#------------------------------------------------------------------------------ #$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2012535.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_2012535 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2002 _journal_volume 58 _journal_page_first m105 _journal_page_last m108 _publ_section_title ; Bis(tetra-n-butylammonium), at 150K - a redetermination, and bis(tetraphenylarsonium), at 300K, bis(1,3-dithiole-2-thione-4,5-dithiolato)zinc(II) ; loop_ _publ_author_name 'Comerlato, Nadia M.' 'Harrison, William T.A.' 'Howie, R. Alan' 'Low, John Nicolson' 'Silvino, Alexandre C.' 'Wardell, James L.' 'Wardell, Solange M.S.V.' _chemical_formula_moiety '(C6 S10 Zn 2-), 2(C24 H20 As +)' _chemical_formula_sum 'C54 H40 As2 S10 Zn' _chemical_formula_weight 1224.67 _chemical_melting_point .478E-305 _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 10.3451(5) _cell_length_b 15.0563(7) _cell_length_c 18.8083(8) _cell_angle_alpha 73.0720(10) _cell_angle_beta 85.8670(10) _cell_angle_gamma 72.2590(10) _cell_volume 2668.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 300(2) _exptl_crystal_density_diffrn 1.524 _diffrn_ambient_temperature 300(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 Zn1 .46443(4) .31624(3) .24779(2) .05534(12) Uani d . 1 . . Zn S1 .60851(9) .38669(7) .28674(6) .0644(3) Uani d . 1 . . S S2 .26338(9) .42316(8) .27927(6) .0723(3) Uani d . 1 . . S S3 .52705(12) .58335(8) .31011(6) .0798(3) Uani d . 1 . . S S4 .24297(12) .61810(8) .29600(6) .0820(3) Uani d . 1 . . S S5 .3427(2) .77712(10) .31257(9) .1408(6) Uani d . 1 . . S C1 .4792(4) .4877(2) .29685(18) .0556(9) Uani d . 1 . . C C2 .3445(4) .5028(3) .29171(19) .0564(9) Uani d . 1 . . C C3 .3679(5) .6661(3) .3068(2) .0828(13) Uani d . 1 . . C S6 .50098(9) .14820(7) .29673(5) .0609(3) Uani d . 1 . . S S7 .47653(10) .31170(7) .12382(5) .0605(2) Uani d . 1 . . S S8 .44669(9) .01920(6) .21430(6) .0610(3) Uani d . 1 . . S S9 .42531(9) .15664(7) .07082(5) .0603(3) Uani d . 1 . . S S10 .39256(10) -.03646(7) .08149(7) .0738(3) Uani d . 1 . . S C4 .4703(3) .1303(2) .21255(19) .0497(8) Uani d . 1 . . C C5 .4595(3) .1952(2) .14478(19) .0494(8) Uani d . 1 . . C C6 .4204(3) .0421(2) .1203(2) .0539(9) Uani d . 1 . . C As1 .09051(3) -.26052(2) .009498(19) .04457(10) Uani d . 1 . . As C7 -.0398(3) -.2595(2) .08742(19) .0480(8) Uani d . 1 . . C C8 -.0067(4) -.3353(3) .1510(2) .0698(11) Uani d . 1 . . C H8 .0790 -.3805 .1568 .084 Uiso calc R 1 . . H C9 -.1004(5) -.3445(3) .2064(2) .0855(13) Uani d . 1 . . C H9 -.0783 -.3969 .2490 .103 Uiso calc R 1 . . H C10 -.2257(4) -.2772(4) .1993(3) .0754(12) Uani d . 