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  • 1.
    Kapilashrami, Mukes
    et al.
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering.
    Rao, K Venkat
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering, Engineering Material Physics.
    Belova, Lyuba
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering, Engineering Material Physics.
    Kloo, Lars
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Inorganic Chemistry.
    Åkerstedt, Josefin
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Inorganic Chemistry.
    Defect induced magnetic anisotropy in undopted ZnO thin filmsArticle in journal (Other academic)
  • 2.
    Åkerstedt, Josefin
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Applied Physical Chemistry.
    Subvalent Cluster Compounds and Synthesis in Alternative Reaction Media2012Doctoral thesis, comprehensive summary (Other academic)
    Abstract [en]

    With the aim of finding alternative reaction media for the synthesis of subvalent main group and transition metal cluster compounds, traditionally made through solid state reactions or in superacidic media, different alternative reaction media have been explored in this work. Room-temperature ionic liquids are amongst the more unconventional reaction media used. The syntheses performed have been aimed at both anionic and cationic cluster and the main tools used for characterization have been different X-ray diffraction and spectroscopic techniques.

    Selected ionic liquids have along with dichloromethane been shown to work as alternative reaction media for room temperature synthesis of the Bi5[GaCl4]3 salt. The salt containing the subvalent naked bismuth polycation Bi5 3+ was isolated from reduction reactions of BiCl3 in Ga/GaCl3-dichloromethane respectively Ga/GaCl3-ioinc liquid media. Three different classes of ionic liquids based on phosphonium-, imidazolium- and pyrrolidinium- salts have been used in synthesis. Homopolyatomic clusters from the lighter Group 15 element arsenic have also been studied. Solutions from the oxidative and reductive reaction routes of arsenic and AsCl3 in Lewis acidic toluene media were studied by EXAFS spectroscopy. The results were evaluated using molecular dynamics simulations of arsenic clusters. A discussion on how the calculated As4 cluster model relates to the experimental data resulted from this study.

    In terms of homopolyatomic anionic clusters the [K+(2,2,2-crypt)]2Ge9 2- compound containing the naked Ge9 2- anionic cluster has been isolated. The crystallographic investigation of [K+(2,2,2-crypt)]2Ge9 2- shows Zintl cluster anion Ge9 2- to be tricapped trigonal-prismatic with a symmetry very close to D3h. A chemical bonding analysis reveals two local minima of D3h symmetry and the cluster interaction scheme to be based on highly delocalised bonding.

    Ligand supported transition metal clusters from tungsten and palladium have also been prepared. Reduction of WCl6 in a reaction mixture of ionic liquid and co-solvent toluene resulted in tritungsten decachloride; W3Cl10(MeCN)3, being formed. Furthermore, palladium sandwich compounds; [Pd2(Ga2Cl7)(C7H8)2], [Pd2(GaCl4)(C9H12)2]∙C9H12 and [Pd2(Ga2Cl7)(C6H5Cl)2] have been prepared using GaCl3-arene reaction media.

  • 3.
    Åkerstedt, Josefin
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Inorganic Chemistry.
    Tailored Reaction Media for the Synthesis of Subvalent Cluster Compounds2010Licentiate thesis, comprehensive summary (Other academic)
    Abstract [en]

    Different synthetic approaches and modifications to reaction media have been applied in order to find new routes to the synthesis of main-group clusters and transition metal compounds. The focus has been on the Group 15 element bismuth and the transition metal palladium. The reactions performed have mainly been Lewis acid-base reactions and the characterization tools used X-ray diffraction and Raman spectroscopy.

    The Bi5[GaCl4]3 salt, previously known form synthesis using other reaction routes, has been isolated from GaCl3-dichloromethane media. The salt containing the subvalent naked bismuth polycation Bi53+ was isolated from the reduction of bismuth(III) chloride. Quantum chemical calculations on the interaction energies of the isolated bismuth cluster show the dichloromethane-cluster interaction energy to be higher than that between benzene and the cluster.

    Ionic liquids have, in addition to dichloromethane, been shown to work as alternative reaction media for room-temperature synthesis of the Bi5[GaCl4]3 salt. Three different classes of ionic liquids have been used; phosphonium-, imidazolium- and pyrrolidinium-based salts. The ionic liquids used have been treated with Lewis acids in order to promote cluster formation.

    In this work three new palladium sandwich compounds have also been isolated, using GaCl3-arene reaction media; [Pd2(Ga2Cl7)(C7H8)2], [Pd2(GaCl4)(C9H12)2]∙C9H12 and [Pd2(Ga2Cl7)(C6H5Cl)2]. Quantum chemical calculations on these palladium sandwiches show the chlorobenzene sandwiching ligands unexpectedly interacting more strongly with the dipalladium unit than the methyl substituted arenes.

  • 4.
    Åkerstedt, Josefin
    et al.
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Inorganic Chemistry (closed 20110630).
    Gorlov, Mikhail
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Organic Chemistry.
    Fischer, Andreas
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Inorganic Chemistry (closed 20110630).
    Kloo, Lars
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Inorganic Chemistry (closed 20110630).
    Synthesis and characterization of binuclear palladium(I) compounds and the influence of competing arenes2010In: Journal of Organometallic Chemistry, ISSN 0022-328X, E-ISSN 1872-8561, Vol. 695, no 10-11, p. 1513-1517Article in journal (Refereed)
    Abstract [en]

    The binuclear palladium(I) compounds, [Pd-2(Ga2Cl7)(2)(C7H8)(2)] (1), [Pd-2(GaCl4)(2)(C9H12)(2)]center dot C9H12 (2) and [Pd-2(Ga2Cl7)(2)(C6H5Cl)(2)] (3), have been prepared from palladium(II) chloride in gallium(III) chloride-arene reaction media. All isolated crystalline solids (1, 2 and 3) have been structurally characterized by single crystal X-ray diffraction and Raman spectroscopy. The results form quantum chemical calculations on the interaction energies of the arenes and the dipalladium unit of these compounds is also presented.

