#------------------------------------------------------------------------------ #$Date: 2009-11-18 14:56:34 +0000 (Wed, 18 Nov 2009) $ #$Revision: 858 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006091.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_2006091 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1997 _journal_volume 53 _journal_page_first 551 _journal_page_last 554 _publ_section_title ; Sodium Bis(2,9-dimethyl-1,10-phenanthroline)-\m-hydroxo-di-\m-thiosulfato-dizinc(II) Pentahydrate Methanol Solvate ; loop_ _publ_author_name 'Baggio, Sergio' 'Pardo, Maria I.' 'Baggio, Ricardo' 'Garland, Maria Teresa' _chemical_formula_moiety ; (Zn 2+)2, (S2 O3 2-)2, (Na 1+), (C14 H12 N2)2, (H1 O1 1-), (C1 H4 O1)0.85, (H2 O)4.35 ; _chemical_formula_sum 'C28.85 H37.1 N4 Na O12.2 S4 Zn2' _[local]_cod_chemical_formula_sum_orig 'C28.85 H37.10 N4 Na O12.20 S4 Zn2' _chemical_formula_iupac '[Na Zn2 (O H) (S2 O3)2 (C14 H12 N2)2 (H2 O)3], 2H2 O, C H4 O' _chemical_formula_weight 933.6 _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 10.358(2) _cell_length_b 13.627(3) _cell_length_c 13.872(3) _cell_angle_alpha 90.160(10) _cell_angle_beta 98.470(10) _cell_angle_gamma 103.230(10) _cell_volume 1883.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.646 _diffrn_ambient_temperature 293(2) _refine_ls_R_factor_obs .039 _refine_ls_wR_factor_obs .095 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_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Zn1 .24809(4) .13460(3) .84121(3) .03656(14) Uani d . 1 . Zn S1 .11971(12) .17430(9) .94796(9) .0532(3) Uani d . 1 . S S2 .11513(10) .32052(8) .91523(8) .0438(3) Uani d . 1 . S O1 .2353(4) .3862(3) .9688(3) .0770(11) Uani d . 1 . O O2 .1118(3) .3315(2) .8119(2) .0560(8) Uani d . 1 . O O3 -.0034(4) .3369(3) .9504(3) .0788(11) Uani d . 1 . O N1 .2466(3) -.0193(2) .8383(2) .0373(8) Uani d . 1 . N N2 .4524(3) .1469(3) .8750(2) .0382(8) Uani d . 1 . N C1 .1443(5) -.0991(3) .8215(3) .0486(11) Uani d . 1 . C C2 .1652(7) -.1973(4) .8187(4) .070(2) Uani d . 1 . C H2A .0903 -.2542 .8037 .091 Uiso d R 1 . H C3 .2922(7) -.2109(4) .8356(4) .074(2) Uani d . 1 . C H3A .3072 -.2778 .8345 .096 Uiso d R 1 . H C4 .4026(6) -.1293(4) .8551(3) .0567(13) Uani d . 1 . C C5 .5411(7) -.1358(5) .8752(4) .075(2) Uani d . 1 . C H5A .5622 -.2009 .8762 .097 Uiso d R 1 . H C6 .6409(6) -.0536(6) .8931(4) .075(2) Uani d . 1 . C H6A .7319 -.0605 .9066 .097 Uiso d R 1 . H C7 .6180(5) .0457(4) .8937(3) .0575(14) Uani d . 1 . C C8 .7176(5) .1360(5) .9124(3) .065(2) Uani d . 