#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2008204.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_2008204 _journal_name_full 'Acta Crystallographica' _journal_year 1999 _journal_volume C55 _journal_page_first 370 _journal_page_last 372 _publ_section_title ; Di-\m-oxo-bis[(2,2'-bipyridine)(difluoroacetato)oxomolybdenum(V)] dihydrate ; loop_ _publ_author_name 'Webb, Thomas R.' 'Talbott, E. Shane' _chemical_formula_sum 'C24 H22 F4 Mo2 N4 O10' _chemical_formula_structural 'Mo2 O4 (C10 H8 N2)2 (O2 C2 H F2)2 (O H2)2' _chemical_formula_iupac '[Mo2 O4 (C2 HF2 O2)2 (C10 H8 N2)2], 2H2O' _chemical_formula_weight 794.34 _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 16.734(3) _cell_length_b 10.267(2) _cell_length_c 17.173(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.34(2) _cell_angle_gamma 90.00 _cell_volume 2766.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _exptl_crystal_density_diffrn 1.907 _diffrn_ambient_temperature 294(2) _refine_ls_R_factor_obs 0.024 _refine_ls_wR_factor_obs 0.056 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 Mo1 0.009470(10) 0.29043(2) 0.179170(10) 0.02557(9) Uani d . 1 . Mo O1 0.08812(11) 0.2521(2) 0.28762(11) 0.0295(4) Uani d . 1 . O O2 0.00217(13) 0.4514(2) 0.15719(12) 0.0388(5) Uani d . 1 . O N1 0.01630(14) 0.0689(2) 0.15606(14) 0.0282(5) Uani d . 1 . N C1 0.0733(2) -0.0115(3) 0.2084(2) 0.0368(7) Uani d . 1 . C H1A 0.1150 0.0236 0.2548 0.044 Uiso calc R 1 . H C2 0.0723(2) -0.1434(3) 0.1959(2) 0.0434(8) Uani d . 1 . C H2A 0.1118 -0.1969 0.2339 0.052 Uiso calc R 1 . H C3 0.0123(2) -0.1954(3) 0.1265(2) 0.0455(8) Uani d . 1 . C H3A 0.0096 -0.2849 0.1175 0.055 Uiso calc R 1 . H C4 -0.0439(2) -0.1137(3) 0.0705(2) 0.0400(7) Uani d . 1 . C H4A -0.0832 -0.1469 0.0218 0.048 Uiso calc R 1 . H C5 -0.0414(2) 0.0183(3) 0.0870(2) 0.0291(6) Uani d . 1 . C C6 -0.0987(2) 0.1147(3) 0.0306(2) 0.0294(6) Uani d . 1 . C C7 -0.1647(2) 0.0815(3) -0.0417(2) 0.0419(7) Uani d . 1 . C H7A -0.1766 -0.0057 -0.0556 0.050 Uiso calc R 1 . H C8 -0.2127(2) 0.1775(4) -0.0928(2) 0.0480(8) Uani d . 1 . C H8A -0.2572 0.1561 -0.1412 0.058 Uiso calc R 1 . H C9 -0.1938(2) 0.3037(4) -0.0710(2) 0.0482(8) Uani d . 1 . C H9A -0.2247 0.3702 -0.1051 0.058 Uiso calc R 1 . H C10 -0.1283(2) 0.3329(3) 0.0020(2) 0.0413(7) Uani d . 1 . C H10A -0.1162 0.4198 0.0165 0.050 Uiso calc R 1 . H N2 -0.08165(14) 0.2404(2) 0.05277(13) 0.0291(5) Uani d . 1 . N O3 0.10958(13) 0.2688(2) 0.12960(12) 0.0359(5) Uani d . 1 . O C11 0.1742(2) 0.3433(3) 0.1480(2) 0.0344(6) Uani d . 