#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2008499.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_2008499 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1999 _journal_volume 55 _publ_section_title ; Sodium hydrogen bis[dichloro(dihydrogen ethylenediaminetetraacetato-O,N,N',O')ruthenium(III)] nonahydrate ; _space_group_IT_number 4 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _[local]_cod_cif_authors_sg_H-M 'P 21' loop_ _publ_author_name 'Stadler, Eduardo' 'Stadler, Carlos C.' 'Peixoto, Carlos R. de M.' 'Vencato, Ivo' _chemical_formula_sum 'C20 H47 Cl4 N4 Na O25 Ru2' _chemical_formula_structural 'NaH[Ru(H~2~edta)Cl~2~]~2~, 9H~2~O' _chemical_formula_iupac 'Na H [Ru Cl2 (C10 H14 N2 O8)]2, 9H2 O' _chemical_formula_weight 1110.55 _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.332(2) _cell_length_b 13.766(3) _cell_length_c 17.264(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00(3) _cell_angle_gamma 90.00 _cell_volume 1980.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.863 _diffrn_ambient_temperature 293(2) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Ru .11442(4) .45125(2) .065277(19) .01975(11) Uani d . 1 . . Ru Cl1 .24002(16) .30796(9) .02004(8) .0328(3) Uani d . 1 . . Cl Cl2 -.03082(16) .35754(11) .15959(8) .0390(3) Uani d . 1 . . Cl O1 -.3766(5) .6747(3) .1416(3) .0448(10) Uani d . 1 . . O O2 -.1434(4) .7398(3) .1784(2) .0359(8) Uani d . 1 . . O H2O -.2051 .7841 .1972 .043 Uiso d . 1 . . H O3 .2924(4) .4772(3) .14152(18) .0284(8) Uani d . 1 . . O O4 .3540(5) .5470(4) .2514(2) .0471(10) Uani d . 1 . . O O5 -.0577(4) .4374(3) -.0172(2) .0295(8) Uani d . 1 . . O O6 -.0881(5) .4305(4) -.1445(2) .0486(12) Uani d . 1 . . O O7 .6310(4) .5845(4) -.0747(2) .0428(10) Uani d . 1 . . O H7O .6766 .6244 -.1231 .051 Uiso d . 1 . . H O8 .4106(5) .6332(4) -.1375(2) .0436(10) Uani d . 1 . . O N1 .0353(5) .5853(3) .1134(2) .0240(8) Uani d . 1 . . N N2 .2116(5) .5386(3) -.0240(2) .0211(8) Uani d . 1 . . N C1 -.2315(6) .6746(4) .1449(3) .0283(11) Uani d . 1 . . C C2 -.1424(6) .5894(4) .1086(3) .0267(10) Uani d . 1 . . C H2A -.1838 .5304 .1321 .040 Uiso calc R 1 . . H H2B -.1713 .5873 .0542 .040 Uiso calc R 1 . . H C3 .2607(6) .5353(4) .1984(3) .0288(11) Uani d . 1 . . C C4 .0992(6) .5861(4) .1943(3) .0289(11) Uani d . 1 . . C H4A .0238 .5536 .2284 .043 Uiso calc R 1 . . H H4B .1107 .6527 .2118 .043 Uiso calc R 1 . . H C5 -.0099(6) .4505(4) -.0878(3) .0289(10) Uani d . 1 . . C C6 .1597(6) .4913(4) -.0975(3) .0273(11) Uani d . 1 . . C H6A .2333 .4393 -.1106 .041 Uiso calc R 1 . . H H6B .1611 .5384 -.1393 .041 Uiso calc R 1 . . H C7 .4751(6) .5937(4) -.0833(3) .0296(11) Uani d . 1 . . C C8 .3892(5) .5447(4) -.0173(3) .0248(10) Uani d . 1 . . C H8A .4312 .4793 -.0122 .037 Uiso calc R 1 . . H H8B .4148 .5793 .0301 .037 Uiso calc R 1 . . H C9 .1179(6) .6641(4) .0675(3) .0271(11) Uani d . 