1 . C H8A .8102 .1332 .9257 .085 Uiso d R 1 . H C9 .6845(5) .2258(5) .9123(4) .0662(14) Uani d . 1 . C H9A .7540 .2865 .9249 .086 Uiso d R 1 . H C10 .5507(4) .2310(4) .8942(3) .0509(11) Uani d . 1 . C C11 .4832(4) .0553(4) .8746(3) .0421(10) Uani d . 1 . C C12 .3759(4) -.0323(3) .8555(3) .0423(10) Uani d . 1 . C C13 .0051(5) -.0820(4) .8042(4) .0652(14) Uani d . 1 . C H13A .0105 -.0109 .8098 .085 Uiso d R 1 . H H13B -.0381 -.1072 .7400 .085 Uiso d R 1 . H H13C -.0458 -.1162 .8518 .085 Uiso d R 1 . H C14 .5120(5) .3297(4) .8957(4) .0711(15) Uani d . 1 . C H14A .4162 .3189 .8814 .092 Uiso d R 1 . H H14B .5428 .3615 .9594 .092 Uiso d R 1 . H H14C .5523 .3724 .8480 .092 Uiso d R 1 . H Zn2 .30668(5) .18452(4) .60064(3) .03922(15) Uani d . 1 . Zn S3 .20962(13) .22117(9) .45180(8) .0537(3) Uani d . 1 . S S4 .12140(12) .33344(8) .49098(8) .0503(3) Uani d . 1 . S O4 .1805(4) .4235(2) .4441(3) .0833(12) Uani d . 1 . O O5 .1463(4) .3460(2) .5952(2) .0692(10) Uani d . 1 . O O6 -.0200(4) .3007(3) .4542(4) .104(2) Uani d . 1 . O N3 .3658(3) .0486(2) .6054(2) .0363(7) Uani d . 1 . N N4 .5142(3) .2398(3) .6325(2) .0430(8) Uani d . 1 . N C15 .2876(4) -.0446(3) .5898(3) .0403(9) Uani d . 1 . C C16 .3453(5) -.1292(3) .5952(3) .0523(11) Uani d . 1 . C H16A .2885 -.1956 .5823 .068 Uiso d R 1 . H C17 .4804(5) -.1159(4) .6183(3) .0565(13) Uani d . 1 . C H17A .5185 -.1740 .6231 .073 Uiso d R 1 . H C18 .5642(4) -.0188(4) .6358(3) .0461(11) Uani d . 1 . C C19 .7071(5) .0026(5) .6594(3) .0603(14) Uani d . 1 . C H19A .7511 -.0524 .6654 .078 Uiso d R 1 . H C20 .7804(5) .0971(5) .6738(3) .0647(15) Uani d . 1 . C H20A .8761 .1091 .6907 .084 Uiso d R 1 . H C21 .7201(4) .1807(4) .6646(3) .0523(12) Uani d . 1 . C C22 .7915(5) .2830(5) .6766(4) .071(2) Uani d . 1 . C H22A .8876 .2982 .6920 .092 Uiso d R 1 . H C23 .7252(5) .3570(4) .6640(4) .070(2) Uani d . 1 . C H23A .7741 .4262 .6710 .090 Uiso d R 1 . H C24 .5852(5) .3355(4) .6412(3) .0567(12) Uani d . 1 . C C25 .5803(4) .1636(3) .6422(3) .0405(10) Uani d . 1 . C C26 .5017(4) .0613(3) .6283(3) .0364(9) Uani d . 1 . C C27 .1399(4) -.0547(3) .5653(4) .0564(12) Uani d . 1 . C H27A .1210 .0110 .5655 .073 Uiso d R 1 . H H27B .1090 -.0867 .5017 .073 Uiso d R 1 . H H27C .0948 -.0948 .6125 .073 Uiso d R 1 . H C28 .5115(6) .4177(4) .6279(4) .082(2) Uani d . 1 . C H28A .4169 .3887 .6131 .107 Uiso d R 1 . H H28B .5297 .4593 .6865 .107 Uiso d R 1 . H H28C .5404 .4580 .5750 .107 Uiso d R 1 . H Na .1774(2) .47746(13) .71169(14) .0574(5) Uani d . 1 . Na O .2183(3) .1824(2) .7123(2) .0471(7) Uani d . 