#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2014310.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_2014310 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2006 _journal_volume 62 _journal_page_first m60 _journal_page_last m62 _publ_section_title ;\ Tetrapiperidinium di-\m-methoxy-di-\m~5~-oxo-tetra-\m~3~-oxo-dodeca-\m~2~-oxo-\ octaoxodecavanadate ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' loop_ _publ_author_name 'Fen Sun' 'Yan-Tuan Li' 'Zhi-Yong Wu' 'Da-Qi Wang' 'Jian-Min Dou' _chemical_formula_moiety '4C5 H12 N + , V10 O28 C2 H6 -' _chemical_formula_sum 'C22 H54 N4 O28 V10' _chemical_formula_iupac '(C5 H12 N)4 [V10 (C1 H3 O1)2 O26]' _chemical_formula_weight 1332.09 _symmetry_cell_setting Monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.546(2) _cell_length_b 12.950(3) _cell_length_c 16.033(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.58(3) _cell_angle_gamma 90.00 _cell_volume 2189.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _exptl_crystal_density_diffrn 2.021 _diffrn_ambient_temperature 296(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 0.55955(5) 0.16947(4) 0.34238(3) 0.03288(15) Uani d . 1 . . V V2 0.29905(5) 0.05938(4) 0.40506(3) 0.03148(15) Uani d . 1 . . V V3 0.48827(6) -0.04982(4) 0.28905(3) 0.03491(16) Uani d . 1 . . V V4 0.71648(5) -0.01575(4) 0.40962(3) 0.03057(15) Uani d . 1 . . V V5 0.53063(5) 0.12000(4) 0.52507(3) 0.02620(14) Uani d . 1 . . V O1 0.5892(2) 0.27549(19) 0.29517(15) 0.0455(6) Uani d . 1 . . O O2 0.1520(2) 0.0890(2) 0.40532(15) 0.0469(6) Uani d . 1 . . O O3 0.4734(3) -0.1153(2) 0.20495(14) 0.0503(7) Uani d . 1 . . O O4 0.8654(2) -0.0404(2) 0.41318(15) 0.0454(6) Uani d . 1 . . O O5 0.5439(2) 0.16155(17) 0.62463(13) 0.0343(5) Uani d . 1 . . O O6 0.3717(2) 0.18438(17) 0.35708(13) 0.0354(5) Uani d . 1 . . O O7 0.5255(2) 0.08004(18) 0.25617(13) 0.0358(5) Uani d . 1 . . O O8 0.71665(19) 0.11729(17) 0.36063(13) 0.0333(5) Uani d . 1 . . O O9 0.5617(2) 0.22085(16) 0.46216(13) 0.0341(5) Uani d . 1 . . O O10 0.3178(2) -0.01297(19) 0.31346(13) 0.0381(5) Uani d . 1 . . O O11 0.6598(2) -0.07721(17) 0.31687(13) 0.0350(5) Uani d . 1 . . O O12 0.70014(19) 0.05908(16) 0.52069(13) 0.0291(5) Uani d . 1 . . O O13 0.35043(19) 0.12186(16) 0.51800(13) 0.0289(5) Uani d . 1 . . O O14 0.50738(18) 0.02909(15) 0.41969(12) 0.0259(4) Uani d . 1 . . O C1 0.3118(5) 0.2851(4) 0.3693(3) 0.0753(14) Uani d . 1 . . C H1A 0.2213 0.2772 0.3681 0.113 Uiso calc R 1 . . H H1B 0.3370 0.3311 0.3255 0.113 Uiso calc R 1 . . H H1C 0.3379 0.3130 0.4222 0.113 Uiso calc R 1 . . H N1 0.9223(3) 0.1709(3) 0.5428(2) 0.0550(9) Uani d . 