#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2202252.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_2202252 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2003 _journal_volume 59 _journal_page_first m162 _journal_page_last m164 _publ_section_title ; Dianilinium tetradecachlorohexamolybdate dihydrate, (PhNH~3~)~2~[(Mo~6~Cl~8~)Cl~6~].2H~2~O ; loop_ _publ_author_name 'Andreas Flemstr\"om ' _chemical_formula_moiety '2C6 H8 N 1+, Mo6 Cl14 2-, 2H2 O1' _chemical_formula_sum 'C12 H20 Cl14 Mo6 N2 O2' _chemical_formula_structural '((Mo6 Cl8) Cl6) (C6 H5 NH3)2 (H2 O)2' _chemical_formula_iupac '2C6 H8 N 1+, Mo6 Cl14 2-, 2H2 O1' _chemical_formula_weight 1296.24 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' 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 20.665(8) _cell_length_b 11.335(3) _cell_length_c 17.347(6) _cell_angle_alpha 90.00 _cell_angle_beta 126.21(5) _cell_angle_gamma 90.00 _cell_volume 3279.(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _exptl_crystal_density_diffrn 2.626 _diffrn_ambient_temperature 293 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 0.425215(18) 0.48452(3) 0.17398(2) 0.02159(12) Uani d . 1 . . Mo Mo2 0.465522(17) 0.36924(3) 0.32710(2) 0.02036(11) Uani d . 1 . . Mo Mo3 0.424981(18) 0.25454(3) 0.17358(2) 0.01952(12) Uani d . 1 . . Mo Cl1 0.39093(5) 0.36952(9) 0.03281(6) 0.0284(2) Uani d . 1 . . Cl Cl2 0.32587(5) 0.36887(9) 0.17906(7) 0.0268(2) Uani d . 1 . . Cl Cl3 0.53322(6) 0.58768(9) 0.17742(7) 0.0303(3) Uani d . 1 . . Cl Cl4 0.46711(5) 0.15080(9) 0.32243(7) 0.0269(2) Uani d . 1 . . Cl Cl5 0.42060(6) 0.36609(11) 0.42975(8) 0.0408(3) Uani d . 1 . . Cl Cl6 0.32670(6) 0.64103(9) 0.07510(8) 0.0404(3) Uani d . 1 . . Cl Cl7 0.32621(6) 0.10384(10) 0.07325(8) 0.0396(3) Uani d . 1 . . Cl N1 0.3396(3) 0.1392(4) -0.5535(4) 0.0649(13) Uani d . 1 . . N HN1 0.3771 0.1192 -0.4930 0.097 Uiso calc R 1 . . H HN2 0.2920 0.1415 -0.5638 0.097 Uiso calc R 1 . . H HN3 0.3508 0.2099 -0.5651 0.097 Uiso calc R 1 . . H C1 0.3376(3) 0.0514(4) -0.6174(4) 0.0452(13) Uani d . 1 . . C C2 0.2847(3) 0.0670(6) -0.7141(5) 0.0632(17) Uani d . 1 . . C H2 0.2508 0.1322 -0.7391 0.095 Uiso calc R 1 . . H C3 0.2825(4) -0.0176(8) -0.7747(5) 0.083(2) Uani d . 1 . . C H3 0.2468 -0.0095 -0.8407 0.125 Uiso calc R 1 . . H C4 0.3337(5) -0.1123(7) -0.7357(7) 0.086(2) Uani d . 1 . . C H4 0.3326 -0.1683 -0.7757 0.129 Uiso calc R 1 . . H C5 0.3858(5) -0.1254(6) -0.6398(6) 0.080(2) Uani d . 1 . . C H5 0.4203 -0.1899 -0.6147 0.120 Uiso calc R 1 . . H C6 0.3883(3) -0.0435(5) -0.5786(5) 0.0560(15) Uani d . 