.62(5) 1_565 3 ? O7 K1 Ge2 123.30(6) . 3 ? Ge3 K1 Ge2 106.04(3) 2_565 3 ? Ge3 K1 Ge2 90.05(2) 6_565 3 ? O5 K1 Ge2 120.39(6) 3 . ? O8 K1 Ge2 81.46(6) 6_565 . ? O8 K1 Ge2 128.55(6) 2_565 . ? O9 K1 Ge2 72.22(6) 2_565 . ? O7 K1 Ge2 106.31(6) 7_565 . ? O1 K1 Ge2 98.14(6) 1_565 . ? O7 K1 Ge2 29.34(5) . . ? Ge3 K1 Ge2 101.61(3) 2_565 . ? Ge3 K1 Ge2 101.50(3) 6_565 . ? Ge2 K1 Ge2 147.52(3) 3 . ? O5 K1 Ge3 72.34(6) 3 4 ? O8 K1 Ge3 104.01(6) 6_565 4 ? O8 K1 Ge3 175.57(6) 2_565 4 ? O9 K1 Ge3 116.02(6) 2_565 4 ? O7 K1 Ge3 82.44(6) 7_565 4 ? O1 K1 Ge3 103.08(6) 1_565 4 ? O7 K1 Ge3 27.29(5) . 4 ? Ge3 K1 Ge3 145.94(3) 2_565 4 ? Ge3 K1 Ge3 101.75(3) 6_565 4 ? Ge2 K1 Ge3 99.51(2) 3 4 ? Ge2 K1 Ge3 48.615(15) . 4 ? O3 K2 O3 59.81(12) 4_455 3_455 ? O3 K2 O1 127.00(8) 4_455 2_565 ? O3 K2 O1 91.53(8) 3_455 2_565 ? O3 K2 O1 91.53(8) 4_455 1_465 ? O3 K2 O1 127.00(8) 3_455 1_465 ? O1 K2 O1 137.49(12) 2_565 1_465 ? O3 K2 O5 75.69(8) 4_455 3_455 ? O3 K2 O5 120.59(8) 3_455 3_455 ? O1 K2 O5 85.32(8) 2_565 3_455 ? O1 K2 O5 88.40(8) 1_465 3_455 ? O3 K2 O5 120.59(8) 4_455 4_455 ? O3 K2 O5 75.69(8) 3_455 4_455 ? O1 K2 O5 88.40(8) 2_565 4_455 ? O1 K2 O5 85.32(8) 1_465 4_455 ? O5 K2 O5 162.63(12) 3_455 4_455 ? O3 K2 O2 65.99(8) 4_455 3_455 ? O3 K2 O2 60.27(8) 3_455 3_455 ? O1 K2 O2 61.04(7) 2_565 3_455 ? O1 K2 O2 149.52(7) 1_465 3_455 ? O5 K2 O2 66.91(7) 3_455 3_455 ? O5 K2 O2 123.33(7) 4_455 3_455 ? O3 K2 O2 60.27(8) 4_455 4_455 ? O3 K2 O2 65.99(8) 3_455 4_455 ? O1 K2 O2 149.52(7) 2_565 4_455 ? O1 K2 O2 61.04(7) 1_465 4_455 ? O5 K2 O2 123.33(7) 3_455 4_455 ? O5 K2 O2 66.91(7) 4_455 4_455 ? O2 K2 O2 117.24(11) 3_455 4_455 ? O3 K2 O4 130.56(7) 4_455 2_565 ? O3 K2 O4 149.78(7) 3_455 2_565 ? O1 K2 O4 59.14(7) 2_565 2_565 ? O1 K2 O4 83.08(8) 1_465 2_565 ? O5 K2 O4 55.13(7) 3_455 2_565 ? O5 K2 O4 107.94(8) 4_455 2_565 ? O2 K2 O4 95.90(7) 3_455 2_565 ? O2 K2 O4 143.78(7) 4_455 2_565 ? O3 K2 O4 149.78(7) 4_455 1_465 ? O3 K2 O4 130.56(7) 3_455 1_465 ? O1 K2 O4 83.08(8) 2_565 1_465 ? O1 K2 O4 59.14(7) 1_465 1_465 ? O5 K2 O4 107.94(8) 3_455 1_465 ? O5 