#------------------------------------------------------------------------------ #$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2007290.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_2007290 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1998 _journal_volume 54 _journal_page_first 616 _journal_page_last 618 _publ_section_title ; [Ni(C~10~H~8~N~2~)~3~]~2~[V~4~O~12~].11H~2~O ; _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _[local]_cod_cif_authors_sg_H-M 'C 2/c' loop_ _publ_author_name 'Guo-Yu Yang' 'Da-Wei Gao' 'Ying Chen' 'Ji-Qing Xu' 'Qing-Xin Zeng' 'Hao-Ran Sun' 'Zhi-Wu Pei' 'Qiang Su' 'Yan Xing' 'Yong-Hua Ling' 'Heng-Qing Jia' _chemical_formula_sum 'C60 H70 N12 Ni2 O23 V4' _chemical_formula_iupac '[Ni(C10 H8 N2)3]2 [V4 O12], 11H2 O' _chemical_formula_weight 1648.46 _symmetry_cell_setting 'monoclinic' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.880(2) _cell_length_b 13.9180(10) _cell_length_c 23.829(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.7450(10) _cell_angle_gamma 90.00 _cell_volume 6984.30(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.568 _diffrn_ambient_temperature 293(2) _refine_ls_R_factor_obs .0376 _refine_ls_wR_factor_obs .1016 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 Ni .16925(2) .46406(3) .26626(2) .02796(12) Uani d . 1 . Ni V1 .0757(3) 1.12991(4) .50351(2) .03257(15) Uani d . 1 . V V2 .03738(3) .93195(4) .42380(2) .03269(15) Uani d . 1 . V O1 .15113(12) 1.1235(2) .53544(11) .0616(8) Uani d . 1 . O O2 .05913(14) 1.2414(2) .48286(11) .0557(7) Uani d . 1 . O O3 .09634(12) .8633(2) .45894(12) .0574(7) Uani d . 1 . O O4 .02408(13) .9125(2) .35370(10) .0517(6) Uani d . 1 . O O5 -.03207(11) .9043(2) .44605(10) .0473(6) Uani d . 1 . O O6 .05479(12) 1.0561(2) .43892(10) .0454(6) Uani d . 1 . O N1 .12319(12) .5412(2) .31785(11) .0310(6) Uani d . 1 . N N2 .1442(2) .5910(2) .21775(10) .0338(6) Uani d . 1 . N N3 .25870(12) .5172(2) .30818(11) .0324(6) Uani d . 1 . N N4 .22366(13) .4107(2) .21224(11) .0346(6) Uani d . 1 . N N5 .17890(12) .3378(2) .31580(10) .0318(6) Uani d . 1 . N N6 .08916(12) .3871(2) .22130(10) .0306(6) Uani d . 1 . N C1 .1150(2) .5132(2) .36911(14) .0407(8) Uani d . 1 . C H1 .1297(2) .4529(2) .38341(14) .080 Uiso calc R 1 . H C2 .0857(2) .5697(3) .4015(2) .0521(10) Uani d . 1 . C H2 .0807(2) .5477(3) .4369(2) .080 Uiso calc R 1 . H C3 .0640(2) .6586(3) .3810(2) .0589(11) Uani d . 1 . C H3 .0438(2) .6977(3) .4021(2) .080 Uiso calc R 1 . H C4 .0724(2) .6893(3) .3285(2) .0525(10) Uani d . 1 . C H4 .0582(2) .7498(3) .3140(2) .080 Uiso calc R 1 . H C5 .10215(15) .6291(2) .29766(13) .0347(7) Uani d . 1 . C C6 .1135(2) .6568(2) .24160(13) .0349(7) Uani d . 1 . C C7 .0937(2) .7432(2) .2143(2) .0495(9) Uani d . 1 . C H7 .0729(2) .7878(2) .2315(2) .080 Uiso calc R 1 . H C8 .1050(2) .7629(3) .1613(2) .0553(10) Uani d . 1 . C H8 .0916(2) .8206(3) .1423(2) .080 Uiso calc R 1 . H C9 .1363(2) .6960(3) .1369(2) .0506(9) Uani d . 1 . C H9 .1449(2) .7077(3) .1013(2) .080 Uiso calc R 1 . H C10 .1547(2) .6117(3) .16630(14) .0439(8) Uani d . 1 . C H10 .1755(2) .5663(3) .14956(14) .080 Uiso calc R 1 . H C11 .2744(2) .5658(2) .35851(15) .0420(8) Uani d . 1 . C H11 .2424(2) .5830(2) .37546(15) .080 Uiso calc R 1 . H C12 .3364(2) .5916(3) .38650(15) .0478(9) Uani d . 