1 . . C H10 -.2885 -.2832 .2370 .090 Uiso calc R 1 . . H C11 -.2570(4) -.2021(4) .1370(3) .0816(13) Uani d . 1 . . C H11 -.3421 -.1562 .1323 .098 Uiso calc R 1 . . H C12 -.1656(3) -.1914(3) .0798(2) .0730(12) Uani d . 1 . . C H12 -.1889 -.1393 .0372 .088 Uiso calc R 1 . . H C13 .2677(3) -.3162(2) .05412(17) .0439(8) Uani d . 1 . . C C14 .3464(3) -.4081(2) .05359(18) .0502(8) Uani d . 1 . . C H14 .3134 -.4455 .0322 .060 Uiso calc R 1 . . H C15 .4747(3) -.4437(3) .08515(19) .0584(9) Uani d . 1 . . C H15 .5282 -.5060 .0859 .070 Uiso calc R 1 . . H C16 .5236(3) -.3877(3) .11534(19) .0598(10) Uani d . 1 . . C H16 .6115 -.4114 .1350 .072 Uiso calc R 1 . . H C17 .4444(4) -.2974(3) .1168(2) .0636(10) Uani d . 1 . . C H17 .4777 -.2605 .1386 .076 Uiso calc R 1 . . H C18 .3165(3) -.2611(2) .0864(2) .0582(10) Uani d . 1 . . C H18 .2625 -.1995 .0875 .070 Uiso calc R 1 . . H C19 .0554(3) -.3344(2) -.04976(18) .0449(8) Uani d . 1 . . C C20 -.0658(3) -.3565(2) -.0428(2) .0594(10) Uani d . 1 . . C H20 -.1261 -.3417 -.0059 .071 Uiso calc R 1 . . H C21 -.0968(4) -.4012(3) -.0920(2) .0740(12) Uani d . 1 . . C H21 -.1785 -.4160 -.0885 .089 Uiso calc R 1 . . H C22 -.0066(5) -.4231(3) -.1452(2) .0767(12) Uani d . 1 . . C H22 -.0286 -.4513 -.1787 .092 Uiso calc R 1 . . H C23 .1160(4) -.4044(3) -.1505(2) .0722(11) Uani d . 1 . . C H23 .1782 -.4232 -.1855 .087 Uiso calc R 1 . . H C24 .1472(3) -.3577(2) -.10374(19) .0562(9) Uani d . 1 . . C H24 .2284 -.3422 -.1084 .067 Uiso calc R 1 . . H C25 .0801(3) -.1356(2) -.05673(18) .0484(8) Uani d . 1 . . C C26 .1940(4) -.1090(3) -.0799(2) .0817(13) Uani d . 1 . . C H26 .2782 -.1500 -.0599 .098 Uiso calc R 1 . . H C27 .1860(4) -.0229(4) -.1320(3) .1075(17) Uani d . 1 . . C H27 .2651 -.0063 -.1475 .129 Uiso calc R 1 . . H C28 .0653(5) .0387(3) -.1618(2) .0808(12) Uani d . 1 . . C H28 .0614 .0981 -.1963 .097 Uiso calc R 1 . . H C29 -.0497(4) .0138(3) -.1411(2) .0801(12) Uani d . 1 . . C H29 -.1329 .0556 -.1620 .096 Uiso calc R 1 . . H C30 -.0437(4) -.0735(3) -.0892(2) .0702(11) Uani d . 1 . . C H30 -.1227 -.0910 -.0758 .084 Uiso calc R 1 . . H As2 -.12845(3) .24463(2) .466014(19) .04693(10) Uani d . 1 . . As C31 -.0549(3) .2143(2) .37682(18) .0459(8) Uani d . 1 . . C C32 .0692(3) .2284(3) .3523(2) .0612(10) Uani d . 1 . . C H32 .1141 .2547 .3781 .073 Uiso calc R 1 . . H C33 .1253(4) .2034(3) .2898(2) .0740(12) Uani d . 1 . . C H33 .2077 .2135 .2726 .089 Uiso calc R 1 . . H C34 .0592(4) .1633(3) .2528(2) .0798(12) Uani d . 1 . . C H34 .0977 .1455 .2109 .096 Uiso calc R 1 . . H C35 -.0627(4) .1491(3) .2769(2) .0774(12) Uani d . 1 . . C H35 -.1059 .1211 .2517 .093 Uiso calc R 1 . . H C36 -.1221(4) .1762(2) .3385(2) .0593(10) Uani d . 