#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/04/2200408.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_2200408 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2001 _journal_volume 57 _journal_page_first m390 _journal_page_last m392 _publ_section_title ; [(CH~3~)~2~NH~2~]~4~[H~4~PMo~12~O~40~]Cl~2~.4H~2~O ; loop_ _publ_author_name 'Wu, Chuan-De' 'Lu, Can-Zhong' 'Lin, Xiang' 'Yang, Wen-Bin' 'Zhuang, Hong-Hui' 'Huang, Jin-Shun' _chemical_formula_moiety '4C2 H6 N H2 1+, H4 P Mo12 O40 2-, 2Cl 1-, 4H2 O' _chemical_formula_sum 'C8 H44 Cl2 Mo12 N4 O44 P' _chemical_formula_iupac '(C2 H6 N H2)4 [H4 P Mo12 O40] Cl2, 4H2 O' _chemical_formula_weight 2153.62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.9803(7) _cell_length_b 15.0682(8) _cell_length_c 22.6217(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5106.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 2.801 _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 Mo1 .52413(3) -.12694(3) .41208(2) .02241(14) Uani d . 1 . . Mo Mo2 .90300(3) -.12836(3) .45329(2) .02278(14) Uani d . 1 . . Mo Mo3 .72576(3) -.12815(3) .34095(2) .02241(14) Uani d . 1 . . Mo Mo4 .49640(4) -.2500 .55895(3) .02137(17) Uani d S 1 . . Mo Mo5 .67296(3) -.13119(3) .61515(2) .01957(13) Uani d . 1 . . Mo Mo6 .87958(4) -.2500 .58057(3) .02083(16) Uani d S 1 . . Mo Mo7 .69432(3) -.00835(3) .47544(2) .02279(13) Uani d . 1 . . Mo Cl1 1.04719(18) -.2500 .30235(11) .0518(6) Uani d S 1 . . Cl Cl2 .68407(15) .2500 .26296(10) .0415(6) Uani d S 1 . . Cl P1 .70035(11) -.2500 .47753(8) .0149(4) Uani d S 1 . . P O1 .9514(3) -.2500 .6371(2) .0323(14) Uani d S 1 . . O O2 .5758(2) -.0218(3) .44803(16) .0256(8) Uani d . 1 . . O O3 .6771(2) -.0641(3) .67374(16) .0307(9) Uani d . 1 . . O O4 .7034(3) .1001(3) .48767(18) .0333(10) Uani d . 1 . . O O5 .8021(3) -.2500 .4856(2) .0209(11) Uani d S 1 . . O O6 .6727(2) -.1660(2) .44290(15) .0203(8) Uani d . 1 . . O O7 .9573(3) -.2500 .4264(2) .0235(12) Uani d S 1 . . O O8 .6694(2) -.0533(3) .55117(16) .0255(9) Uani d . 1 . . O O9 .9346(2) -.1613(3) .53001(15) .0243(9) Uani d . 1 . . O O10 .6548(3) -.2500 .5391(2) .0187(11) Uani d S 1 . . O O11 .5476(2) -.1603(3) .60879(15) .0224(8) Uani d . 1 . . O O12 .7923(2) -.1618(3) .60303(16) .0234(8) Uani d . 1 . . O O13 .8357(2) -.1380(3) .37983(16) .0247(9) Uani d . 1 . . O O14 .8142(2) -.0489(3) .47890(16) .0258(9) Uani d . 1 . . O O15 .6001(2) -.1139(3) .34373(16) .0248(9) Uani d . 1 . . O O16 .3909(3) -.2500 .5835(2) .0280(13) Uani d S 1 . . O O17 .5123(3) -.2500 .3971(2) .0238(12) Uani d S 1 . . O O18 .7188(3) -.2500 .3262(2) .0261(12) Uani d S 1 . . O O19 .4928(2) -.1605(3) .49627(16) .0302(9) Uani d . 