K2 O4 55.13(7) 4_455 1_465 ? O2 K2 O4 143.78(7) 3_455 1_465 ? O2 K2 O4 95.90(7) 4_455 1_465 ? O4 K2 O4 58.28(9) 2_565 1_465 ? O3 K2 Ge1 30.71(6) 4_455 4_455 ? O3 K2 Ge1 55.97(6) 3_455 4_455 ? O1 K2 Ge1 145.94(6) 2_565 4_455 ? O1 K2 Ge1 76.42(5) 1_465 4_455 ? O5 K2 Ge1 101.87(6) 3_455 4_455 ? O5 K2 Ge1 92.38(6) 4_455 4_455 ? O2 K2 Ge1 90.91(6) 3_455 4_455 ? O2 K2 Ge1 29.73(5) 4_455 4_455 ? O4 K2 Ge1 149.80(5) 2_565 4_455 ? O4 K2 Ge1 124.46(5) 1_465 4_455 ? O3 K2 Ge1 55.97(6) 4_455 3_455 ? O3 K2 Ge1 30.71(6) 3_455 3_455 ? O1 K2 Ge1 76.42(5) 2_565 3_455 ? O1 K2 Ge1 145.94(6) 1_465 3_455 ? O5 K2 Ge1 92.38(6) 3_455 3_455 ? O5 K2 Ge1 101.87(6) 4_455 3_455 ? O2 K2 Ge1 29.73(5) 3_455 3_455 ? O2 K2 Ge1 90.91(6) 4_455 3_455 ? O4 K2 Ge1 124.46(5) 2_565 3_455 ? O4 K2 Ge1 149.80(5) 1_465 3_455 ? Ge1 K2 Ge1 70.09(3) 4_455 3_455 ? O1 Eu1 O1 104.02(13) 1_565 2_565 ? O1 Eu1 O9 75.39(9) 1_565 2_565 ? O1 Eu1 O9 82.50(9) 2_565 2_565 ? O1 Eu1 O9 82.50(9) 1_565 1_565 ? O1 Eu1 O9 75.39(9) 2_565 1_565 ? O9 Eu1 O9 143.77(12) 2_565 1_565 ? O1 Eu1 O2 144.35(9) 1_565 3_455 ? O1 Eu1 O2 76.17(9) 2_565 3_455 ? O9 Eu1 O2 69.25(9) 2_565 3_455 ? O9 Eu1 O2 130.09(9) 1_565 3_455 ? O1 Eu1 O2 76.17(9) 1_565 4 ? O1 Eu1 O2 144.35(9) 2_565 4 ? O9 Eu1 O2 130.09(9) 2_565 4 ? O9 Eu1 O2 69.25(8) 1_565 4 ? O2 Eu1 O2 124.47(12) 3_455 4 ? O1 Eu1 O4 97.52(9) 1_565 4 ? O1 Eu1 O4 149.60(9) 2_565 4 ? O9 Eu1 O4 82.48(8) 2_565 4 ? O9 Eu1 O4 129.25(8) 1_565 4 ? O2 Eu1 O4 73.83(8) 3_455 4 ? O2 Eu1 O4 61.75(8) 4 4 ? O1 Eu1 O4 149.60(9) 1_565 3_455 ? O1 Eu1 O4 97.52(9) 2_565 3_455 ? O9 Eu1 O4 129.25(8) 2_565 3_455 ? O9 Eu1 O4 82.48(8) 1_565 3_455 ? O2 Eu1 O4 61.75(8) 3_455 3_455 ? O2 Eu1 O4 73.83(8) 4 3_455 ? O4 Eu1 O4 72.40(12) 4 3_455 ? O1 Eu1 Ge1 168.35(7) 1_565 3_455 ? O1 Eu1 Ge1 84.29(7) 2_565 3_455 ? O9 Eu1 Ge1 98.00(6) 2_565 3_455 ? O9 Eu1 Ge1 107.78(6) 1_565 3_455 ? O2 Eu1 Ge1 29.19(6) 3_455 3_455 ? O2 Eu1 Ge1 101.96(6) 4 3_455 ? O4 Eu1 Ge1 71.85(6) 4 3_455 ? O4 Eu1 Ge1 32.64(6) 3_455 3_455 ? O1 Eu1 Ge1 84.29(7) 1_565 4 ? O1 Eu1 Ge1 168.35(7) 2_565 4 ? O9 