1 . . C H36 -.2066 .1688 .3539 .071 Uiso calc R 1 . . H C37 .0163(3) .1883(2) .53869(18) .0484(8) Uani d . 1 . . C C38 .0233(4) .2348(3) .5906(2) .0649(10) Uani d . 1 . . C H38 -.0399 .2942 .5898 .078 Uiso calc R 1 . . H C39 .1266(5) .1914(3) .6442(2) .0859(13) Uani d . 1 . . C H39 .1343 .2228 .6789 .103 Uiso calc R 1 . . H C40 .2171(4) .1027(3) .6461(2) .0813(13) Uani d . 1 . . C H40 .2852 .0737 .6826 .098 Uiso calc R 1 . . H C41 .2082(4) .0563(3) .5948(2) .0744(12) Uani d . 1 . . C H41 .2690 -.0044 .5970 .089 Uiso calc R 1 . . H C42 .1094(3) .0998(3) .5401(2) .0627(10) Uani d . 1 . . C H42 .1051 .0696 .5041 .075 Uiso calc R 1 . . H C43 -.2685(3) .1839(3) .50079(19) .0495(8) Uani d . 1 . . C C44 -.2364(4) .0975(3) .5569(2) .0649(10) Uani d . 1 . . C H44 -.1509 .0725 .5796 .078 Uiso calc R 1 . . H C45 -.3317(5) .0485(3) .5791(3) .0844(13) Uani d . 1 . . C H45 -.3106 -.0098 .6168 .101 Uiso calc R 1 . . H C46 -.4558(6) .0853(4) .5461(3) .0971(17) Uani d . 1 . . C H46 -.5192 .0513 .5610 .117 Uiso calc R 1 . . H C47 -.4898(4) .1710(4) .4915(3) .0944(16) Uani d . 1 . . C H47 -.5765 .1958 .4702 .113 Uiso calc R 1 . . H C48 -.3948(4) .2220(3) .4674(2) .0722(11) Uani d . 1 . . C H48 -.4167 .2803 .4297 .087 Uiso calc R 1 . . H C49 -.1865(3) .3800(2) .45792(18) .0487(8) Uani d . 1 . . C C50 -.2910(3) .4166(3) .5012(2) .0601(10) Uani d . 1 . . C H50 -.3422 .3778 .5288 .072 Uiso calc R 1 . . H C51 -.3188(4) .5125(3) .5030(2) .0734(12) Uani d . 1 . . C H51 -.3887 .5376 .5322 .088 Uiso calc R 1 . . H C52 -.2443(5) .5694(3) .4624(2) .0814(13) Uani d . 1 . . C H52 -.2634 .6332 .4641 .098 Uiso calc R 1 . . H C53 -.1418(5) .5335(3) .4193(2) .0826(13) Uani d . 1 . . C H53 -.0917 .5730 .3914 .099 Uiso calc R 1 . . H C54 -.1119(4) .4385(3) .4166(2) .0686(11) Uani d . 1 . . C H54 -.0418 .4142 .3872 .082 Uiso calc R 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 Zn1 .0551(2) .0473(3) .0651(3) -.01599(19) -.0011(2) -.0167(2) S1 .0547(6) .0607(7) .0760(7) -.0200(5) -.0117(5) -.0105(5) S2 .0533(6) .0750(7) .1034(9) -.0200(5) .0032(5) -.0469(7) S3 .1210(9) .0772(8) .0609(7) -.0575(7) -.0091(6) -.0174(6) S4 .1028(9) .0671(7) .0768(8) -.0101(6) .0011(6) -.0372(6) S5 .254(2) .0762(10) .1161(12) -.0655(11) .0303(12) -.0529(9) C1 .078(3) .051(2) .042(2) -.0281(19) -.0060(18) -.0079(17) C2 .064(2) .059(2) .051(2) -.0159(18) -.0027(18) -.0236(19) C3 .132(4) .067(3) .054(3) -.029(3) .007(2) -.025(2) S6 .0701(6) .0476(6) .0603(6) -.0158(5) -.0059(5) -.0086(5) S7 .0742(6) .0477(6) .0599(6) -.0236(5) .0033(5) -.0106(5) S8 .0628(6) .0433(6) .0751(7) -.0160(4) .0047(5) -.0145(5) S9 .0618(6) .0563(6) .0649(6) -.0171(5) -.0003(5) -.0204(5) S10 .0619(6) .0631(7) .1069(9) -.0168(5) -.0004(6) -.0411(6) C4 .0461(19) .038(2) .061(2) -.0080(15) .0018(17) -.0130(18) C5 .0428(19) .043(2) .060(2) -.0094(15) .0021(17) -.0146(18) C6 .0331(17) .052(2) .077(3) -.0055(15) .0002(17) -.026(2) As1 .03888(18) .0435(2) .0527(2) -.01203(15) -.00089(16) -.01553(17) C7 .045(2) .056(2) .049(2) -.0172(17) .0006(17) -.0206(19) C8 .071(3) .068(3) .058(3) -.010(2) .012(2) -.013(2) C9 .108(4) .080(3) .062(3) -.031(3) .018(3) -.012(2) C10 .074(3) .110(4) .070(3) -.055(3) .026(2) -.044(3) C11 .044(2) .110(4) .094(4) -.016(2) .005(2) -.044(3) C12 .050(2) .087(3) .065(3) -.006(2) .004(2) -.013(2) C13 .0402(18) .046(2) .047(2) -.0158(15) .0017(15) -.0132(17) C14 .052(2) .041(2) .057(2) -.0117(16) -.0065(17) -.0137(17) C15 .056(2) .043(2) .064(2) -.0019(17) -.0055(19) -.0079(19) C16 .046(2) .064(3) .060(2) -.0130(19) -.0154(18) -.002(2) C17 .064(2) .064(3) .070(3) -.025(2) -.017(2) -.019(2) C18 .054(2) .046(2) .077(3) -.0083(17) -.0087(19) -.025(2) C19 .0418(18) .044(2) .049(2) -.0114(15) -.0063(16) -.0132(16) C20 .047(2) .058(2) .079(3) -.0195(18) .0037(19) -.024(2) C21 .062(3) .068(3) .103(4) -.027(2) -.013(2) -.029(3) C22 .090(3) .062(3) .086(3) -.016(2) -.027(3) -.033(2) C23 .080(3) .071(3) .069(3) -.012(2) -.004(2) -.034(2) C24 .052(2) .058(2) .061(2) -.0169(18) -.0010(19) -.021(2) C25 .0429(19) .047(2) .055(2) -.0121(16) .0036(17) -.0165(17) C26 .045(2) .066(3) .109(4) -.011(2) .002(2) .009(3) C27 .065(3) .081(4) .145(5) -.028(3) .014(3) .020(3) C28 .093(3) .053(3) .079(3) -.019(3) .018(3) .000(2) C29 .064(3) .063(3) .084(3) .001(2) .004(2) .001(2) C30 .051(2) .069(3) .076(3) -.015(2) .002(2) -.002(2) As2 .0499(2) .0444(2) .0495(2) -.01694(16) .00489(17) -.01579(17) C31 .0457(19) .047(2) .045(2) -.0136(16) .0052(16) -.0141(16) C32 .057(2) .072(3) .061(3) -.0202(19) .005(2) -.028(2) C33 .055(2) .089(3) .073(3) -.015(2) .012(2) -.023(3) C34 .080(3) .093(3) .063(3) -.013(3) .014(2) -.034(3) C35 .090(3) .085(3) .069(3) -.025(2) -.002(2) -.040(3) C36 .059(2) .062(3) .063(3) -.0208(19) .0047(19) -.025(2) C37 .050(2) .050(2) .046(2) -.0171(17) .0041(16) -.0142(17) C38 .080(3) .054(2) .055(2) -.007(2) -.009(2) -.017(2) C39 .113(4) .078(3) .063(3) -.017(3) -.019(3) -.021(2) C40 .070(3) .094(4) .065(3) -.020(3) -.016(2) -.001(3) C41 .058(3) .061(3) .090(3) -.006(2) -.007(2) -.012(2) C42 .057(2) .056(2) .077(3) -.0104(19) -.001(2) -.027(2) C43 .055(2) .053(2) .048(2) -.0232(17) .0145(17) -.0204(18) C44 .072(3) .056(3) .070(3) -.023(2) .023(2) -.024(2) C45 .103(4) .062(3) .091(3) -.040(3) .044(3) -.021(3) C46 .100(4) .111(5) .117(5) -.070(4) .051(4) -.059(4) C47 .061(3) .144(5) .100(4) -.049(3) .016(3) -.052(4) C48 .062(3) .088(3) .069(3) -.028(2) .008(2) -.021(2) C49 .056(2) .043(2) .045(2) -.0130(17) -.0051(17) -.0101(17) C50 .066(2) .052(2) .058(2) -.0138(19) .0027(19) -.015(2) C51 .088(3) .053(3) .069(3) -.001(2) .000(2) -.022(2) C52 .119(4) .048(3) .079(3) -.021(3) -.010(3) -.022(2) C53 .111(4) .058(3) .088(3) -.043(3) .006(3) -.017(3) C54 .083(3) .058(3) .067(3) -.026(2) .017(2) -.018(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 Zn1 S1 . 