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Arnold M Guloy

Publications and source records attributed to Arnold M Guloy.

10 recordsLinked to original sources

A guest-free germanium clathrate.

The challenges associated with synthesizing expanded semiconductor frameworks with cage-like crystal structures continue to be of interest. Filled low-density germanium and silicon framework structures have distinct properties that address important issues in thermoelectric phonon glass-electron crystals, superconductivity and the possibility of Kondo insulators. Interest in empty framework structures of silicon and germanium is motivated by their predicted wide optical bandgaps of the same magnitude as quantum dots and porous silicon, making them and their alloys promising materials for silicon-based optoelectronic devices. Although almost-empty Na(1-x)Si136 has already been reported, the synthesis of guest-free germanium clathrate has so far been unsuccessful. Here we report the high-yield synthesis and characteristics of germanium with the empty clathrate-II structure through the oxidation of Zintl anions in ionic liquids under ambient conditions. The approach demonstrates the potential of ionic liquids as media for the reactions of polar intermetallic phases.

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Layered organic-based metal iodide-polyiodide with unique mixed-valent gold(I/III) iodide chains.

We report the synthesis, optical spectrum, and crystal and electronic structures of a new organic-inorganic hybrid compound, [(p-NH3C6H4)2CH2]4 [(AuI2)(AuI4)(I2)2(I5)2Cl4], with unique mixed-valent gold(I/III) chains. The chains feature face-shared octahedral [AuIAu(III)I6]2- units and are embedded within polyiodide layers. The new mixed-valent gold iodide crystallizes in the orthorhombic space group Pnnm, with a = 27.0703(2), b = 8.9363(5), c = 18.4280(1) angstroms, Z = 2, and exhibits an optical band gap of 0.53 eV.

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Li17Ag3Sn6: a polar intermetallic pi-system with carbonate-like [AgSn3]11- anions and trefoil aromatic [Ag2Sn3]6- layers.

A new lithium silver stannide, Li17Ag3Sn6, was synthesized from high-temperature reactions of the pure elements in tantalum containers. Its crystal structure, in the space group, P31m, with a = 8.063(3) A, c = 8.509(4) A, Z = 1, features two distinct AgSn-based anionic layers. Defect graphitic layers of Ag2Sn3, with ordered vacancies at one-third of the Ag sites, are alternately stacked with Kagome-like nets of isolated trigonal planar AgSn3 units. Double layers of Li ions are sandwiched between the stacked AgSn-based layers. Theoretical calculations show unusual pi-interactions within both anionic layers, with the trigonal planar [AgSn3]11- units being isoelectronic with CO(3)2-. In addition, the chemical bonding of the layered [Ag2Sn3]6- pi-network features incompletely filled lone-pair Sn states involved in in-plane trefoil aromatic interactions. Transport and magnetic susceptibility measurements on Li17Ag3Sn6 indicate excellent metallic behavior and temperature-independent paramagnetism consistent with results from band structure calculations. The "trefoil" aromaticity, previously postulated for aromatic molecular systems, is finally observed, albeit in a polar intermetallic solid-state structure that lies at the border between metals and nonmetals.

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The role of sequestering agents in the formation and structure of germanium anion cluster polymers.

Large blue-green, transparent crystalline needles of [K-(2,2)diaza-[18]-crown-6]KGe(9).3en are prepared, in high yield, from the reaction of (2,2)diaza[18]-crown-6 in toluene with a solution of "KGe(4)" in ethylenediamine (en). The compound crystallizes in the orthorhombic space group Pnma (a = 10.9763(12) A, b = 27.265(3) A, c = 13.880(1) A; Z = 4). The crystal structure of [K-(2,2)diaza-[18]-crown-6]KGe(9).2en features one-dimensional [KGe(9)](-) bare intermetallic chains formed from the linking, via exo-bonds, of nido-Ge(9)(2-) clusters. Uncomplexed K atoms effectively cap the square bases of the monocapped square antiprismatic [Ge(9)](2-) clusters. The optical band gap of the title compound is 1.25 eV. The use of weaker sequestering agents in the isolation of Ge cluster anions from en solutions provides an additional handle in a controlled molecular route to preparing new low-dimensional Zintl phases.

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Synthesis and structure of Ca(18)Li(5)In(25.07): a novel intergrowth of Li-centered in(12) icosahedral clusters and electron-precise Zintl layers.

A new ternary polar intermetallic, Ca(18)Li(5)In(25.07), was obtained from high-temperature reactions of the elements in welded Nb tubes. Its crystal structure, established by single-crystal X-ray diffraction, was found to crystallize in the orthorhombic space group Cmmm (No. 65). Unit cell parameters are a = 9.9151(6) A, b = 26.432(2) A, and c = 10.2116(6) A; Z = 2. The structure of Ca(18)Li(5)In(25.07) features two distinct types of indium anionic layers. An "electron-deficient" layer is made up of Li-centered In(12) icosahedra that are interconnected by bridging planar In(4) units and In atoms. A second In(3)(5-) layer is an electron-precise Zintl layer formed by fused four-, five-, and six-membered rings of three- and four-bonded indium atoms. The two distinct layers are alternately stacked and linked into a complex three-dimensional network. Vacancies are observed to occur only at the In(12) icosahedral and the bridging indium units within the "electron-deficient" layers. Magnetic property measurements indicate that Ca(18)Li(5)In(25.07) exhibits temperature-independent paramagnetism consistent with metallic behavior. Band structure calculations were performed to elucidate the role of defects and vacancies in the electronic structure of the electron-deficient "metallic" Zintl phase.