  • 5.
    Åkerstedt, Josefin
    et al.
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Applied Physical Chemistry.
    Gorlov, Mikhail
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Applied Physical Chemistry.
    Kloo, Lars
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Applied Physical Chemistry.
    Room-Temperature Synthesis of the Bi-5[GaCl4](3) Salt From Three Different Classes of Ionic Liquids2013In: Journal of cluster science, ISSN 1040-7278, E-ISSN 1572-8862, Vol. 24, no 1, p. 157-164Article in journal (Refereed)
    Abstract [en]

    Following the development in the synthesis of subvalent cluster compounds, we report on the use of three different classes of room-temperature ionic liquids for the synthesis of the pentabismuth-tris(tetragallate) salt, Bi-5[GaCl4](3), characterized by X-ray diffraction. The Bi-5[GaCl4](3) salt was prepared by reduction of BiCl3 using gallium metal in ionic liquid reaction media containing a strong Lewis acid, GaCl3. The ionic liquids; trihexyltetradecyl phosphonium chloride [Th-Td-P+]Cl-, 1-dodecyl-3-methylimidazolium chloride [Dod-Me-Im(+)]Cl- and N-butyl-N-methylpyrrolidinium chloride [Bu-Me-Pyrr(+)]Cl- from three of the main classes of ionic liquids were used in synthesis. Reactions using ionic liquids composed of the trihexyltetradecyl phosphonium cation [Th-Td-P+] and the anions; tetrafluoroborate [BF4 (-)], bis(trifluoro-methyl sulfonyl) imide [(Tf)(2)N-] and hexafluorophosphate [PF6 (-)] were also investigated.

  • 6.
    Åkerstedt, Josefin
    et al.
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Inorganic Chemistry (closed 20110630).
    Gorlov, Mikhail
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Organic Chemistry.
    Kloo, Lars
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Inorganic Chemistry (closed 20110630).
    Synthesis of Bi5[GaCl4]3 from room-temperature ionic liquid reaction mediaManuscript (preprint) (Other academic)
  • 7.
    Åkerstedt, Josefin
    et al.
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Inorganic Chemistry.
    Ponou, Simeon
    Kloo, Lars
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Inorganic Chemistry.
    Lidin, Sven
    Structural Investigation of a Fully Ordered closo-Ge(9)(2-) Cluster in the Compound [K(+)(2,2,2-crypt)](2)Ge(9)(2-)2011In: European Journal of Inorganic Chemistry, ISSN 1434-1948, E-ISSN 1099-1948, no 26, p. 3999-4005Article in journal (Refereed)
    Abstract [en]

    [K(+)(2,2,2-crypt)] (2)Ge(9)(2-) containing the deltahedral Zintl anion Ge(9)(2-) has been isolated from a solution of K(4)Ge(9) in ethylenediamine in the presence of 2,2,2-crypt, intended as an intermediate in mixed-cluster synthesis. The subsequent crystallographic characterisation shows the closo-Ge(9)(2-) cluster unit to be tricapped trigonal-prismatic with a symmetry very close to D(3h). Each Ge(9)(2-) unit is surrounded by two 2,2,2-crypt units, each with a chelated K(+) cation, viz. [K(+)(2,2,2-crypt)]. The structure characterisation of this ordered Ge(9)(2-) cluster is surprisingly enough the first one reported. A chemical bonding analysis reveals two local minima of D(3h) symmetry, with that of lowest energy being highly similar to that resulting from the crystallographic analysis of low-temperature data. The cluster interaction scheme is based on highly delocalised bonding.

  • 8.
    Åkerstedt, Josefin
    et al.
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Applied Physical Chemistry.
    Rosdahl, Jan
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Applied Physical Chemistry.
    Persson, Per
    Umeå University.
    Kloo, Lars
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Applied Physical Chemistry.
    Arsenic Clusters in Solution: An Experimental and A Priori Theoretical EXAFS StudyManuscript (preprint) (Other academic)
  • 9.
    Åkerstedt, Josefin
    et al.
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Applied Physical Chemistry.
    Ruck, M.
    Kloo, Lars
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Applied Physical Chemistry.
    Long, J. R.
    Tungsten Chloride W3Cl10(CH3CN)3 fromRoom-temperature Synthesis in Ionic liquid using an Organic Co-solventManuscript (preprint) (Other academic)
  • 10.
    Åkerstedt, Josefin
    et al.
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Inorganic Chemistry.
    Zaffaroni, Riccardo
    Kloo, Lars
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Inorganic Chemistry.
    Dichloromethane as solvent for the synthesis of polycationic clusters at room temperature: a link to standard organometallic chemistry2010In: Dalton Transactions, ISSN 1477-9226, E-ISSN 1477-9234, Vol. 39, no 35, p. 8132-8134Article in journal (Refereed)
    Abstract [en]

    Dichloromethane (DCM), CH2Cl2 has been identified as an alternative reaction medium for room-temperature synthesis of subvalent homopolyatomic clusters of the group 15 element bismuth.

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