1 . . C H9A .0582 .7243 .0723 .041 Uiso calc R 1 . . H H9B .2248 .6747 .0880 .041 Uiso calc R 1 . . H C10 .1285(6) .6355(4) -.0160(3) .0261(10) Uani d . 1 . . C H10A .1878 .6845 -.0445 .039 Uiso calc R 1 . . H H10B .0215 .6314 -.0379 .039 Uiso calc R 1 . . H Ru' .09192(4) .50674(2) -.440683(18) .01676(11) Uani d . 1 . . Ru Cl1' .24922(14) .64359(9) -.46813(7) .0264(3) Uani d . 1 . . Cl Cl2' -.03747(15) .59542(10) -.33844(7) .0331(3) Uani d . 1 . . Cl O1' -.4314(4) .2936(3) -.3951(2) .0354(8) Uani d . 1 . . O H1O' -.4956 .2343 -.3755 .042 Uiso d . 1 . . H O2' -.2119(4) .2211(3) -.3470(2) .0348(8) Uani d . 1 . . O O3' .2581(3) .4598(3) -.36135(17) .0237(7) Uani d . 1 . . O O4' .2852(4) .3723(3) -.25346(19) .0310(8) Uani d . 1 . . O O5' -.0760(4) .5423(3) -.51984(18) .0232(7) Uani d . 1 . . O O6' -.1210(4) .5548(3) -.6467(2) .0402(10) Uani d . 1 . . O O7' .5952(4) .3713(4) -.5912(2) .0453(11) Uani d . 1 . . O H7O' .6297 .3250 -.6340 .054 Uiso d . 1 . . H O8' .3733(4) .3276(3) -.6560(2) .0345(8) Uani d . 1 . . O N1' -.0111(4) .3721(3) -.4057(2) .0202(8) Uani d . 1 . . N N2' .1789(4) .4275(3) -.5375(2) .0189(8) Uani d . 1 . . N C1' -.2759(6) .2864(4) -.3820(3) .0254(10) Uani d . 1 . . C C2' -.1882(5) .3729(4) -.4156(3) .0230(9) Uani d . 1 . . C H2'1 -.2120 .3764 -.4705 .034 Uiso calc R 1 . . H H2'2 -.2302 .4314 -.3917 .034 Uiso calc R 1 . . H C3' .2057(5) .3987(4) -.3108(3) .0221(9) Uani d . 1 . . C C4' .0376(5) .3582(4) -.3234(3) .0248(10) Uani d . 1 . . C H4'1 .0359 .2896 -.3107 .037 Uiso calc R 1 . . H H4'2 -.0377 .3913 -.2897 .037 Uiso calc R 1 . . H C5' -.0354(6) .5295(4) -.5928(3) .0240(11) Uani d . 1 . . C C6' .1262(6) .4847(3) -.6066(2) .0238(11) Uani d . 1 . . C H6'1 .1210 .4423 -.6515 .036 Uiso calc R 1 . . H H6'2 .2040 .5353 -.6173 .036 Uiso calc R 1 . . H C7' .4381(6) .3662(4) -.6022(3) .0264(10) Uani d . 1 . . C C8' .3554(6) .4162(4) -.5332(3) .0256(10) Uani d . 1 . . C H8'1 .3804 .3795 -.4868 .038 Uiso calc R 1 . . H H8'2 .4023 .4803 -.5271 .038 Uiso calc R 1 . . H C9' .0704(6) .2963(4) -.4549(3) .0233(10) Uani d . 1 . . C H9'1 .1750 .2816 -.4333 .035 Uiso calc R 1 . . H H9'2 .0072 .2372 -.4546 .035 Uiso calc R 1 . . H C10' .0898(5) .3313(4) -.5371(3) .0228(9) Uani d . 1 . . C H10C -.0148 .3394 -.5608 .034 Uiso calc R 1 . . H H10D .1493 .2837 -.5669 .034 Uiso calc R 1 . . H Na .5087(3) .7265(2) .75731(13) .0378(4) Uani d . 1 . . Na O1W .2449(5) .7650(3) .6982(2) .0429(10) Uani d . 1 . . O H1W1 .2068 .7151 .6804 .051 Uiso d . 1 . . H H2W1 .1628 .7941 .7223 .051 Uiso d . 1 . . H O2W .2253(5) .1833(4) .1895(2) .0441(10) Uani d . 1 . . O H1W2 .1635 .2384 .1789 .053 Uiso d . 1 . . H H2W2 .1932 .1672 .2370 .053 Uiso d . 1 . . H O3W .4408(6) .8602(4) .8425(3) .0628(14) Uani d . 