2.3360(10) yes Zn1 S6 . 2.3458(10) yes Zn1 S7 . 2.3458(10) yes Zn1 S2 . 2.3674(10) yes S1 C1 . 1.740(4) yes S2 C2 . 1.733(4) yes S3 C3 . 1.728(4) yes S3 C1 . 1.745(3) yes S4 C3 . 1.711(5) yes S4 C2 . 1.755(3) yes S5 C3 . 1.646(4) yes C1 C2 . 1.347(4) yes S6 C4 . 1.747(3) yes S7 C5 . 1.743(3) yes S8 C6 . 1.725(4) yes S8 C4 . 1.754(3) yes S9 C6 . 1.719(4) yes S9 C5 . 1.751(3) yes S10 C6 . 1.660(3) yes C4 C5 . 1.349(4) yes As1 C25 . 1.906(3) ? As1 C19 . 1.908(3) ? As1 C13 . 1.908(3) ? As1 C7 . 1.918(3) ? C7 C8 . 1.370(5) ? C7 C12 . 1.376(4) ? C8 C9 . 1.376(5) ? C8 H8 . .9300 ? C9 C10 . 1.367(5) ? C9 H9 . .9300 ? C10 C11 . 1.348(5) ? C10 H10 . .9300 ? C11 C12 . 1.386(5) ? C11 H11 . .9300 ? C12 H12 . .9300 ? C13 C14 . 1.378(4) ? C13 C18 . 1.380(4) ? C14 C15 . 1.377(4) ? C14 H14 . .9300 ? C15 C16 . 1.367(5) ? C15 H15 . .9300 ? C16 C17 . 1.364(4) ? C16 H16 . .9300 ? C17 C18 . 1.365(4) ? C17 H17 . .9300 ? C18 H18 . .9300 ? C19 C20 . 1.380(4) ? C19 C24 . 1.386(4) ? C20 C21 . 1.397(5) ? C20 H20 . .9300 ? C21 C22 . 1.360(5) ? C21 H21 . .9300 ? C22 C23 . 1.371(5) ? C22 H22 . .9300 ? C23 C24 . 1.383(4) ? C23 H23 . .9300 ? C24 H24 . .9300 ? C25 C26 . 1.360(5) ? C25 C30 . 1.392(4) ? C26 C27 . 1.362(5) ? C26 H26 . .9300 ? C27 C28 . 1.351(5) ? C27 H27 . .9300 ? C28 C29 . 1.352(5) ? C28 H28 . .9300 ? C29 C30 . 1.377(5) ? C29 H29 . .9300 ? C30 H30 . .9300 ? As2 C49 . 1.904(3) ? As2 C31 . 1.911(3) ? As2 C37 . 1.917(3) ? As2 C43 . 1.919(3) ? C31 C36 . 1.373(4) ? C31 C32 . 1.389(4) ? C32 C33 . 1.375(5) ? C32 H32 . .9300 ? C33 C34 . 1.372(5) ? C33 H33 . .9300 ? C34 C35 . 1.366(5) ? C34 H34 . .9300 ? C35 C36 . 1.381(5) ? C35 H35 . .9300 ? C36 H36 . .9300 ? C37 C38 . 1.374(4) ? C37 C42 . 1.380(4) ? C38 C39 . 1.391(5) ? C38 H38 . .9300 ? C39 C40 . 1.370(5) ? C39 H39 . .9300 ? C40 C41 . 1.368(5) ? C40 H40 . .9300 ? C41 C42 . 1.372(5) ? C41 H41 . .9300 ? C42 H42 . .9300 ? C43 C48 . 1.372(5) ? C43 C44 . 1.380(5) ? C44 C45 . 1.376(5) ? C44 H44 . .9300 ? C45 C46 . 1.350(6) ? C45 H45 . .9300 ? C46 C47 . 1.359(6) ? C46 H46 . .9300 ? C47 C48 . 1.398(6) ? C47 H47 . .9300 ? C48 H48 . .9300 ? C49 C54 . 1.380(5) ? C49 C50 . 1.380(4) ? C50 C51 . 1.393(5) ? C50 H50 . .9300 ? C51 C52 . 1.359(6) ? C51 H51 . .9300 ? C52 C53 . 1.363(5) ? C52 H52 . .9300 ? C53 C54 . 1.382(5) ? C53 H53 . .9300 ? C54 H54 . .9300 ? _cod_database_code 2012535