1 . . N H1D 0.9806 0.1201 0.5440 0.066 Uiso calc R 1 . . H H1E 0.8481 0.1432 0.5259 0.066 Uiso calc R 1 . . H C2 0.9617(4) 0.2507(4) 0.4821(3) 0.0681(13) Uani d . 1 . . C H2A 0.9626 0.2209 0.4266 0.082 Uiso calc R 1 . . H H2B 1.0471 0.2735 0.4956 0.082 Uiso calc R 1 . . H C3 0.8744(5) 0.3413(4) 0.4826(3) 0.0674(12) Uani d . 1 . . C H3A 0.7912 0.3200 0.4628 0.081 Uiso calc R 1 . . H H3B 0.9059 0.3937 0.4449 0.081 Uiso calc R 1 . . H C4 0.8631(5) 0.3867(3) 0.5695(3) 0.0652(12) Uani d . 1 . . C H4A 0.9445 0.4141 0.5875 0.078 Uiso calc R 1 . . H H4B 0.8022 0.4428 0.5688 0.078 Uiso calc R 1 . . H C5 0.8209(4) 0.3045(4) 0.6289(3) 0.0640(12) Uani d . 1 . . C H5A 0.8179 0.3331 0.6847 0.077 Uiso calc R 1 . . H H5B 0.7359 0.2824 0.6136 0.077 Uiso calc R 1 . . H C6 0.9075(4) 0.2132(4) 0.6287(3) 0.0656(13) Uani d . 1 . . C H6A 0.9899 0.2334 0.6506 0.079 Uiso calc R 1 . . H H6B 0.8736 0.1600 0.6648 0.079 Uiso calc R 1 . . H N2 0.8609(3) 0.1875(2) 0.2268(2) 0.0506(8) Uani d . 1 . . N H2C 0.8684 0.2557 0.2364 0.061 Uiso calc R 1 . . H H2D 0.8126 0.1608 0.2674 0.061 Uiso calc R 1 . . H C7 0.9880(4) 0.1401(4) 0.2321(3) 0.0593(11) Uani d . 1 . . C H7A 1.0451 0.1770 0.1955 0.071 Uiso calc R 1 . . H H7B 1.0204 0.1464 0.2887 0.071 Uiso calc R 1 . . H C8 0.9851(5) 0.0301(4) 0.2082(3) 0.0753(14) Uani d . 1 . . C H8A 0.9371 -0.0084 0.2491 0.090 Uiso calc R 1 . . H H8B 1.0710 0.0031 0.2082 0.090 Uiso calc R 1 . . H C9 0.9248(6) 0.0149(4) 0.1214(3) 0.0876(17) Uani d . 1 . . C H9A 0.9754 0.0491 0.0795 0.105 Uiso calc R 1 . . H H9B 0.9206 -0.0581 0.1080 0.105 Uiso calc R 1 . . H C10 0.7934(5) 0.0603(4) 0.1226(3) 0.0785(15) Uani d . 1 . . C H10A 0.7545 0.0524 0.0679 0.094 Uiso calc R 1 . . H H10B 0.7423 0.0226 0.1623 0.094 Uiso calc R 1 . . H C11 0.7948(4) 0.1724(3) 0.1457(3) 0.0602(11) Uani d . 1 . . C H11A 0.8375 0.2117 0.1028 0.072 Uiso calc R 1 . . H H11B 0.7084 0.1976 0.1495 0.072 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 V1 0.0343(3) 0.0323(3) 0.0321(3) 0.0013(2) 0.0042(2) 0.0060(2) V2 0.0240(3) 0.0392(3) 0.0311(3) 0.0025(2) -0.0030(2) 0.0046(2) V3 0.0400(3) 0.0383(3) 0.0263(3) -0.0009(3) -0.0003(2) -0.0031(2) V4 0.0235(3) 0.0373(3) 0.0310(3) 0.0028(2) 0.0041(2) 0.0030(2) V5 0.0262(3) 0.0250(3) 0.0274(3) -0.0012(2) 0.0007(2) -0.0020(2) O1 0.0525(15) 0.0389(14) 0.0451(14) -0.0004(12) 0.0047(11) 0.0105(11) O2 0.0271(12) 0.0667(17) 0.0466(14) 0.0085(12) -0.0058(10) 0.0084(13) O3 0.0632(17) 0.0550(16) 0.0328(13) -0.0058(13) -0.0003(12) -0.0105(12) O4 0.0258(12) 0.0628(17) 0.0476(14) 0.0078(11) 0.0059(10) 0.0110(12) O5 0.0385(13) 0.0313(12) 0.0329(12) -0.0032(10) -0.0011(9) -0.0045(10) O6 0.0348(12) 0.0352(12) 0.0363(12) 0.0074(10) 0.0006(9) 0.0092(10) O7 0.0372(13) 0.0424(13) 0.0279(11) 0.0016(10) -0.0002(9) 0.0061(10) O8 0.0276(11) 