Trifluoromethanesulfonate

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  • hydration and hydrolysis of thorium iv in aqueous solution and the structures of two crystalline thorium iv hydrates
    Inorganic Chemistry, 2009
    Co-Authors: Natallia Torapava, Lars Eriksson, Ingmar Persson, Daniel Lundberg
    Abstract:

    Solid octaaqua(κ2O-perchlorato)thorium(IV) perchlorate hydrate, [Th(H2O)8(ClO4)](ClO4)3·H2O, 1, and aquaoxonium hexaaquatris(κO-trifluoromethanesulfonato)thorium(IV) trisaquahexakis(κO-trifluoromethanesulfonato)thorinate(IV), H5O2[Th(H2O)6(OSO2CF3)3][Th(H2O)3(OSO2CF3)6], 2, were crystallized from concentrated perchloric and trifluoromethanesulfonic acid solutions, respectively. 1 adopts a severely distorted tricapped trigonal prismatic configuration with an additional oxygen from the perchlorate ion at a longer distance. 2 consists of individual hexaaquatris(κO-trifluoromethanesulfonato)thorium(IV) and trisaquahexakis(κO-trifluoromethanesulfonato)thorinate(IV) ions and an aquaoxonium ion bridging these two ions through hydrogen bonding. The hydrated thorium(IV) ion is nine-coordinated in aqueous solution as determined by extended X-ray absorption fine structure (EXAFS) and large angle X-ray scattering (LAXS). The LAXS studies also showed a second hydration sphere of about 18 water molecules, and traces of...

  • a structural study of the hydrated and the dimethylsulfoxide n n dimethylpropyleneurea acetonitrile pyridine and n n dimethylthioformamide solvated nickel ii ion in solution and solid state
    Inorganica Chimica Acta, 2003
    Co-Authors: Olof Kristiansson, Ingmar Persson, Dorota Bobicz
    Abstract:

    Abstract The structure of the solvated nickel(II) ion has been studied in solution by EXAFS in a series of solvents with different coordinating properties. The solvents studied are water, dimethylsulfoxide, N,N′-dimethylpropyleneurea (oxygen donors), acetonitrile, pyridine (nitrogen donors) and N,N-dimethylthioformamide (sulfur donor). A number of solid solvate structures has been determined crystallographically, hexakis(dimethylsulfoxide)nickel(II) perchlorate, [Ni(OS(CH3)2)6](ClO4)2, tetrakis(dimethylsulfoxide)bis(N,N′-dimethylpropyleneurea)nickel(II) perchlorate, [Ni(OS(CH3)2)4(OCN2(CH3)2(CH2)3)2](ClO4)2, tetrakis(pyridine)bis(trifluoromethanesulfonato)nickel(II), [Ni(NC5H5)4(O3SCF3)2], bisaquatetrakis(pyridine)nickel(II) perchlorate pyridine solvate, Ni(NC5H5)4(OH2)2(ClO4)2·C5H5N, and hexakis(N,N-dimethylthioformamide)nickel(II) perchlorate, [Ni(SCHN(CH3)2)6](ClO4)2, in order to be used as model compounds in the EXAFS studies of the solutions. The hydrated and the dimethylsulfoxide, acetonitrile and N,N-dimethylthioformamide solvated nickel(II) ions are all octahedral in solution with Nisolvent bond distances of 2.055(2), 2.064(2), 2.062(2) and 2.454(2) A, respectively. Pyridine has too low permittivity to allow dissociation of nickel(II) salts. The nickel(II) Trifluoromethanesulfonate complex is solvated by four pyridines in the equatorial plane with two oxygen atoms from the Trifluoromethanesulfonate anions in the axial positions completing the octahedron, and the perchlorate salt takes up water very easily, forming a bisaqua(tetrakispyridine)nickel(II) solvate in both solid state and pyridine solution. The NiN and NiO bond distances are approximately 2.10 A in these complexes. The nickel(II) ion is five-coordinated, probably in square-pyramidal fashion, in N,N′-dimethylpropyleneurea with a mean NiO bond distance of 2.000(2) A. The reason for this lower coordination number is certainly sterical due to the bulkiness of the N,N′-dimethylpropyleneurea molecule. The octahedral complexes with oxygen and sulfur donor solvents are green, while with nitrogen donor solvents they are blue due to different ligand field splitting ability versus the nickel(II) ion. The five-coordinated N,N′-dimethylpropyleneurea solvated nickel(II) ion has a deep red color.

