#------------------------------------------------------------------------------ #$Date: 2011-09-28 16:24:46 +0200 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/15/2011595.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_2011595 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2000 _journal_volume 56 _journal_page_first 1411 _journal_page_last 1412 _publ_section_title ; [NH~4~]~3~[VO~2~(SO~4~)~2~(OH~2~)~2~].1.5H~2~O ; loop_ _publ_author_name 'Hashimoto, Masato' 'Kubata, Michiru' 'Yagasaki, Atsushi' _chemical_formula_moiety '3NH4 + , H14 O12 S2 V 3- , 1.5H2 O' _chemical_formula_sum 'H19 N3 O13.5 S2 V' _[local]_cod_chemical_formula_sum_orig 'H19 N3 O13.50 S2 V' _chemical_formula_structural ' (N H4)3 (V(O2 (S O4)2 (O H2)2)) (H2 O)1.5' _chemical_formula_iupac '(N H4)3 , [VO2 (SO4 )2 (OH2 )2 ], 1.5H2 O' _chemical_formula_weight 392.24 _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 7.748(2) _cell_length_b 14.164(3) _cell_length_c 6.268(2) _cell_angle_alpha 91.54(2) _cell_angle_beta 95.30(2) _cell_angle_gamma 88.25(2) _cell_volume 684.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.903 _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 V1 .41406(2) .232330(13) .46950(3) .01946(5) Uani d . 1 . . V S1 .14518(4) .37785(2) .23438(6) .02690(7) Uani d . 1 . . S S2 .74810(3) .098593(18) .58459(4) .01907(5) Uani d . 1 . . S O1 .55752(13) .31019(7) .42587(18) .02993(18) Uani d . 1 . . O O2 .38995(14) .17176(8) .24622(17) .0329(2) Uani d . 1 . . O OW1 .22757(12) .14909(7) .63305(19) .02893(18) Uani d . 1 . . O OW2 .41290(14) .30238(7) .79675(17) .03127(19) Uani d . 1 . . O O11 .19843(12) .31434(7) .42029(17) .02863(18) Uani d . 1 . . O O12 .13178(16) .31852(9) .0373(2) .0379(2) Uani d . 1 . . O O13 -.02344(14) .42014(9) .2745(2) .0403(3) Uani d . 1 . . O O14 .27415(17) .45012(9) .2239(3) .0499(4) Uani d . 1 . . O O21 .57481(11) .14075(7) .63211(15) .02478(16) Uani d . 1 . . O O22 .72938(15) .04146(7) .38645(17) .03152(19) Uani d . 1 . . O O23 .86817(12) .17500(7) .5614(2) .0338(2) Uani d . 1 . . O O24 .80695(13) .04067(7) .76919(17) .03013(19) Uani d . 1 . . O N1 .00854(17) .13172(9) .1252(2) .0333(2) Uani d . 1 . . N N2 .8812(2) .36879(10) .6918(2) .0385(3) Uani d . 1 . . N N3 .6224(2) .49888(12) .2242(4) .0543(5) Uani d . 1 . . N OW3 .72234(18) .26757(14) .0540(2) .0547(4) Uani d . 1 . . O OW4 .5000 .0000 .0000 .0435(4) Uani d S 1 . . O H11 .2449 .0954 .6185 .060 Uiso d . 1 . . H H12 .1249 .1579 .6088 .060 Uiso d . 1 . . H H21 .3351 .2968 .8714 .060 Uiso d . 1 . . H H22 .5017 .2938 .8831 .060 Uiso d . 1 . . H H31 .6830 .2731 .1738 .110 Uiso d . 1 . . H H32 .8044 .3106 .1203 .110 Uiso d . 1 . . H H41 .5735 .0210 .1079 .090 Uiso d P .50 . . H H42 .6051 .0109 -.0352 .090 Uiso d P .50 . . H H51 -.0432 .1140 .0217 .070 Uiso d . 1 . . H H52 .0649 .1761 .1060 .070 Uiso d . 1 . . H H53 .0814 .0903 .1694 .070 Uiso d . 1 . . H H54 -.0488 .1498 .2257 .070 Uiso d . 1 . . H H61 .8299 .4166 .7110 .080 Uiso d . 1 . . H H62 .9573 .3607 .7914 .080 Uiso d . 1 . . H H63 .8445 .3244 .6534 .080 Uiso d . 1 . . H H64 .9354 .3894 .5880 .080 Uiso d . 1 . . H H71 .7177 .4646 .2001 .110 Uiso d . 1 . . H H72 .5388 .4600 .2383 .110 Uiso d . 1 . . H H73 .6402 .5061 .3490 .110 Uiso d . 