0.0378(13) 0.0345(12) -0.0033(9) 0.0047(9) 0.0054(10) O9 0.0383(13) 0.0277(12) 0.0365(12) -0.0037(10) 0.0030(9) 0.0008(9) O10 0.0328(12) 0.0499(14) 0.0314(12) -0.0056(11) -0.0062(9) 0.0008(10) O11 0.0370(13) 0.0385(13) 0.0297(11) 0.0051(10) 0.0063(9) -0.0007(10) O12 0.0226(10) 0.0328(12) 0.0318(11) -0.0036(9) -0.0026(8) 0.0020(9) O13 0.0263(11) 0.0293(11) 0.0311(11) 0.0045(9) 0.0020(8) 0.0006(9) O14 0.0231(10) 0.0297(11) 0.0249(10) -0.0006(9) 0.0000(8) 0.0011(9) C1 0.067(3) 0.067(3) 0.092(4) 0.010(2) 0.015(3) 0.013(3) N1 0.0315(16) 0.050(2) 0.084(2) 0.0024(14) -0.0167(16) -0.0081(18) C2 0.056(3) 0.084(3) 0.064(3) -0.004(2) 0.018(2) -0.013(3) C3 0.081(3) 0.065(3) 0.056(3) 0.008(2) 0.006(2) 0.009(2) C4 0.074(3) 0.049(3) 0.072(3) 0.004(2) 0.005(2) -0.007(2) C5 0.053(3) 0.088(3) 0.051(2) -0.021(2) 0.0053(19) -0.025(2) C6 0.064(3) 0.072(3) 0.060(3) -0.020(2) -0.021(2) 0.011(2) N2 0.0508(19) 0.0467(19) 0.0547(19) -0.0080(15) 0.0131(15) 0.0082(15) C7 0.055(3) 0.067(3) 0.056(2) 0.003(2) 0.0013(19) 0.013(2) C8 0.087(4) 0.061(3) 0.079(3) 0.017(3) 0.007(3) 0.016(3) C9 0.131(5) 0.053(3) 0.080(4) 0.008(3) 0.021(3) -0.009(3) C10 0.092(4) 0.075(3) 0.069(3) -0.027(3) -0.011(3) 0.001(3) C11 0.052(2) 0.067(3) 0.061(3) -0.003(2) -0.001(2) 0.014(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 V1 O1 . 1.600(2) y V1 O6 . 2.007(2) y V1 O7 . 1.836(2) y V1 O8 . 1.810(2) y V1 O9 . 2.033(2) y V1 O14 . 2.271(2) y V2 O2 . 1.598(2) y V2 O6 . 1.952(2) y V2 O10 . 1.755(2) y V2 O12 3_656 1.942(2) y V2 O13 . 2.051(2) y V2 O14 . 2.242(2) y V3 O3 . 1.600(2) y V3 O5 3_656 2.033(2) y V3 O7 . 1.807(2) y V3 O10 . 1.904(2) y V3 O11 . 1.893(2) y V3 O14 . 2.337(2) y V4 O4 . 1.603(2) y V4 O8 . 1.893(2) y V4 O11 . 1.784(2) y V4 O12 . 2.036(2) y V4 O13 3_656 1.936(2) y V4 O14 . 2.288(2) y V5 O5 . 1.689(2) y V5 O9 . 1.684(2) y V5 O12 . 1.956(2) y V5 O13 . 1.903(2) y V5 O14 . 2.072(2) y V5 O14 3_656 2.163(2) y O6 C1 . 1.463(5) ? C1 H1A . 0.9600 ? C1 H1B . 0.9600 ? C1 H1C . 0.9600 ? N1 C2 . 1.482(6) ? N1 C6 . 1.491(6) ? N1 H1D . 0.9000 ? N1 H1E . 0.9000 ? C2 C3 . 1.491(6) ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? C3 C4 . 1.517(6) ? C3 H3A . 0.9700 ? C3 H3B . 0.9700 ? C4 C5 . 1.498(6) ? C4 H4A . 0.9700 ? C4 H4B . 0.9700 ? C5 C6 . 1.494(6) ? C5 H5A . 0.9700 ? C5 H5B . 0.9700 ? C6 H6A . 0.9700 ? C6 H6B . 0.9700 ? N2 C7 . 1.476(5) ? N2 C11 . 1.481(5) ? N2 H2C . 0.9000 ? N2 H2D . 0.9000 ? C7 C8 . 1.475(6) ? C7 H7A . 0.9700 ? C7 H7B . 0.9700 ? C8 C9 . 1.538(7) ? C8 H8A . 0.9700 ? C8 H8B . 0.9700 ? C9 C10 . 1.505(7) ? C9 H9A . 0.9700 ? C9 H9B . 0.9700 ? C10 C11 . 1.499(6) ? C10 H10A . 0.9700 ? C10 H10B . 0.9700 ? C11 H11A . 0.9700 ? C11 H11B . 0.9700 ? _cod_database_code 2014310