1 . . C H6 0.4236 -0.0529 -0.5127 0.084 Uiso calc R 1 . . H O1 0.4405(4) 0.1188(5) -0.3535(5) 0.1147(18) Uani d D 1 . . O HW1 0.416(5) 0.177(5) -0.345(8) 0.172 Uiso d D 1 . . H HW2 0.417(6) 0.051(4) -0.355(9) 0.172 Uiso d 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 Mo1 0.01705(19) 0.0265(2) 0.0198(2) 0.00297(13) 0.01005(17) 0.00258(13) Mo2 0.01682(18) 0.0287(2) 0.01668(19) -0.00060(13) 0.01050(15) -0.00134(14) Mo3 0.01425(19) 0.0266(2) 0.0154(2) -0.00133(12) 0.00749(16) -0.00139(12) Cl1 0.0223(5) 0.0419(5) 0.0155(5) 0.0024(4) 0.0081(4) 0.0031(4) Cl2 0.0153(4) 0.0383(5) 0.0254(5) 0.0013(4) 0.0112(4) -0.0004(4) Cl3 0.0303(5) 0.0312(5) 0.0322(6) -0.0007(4) 0.0199(5) 0.0072(4) Cl4 0.0248(5) 0.0316(5) 0.0254(5) -0.0023(4) 0.0154(4) 0.0039(4) Cl5 0.0422(6) 0.0602(7) 0.0350(6) -0.0088(5) 0.0311(5) -0.0093(5) Cl6 0.0311(5) 0.0401(6) 0.0478(7) 0.0137(5) 0.0220(5) 0.0169(6) Cl7 0.0306(5) 0.0476(6) 0.0334(6) -0.0150(5) 0.0149(5) -0.0119(5) N1 0.058(3) 0.069(3) 0.091(4) -0.008(2) 0.057(3) -0.003(3) C1 0.036(3) 0.053(3) 0.055(4) -0.008(2) 0.031(3) 0.002(3) C2 0.039(3) 0.079(4) 0.066(5) -0.006(3) 0.028(3) 0.024(3) C3 0.065(4) 0.131(7) 0.050(5) -0.049(5) 0.032(4) -0.005(4) C4 0.102(6) 0.101(6) 0.094(6) -0.048(5) 0.079(5) -0.033(5) C5 0.101(5) 0.071(4) 0.110(7) 0.005(4) 0.086(5) 0.001(4) C6 0.050(3) 0.068(4) 0.054(4) 0.010(3) 0.034(3) 0.022(3) O1 0.115(5) 0.088(3) 0.127(5) 0.008(3) 0.064(4) 0.002(4) 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 Cl6 . 2.4714(15) no Mo1 Cl3 2_655 2.4767(14) no Mo1 Cl1 . 2.4795(13) no Mo1 Cl2 . 2.4809(11) no Mo1 Cl3 . 2.4889(12) no Mo1 Mo3 . 2.6069(8) no Mo1 Mo2 . 2.6158(11) no Mo1 Mo2 2_655 2.6184(9) no Mo1 Mo1 2_655 2.623(2) no Mo2 Cl5 . 2.4467(13) no Mo2 Cl3 2_655 2.4779(12) no Mo2 Cl4 . 2.4782(12) no Mo2 Cl2 . 2.483(2) no Mo2 Cl1 2_655 2.488(2) no Mo2 Mo3 2_655 2.6157(9) no Mo2 Mo3 . 2.6168(11) no Mo2 Mo1 2_655 2.6184(9) no Mo3 Cl7 . 2.4323(15) no Mo3 Cl2 . 2.4725(11) no Mo3 Cl1 . 2.4753(13) no Mo3 Cl4 . 2.4803(14) no Mo3 Cl4 2_655 2.4856(12) no Mo3 Mo2 2_655 2.6157(9) no Mo3 Mo3 2_655 2.633(2) no Cl1 Mo2 2_655 2.488(2) no Cl3 Mo1 2_655 2.4767(14) no Cl3 Mo2 2_655 2.4779(12) no Cl4 Mo3 2_655 2.4856(12) no N1 C1 . 1.472(7) no N1 HN1 . 0.89 no N1 HN2 . 0.89 no N1 HN3 . 0.89 no C1 C2 . 1.368(8) no C1 C6 . 1.370(7) no C2 C3 . 1.405(10) no C2 H2 . 0.93 no C3 C4 . 1.373(11) no C3 H3 . 0.93 no C4 C5 . 1.354(11) no C4 H4 . 0.93 no C5 C6 . 1.388(9) no C5 H5 . 0.93 no C6 H6 . 0.93 no O1 HW1 . 0.90(2) no O1 HW2 . 0.90(2) no