1 . C H12 .3458(2) .6249(3) .42165(15) .080 Uiso calc R 1 . H C13 .3835(2) .5669(3) .3612(2) .0475(9) Uani d . 1 . C H13 .4256(2) .5828(3) .3790(2) .080 Uiso calc R 1 . H C14 .3675(2) .5182(3) .3088(2) .0447(9) Uani d . 1 . C H14 .3988(2) .5014(3) .2909(2) .080 Uiso calc R 1 . H C15 .3051(2) .4943(2) .28300(14) .0342(7) Uani d . 1 . C C16 .2844(2) .4407(2) .22731(14) .0341(7) Uani d . 1 . C C17 .3241(2) .4224(3) .1918(2) .0477(9) Uani d . 1 . C H17 .3659(2) .4439(3) .2027(2) .080 Uiso calc R 1 . H C18 .3017(2) .3730(3) .1410(2) .0581(11) Uani d . 1 . C H18 .3278(2) .3615(3) .1167(2) .080 Uiso calc R 1 . H C19 .2399(2) .3404(3) .1260(2) .0566(10) Uani d . 1 . C H19 .2239(2) .3055(3) .0919(2) .080 Uiso calc R 1 . H C20 .2027(2) .3604(3) .16235(15) .0471(9) Uani d . 1 . C H20 .1610(2) .3382(3) .15217(15) .080 Uiso calc R 1 . H C21 .2220(2) .3203(3) .36687(14) .0413(8) Uani d . 1 . C H21 .2534(2) .3659(3) .38130(14) .080 Uiso calc R 1 . H C22 .2217(2) .2380(3) .39874(15) .0494(9) Uani d . 1 . C H22 .2517(2) .2290(3) .43438(15) .080 Uiso calc R 1 . H C23 .1758(2) .1687(3) .3766(2) .0535(10) Uani d . 1 . C H23 .1745(2) .1123(3) .3972(2) .080 Uiso calc R 1 . H C24 .1322(2) .1849(2) .32363(15) .0427(8) Uani d . 1 . C H24 .1017(2) .1389(2) .30755(15) .080 Uiso calc R 1 . H C25 .13451(14) .2705(2) .29465(13) .0319(7) Uani d . 1 . C C26 .08730(14) .2955(2) .23851(12) .0309(7) Uani d . 1 . C C27 .0453(2) .2295(2) .20596(13) .0382(8) Uani d . 1 . C H27 .0444(2) .1668(2) .21919(13) .080 Uiso calc R 1 . H C28 .0042(2) .2579(3) .15320(14) .0422(8) Uani d . 1 . C H28 -.0234(2) .2140(3) .12981(14) .080 Uiso calc R 1 . H C29 .0052(2) .3517(3) .13641(14) .0412(8) Uani d . 1 . C H29 -.0225(2) .3730(3) .10175(14) .080 Uiso calc R 1 . H C30 .0475(2) .4142(2) .17142(13) .0385(8) Uani d . 1 . C H30 .0473(2) .4781(2) .15996(13) .080 Uiso calc R 1 . H OW1 .2501(2) 1.0295(3) .5062(2) .1075(13) Uani d . 1 . O OW2 .0599(2) .4843(2) .0411(2) .0924(12) Uani d . 1 . O OW3 .1405(2) 1.3939(2) .5029(2) .0925(11) Uani d . 1 . O OW4 .2241(2) .8370(3) .50895(14) .0835(10) Uani d . 1 . O OW5 -.07190(15) 1.2835(2) .46639(14) .0721(8) Uani d . 1 . O OW6 0 1.0125(3) .25000 .0593(10) Uani d S 1 . 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 _atom_site_aniso_type_symbol Ni .0298(2) .0289(2) .0250(2) -.0003(2) .0072(2) -.0002(2) Ni V1 .0343(3) .0332(3) .0277(3) -.0015(2) .0042(2) -.0061(2) V V2 .0383(3) .0337(3) .0257(3) -.0021(2) .0082(2) -.0016(2) V O1 .0349(14) .089(2) .054(2) -.0033(15) -.0001(12) -.0064(14) O O2 .080(2) .0340(13) .0493(15) .0022(12) .0111(14) -.0035(13) O O3 .048(2) .058(2) .062(2) .0123(14) .0094(13) .0101(13) O O4 .072(2) .053(2) .0320(12) -.0080(11) .0175(12) -.0010(14) O O5 .0506(15) .055(2) .0393(13) -.0049(12) .0178(11) -.0137(12) O O6 .059(2) .0405(13) .0365(13) -.0076(10) .0136(12) -.0118(12) O N1 .0325(14) .0324(14) .0288(13) -.0002(11) .0093(11) .0032(11) N N2 .040(2) .0318(14) .0285(13) .0026(11) .0079(12) -.0013(12) N N3 .0327(14) .0332(15) .0302(14) -.0020(11) .0067(11) -.0027(11) N N4 .0382(15) .0354(15) .0312(14) -.0035(12) .0113(12) .0003(12) N N5 .0328(14) .0335(14) .0279(13) .0007(11) .0064(11) .0041(12) N N6 .0313(14) .0325(14) .0268(13) -.0003(11) .0059(11) .0007(11) N