Eu1 Ge1 107.78(6) 2_565 4 ? O9 Eu1 Ge1 98.00(6) 1_565 4 ? O2 Eu1 Ge1 101.96(6) 3_455 4 ? O2 Eu1 Ge1 29.19(6) 4 4 ? O4 Eu1 Ge1 32.64(6) 4 4 ? O4 Eu1 Ge1 71.85(6) 3_455 4 ? Ge1 Eu1 Ge1 88.756(16) 3_455 4 ? O1 Eu1 Ge1 22.65(7) 1_565 1_565 ? O1 Eu1 Ge1 84.01(7) 2_565 1_565 ? O9 Eu1 Ge1 82.83(6) 2_565 1_565 ? O9 Eu1 Ge1 66.79(6) 1_565 1_565 ? O2 Eu1 Ge1 147.39(6) 3_455 1_565 ? O2 Eu1 Ge1 86.28(6) 4 1_565 ? O4 Eu1 Ge1 119.98(6) 4 1_565 ? O4 Eu1 Ge1 147.90(6) 3_455 1_565 ? Ge1 Eu1 Ge1 168.055(14) 3_455 1_565 ? Ge1 Eu1 Ge1 102.388(4) 4 1_565 ? O1 Eu1 Ge1 84.01(7) 1_565 2_565 ? O1 Eu1 Ge1 22.65(7) 2_565 2_565 ? O9 Eu1 Ge1 66.79(6) 2_565 2_565 ? O9 Eu1 Ge1 82.83(6) 1_565 2_565 ? O2 Eu1 Ge1 86.28(6) 3_455 2_565 ? O2 Eu1 Ge1 147.39(6) 4 2_565 ? O4 Eu1 Ge1 147.90(6) 4 2_565 ? O4 Eu1 Ge1 119.98(6) 3_455 2_565 ? Ge1 Eu1 Ge1 102.388(4) 3_455 2_565 ? Ge1 Eu1 Ge1 168.055(14) 4 2_565 ? Ge1 Eu1 Ge1 66.876(14) 1_565 2_565 ? O8 Eu2 O5 99.09(9) 4_455 3_455 ? O8 Eu2 O2 92.21(10) 4_455 3_455 ? O5 Eu2 O2 89.93(10) 3_455 3_455 ? O8 Eu2 O9 161.64(10) 4_455 2_565 ? O5 Eu2 O9 91.99(9) 3_455 2_565 ? O2 Eu2 O9 73.10(9) 3_455 2_565 ? O8 Eu2 O6 90.32(10) 4_455 7_465 ? O5 Eu2 O6 97.08(9) 3_455 7_465 ? O2 Eu2 O6 172.08(9) 3_455 7_465 ? O9 Eu2 O6 102.86(9) 2_565 7_465 ? O8 Eu2 O6 86.06(9) 4_455 . ? O5 Eu2 O6 171.25(9) 3_455 . ? O2 Eu2 O6 96.97(9) 3_455 . ? O9 Eu2 O6 84.91(9) 2_565 . ? O6 Eu2 O6 75.71(10) 7_465 . ? O8 Eu2 Ge2 121.65(7) 4_455 3_455 ? O5 Eu2 Ge2 24.71(7) 3_455 3_455 ? O2 Eu2 Ge2 98.28(7) 3_455 3_455 ? O9 Eu2 Ge2 72.48(6) 2_565 3_455 ? O6 Eu2 Ge2 86.75(6) 7_465 3_455 ? O6 Eu2 Ge2 147.55(7) . 3_455 ? O8 Eu2 Ge3 22.51(7) 4_455 4_455 ? O5 Eu2 Ge3 82.69(7) 3_455 4_455 ? O2 Eu2 Ge3 76.85(6) 3_455 4_455 ? O9 Eu2 Ge3 149.49(7) 2_565 4_455 ? O6 Eu2 Ge3 107.60(7) 7_465 4_455 ? O6 Eu2 Ge3 104.08(7) . 4_455 ? Ge2 Eu2 Ge3 107.209(11) 3_455 4_455 ? O8 Eu2 Ge3 173.10(7) 4_455 2_565 ? O5 Eu2 Ge3 74.66(7) 3_455 2_565 ? O2 Eu2 Ge3 90.74(7) 3_455 2_565 ? O9 Eu2 Ge3 24.63(6) 2_565 2_565 ? O6 Eu2 Ge3 87.59(7) 7_465 2_565 ? O6 Eu2 Ge3 99.77(7) . 