1 . . O H1W3 .4126 .8530 .8913 .075 Uiso d . 1 . . H H2W3 .5385 .9022 .8394 .075 Uiso d . 1 . . H O4W .4723(4) .0809(3) .3198(2) .0411(9) Uani d . 1 . . O H1W4 .4049 .1113 .3627 .049 Uiso d . 1 . . H H2W4 .5644 .0520 .3377 .049 Uiso d . 1 . . H O5W .3440(5) .8389(4) .0011(2) .0471(10) Uani d . 1 . . O H1W5 .2446 .8615 -.0004 .057 Uiso d . 1 . . H H2W5 .3906 .8406 .0461 .057 Uiso d . 1 . . H O6W .3584(5) .1393(4) .4643(3) .0544(12) Uani d . 1 . . O H1W6 .2702 .1052 .4873 .065 Uiso d . 1 . . H H2W6 .4007 .1411 .5145 .065 Uiso d . 1 . . H O7W .4797(6) .8440(5) .1319(3) .0691(16) Uani d . 1 . . O H1W7 .5278 .7892 .1347 .083 Uiso d . 1 . . H H2W7 .4478 .8779 .1827 .083 Uiso d . 1 . . H O8W .4337(6) .1318(5) .6435(4) .085(2) Uani d . 1 . . O H1W8 .3394 .1073 .6438 .102 Uiso d . 1 . . H H2W8 .4818 .1141 .6824 .102 Uiso d . 1 . . H O9W .3442(4) .9325(3) .2356(2) .0468(11) Uani d . 1 . . O H1W9 .3777 .9722 .2709 .056 Uiso d . 1 . . H H2W9 .2520 .9493 .2174 .056 Uiso d . 1 . . H 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 Ru .02184(18) .0178(2) .01965(19) -.00052(15) .00019(13) .00097(14) Cl1 .0373(7) .0225(6) .0387(7) .0056(5) .0032(5) -.0030(5) Cl2 .0388(7) .0330(8) .0451(7) -.0001(6) .0128(6) .0149(6) O1 .029(2) .041(2) .065(3) .0018(18) .0089(18) -.011(2) O2 .0328(18) .036(2) .0386(19) .0073(16) -.0027(15) -.0173(17) O3 .0287(17) .033(2) .0240(16) .0034(14) -.0030(13) .0001(14) O4 .044(2) .067(3) .0304(18) -.002(2) -.0105(16) -.009(2) O5 .0274(16) .030(2) .0310(17) -.0035(15) -.0035(13) -.0031(15) O6 .039(2) .071(3) .036(2) .003(2) -.0117(17) -.015(2) O7 .0283(19) .050(3) .050(2) -.0024(19) .0034(16) .012(2) O8 .039(2) .056(3) .036(2) -.003(2) .0029(17) .020(2) N1 .028(2) .023(2) .0211(19) -.0026(17) .0053(16) .0004(17) N2 .0275(19) .0167(19) .0190(17) .0006(16) -.0008(15) .0016(15) C1 .036(3) .028(3) .021(2) .009(2) .0045(19) .003(2) C2 .026(2) .022(2) .033(2) .001(2) .0006(19) -.002(2) C3 .034(3) .033(3) .019(2) -.007(2) -.0008(19) .004(2) C4 .033(3) .035(3) .019(2) .003(2) -.0005(19) -.007(2) C5 .031(2) .030(3) .026(2) .007(2) -.0067(19) -.006(2) C6 .032(2) .029(3) .021(2) -.004(2) .0015(18) -.002(2) C7 .036(3) .024(3) .030(2) -.001(2) .005(2) -.001(2) C8 .024(2) .024(2) .026(2) -.0012(19) .0017(18) -.001(2) C9 .026(3) .024(3) .032(3) .000(2) .008(2) .001(2) C10 .030(2) .022(2) .027(2) .002(2) .0021(19) .002(2) Ru' .01860(17) .01519(19) .01649(17) .00013(14) .00027(12) -.00033(14) Cl1' .0293(6) .0194(6) .0306(6) -.0047(5) .0012(5) .0038(5) Cl2' .0363(6) .0326(7) .0302(6) .0005(5) .0101(5) -.0108(6) O1' .0180(16) .040(2) .048(2) -.0046(15) -.0020(15) .0077(18) O2' .0329(18) .031(2) .041(2) -.0081(16) -.0051(15) .0112(17) O3' .0226(15) .0251(17) .0235(14) -.0051(15) -.0035(12) .0044(15) O4' .0297(17) .038(2) .0256(16) -.0089(16) -.0095(14) .0118(16) O5' .0196(15) .0257(18) .0244(16) .0032(13) -.0022(12) .0002(14) O6' .0343(19) .058(3) .0287(18) .0151(19) -.0047(15) .0054(19) O7' .0227(18) .068(3) .045(2) .0068(19) .0032(16) -.019(2) O8' .0359(19) .039(2) .0287(18) .0047(17) .0041(15) -.0089(17) N1' .0164(18) .0192(19) .0251(19) -.0028(15) .0001(14) .0003(16) N2' .0183(17) .019(2) .0189(17) .0016(15) .0025(13) .0006(15) C1' .028(2) .027(3) .022(2) -.004(2) -.0029(18) -.004(2) C2' .021(2) .025(2) .023(2) -.0019(19) -.0043(17) .0006(19) C3' .026(2) .019(2) .021(2) -.004(2) -.0002(18) -.0006(19) C4' .021(2) .031(3) .022(2) -.007(2) .0004(17) .003(2) C5' .030(2) .024(3) .018(2) .0016(19) -.0026(18) .0029(18) C6' .030(2) .026(3) .0154(19) .0048(18) -.0014(17) .0038(18) C7' .026(2) .028(3) .025(2) .009(2) .0053(19) -.001(2) C8' .020(2) .031(3) .025(2) .005(2) .0022(18) -.005(2) C9' .021(2) .014(2) .035(2) .0020(18) .0018(19) .000(2) C10' .025(2) .021(2) .022(2) -.0005(19) -.0005(17) -.0042(19) Na .0427(11) .0384(10) .0324(10) -.0026(9) .0049(8) .0080(8) O1W .037(2) .043(2) .048(2) -.0143(19) .0136(18) -.016(2) O2W .043(2) .053(3) .036(2) .017(2) .0135(17) .011(2) O3W .046(3) .071(4) .071(3) -.020(2) .010(2) -.025(3) O4W .0311(19) .050(2) .042(2) .0086(18) -.0029(16) .0069(19) O5W .034(2) .058(3) .049(2) .005(2) -.0046(17) -.010(2) O6W .035(2) .078(3) .050(2) -.012(2) -.0005(18) .013(3) O7W .079(3) .072(4) .057(3) .037(3) -.024(2) -.019(3) O8W .057(3) .090(5) .108(4) -.041(3) -.041(3) .061(4) O9W .0337(19) .062(3) .045(2) .0059(19) -.0079(16) -.005(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru O3 . 2.015(3) ? Ru O5 . 2.030(3) ? Ru N2 . 2.116(4) ? Ru N1 . 2.128(4) ? Ru Cl1 . 2.3656(14) ? Ru Cl2 . 2.4041(14) ? O1 C1 . 1.210(6) ? O2 C1 . 1.295(7) ? O3 C3 . 1.293(6) ? O4 C3 . 1.213(6) ? O5 C5 . 1.295(6) ? O6 C5 . 1.209(6) ? O7 C7 . 1.313(6) ? O8 C7 . 1.209(7) ? O8 Na 1_554 2.369(4) ? N1 C2 . 1.484(6) ? N1 C4 . 1.496(6) ? N1 C9 . 1.508(6) ? N2 C8 . 1.486(6) ? N2 C6 . 1.489(6) ? N2 C10 . 1.509(6) ? C1 C2 . 1.524(7) ? C3 C4 . 1.518(7) ? C5 C6 . 1.530(7) ? C7 C8 . 1.505(7) ? C9 C10 . 1.498(6) ? Ru' O5' . 2.016(3) ? Ru' O3' . 2.052(3) ? Ru' N2' . 2.123(4) ? Ru' N1' . 2.129(4) ? Ru' Cl1' . 2.3433(13) ? Ru' Cl2' . 2.4017(13) ? O1' C1' . 1.318(6) ? O2' C1' . 1.208(6) ? O3' C3' . 1.288(6) ? O4' C3' . 1.246(6) ? O5' C5' . 1.316(6) ? O6' C5' . 1.223(6) ? O7' C7' . 1.324(6) ? O8' C7' . 1.199(6) ? O8' Na 2_645 2.442(4) ? N1' C2' . 1.486(5) ? N1' C4' . 1.490(6) ? N1' C9' . 1.507(6) ? N2' C8' . 1.481(6) ? N2' C6' . 1.495(5) ? N2' C10' . 1.518(6) ? C1' C2' . 1.513(7) ? C3' C4' . 1.523(6) ? C5' C6' . 1.500(6) ? C7' C8' . 1.539(6) ? C9' C10' . 1.506(6) ? Na O8 1_556 2.369(4) ? Na O4W 2_656 2.411(5) ? Na O3W . 2.423(6) ? Na O8' 2_655 2.442(4) ? Na O2W 2_656 2.472(5) ? Na O1W . 2.481(5) ? O2W Na 2_646 2.472(5) ? O4W Na 2_646 2.411(5) ?