1 . . H H74 .5985 .5524 .1314 .110 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 V1 .01595(7) .01890(8) .02329(8) .00197(5) .00110(5) .00121(6) S1 .02039(12) .02187(12) .03869(16) .00533(9) .00381(10) .00802(11) S2 .01539(9) .01541(10) .02601(12) .00138(7) .00016(8) .00099(8) O1 .0242(4) .0284(4) .0379(5) -.0037(3) .0038(3) .0060(4) O2 .0321(5) .0344(5) .0303(4) .0061(4) -.0021(4) -.0074(4) OW1 .0198(3) .0206(3) .0466(5) -.0001(3) .0037(3) .0031(3) OW2 .0309(4) .0310(4) .0323(5) -.0010(4) .0064(4) -.0055(4) O11 .0231(4) .0274(4) .0356(5) .0081(3) .0040(3) .0080(3) O12 .0362(5) .0422(6) .0354(5) .0077(4) .0046(4) .0058(4) O13 .0273(5) .0412(6) .0524(7) .0178(4) .0074(4) .0105(5) O14 .0351(6) .0270(5) .0892(11) -.0024(4) .0081(6) .0184(6) O21 .0168(3) .0267(4) .0309(4) .0058(3) .0033(3) .0064(3) O22 .0388(5) .0252(4) .0295(4) .0045(4) .0004(4) -.0051(3) O23 .0198(4) .0224(4) .0601(7) -.0041(3) .0065(4) .0013(4) O24 .0301(4) .0270(4) .0316(4) .0078(3) -.0053(3) .0059(3) N1 .0305(5) .0304(5) .0377(6) .0001(4) -.0033(4) .0020(4) N2 .0452(7) .0302(6) .0387(6) -.0011(5) -.0027(5) -.0047(5) N3 .0362(7) .0389(7) .0888(14) -.0022(6) .0059(8) .0203(8) OW3 .0319(6) .0885(12) .0441(7) .0032(6) .0045(5) .0101(7) OW4 .0360(8) .0578(11) .0363(8) -.0043(7) .0024(6) -.0054(7) 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 V1 O2 . 1.6206(11) y V1 O1 . 1.6352(10) y V1 O21 . 2.0026(10) y V1 O11 . 2.0103(10) y V1 OW1 . 2.2296(11) y V1 OW2 . 2.2551(12) y S1 O14 . 1.4591(13) y S1 O13 . 1.4608(11) y S1 O12 . 1.4725(14) y S1 O11 . 1.5107(11) y S2 O22 . 1.4622(11) y S2 O24 . 1.4665(11) y S2 O23 . 1.4672(10) y S2 O21 . 1.5045(9) y O1 OW2 . 2.6785(17) n O1 OW3 . 2.803(2) n O1 N2 . 3.006(2) n O1 N3 . 3.062(2) n O2 OW1 . 2.8627(18) n O2 OW4 . 2.9904(12) n O2 N1 . 3.0488(19) n OW1 O21 . 2.6899(14) n OW1 O22 2_656 2.7103(15) n OW1 O11 . 2.7180(15) n OW1 OW2 . 2.7617(16) n OW1 O23 1_455 2.7939(15) n OW1 H11 . .7727 n OW1 H12 . .8025 n OW2 O12 1_556 2.7620(17) n OW2 O11 . 2.7637(17) n OW2 O21 . 2.7957(15) n OW2 OW3 1_556 2.8015(19) n OW2 N3 2_666 2.825(2) n OW2 H21 . .8035 n OW2 H22 . .8430 n O11 N2 1_455 3.181(2) n O12 OW2 1_554 2.7620(17) n O12 N2 1_454 2.862(2) n O12 N1 . 2.923(2) n O13 N2 1_455 2.899(2) n O13 N3 1_455 2.923(2) n O13 OW3 1_455 3.171(2) n O13 N2 2_666 3.212(2) n O14 N3 . 2.805(2) n O14 N2 2_666 2.857(2) n O14 N3 2_665 3.101(3) n O21 OW4 1_556 3.1926(12) n O22 OW1 2_656 2.7103(15) n O22 OW4 . 2.9263(14) n O22 N1 1_655 3.151(2) n O23 OW1 1_655 2.7939(15) n O23 N2 . 2.8450(18) n O23 N1 1_655 3.074(2) n O24 N1 2_656 2.8536(17) n O24 N1 1_656 2.8994(18) n O24 OW4 1_556 2.9740(14) n N1 O24 2_656 2.8536(17) n N1 O24 1_454 2.8994(18) n N1 OW3 1_455 2.902(2) n N1 O23 1_455 3.074(2) n N1 O22 1_455 3.151(2) n N1 H51 . .7706 n N1 H52 . .7942 n N1 H53 . .8362 n N1 H54 . .8342 n N2 O14 2_666 2.857(2) n N2 O12 1_656 2.862(2) n N2 O13 1_655 2.899(2) n N2 OW3 1_556 3.087(2) n N2 O11 1_655 3.181(2) n N2 H61 . .7869 n N2 H62 . .8260 n N2 H63 . .7241 n N2 H64 . .8674 n N3 OW2 2_666 2.825(2) n N3 O13 1_655 2.923(2) n N3 O14 2_665 3.101(3) n N3 H71 . .8939 n N3 H72 . .8747 n N3 H73 . .786 n N3 H74 . .9709 n OW3 OW2 1_554 2.8015(19) n OW3 N1 1_655 2.902(2) n OW3 N2 1_554 3.087(2) n OW3 O13 1_655 3.171(2) n OW3 H31 . .8368 n OW3 H32 . .9536 n OW4 O22 2_655 2.9263(14) n OW4 O24 2_656 2.9740(13) n OW4 O24 1_554 2.9740(13) n OW4 O2 2_655 2.9904(12) n OW4 O21 2_656 3.1926(12) n OW4 O21 1_554 3.1926(12) n OW4 H41 . .8936 n OW4 H42 . .8822 n _cod_database_code 2011595