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Nine hexagonal ca(5)pb(3)z phases in stuffed mn(5)si(3)-type structures with transition metal interstitial atoms z. Problems with classical valence States in possible zintl phases.

Ternary hexagonal Ae(5)Tt(3)Z phases have been obtained from high-temperature reactions (1000-1300 degrees C in Ta) only for Ae (alkaline-earth metal) = Ca, Tt (tetrel) = Pb, and Z = V, Cr, Mn, Fe, Co, Ni, Zn, Ru, or Cd. The hexagonal crystal structures (stuffed Mn(5)Si(3)-type, P6(3)/mcm, Z = 2) were refined for Z = Mn and Fe (a = 9.3580(3), 9.3554(5) A, c = 7.009(1), 7.009(1) A, respectively). In contrast, Ca(5)Pb(3)Z for Z = Cu or Ag form only with a trigonal structure (P3c1, Z = 2, a = 9.4130(3) A, c = 7.052(1) A for Cu) in which regular displacements of only the linear strings of Ca1 atoms occur. The existence of these compounds stands in contrast to the nonexistence of all binary Ae(5)Tt(3) products from Ca to Ba (Ae) and Si to Pb (Tt) with a Mn(5)Si(3)-type structure. Therefore, it once seemed attractive to consider the Z elements in these Ca(5)Pb(3)Z compounds as reducing agents (electron donors). The Mn and Fe structures appropriately exhibit greatly enlarged antiprismatic calcium cavities about Z. Other indications of relatively electron-poor environments around Fe are found in its properties, which include soft ferromagnetism with an elevated magnetic moment (6.3 micro(B)) and a large Fe 3p(3/2) binding energy relative to that in La(5)Ge(3)Fe, La(15)Ge(9)Fe, etc. The Ca(5)Pb(3)Mn phase exhibits metallic behavior (rho(295) = 135 microOmega cm) and temperature-independent Pauli paramagnetism. These properties are supported by ab initio band structure calculations for Ca(5)Pb(3)Mn, which show strong Ca-Pb bonding and a broad Pb-based band, with appreciable Ca-Mn and Ca-Pb bonding states at and above E(F). Distortion of the Cu analogue gives strengthened Ca-Pb bonding and reduced Cu-Ca1 repulsions. A Zintl phase description of these compounds and some related compounds in terms of closed Pb bands is not appropriate.

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X-ray and neutron diffraction studies on "Li4.4Sn".

A chemical analysis and detailed structural characterization, using X-ray single crystal and neutron powder diffraction, of the binary lithium-tin compound "Li(4.4)Sn" is presented. Phase analyses and subsequent structural refinements result in the reformulation of "Li(4.4)Sn" as Li(17)Sn(4). The lithium-rich binary phase crystallizes with a complex cubic structure in the space group Ffourmacr;3m, with a = 19.6907(11) A, Z = 20. The improved crystal structure determination indicates well-defined lithium atom positions, some of which differ from those previously reported. The nearly Zintl phase Li(17)Sn(4) exhibits poor metallic behavior similar to that of heavily doped semiconductors. Comparisons of the refined crystal structure with previously reported X-ray crystal structures associated with "Li(4.4)Sn" are discussed.

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SrInGe and EuInGe: new Zintl phases with an unusual anionic network derived from the ThSi(2) structure.

Two new isostructural Zintl phases, EuInGe and SrInGe, are obtained from high-temperature reactions of the pure elements in welded Ta tubes. Both ternary phases crystallize in a new structure type in space group Pnma (No. 62), with a = 4.921(1) A, b = 3.9865(9) A, and c = 16.004(3) A for EuInGe; and a = 5.021(1) A, b = 4.0455(9) A, and c = 16.188(4) A for SrInGe. The crystal structures established by single-crystal X-ray diffraction feature zigzag chains of 3-bonded Ge atoms and puckered layers of 4-bonded In atoms. The two structural units are linked into an anionic network with channels composed of 5-membered and 7-membered rings. The channels are filled by the respective divalent cations. The chemical bonding of the anionic [InGe](2)(-) network, derived from a one-electron oxidative distortion of the alpha-ThSi(2) structure, is explained using extended-Hückel band structure calculations. Magnetic measurements indicate that EuInGe exhibits Curie-Weiss paramagnetic behavior above 35 K and antiferromagnetic behavior below 35 K. The calculated effective moment, mu(eff) = 8.11 mu(B), of EuInGe and the diamagnetic behavior of SrInGe are consistent with the oxidation states of Eu(II) and Sr(II), respectively.

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