2_565 ? Ge2 Eu2 Ge3 51.670(10) 3_455 2_565 ? Ge3 Eu2 Ge3 154.206(14) 4_455 2_565 ? O8 Eu2 Ge2 88.41(7) 4_455 7_465 ? O5 Eu2 Ge2 75.35(7) 3_455 7_465 ? O2 Eu2 Ge2 165.17(7) 3_455 7_465 ? O9 Eu2 Ge2 108.64(6) 2_565 7_465 ? O6 Eu2 Ge2 22.41(6) 7_465 7_465 ? O6 Eu2 Ge2 97.86(6) . 7_465 ? Ge2 Eu2 Ge2 69.033(11) 3_455 7_465 ? Ge3 Eu2 Ge2 99.064(10) 4_455 7_465 ? Ge3 Eu2 Ge2 87.156(10) 2_565 7_465 ? O8 Eu2 Eu2 87.71(7) 4_455 7_465 ? O5 Eu2 Eu2 134.79(7) 3_455 7_465 ? O2 Eu2 Eu2 134.71(7) 3_455 7_465 ? O9 Eu2 Eu2 94.85(6) 2_565 7_465 ? O6 Eu2 Eu2 37.90(6) 7_465 7_465 ? O6 Eu2 Eu2 37.81(6) . 7_465 ? Ge2 Eu2 Eu2 119.936(10) 3_455 7_465 ? Ge3 Eu2 Eu2 110.211(10) 4_455 7_465 ? Ge3 Eu2 Eu2 94.648(9) 2_565 7_465 ? Ge2 Eu2 Eu2 60.118(8) 7_465 7_465 ? O8 Eu2 Eu1 126.17(7) 4_455 . ? O5 Eu2 Eu1 96.89(7) 3_455 . ? O2 Eu2 Eu1 36.77(6) 3_455 . ? O9 Eu2 Eu1 37.09(6) 2_565 . ? O6 Eu2 Eu1 137.83(6) 7_465 . ? O6 Eu2 Eu1 85.58(6) . . ? Ge2 Eu2 Eu1 89.738(9) 3_455 . ? Ge3 Eu2 Eu1 113.530(9) 4_455 . ? Ge3 Eu2 Eu1 58.464(8) 2_565 . ? Ge2 Eu2 Eu1 145.419(9) 7_465 . ? Eu2 Eu2 Eu1 114.837(8) 7_465 . ? O1 Ge1 O2 118.41(13) . . ? O1 Ge1 O3 111.12(13) . . ? O2 Ge1 O3 112.18(12) . . ? O1 Ge1 O4 116.63(13) . . ? O2 Ge1 O4 96.04(12) . . ? O3 Ge1 O4 100.33(12) . . ? O1 Ge1 Eu1 136.57(9) . 3_545 ? O2 Ge1 Eu1 43.91(8) . 3_545 ? O3 Ge1 Eu1 112.23(9) . 3_545 ? O4 Ge1 Eu1 52.26(8) . 3_545 ? O1 Ge1 K2 132.01(9) . 3_545 ? O2 Ge1 K2 60.19(9) . 3_545 ? O3 Ge1 K2 52.42(8) . 3_545 ? O4 Ge1 K2 110.96(9) . 3_545 ? Eu1 Ge1 K2 79.214(15) 3_545 3_545 ? O1 Ge1 K2 52.06(9) . 1_645 ? O2 Ge1 K2 111.23(9) . 1_645 ? O3 Ge1 K2 135.74(9) . 1_645 ? O4 Ge1 K2 66.77(9) . 1_645 ? Eu1 Ge1 K2 93.266(18) 3_545 1_645 ? K2 Ge1 K2 171.26(3) 3_545 1_645 ? O1 Ge1 Eu1 31.85(9) . 1_545 ? O2 Ge1 Eu1 136.19(9) . 1_545 ? O3 Ge1 Eu1 79.27(9) . 1_545 ? O4 Ge1 Eu1 124.38(9) . 1_545 ? Eu1 Ge1 Eu1 168.055(14) 3_545 1_545 ? K2 Ge1 Eu1 111.515(17) 3_545 1_545 ? K2 Ge1 Eu1 75.596(16) 1_645 1_545 ? O5 Ge2 O6 116.86(13) . . ? O5 Ge2 O7 109.06(13) . . ? O6 Ge2 O7 107.17(12) . . ? O5 Ge2 O4 107.96(13) . 