1 . C O4 0.1975(2) 0.4261(3) 0.20127(15) 0.0548(6) Uani d . 1 . O C12 0.2267(2) 0.3181(3) 0.0921(2) 0.0396(7) Uani d . 1 . C H12A 0.2474 0.2280 0.0983 0.048 Uiso calc R 1 . H F1 0.17797(14) 0.3424(2) 0.01230(12) 0.0614(6) Uani d . 1 . F F2 0.29258(13) 0.4020(2) 0.10945(14) 0.0648(6) Uani d . 1 . F O5 0.1546(2) 0.5853(3) 0.3156(2) 0.0708(8) Uani d . 1 . O H5A 0.160(3) 0.540(5) 0.277(3) 0.091(17) Uiso d . 1 . H H5B 0.102(4) 0.573(7) 0.319(4) 0.15(3) 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 Mo1 0.02441(13) 0.02895(14) 0.02338(13) -0.00185(10) 0.00836(9) -0.00012(10) O1 0.0237(9) 0.0381(11) 0.0250(9) -0.0012(8) 0.0065(8) -0.0012(8) O2 0.0444(12) 0.0336(11) 0.0386(11) -0.0022(9) 0.0147(10) 0.0027(9) N1 0.0257(12) 0.0315(12) 0.0284(12) 0.0005(10) 0.0106(10) 0.0014(10) C1 0.034(2) 0.044(2) 0.033(2) 0.0059(14) 0.0126(13) 0.0017(14) C2 0.047(2) 0.041(2) 0.047(2) 0.014(2) 0.022(2) 0.0081(15) C3 0.053(2) 0.030(2) 0.063(2) 0.0019(14) 0.032(2) -0.003(2) C4 0.040(2) 0.037(2) 0.048(2) -0.0088(14) 0.0214(14) -0.0111(14) C5 0.0261(14) 0.0339(15) 0.0317(14) -0.0033(12) 0.0156(12) -0.0012(12) C6 0.0246(13) 0.040(2) 0.0258(13) -0.0055(12) 0.0115(11) -0.0019(12) C7 0.038(2) 0.052(2) 0.033(2) -0.0090(15) 0.0090(14) -0.0064(14) C8 0.037(2) 0.070(2) 0.031(2) -0.001(2) 0.0040(13) -0.001(2) C9 0.043(2) 0.062(2) 0.034(2) 0.014(2) 0.0055(14) 0.010(2) C10 0.043(2) 0.043(2) 0.036(2) 0.0056(14) 0.0107(14) 0.0039(14) N2 0.0276(12) 0.0358(13) 0.0230(11) 0.0003(10) 0.0078(9) 0.0013(10) O3 0.0351(11) 0.0414(12) 0.0367(11) -0.0093(9) 0.0196(9) -0.0062(9) C11 0.034(2) 0.040(2) 0.0316(15) -0.0037(13) 0.0146(13) 0.0021(13) O4 0.0514(14) 0.067(2) 0.0517(14) -0.0233(13) 0.0253(12) -0.0239(13) C12 0.035(2) 0.041(2) 0.047(2) -0.0061(13) 0.0199(14) 0.0011(14) F1 0.0663(13) 0.084(2) 0.0402(11) -0.0104(12) 0.0268(10) -0.0050(10) F2 0.0479(12) 0.079(2) 0.0780(15) -0.0242(11) 0.0357(11) -0.0111(12) O5 0.083(2) 0.057(2) 0.072(2) -0.010(2) 0.026(2) -0.021(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 O2 . 1.690(2) y Mo1 O1 . 1.911(2) y Mo1 O1 2 1.948(2) y Mo1 O3 . 2.138(2) y Mo1 N2 . 2.236(2) y Mo1 N1 . 2.318(2) y Mo1 Mo1 2 2.5601(7) y O1 Mo1 2 1.948(2) n N1 C1 . 1.343(4) no N1 C5 . 1.347(3) no C1 C2 . 1.370(4) no C2 C3 . 1.372(5) no C3 C4 . 1.372(5) no C4 C5 . 1.382(4) no C5 C6 . 1.480(4) no C6 N2 . 1.348(4) no C6 C7 . 1.388(4) no C7 C8 . 1.377(5) no C8 C9 . 1.356(5) no C9 C10 . 1.381(4) no C10 N2 . 1.341(4) no O3 C11 . 1.271(3) no C11 O4 . 1.210(4) no C11 C12 . 1.532(4) no C12 F2 . 1.348(3) no C12 F1 . 1.353(4) no