Na12Ge17: A compound with the zintl anions [Ge-4](4-) and [Ge-9](4-) - Synthesis, crystal structure, and Raman spectrum

2003-04-01
CARRILLO-CABRERA, W
GIL, RC
SOMER, M
Persil Çetinkol, Özgül
VON SCHNERING, HG
Na12Ge17 is prepared from the elements at 1025 K in sealed niobium ampoules. The crystal structure reinvestigation reveals a doubling of the unit cell (space group:P2(1)/c; a = 22.117(3) Angstrom, b = 12.803(3) Angstrom, c = 41.557(6) Angstrom, beta = 91.31(2)degrees, Z = 16; Pearson code: mP464), furthermore, weak superstructure reflections indicate an even larger C-centred monoclinic cell. The characteristic structural units are the isolated cluster anions [Ge-9](4-) and [Ge-4](4-) in ratio 1:2, respectively The crystal structure represents a hierarchical cluster replacement structure of the hexagonal Laves phase MgZn2 in which the Mg and Zn atoms are replaced by the Ge-9 and Ge-4 units, respectively The Raman spectrum of Na12Ge17 exhibits the characteristic breathing modes of the constituent cluster anions at v = 274 cm(-1) ([Ge-9](4-)) and v = 222 cm(-1) ([Ge-4](4-)) which may be used for identification of these clusters in solid phases and in solutions. Raman spectra further prove that Na12Ge17 is partial soluble both in ethylenediamine and liquid ammonia. The solution and the solid extract contain solely [Ge-9](4-). The remaining insoluble residue is Na4Ge4. By heating the solvate Na4Ge9(NH3)(n) releases NH3 and decomposes irreversibly at 742 K, yielding Na12Ge17 and Ge.
ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE

Suggestions

Ruthenium(III) acetylacetonate; a homogeneous catalyst in the hydrolysis of sodium borohydride
Keçeli, Ezgi; Özkar, Saim; Department of Chemistry (2006)
Ruthenium(III) acetylacetonate was employed for the first time as homogeneous catalyst in the hydrolysis of sodium borohydride. Ruthenium(III) acetylacetonate was not reduced by sodium borohydride under the experimental conditions and remains unchanged after the catalysis, as shown by FT-IR and UV-Vis spectroscopic characterization. Poisoning experiments with mercury, carbon disulfide or trimethylphosphite provide compelling evidence that ruthenium(III) acetylacetonate is indeed a homogenous catalyst in the...
Rhodium(0) nanoparticles supported on hydroxyapatite: preparation, characterization and catalytic use in hydrogen generation from hydrolysis of hydrazine borane and ammonia borane
Çelik, Derya; Özkar, Saim; Department of Chemistry (2012)
This dissertation presents the preparation and characterization of rhodium(0) nanoparticles supported on hydroxyapatite, and investigation of their catalytic activity in hydrogen generation from the hydrolysis of hydrazine-borane and ammonia-borane. Rh+3 ions were impregnated on hydroxyapatite by ion-exchange; then rhodium(0) nanoparticles supported on hydroxyapatite were formed in-situ during the hydrolysis of hydrazine-borane at room temperature. The rhodium(0) nanoparticles supported on hydroxyapatite we...
Aminophosphine-palladium(II) complexes: Synthsesis, structure and applications in Suzuki and Heck cross-coupling reactions
AYDEMİR, MURAT; BAYSAL, AKIN; ŞAHİN, Ertan; Gumgum, Bahattin; Özkar, Saim (Elsevier BV, 2011-11-30)
Reaction of furfurylamine with 1 or 2 equivalents of PPh2Cl in the presence of Et3N, proceeds under anaerobic conditions in thf to give furfuryl-2-(N-diphenylphosphino)amine, Ph2PNHCH2-C4H3O, 1 and furfuryl-2-(N,N-bis(diphenylphosphino)amine), (Ph2P)(2)NCH2-C4H3O, 2, respectively. The reactions of 1 and 2 with MCl2(cod) (M = Pd, Pt; cod = 1,5-cyclooctadiene) or Pt(CH3)(2)(cod) yield complexes [M(Ph2PNHCH2-C4H3O)(2)Cl-2] (M= Pd 1a, Pt 1b), [Pt(Ph2PNHCH2-C4H3O)(2)(CH3)(2)] (1c), and [M((Ph2P)(2) NCH2-C4H3O)Cl...
ELECTRONIC ABSORPTION AND MAGNETIC CIRCULAR-DICHROISM SPECTRA FOR BINUCLEAR PT2(SO4)4X2N- AND PT2(HPO4)4X2N- IONS IN AQUEOUS-SOLUTION
GOKAGAC, G; ISCI, H; MASON, WR (American Chemical Society (ACS), 1992-05-27)
Electronic absorption and 7-T magnetic circular dichroism (MCD) spectra in the UV-visible region are reported for the binuclear diplatinum(III) ions: Pt2(SO4)4X2n-, n = 2, X = H2O, NH3; n = 4, X = Cl-, Br-, OH-. Pt2(HPO4)4X2n-, n = 2, X = H2O, Me2S; n = 4, X = Cl-, Br-. Both the absorption spectra and the MCD spectra for complexes with the same axial ligand X are similar for oxo-bridging SO42- or HPO42-. However, the MCD spectra show marked differences depending upon the nature of the X ligand. The mos...
Synthesis of ferrocenyl quinolines
Zora, Metin (Elsevier BV, 2008-06-01)
A convenient one-pot synthesis of ferrocenyl-substituted quinolines via a molecular iodine-catalyzed reaction of ferrocenylimines with enolizable aldehydes is reported. First, nucleophilic addition of the in situ generated enol to ferrocenylimine produces beta-anilinopropionaldehyde, which then undergoes intramolecular Friedel-Crafts reaction to give dihydroquinoline derivative. Finally, subsequent dehydration and aerobic oxidation affords ferrocenyl quinolines.
Citation Formats
W. CARRILLO-CABRERA, R. GIL, M. SOMER, Ö. Persil Çetinkol, and H. VON SCHNERING, “Na12Ge17: A compound with the zintl anions [Ge-4](4-) and [Ge-9](4-) - Synthesis, crystal structure, and Raman spectrum,” ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, pp. 601–608, 2003, Accessed: 00, 2020. [Online]. Available: https://hdl.handle.net/11511/48243.