4 ? O6 Ge2 O4 109.27(12) . 4 ? O7 Ge2 O4 106.01(13) . 4 ? O5 Ge2 Eu2 33.66(9) . 3_545 ? O6 Ge2 Eu2 132.95(9) . 3_545 ? O7 Ge2 Eu2 75.59(9) . 3_545 ? O4 Ge2 Eu2 114.97(9) 4 3_545 ? O5 Ge2 K1 46.42(9) . 3_445 ? O6 Ge2 K1 73.11(9) . 3_445 ? O7 Ge2 K1 140.52(10) . 3_445 ? O4 Ge2 K1 111.02(9) 4 3_445 ? Eu2 Ge2 K1 76.823(18) 3_545 3_445 ? O5 Ge2 K1 165.49(9) . . ? O6 Ge2 K1 75.23(9) . . ? O7 Ge2 K1 57.72(9) . . ? O4 Ge2 K1 73.06(9) 4 . ? Eu2 Ge2 K1 132.271(19) 3_545 . ? K1 Ge2 K1 147.52(3) 3_445 . ? O5 Ge2 Eu2 113.18(9) . 7_465 ? O6 Ge2 Eu2 31.58(9) . 7_465 ? O7 Ge2 Eu2 79.94(9) . 7_465 ? O4 Ge2 Eu2 133.72(9) 4 7_465 ? Eu2 Ge2 Eu2 110.967(11) 3_545 7_465 ? K1 Ge2 Eu2 84.223(18) 3_445 7_465 ? K1 Ge2 Eu2 72.410(17) . 7_465 ? O5 Ge2 K2 47.32(9) . 3_545 ? O6 Ge2 K2 124.83(9) . 3_545 ? O7 Ge2 K2 127.95(9) . 3_545 ? O4 Ge2 K2 61.30(9) 4 3_545 ? Eu2 Ge2 K2 68.120(17) 3_545 3_545 ? K1 Ge2 K2 63.632(19) 3_445 3_545 ? K1 Ge2 K2 133.86(2) . 3_545 ? Eu2 Ge2 K2 147.489(13) 7_465 3_545 ? O8 Ge3 O9 115.31(13) . . ? O8 Ge3 O3 110.98(12) . . ? O9 Ge3 O3 111.60(13) . . ? O8 Ge3 O7 107.73(13) . 4_545 ? O9 Ge3 O7 107.87(13) . 4_545 ? O3 Ge3 O7 102.41(13) . 4_545 ? O8 Ge3 K1 56.87(9) . 2_545 ? O9 Ge3 K1 59.00(9) . 2_545 ? O3 Ge3 K1 125.63(9) . 2_545 ? O7 Ge3 K1 131.93(9) 4_545 2_545 ? O8 Ge3 K1 53.37(9) . 6_566 ? O9 Ge3 K1 107.84(9) . 6_566 ? O3 Ge3 K1 140.25(9) . 6_566 ? O7 Ge3 K1 59.82(9) 4_545 6_566 ? K1 Ge3 K1 79.61(3) 2_545 6_566 ? O8 Ge3 Eu2 30.18(9) . 4_445 ? O9 Ge3 Eu2 132.95(9) . 4_445 ? O3 Ge3 Eu2 80.91(9) . 4_445 ? O7 Ge3 Eu2 113.37(9) 4_545 4_445 ? K1 Ge3 Eu2 76.587(19) 2_545 4_445 ? K1 Ge3 Eu2 75.963(18) 6_566 4_445 ? O8 Ge3 Eu2 124.54(9) . 2_545 ? O9 Ge3 Eu2 34.70(9) . 2_545 ? O3 Ge3 Eu2 123.12(9) . 2_545 ? O7 Ge3 Eu2 73.33(9) 4_545 2_545 ? K1 Ge3 Eu2 80.937(19) 2_545 2_545 ? K1 Ge3 Eu2 87.753(19) 6_566 2_545 ? Eu2 Ge3 Eu2 154.206(14) 4_445 2_545 ? O8 Ge3 Eu1 119.95(9) . 1_545 ? O9 Ge3 Eu1 35.08(9) . 1_545 ? O3 Ge3 Eu1 78.62(9) . 