  • Structure and bonding of bisaquamercury(II) and trisaquathallium(III) Trifluoromethanesulfonate
    J. Chem. Soc. Dalton Trans., 2002
    Co-Authors: Alireza Molla-abbassi, Lars Eriksson, János Mink, Ingmar Persson, Magnus Sandström, Mikhail Yu. Skripkin, Ann-sofi Ullström, Patric Lindqvist-reis
    Abstract:

    The structure and bonding in bisaquamercury(II) Trifluoromethanesulfonate, [Hg(OH2)2(CF3SO3)2]∞, and trisaquathallium(III) Trifluoromethanesulfonate, [Tl(OH2)3(CF3SO3)3], have been studied by means of single-crystal X-ray diffraction, EXAFS and vibrational spectroscopy. The crystal structure of bisaquamercury(II) Trifluoromethanesulfonate shows an unusual connectivity pattern. The mercury(II) ion strongly binds two water molecules axially with the Hg–O bond distance 2.11 A, and four oxygen atoms from four Trifluoromethanesulfonate ions complete a tetragonally compressed octahedral coordination geometry, at the mean Hg–O distance 2.53 A. Two Trifluoromethanesulfonate ions form double bridges between the bisaquamercury(II) entities giving rise to infinite >Hg(OH2)2 Hg(OH2)2< chains. The parallel chains are held together in layers by relatively strong hydrogen bonds with O(–H)⋯O distances in the range 2.688(9)–2.735(9) A. The O–D stretching vibrational frequencies of the hydrogen bonds in the partly deuterated compound occur in a broad band at about 2400 cm−1, bandwidth ca. 170 cm−1. The layers are connected only via van der Waals interactions between the protruding CF3 groups, consistent with the fragile sheet-like structure of the crystalline compound. Trisaquathallium(III) Trifluoromethanesulfonate crystallises as molecular complexes where each thallium(III) ion binds three water molecules and three oxygen atoms from Trifluoromethanesulfonate ions, with Tl–O bond distances in the range 2.18–2.24 A. A hydrogen bond network between the water molecules and Trifluoromethanesulfonate ions with O(–H)⋯O distances in the range 2.65(1)–2.80(1) A holds the structure together. Raman and infrared spectra have been recorded and analysed. The changes in force constants and vibrational frequencies have been correlated with bond lengths for the S–O bond in the coordinated Trifluoromethanesulfonate ion and for the Hg–O and Tl–O bonds, also including the hexaaquaions in the comparisons.

  • crystal structure of n n dimethylthioformamide solvates of the divalent group 12 ions with linear coordination geometry for mercury ii tetrahedral for zinc ii and octahedral for cadmium ii
    Inorganic Chemistry, 1997
    Co-Authors: M Sandstrom, Christina M V Stalhandske, Ingmar Persson
    Abstract:

    : The crystalline solvates of the divalent group 12 metal ions with the soft sulfur donor N,N-dimethylthioformamide display an unusual variation in coordination number and geometry with two, four, and six ligands attached to the mercury(II), zinc(II), and cadmium(II), ions, respectively. Bis(N,N-dimethylthioformamide)mercury(II) perchlorate precipitates from acetonitrile solution when adding less than 2 equiv of N,N-dimethylthioformamide, while the zinc and cadmium solvates crystallize from saturated N,N-dimethylthioformamide solutions. The disolvate [Hg(SCHN(CH(3))(2))(2)](ClO(4))(2) crystallizes in the monoclinic space group P2(1)/n (No. 14) with a = 6.208(1) A, b = 15.239(7) A, c = 8.681(2) A, beta = 99.30(3) degrees, and Z = 2. Centrosymmetric mercury(II) complexes with strong collinear bonds to two N,N-dimethylthioformamide molecules, Hg-S 2.350(2) A, are joined by double bridges of perchlorate ions in chains along the a-axis by four weak interactions between the mercury and the perchlorate oxygen atoms, mean Hg-O distance 2.84 A. Tetrakis(N,N-dimethylthioformamide)zinc Trifluoromethanesulfonate, [Zn(SCHN(CH(3))(2))(4)](CF(3)SO(3))(2), crystallizes in the triclinic space group Po (No. 2) with a = 10.487(3) A, b = 12.910(3) A, c = 13.489(5) A, alpha = 68.800(4) degrees, beta = 69.260(4) degrees, gamma = 74.06(1) degrees, and Z = 2, with the zinc ions tetrahedrally surrounded by four N,N-dimethylthioformamide ligands, mean Zn-S distance 2.34 A. Also the cadmium solvate of corresponding composition, [Cd(SCHN(CH(3))(2))(4)(CF(3)SO(3))(2)], crystallizes in the space group Po, with a = 8.670(1) A, b = 9.529(1) A, c = 10.685(1) A, alpha = 75.20(1) degrees, beta = 66.97(1) degrees, gamma = 65.31(1) degrees, and Z = 1, although the structure comprises centrosymmetric tetrakis(N,N-dimethylthioformamide)bis(trifluoromethanesulfonato)cadmium(II) complexes in which four Cd-S bonds (mean 2.65 A) and two weaker Cd-O bonds at 2.470(2) A to the Trifluoromethanesulfonate ions give rise to a pseudo-octahedral coordination around the cadmium ion. When using perchlorate instead as counterion, hexakis(N,N-dimethylthioformamide)cadmium perchlorate, [Cd(SCHN(CH(3))(2))(6)](ClO(4))(2), crystallizes in the space group P2(1)/n with a = 12.757(1) A, b = 7.4681(6) A, c = 19.732(2) A, beta = 96.31(1) degrees, and Z = 2. The mean Cd-S bond distance increases to 2.715 A in the fully solvated cadmium ion with almost regular octahedral coordination geometry to its six centrosymmetrically related ligands. The effect of the weak internal hydrogen bonding occuring between the hydrogen atom of a -CHS group and the sulfur atom of neighboring N,N-dimethylthioformamide ligands is discussed.

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