1 . O H .1750(10) .2230(10) .7090(10) .061 Uiso d R 1 . H O1W .3484(4) .5371(4) .8382(3) .0918(14) Uani d D 1 . O H1WB .332(7) .508(6) .888(6) .119 Uiso d D 1 . H H1WA .431(8) .555(6) .845(5) .119 Uiso d D 1 . H O2W .0148(4) .5584(3) .7362(3) .0718(10) Uani d D 1 . O H2WA -.035(6) .540(5) .776(5) .093 Uiso d D 1 . H H2WB -.030(6) .578(5) .690(5) .093 Uiso d D 1 . H O3W .2299(4) .5918(3) .5829(3) .0787(11) Uani d D 1 . O H3WA .165(6) .616(5) .571(5) .102 Uiso d D 1 . H H3WB .221(7) .549(5) .540(5) .102 Uiso d D 1 . H O4W -.1319(5) .4914(4) .8842(3) .0835(12) Uani d D 1 . O H4WA -.144(7) .525(6) .929(5) .108 Uiso d D 1 . H H4WB -.076(7) .461(6) .906(5) .108 Uiso d D 1 . H C1X .6874(14) .6588(11) .7827(9) .210(7) Uani d PD .85(5) . C H1XA .6523 .7119 .7554 .316 Uiso d PR .85 . H H1XB .7757 .6791 .8143 .316 Uiso d PR .85 . H H1XC .6735 .6032 .7387 .316 Uiso d PR .85 . H O1X .6131(6) .6242(5) .8545(5) .103(2) Uani d PD .85(5) . O H1X .654(9) .580(7) .870(7) .134 Uiso d P .85 . H O5W .4690(15) .3386(12) .3388(10) .130(5) Uani d P .35(7) . O 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 Zn1 .0375(3) .0367(3) .0389(3) .0134(2) .0095(2) .0056(2) S1 .0670(8) .0535(7) .0548(7) .0330(6) .0300(6) .0174(6) S2 .0437(6) .0427(6) .0476(6) .0165(5) .0058(5) -.0034(5) O1 .071(2) .073(2) .072(2) -.001(2) -.011(2) -.008(2) O2 .082(2) .042(2) .046(2) .023(2) .002(2) .0056(14) O3 .074(2) .061(2) .121(3) .037(2) .046(2) .010(2) N1 .049(2) .033(2) .032(2) .011(2) .0098(15) .0091(14) N2 .037(2) .046(2) .035(2) .013(2) .0096(14) .006(2) C1 .066(3) .043(3) .036(2) .009(2) .011(2) .003(2) C2 .115(5) .036(3) .055(3) .011(3) .013(3) .004(2) C3 .141(6) .043(3) .051(3) .045(4) .022(3) .006(2) C4 .092(4) .055(3) .037(3) .040(3) .018(2) .010(2) C5 .117(5) .092(4) .050(3) .081(4) .032(3) .026(3) C6 .076(4) .128(6) .047(3) .069(4) .019(3) .029(3) C7 .060(3) .098(4) .030(2) .046(3) .011(2) .018(2) C8 .033(3) .121(5) .041(3) .015(3) .009(2) .015(3) C9 .048(3) .090(4) .054(3) .003(3) .010(2) .005(3) C10 .039(2) .070(3) .038(2) .001(2) .009(2) .004(2) C11 .044(2) .067(3) .022(2) .024(2) .008(2) .008(2) C12 .063(3) .047(3) .028(2) .030(2) .015(2) .009(2) C13 .058(3) .060(3) .066(3) -.010(2) .009(2) -.001(3) C14 .068(3) .052(3) .086(4) -.007(3) .019(3) -.006(3) Zn2 .0405(3) .0394(3) .0371(3) .0081(2) .0051(2) .0041(2) S3 .0702(8) .0559(7) .0377(6) .0257(6) -.0004(5) -.0011(5) S4 .0671(8) .0318(6) .0480(7) .0125(5) -.0055(5) .0048(5) O4 .143(4) .036(2) .066(2) .008(2) .022(2) .017(2) O5 .120(3) .050(2) .048(2) .041(2) .013(2) .008(2) O6 .070(3) .065(3) .169(5) .032(2) -.035(3) -.027(3) N3 .039(2) .040(2) .029(2) .008(2) .0069(14) .0044(14) N4 .045(2) .044(2) .034(2) -.002(2) .006(2) .005(2) C15 .048(2) .038(2) .034(2) .006(2) .010(2) .003(2) C16 .073(3) .038(2) .046(3) .011(2) .014(2) .000(2) C17 .084(4) .059(3) .038(3) .039(3) .013(2) .006(2) C18 .056(3) .061(3) .029(2) .028(2) .009(2) .003(2) C19 .059(3) .094(4) .041(3) .045(3) .008(2) .001(3) C20 .037(3) .112(5) .049(3) .025(3) .003(2) -.001(3) C21 .039(2) .081(4) .032(2) .005(2) .003(2) .000(2) C22 .041(3) .106(5) .052(3) -.005(3) -.002(2) .010(3) C23 .056(3) .067(4) .063(3) -.027(3) .001(3) .006(3) C24 .057(3) .053(3) .050(3) -.008(2) .008(2) .007(2) C25 .039(2) .054(3) .027(2) .007(2) .006(2) .002(2) C26 .035(2) .051(3) .022(2) .009(2) .004(2) .000(2) C27 .047(3) .044(3) .070(3) -.005(2) .010(2) -.001(2) C28 .093(4) .042(3) .094(4) -.010(3) -.002(3) .000(3) Na .0622(11) .0427(10) .0633(12) .0114(8) -.0029(9) -.0007(9) O .060(2) .050(2) .043(2) .0302(15) .0168(14) .0140(14) O1W .076(3) .079(3) .100(3) .000(2) -.025(2) .015(2) O2W .074(2) .070(2) .072(3) .025(2) .001(2) .014(2) O3W .099(3) .047(2) .088(3) .014(2) .015(2) .010(2) O4W .110(3) .093(3) .062(2) .055(3) .013(2) -.010(2) C1X .231(17) .187(15) .197(16) .074(13) -.054(13) -.038(12) O1X .074(4) .130(6) .085(4) -.003(3) -.014(3) .023(4) O5W .186(16) .097(11) .105(11) .025(10) .027(11) .008(9) 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 Zn1 O . 1.912(3) Y Zn1 N2 . 2.067(3) Y Zn1 N1 . 2.094(3) Y Zn1 S1 . 2.2713(12) Y S1 S2 . 2.054(2) Y S2 O2 . 1.437(3) Y S2 O3 . 1.448(3) Y S2 O1 . 1.455(4) Y O2 Na . 2.455(3) no N1 C1 . 1.325(5) N N1 C12 . 1.378(5) N N2 C10 . 1.344(5) N N2 C11 . 1.358(5) N C1 C2 . 1.406(7) N C1 C13 . 1.497(7) N C2 C3 . 1.357(8) N C3 C4 . 1.394(8) N C4 C12 . 1.411(6) N C4 C5 . 1.444(8) N C5 C6 . 1.334(8) N C6 C7 . 1.426(8) N C7 C8 . 1.408(7) N C7 C11 . 1.418(6) N C8 C9 . 1.344(8) N C9 C10 . 1.389(7) N C10 C14 . 1.489(7) N C11 C12 . 1.427(6) N Zn2 O . 1.908(3) Y Zn2 N3 . 2.077(3) Y Zn2 N4 . 2.088(3) Y Zn2 S3 . 2.2688(13) Y S3 S4 . 2.062(2) Y S4 O5 . 1.434(3) Y S4 O4 . 1.443(3) Y S4 O6 . 1.443(4) Y O5 Na . 2.343(4) no N3 C15 . 1.339(5) N N3 C26 . 1.368(5) N N4 C24 . 1.338(6) N N4 C25 . 1.366(5) N C15 C16 . 1.413(6) N C15 C27 . 1.491(6) N C16 C17 . 1.359(7) N C17 C18 . 1.406(7) N C18 C26 . 1.387(6) N C18 C19 . 1.429(6) N C19 C20 . 1.335(7) N C20 C21 . 1.417(7) N C21 C25 . 1.400(6) N C21 C22 . 1.418(7) N C22 C23 . 1.342(8) N C23 C24 . 1.399(7) N C24 C28 . 1.491(7) N C25 C26 . 1.441(6) N Na O2W . 2.278(4) no Na O1W . 2.301(4) no Na O3W . 2.414(5) no C1X O1X . 1.366(9) N