1_545 ? O7 Ge3 Eu1 128.55(9) 4_545 1_545 ? K1 Ge3 Eu1 69.560(18) 2_545 1_545 ? K1 Ge3 Eu1 140.94(2) 6_566 1_545 ? Eu2 Ge3 Eu1 117.453(12) 4_445 1_545 ? Eu2 Ge3 Eu1 64.686(8) 2_545 1_545 ? O8 Ge3 K1 89.10(9) . 4_545 ? O9 Ge3 K1 153.77(9) . 4_545 ? O3 Ge3 K1 64.20(9) . 4_545 ? O7 Ge3 K1 52.18(9) 4_545 4_545 ? K1 Ge3 K1 145.94(3) 2_545 4_545 ? K1 Ge3 K1 78.25(3) 6_566 4_545 ? Eu2 Ge3 K1 73.142(17) 4_445 4_545 ? Eu2 Ge3 K1 123.445(18) 2_545 4_545 ? Eu1 Ge3 K1 139.633(19) 1_545 4_545 ? Ge1 O1 Eu1 125.50(14) . 1_545 ? Ge1 O1 K2 99.13(11) . 1_645 ? Eu1 O1 K2 115.85(10) 1_545 1_645 ? Ge1 O1 K1 129.03(13) . 1_545 ? Eu1 O1 K1 97.07(9) 1_545 1_545 ? K2 O1 K1 82.95(7) 1_645 1_545 ? Ge1 O2 Eu2 138.95(14) . 3_545 ? Ge1 O2 Eu1 106.91(12) . 3_545 ? Eu2 O2 Eu1 109.16(10) 3_545 3_545 ? Ge1 O2 K2 90.08(10) . 3_545 ? Eu2 O2 K2 98.34(9) 3_545 3_545 ? Eu1 O2 K2 105.75(9) 3_545 3_545 ? Ge3 O3 Ge1 116.82(14) . . ? Ge3 O3 K2 145.30(14) . 3_545 ? Ge1 O3 K2 96.87(11) . 3_545 ? Ge2 O4 Ge1 122.59(14) 4_545 . ? Ge2 O4 Eu1 138.29(13) 4_545 3_545 ? Ge1 O4 Eu1 95.10(10) . 3_545 ? Ge2 O4 K2 89.72(10) 4_545 1_645 ? Ge1 O4 K2 82.12(9) . 1_645 ? Eu1 O4 K2 114.66(9) 3_545 1_645 ? Ge2 O5 Eu2 121.63(14) . 3_545 ? Ge2 O5 K1 106.36(12) . 3_445 ? Eu2 O5 K1 123.77(11) 3_545 3_445 ? Ge2 O5 K2 106.27(12) . 3_545 ? Eu2 O5 K2 103.73(10) 3_545 3_545 ? K1 O5 K2 87.78(8) 3_445 3_545 ? Ge2 O6 Eu2 126.00(13) . 7_465 ? Ge2 O6 Eu2 128.98(13) . . ? Eu2 O6 Eu2 104.29(10) 7_465 . ? Ge2 O7 Ge3 119.14(15) . 4 ? Ge2 O7 K1 146.92(14) . 7_565 ? Ge3 O7 K1 89.02(10) 4 7_565 ? Ge2 O7 K1 92.94(11) . . ? Ge3 O7 K1 100.53(12) 4 . ? K1 O7 K1 98.85(8) 7_565 . ? Ge3 O8 Eu2 127.31(14) . 4_445 ? Ge3 O8 K1 97.19(11) . 6_566 ? Eu2 O8 K1 117.29(11) 4_445 6_566 ? Ge3 O8 K1 93.28(11) . 2_545 ? Eu2 O8 K1 114.77(11) 4_445 2_545 ? K1 O8 K1 101.99(9) 6_566 2_545 ? Ge3 O9 Eu2 120.67(13) . 2_545 ? Ge3 O9 Eu1 120.79(13) . 1_545 ? Eu2 O9 Eu1 107.02(10) 2_545 1_545 ? Ge3 O9 K1 90.71(10) . 2_545 ? Eu2 O9 K1 117.54(10) 2_545 2_545 ? Eu1 O9 K1 96.87(9) 1_545 2_545 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.938 _refine_diff_density_min -1.427 _refine_diff_density_rms 0.307