C1 .049(2) .044(2) .033(2) .0021(15) .017(2) .001(2) C C2 .068(3) .059(2) .037(2) -.004(2) .028(2) .003(2) C C3 .081(3) .052(2) .052(2) -.015(2) .032(2) .012(2) C C4 .064(2) .041(2) .055(2) -.010(2) .021(2) .009(2) C C5 .037(2) .031(2) .035(2) -.0036(13) .0074(14) -.0005(14) C C6 .037(2) .029(2) .034(2) -.0007(14) .0023(14) -.0027(14) C C7 .059(2) .035(2) .050(2) .006(2) .008(2) .010(2) C C8 .062(3) .044(2) .052(2) .017(2) .001(2) .004(2) C C9 .061(2) .051(2) .036(2) .014(2) .008(2) -.006(2) C C10 .055(2) .046(2) .033(2) .004(2) .015(2) -.002(2) C C11 .045(2) .044(2) .038(2) -.007(2) .013(2) -.005(2) C C12 .052(2) .050(2) .037(2) -.005(2) .003(2) -.013(2) C C13 .035(2) .048(2) .053(2) .008(2) .001(2) -.010(2) C C14 .034(2) .050(2) .050(2) .002(2) .013(2) -.004(2) C C15 .038(2) .031(2) .035(2) .0043(14) .0116(15) -.0007(14) C C16 .037(2) .030(2) .036(2) .0034(14) .0130(14) .0045(14) C C17 .047(2) .052(2) .052(2) .000(2) .026(2) .000(2) C C18 .067(3) .067(3) .052(2) -.008(2) .036(2) .003(2) C C19 .072(3) .059(2) .046(2) -.016(2) .029(2) -.003(2) C C20 .053(2) .050(2) .041(2) -.014(2) .017(2) -.008(2) C C21 .039(2) .044(2) .035(2) .005(2) .0012(15) .007(2) C C22 .051(2) .051(2) .040(2) .010(2) .002(2) .011(2) C C23 .064(3) .043(2) .053(2) .019(2) .015(2) .008(2) C C24 .048(2) .034(2) .044(2) .005(2) .011(2) -.002(2) C C25 .032(2) .033(2) .032(2) -.0021(13) .0117(13) .0029(14) C C26 .032(2) .034(2) .028(2) -.0007(13) .0113(13) .0027(14) C C27 .042(2) .039(2) .034(2) -.0062(14) .0106(15) -.006(2) C C28 .041(2) .052(2) .034(2) -.011(2) .0105(15) -.010(2) C C29 .034(2) .058(2) .028(2) -.006(2) .0031(14) -.001(2) C C30 .036(2) .043(2) .034(2) .0022(15) .0038(14) .004(2) C OW1 .070(2) .125(3) .139(4) -.010(3) .049(2) .001(2) O OW2 .147(4) .066(2) .079(2) -.002(2) .056(2) -.008(2) O OW3 .089(3) .060(2) .137(3) .007(2) .044(2) -.011(2) O OW4 .075(2) .107(3) .072(2) .017(2) .027(2) .026(2) O OW5 .080(2) .058(2) .081(2) .014(2) .026(2) .005(2) O OW6 .086(3) .045(2) .057(2) .000 .037(2) .000 O 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 Ni N3 . 2.077(3) yes Ni N6 . 2.085(2) yes Ni N1 . 2.086(2) yes Ni N5 . 2.095(3) yes Ni N2 . 2.101(3) yes Ni N4 . 2.112(2) yes V1 O1 . 1.621(2) yes V1 O2 . 1.638(2) yes V1 O5 5_576 1.790(2) yes V1 O6 . 1.803(2) yes V2 O4 . 1.638(2) yes V2 O3 . 1.641(3) yes V2 O5 . 1.782(2) yes V2 O6 . 1.784(2) yes O5 V1 5_576 1.790(2) yes N1 C1 . 1.340(4) yes N1 C5 . 1.349(4) yes N2 C10 . 1.338(4) yes N2 C6 . 1.349(4) yes N3 C11 . 1.338(4) no N3 C15 . 1.350(4) no N4 C20 . 1.348(4) no N4 C16 . 1.345(4) no N5 C25 . 1.345(4) no N5 C21 . 1.344(4) no N6 C30 . 1.340(4) no N6 C26 . 1.344(4) no C1 C2 . 1.376(5) yes C2 C3 . 1.367(5) yes C3 C4 . 1.382(5) yes C4 C5 . 1.388(5) yes C5 C6 . 1.474(4) yes C6 C7 . 1.380(5) yes C7 C8 . 1.379(5) yes C8 C9 . 1.375(5) yes C9 C10 . 1.370(5) yes C11 C12 . 1.386(5) no C12 C13 . 1.373(5) no C13 C14 . 1.380(5) no C14 C15 . 1.377(5) no C15 C16 . 1.482(4) no C16 C17 . 1.391(4) no C17 C18 . 1.364(5) no C18 C19 . 1.377(6) no C19 C20 . 1.369(5) no C21 C22 . 1.375(5) no C22 C23 . 1.389(5) no C23 C24 . 1.379(5) no C24 C25 . 1.384(4) no C25 C26 . 1.493(4) no C26 C27 . 1.380(4) no C27 C28 . 1.390(5) no C28 C29 . 1.368(5) no C29 C30 . 1.376(5) no _cod_database_code 2007290