1 . . O O20 .4279(3) -.0872(3) .38600(18) .0346(10) Uani d . 1 . . O O21 .6718(3) -.2500 .6649(2) .0221(12) Uani d S 1 . . O O22 .9877(3) -.0626(3) .43334(17) .0360(11) Uani d . 1 . . O O23 .7495(3) -.0881(3) .27354(17) .0343(10) Uani d . 1 . . O O24 .7223(2) -.0052(3) .38493(15) .0254(9) Uani d . 1 . . O O101 .5965(3) .0864(3) .32466(17) .0330(10) Uani d . 1 . . O O102 .6143(9) .2500 .7104(5) .125(4) Uani d S 1 . . O O103 .4613(5) .2500 .2462(3) .088(3) Uani d S 1 . . O N1 .5509(3) -.0347(4) .2284(2) .0383(13) Uani d . 1 . . N N2 .3499(6) .2500 .1476(4) .057(2) Uani d S 1 . . N N3 .7597(10) .2500 .6511(7) .129(6) Uani d S 1 . . N C1 .4530(4) -.0237(6) .2277(3) .058(2) Uani d . 1 . . C H1A .4267 -.0619 .2569 .087 Uiso calc R 1 . . H H1B .4304 -.0391 .1893 .087 Uiso calc R 1 . . H H1C .4382 .0369 .2364 .087 Uiso calc R 1 . . H C2 .5965(5) .0230(6) .1847(3) .063(2) Uani d . 1 . . C H2A .6598 .0135 .1869 .095 Uiso calc R 1 . . H H2B .5836 .0841 .1934 .095 Uiso calc R 1 . . H H2C .5757 .0090 .1457 .095 Uiso calc R 1 . . H C3 .3517(7) .1708(8) .1111(6) .116(4) Uani d . 1 . . C H3A .3503 .1191 .1359 .174 Uiso calc R 1 . . H H3B .4054 .1704 .0879 .174 Uiso calc R 1 . . H H3C .3008 .1706 .0853 .174 Uiso calc R 1 . . H C4 .7657(10) .1759(17) .6131(8) .289(17) Uani d . 1 . . C H4A .7593 .1224 .6357 .434 Uiso calc R 1 . . H H4B .8228 .1760 .5937 .434 Uiso calc R 1 . . H H4C .7192 .1790 .5840 .434 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 Mo1 .0196(2) .0251(3) .0226(3) .0038(2) -.00269(18) -.0011(2) Mo2 .0187(2) .0298(3) .0199(3) -.0037(2) .00098(18) .0018(2) Mo3 .0238(3) .0269(3) .0165(2) .0001(2) .00005(18) .00272(19) Mo4 .0159(3) .0302(4) .0179(3) .000 .0019(3) .000 Mo5 .0194(2) .0227(3) .0166(2) -.00018(19) .00151(17) -.00262(19) Mo6 .0153(3) .0304(4) .0167(3) .000 -.0014(2) .000 Mo7 .0271(3) .0201(3) .0212(2) -.0003(2) .00027(19) .00061(19) Cl1 .0616(15) .0495(16) .0445(14) .000 .0158(12) .000 Cl2 .0421(12) .0495(15) .0330(12) .000 .0087(9) .000 P1 .0138(8) .0185(11) .0123(8) .000 .0004(7) .000 O1 .024(3) .048(4) .025(3) .000 -.005(2) .000 O2 .027(2) .025(2) .024(2) .0048(18) -.0001(16) -.0019(17) O3 .033(2) .037(3) .021(2) -.0010(19) .0025(16) -.0068(18) O4 .042(2) .021(2) .036(2) -.0032(19) .0026(19) .0005(19) O5 .017(2) .028(3) .018(3) .000 -.003(2) .000 O6 .0202(18) .023(2) .0177(18) -.0002(16) .0007(14) .0022(16) O7 .018(2) .027(3) .026(3) .000 .003(2) .000 O8 .028(2) .028(2) .0205(19) .0004(17) .0018(15) -.0019(17) O9 .0159(18) .036(2) .0214(19) -.0019(17) -.0001(15) .0005(17) O10 .016(2) .027(3) .014(2) .000 .0027(19) .000 O11 .0197(18) .028(2) .0199(18) .0002(17) .0034(15) -.0015(16) O12 .0211(18) .028(2) .0209(19) -.0026(17) .0000(15) -.0024(16) O13 .025(2) .029(2) .0197(19) .0014(17) .0016(15) .0024(16) O14 .0273(19) .027(2) .0234(19) .0010(18) -.0021(15) -.0018(17) O15 .026(2) .029(2) .0192(19) .0009(17) -.0026(15) .0010(17) O16 .020(3) .040(4) .023(3) .000 .004(2) .000 O17 .023(3) .030(3) .019(3) .000 -.001(2) .000 O18 .025(3) .033(3) .020(3) .000 .000(2) .000 O19 .0226(19) .048(3) .0198(19) .0021(19) .0006(15) .0070(19) O20 .028(2) .040(3) .036(2) .010(2) -.0051(18) -.001(2) O21 .024(3) .028(3) .014(2) .000 .003(2) .000 O22 .029(2) .047(3) .032(2) -.014(2) .0030(17) .005(2) O23 .037(2) .043(3) .023(2) .000(2) .0030(17) .0086(19) O24 .0295(19) .027(2) .0201(19) -.0007(18) .0024(16) .0009(16) O101 .039(2) .029(2) .031(2) .004(2) -.0027(18) .0005(19) O102 .172(12) .121(10) .082(8) .000 -.028(7) .000 O103 .045(4) .184(11) .035(4) .000 .011(3) .000 N1 .037(3) .043(4) .035(3) -.003(3) -.004(2) .003(2) N2 .044(5) .071(7) .057(6) .000 -.006(4) .000 N3 .120(12) .173(17) .094(11) .000 -.028(9) .000 C1 .040(4) .078(6) .056(5) .002(4) .004(3) -.020(4) C2 .069(5) .086(6) .034(4) -.030(5) .001(3) .016(4) C3 .082(7) .121(10) .145(11) -.051(8) -.019(7) -.032(9) C4 .116(12) .51(4) .24(2) -.127(18) .045(13) -.24(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 Mo1 O20 . 1.668(4) yes Mo1 O17 . 1.8930(10) yes Mo1 O15 . 1.930(4) yes Mo1 O2 . 1.941(4) yes Mo1 O19 . 2.026(4) yes Mo1 O6 . 2.406(3) yes Mo2 O22 . 1.672(4) yes Mo2 O9 . 1.866(4) yes Mo2 O14 . 1.881(4) yes Mo2 O13 . 1.949(4) yes Mo2 O7 . 2.096(2) yes Mo2 O5 . 2.486(3) yes Mo3 O23 . 1.678(4) yes Mo3 O18 . 1.8690(10) yes Mo3 O13 . 1.873(4) yes Mo3 O15 . 1.896(4) yes Mo3 O24 . 2.104(4) yes Mo3 O6 . 2.505(3) yes Mo4 O16 . 1.676(5) yes Mo4 O11 . 1.921(4) yes Mo4 O11 7 1.921(4) no Mo4 O19 7 1.958(4) no Mo4 O19 . 1.958(4) yes Mo4 O10 . 2.415(5) yes Mo5 O3 . 1.669(4) yes Mo5 O8 . 1.865(4) yes Mo5 O12 . 1.866(3) yes Mo5 O11 . 1.933(3) yes Mo5 O21 . 2.115(3) yes Mo5 O10 . 2.497(3) yes Mo6 O1 . 1.672(5) yes Mo6 O12 7 1.933(4) no Mo6 O12 . 1.933(4) yes Mo6 O9 . 1.943(4) yes Mo6 O9 7 1.943(4) no Mo6 O5 . 2.442(5) yes Mo7 O4 . 1.663(4) yes Mo7 O8 . 1.879(4) yes Mo7 O2 . 1.892(4) yes Mo7 O14 . 1.899(4) yes Mo7 O24 . 2.090(3) yes Mo7 O6 . 2.508(4) yes P1 O5 . 1.535(5) yes P1 O6 . 1.545(4) yes P1 O6 7 1.545(4) no P1 O10 . 1.552(5) yes O5 Mo2 7 2.486(3) no O7 Mo2 7 2.096(2) no O10 Mo5 7 2.497(3) no O17 Mo1 7 1.8933(11) no O18 Mo3 7 1.8690(11) no O21 Mo5 7 2.115(3) no N1 C1 . 1.477(8) no N1 C2 . 1.482(8) no N2 C3 . 1.452(12) no N2 C3 7_565 1.452(12) no N3 C4 . 1.413(18) no N3 C4 7_565 1.413(18) no _cod_database_code 2200408