#------------------------------------------------------------------------------ #$Date: 2008-11-20 19:58:43 +0000 (Thu, 20 Nov 2008) $ #$Revision: 481 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006531.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2006531 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1997 _journal_volume 53 _journal_page_first 1166 _journal_page_last 1170 _publ_section_title ; A Tricapped Trigonal Prismatic EuO(H~2~O)~8~ Site in Trihydrogen Tris(octaaquaeuropium) Dipotassium Digermanohexatitanooctadecatungstate(14-) Tridecahydrate ; loop_ _publ_author_name 'Sugeta, Moriyasu' 'Yamase, Toshihiro ' _chemical_formula_sum 'K2 [Eu(H2 O)8]3 H3[(GeTi3 W9 O37)2 O3].13H2 O' _chemical_formula_structural ; (Eu (H2 O)8)3 K2 H3 ((Ge Ti3 W9 O37)2 O3)1 (H2 O)13 ; _chemical_formula_weight 6177.5 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m' loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y, -z' ' -x, -y, -z' ' +x,1/2-y, +z' _cell_length_a 13.177(2) _cell_length_b 18.645(3) _cell_length_c 21.800(3) _cell_angle_alpha 90 _cell_angle_beta 99.820(10) _cell_angle_gamma 90 _cell_volume 5277.0(10) _cell_formula_units_Z 2.00 _cell_measurement_temperature 23.0 _exptl_crystal_density_diffrn 3.89 _diffrn_ambient_temperature 296 _refine_ls_R_factor_obs .0660 _refine_ls_wR_factor_obs .0570 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom W1 -.27698(7) .15945(7) .35247(4) .0259(3) Uani ? ? W2 -.47010(10) .2500 .40005(6) .0228(4) Uani ? ? W3 -.01370(7) .15968(7) .44902(4) .0242(3) Uani ? ? W4 -.22973(8) .05854(6) .50312(5) .0251(3) Uani ? ? W5 -.42066(7) .14950(6) .55094(4) .0222(3) Uani ? ? W6 .33321(8) .16071(9) .81384(5) .0429(4) Uani ? ? W7 .12446(9) .05984(8) .87476(6) .0432(4) Uani ? ? W8 -.06228(8) .14950(8) .92783(5) .0385(4) Uani ? ? W9 .32466(9) .15990(10) .98421(5) .0572(4) Uani ? ? W10 .13740(10) .2500 1.03778(7) .0521(6) Uani ? ? Eu1 .56830(10) .01900(10) .80097(9) .0580(6) Uani ? ? Eu2 -.0071(2) .2500 1.18960(10) .0720(10) Uani ? ? Ge1 -.2256(3) .2500 .4970(2) .0190(10) Uani ? ? Ge2 .1356(3) .2500 .8763(2) .0340(10) Uani ? ? Ti1 .0174(5) .2500 .5797(3) .0230(10) Uani ? ? Ti2 -.1860(3) .1524(3) .6328(2) .0240(10) Uani ? ? Ti3 .1541(5) .2500 .7218(3) .0280(10) Uani ? ? Ti4 -.0461(3) .1522(3) .7781(2) .030(10) Uani ? ? K1 .0500(10) .0418(7) .5999(6) .142(6) Uanij ? ? O1 -.2790(10) .1000(10) .2912(9) .042(5) Uiso ? ? O2 -.598(2) .2500 .3700(10) .036(7) Uiso ? ? O3 .0550(10) .1010(10) .4140(8) .038(5) Uiso ? ? O4 -.2210(10) -.0310(10) .4840(8) .032(4) Uiso ? ? O5 -.5400(10) .1190(10) .5628(7) .029(4) Uiso ? ? O6 .427(2) .1020(10) .8017(9) .049(6) Uiso ? ? O7 .164(2) -.0290(10) .8823(9) .056(6) Uiso ? ? O8 -.1530(10) .1170(10) .9702(9) .043(5) Uiso ? ? O9 .414(2) .1020(10) 1.0230(10) .059(6) Uiso ? ? O10 .102(2) .2500 1.1100(10) .054(9) Uiso ? ? O11 -.271(2) .2500 .3100(10) .038(7) Uiso ? ? O12 -.4230(10) .1770(9) .3438(7) .029(4) Uiso ? ? O13 -.1350(10) .1675(9) .3820(7) .020(4) Uiso ? ? O14 -.2830(10) .0983(9) .4186(7) .025(4) Uiso ? ? O15 -.4620(10) .1807(9) .4629(7) .021(4) Uiso ? ? O16 .026(2) .2500 .4170(10) .026(6) Uiso ? ? O17 -.1000(10) .0954(9) .4847(7) .021(4) Uiso ? ? O18 -.3740(10) .0650(10) .5179(8) .032(4) Uiso ? ? O19 -.429(2) .2500 .5670(10) .020(5) Uiso ? ? O20 .0690(10) .1763(9) .5237(7) .023(4) Uiso ? ? O21 -.1820(10) .0581(9) .5876(7) .022(4) Uiso ? ? O22 -.3380(10) .1322(8) .6257(7) .020(4) Uiso ? ? O23 -.0610(10) .1786(9) .6094(7) .021(4) Uiso ? ? O24 -.213(2) .2500 .6490(10) .020(5) Uiso ? ? O25 -.294(2) .2500 .4220(10) .017(5) Uiso ? ? O26 -.095(2) .2500 .4950(10) .017(5) Uiso ? ? O27 -.2560(10) .1748(8) .5354(6) .012(3) Uiso ? ? O28 .135(2) .2500 .6370(10) .024(6) Uiso ? ? O29 -.1430(10) .1198(9) .7128(7) .021(4) Uiso ? ? O30 .0620(10) .1804(9) .7393(7) .029(4) Uiso ? ? O31 -.085(2) .2500 .7840(10) .041(7) Uiso ? ? O32 .2660(10) .1767(9) .7339(7) .030(4) Uiso ? ? O33 .0250(10) .0610(10) .8041(8) .031(4) Uiso ? ? O34 -.1270(10) .1317(9) .8481(7) .030(4) Uiso ? ? O35 .407(2) .2500 .8150(10) .041(7) Uiso ? ? O36 .2250(10) .1000(10) .8297(8) .035(5) Uiso ? ? O37 .0150(10) .0630(10) .9268(9) .047(5) Uiso ? ? O38 -.090(2) .2500 .9220(10) .033(6) Uiso ? ? O39 .3650(10) .1670(10) .9047(8) .043(5) Uiso ? ? O40 .2190(10) .0990(10) .9471(8) .036(5) Uiso ? ? O41 .0510(10) .1800(10) .9963(8) .037(5) Uiso ? ? O42 .393(2) .2500 1.0060(10) .050(8) Uiso ? ? O43 .2460(10) .1800(10) 1.0514(8) .040(5) Uiso ? ? O44 .220(2) .2500 .8240(10) .022(5) Uiso ? ? O45 .0580(10) .1749(9) .8669(7) .026(4) Uiso ? ? O46 .209(2) .2500 .9510(10) .034(7) Uiso ? ? O47 .656(2) .131(2) .8360(10) .120(10) Uiso ? ? O48 .668(3) -.083(2) .850(2) .150(10) Uiso ? ? O49 .725(2) .012(2) .7540(10) .120(10) Uiso ? ? O50 .528(2) .033(2) .9070(10) .090(9) Uiso ? ? O51 .573(3) -.079(2) .728(2) .160(10) Uiso ? ? O52 .576(3) .113(3) .723(2) .21(2) Uiso ? ? O53 .423(3) -.058(2) .809(2) .130(10) Uiso ? ? O54 .427(4) .023(3) .685(2) .24(2) Uiso ? ? O55 .063(2) .121(2) 1.1840(10) .130(10) Uiso ? ? O56 -.107(2) .180(2) 1.1070(10) .130(10) Uiso ? ? O57 -.028(2) .171(2) 1.2760(10) .110(10) Uiso ? ? O58 -.187(4) .2500 1.196(2) .15(2) Uiso ? ? O59 .165(5) .2500 1.252(3) .19(2) Uiso ? ? O60 .598(4) .2500 .907(2) .13(2) Uiso ? ? O61 .420(3) .2500 .664(2) .12(2) Uiso ? ? O62 .667(5) .2500 .758(3) .23(2) Uiso ? ? O63 .2690(10) .1520(10) .5887(9) .052(6) Uiso ? ? O64 -.533(2) .0420(10) .4030(10) .076(8) Uiso ? ? O65 .112(2) .0570(10) 1.0820(10) .074(8) Uiso ? ? O66 -.038(3) .041(3) 1.286(2) .20(2) Uiso ? ? O67 .211(3) .2500 1.374(2) .090(10) Uiso ? ? O68 .345(6) .2500 1.198(3) .25(2) Uiso ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 W1 .0246(5) .0372(7) .0154(5) .0008(5) .0022(4) -.0064(5) W2 .0186(7) .0330(10) .0165(7) .0000 .0010(6) .0000 W3 .0215(5) .0341(7) .0175(5) .0032(5) .0049(4) -.0055(5) W4 .0292(6) .0225(6) .0239(6) .0010(5) .0056(4) -.0043(5) W5 .0200(5) .0263(6) .0207(5) -.0029(5) .0044(4) .0016(5) W6 .0238(5) .0870(10) .0189(5) .0161(7) .0066(4) .0122(7) W7 .0307(6) .0720(10) .0276(6) .0161(7) .0065(5) .0193(7) W8 .0248(5) .0740(10) .0176(5) .0013(6) .0070(4) .0105(6) W9 .0240(6) .131(2) .0162(5) .0149(8) .0027(4) .0182(8) W10 .0240(8) .122(2) .0112(7) .0000 .0051(6) .0000 Eu1 .0650(10) .0420(10) .0740(10) -.0020(10) .0310(10) .0110(10) Eu2 .061(2) .131(3) .0310(10) .0000 .0270(10) .0000 Ge1 .017(2) .025(2) .013(2) .0000 .0020(10) .0000 Ge2 .018(2) .071(4) .013(2) .0000 .003(2) .0000 Ti1 .018(3) .035(4) .015(3) .0000 .002(2) .0000 Ti2 .023(2) .033(3) .016(2) -.003(2) .002(2) .002(2) Ti3 .026(3) .048(5) .010(3) .0000 .001(3) .0000 Ti4 .024(2) .049(4) .018(2) -.002(2) .001(2) .009(2) K1 .140(10) .130(10) .160(10) .050(10) .070(10) .030(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag W1 O1 . . 1.74(2) ? W1 O11 . . 1.930(10) ? W1 O12 . . 1.93(2) ? W1 O13 . . 1.880(10) ? W1 O14 . . 1.85(2) ? W1 O25 . . 2.310(10) ? W2 O2 . . 1.70(2) ? W2 O12 . . 2.00(2) ? W2 O15 . . 1.87(2) ? W2 O25 . . 2.29(2) ? W3 O3 . . 1.68(2) ? W3 O13 . . 1.980(10) ? W3 O16 . . 1.930(10) ? W3 O17 . . 1.90(2) ? W3 O20 . . 1.820(10) ? W3 O26 . . 2.31(2) ? W4 O4 . . 1.72(2) ? W4 O14 . . 2.00(2) ? W4 O17 . . 1.95(2) ? W4 O18 . . 1.98(2) ? W4 O21 . . 1.840(10) ? W4 O27 . . 2.320(10) ? W5 O5 . . 1.73(2) ? W5 O15 . . 1.990(10) ? W5 O18 . . 1.88(2) ? W5 O19 . . 1.912(5) ? W5 O22 . . 1.830(10) ? W5 O27 . . 2.310(10) ? W6 O6 . . 1.70(2) ? W6 O32 . . 1.84(2) ? W6 O35 . . 1.930(10) ? W6 O36 . . 1.90(2) ? W6 O39 . . 1.96(2) ? W6 O44 . . 2.27(2) ? W7 O7 . . 1.73(2) ? W7 O33 . . 1.84(2) ? W7 O36 . . 1.93(2) ? W7 O37 . . 1.99(2) ? W7 O40 . . 1.97(2) ? W7 O45 . . 2.31(2) ? W8 O8 . . 1.74(2) ? W8 O34 . . 1.83(2) ? W8 O37 . . 1.91(2) ? W8 O38 . . 1.910(10) ? W8 O41 . . 2.00(2) ? W8 O45 . . 2.29(2) ? W9 O9 . . 1.70(2) ? W9 O39 . . 1.91(2) ? W9 O40 . . 1.87(2) ? W9 O42 . . 1.930(10) ? W9 O43 . . 1.97(2) ? W9 O46 . . 2.30(2) ? W10 O10 . . 1.71(3) ? W10 O41 . . 1.87(2) ? W10 O43 . . 1.92(2) ? W10 O46 . . 2.25(3) ? Eu1 O6 . . 2.43(2) yes Eu1 O47 . . 2.44(3) yes Eu1 O48 . . 2.44(4) yes Eu1 O49 . . 2.46(3) yes Eu1 O50 . . 2.48(3) yes Eu1 O51 . . 2.43(4) yes Eu1 O52 . . 2.45(5) yes Eu1 O53 . . 2.42(3) yes Eu1 O54 . . 2.88(5) yes Eu2 O10 . . 2.44(3) yes Eu2 O55 . . 2.59(3) yes Eu2 O56 . . 2.42(3) yes Eu2 O57 . . 2.45(3) yes Eu2 O58 . . 2.40(5) yes Eu2 O59 . . 2.44(6) yes Ge1 O25 . . 1.73(2) ? Ge1 O26 . . 1.73(2) ? Ge1 O27 . . 1.710(10) ? Ge2 O44 . . 1.73(2) ? Ge2 O45 . . 1.72(2) ? Ge2 O46 . . 1.75(2) ? Ti1 O20 . . 2.03(2) ? Ti1 O23 . . 1.86(2) ? Ti1 O26 . . 2.17(2) ? Ti1 O28 . . 1.82(2) ? Ti2 O21 . . 2.02(2) ? Ti2 O22 . . 2.01(2) ? Ti2 O23 . . 1.88(2) ? Ti2 O24 . . 1.901(8) ? Ti2 O27 . . 2.210(10) ? Ti2 O29 . . 1.84(2) ? Ti3 O28 . . 1.82(2) ? Ti3 O30 . . 1.86(2) ? Ti3 O32 . . 2.00(2) ? Ti3 O44 . . 2.24(2) ? Ti4 O29 . . 1.840(10) ? Ti4 O30 . . 1.85(2) ? Ti4 O31 . . 1.900(10) ? Ti4 O33 . . 1.98(2) ? Ti4 O34 . . 2.04(2) ? Ti4 O45 . . 2.21(2) ? K1 O3 . 3_556 3.00(2) yes K1 O4 . 3_556 3.14(2) yes K1 O17 . . 3.08(2) yes K1 O17 . 3_556 3.29(2) yes K1 O20 . . 3.04(2) yes K1 O21 . . 3.03(2) yes K1 O23 . . 2.96(2) yes K1 O66 . 3_557 2.96(5) yes