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1.
Acta Crystallogr E Crystallogr Commun ; 79(Pt 10): 942-945, 2023 Oct 01.
Article in English | MEDLINE | ID: mdl-37817955

ABSTRACT

A new solid-state inorganic compound, indium dilead penta-chloride, InPb2Cl5, was synthesized by melting InCl and PbCl2 in a vacuum-sealed quartz ampoule. The ampoule was heated to 793 K and then slowly cooled to room temperature to induce crystallization of InPb2Cl5. InPb2Cl5 crystallizes in the monoclinic crystal system adopting a space group of type P21/c, which is isostructural with other metal halides such as RbPb2Cl5, KPb2Cl5 and TlPb2Cl5. The bulk InPb2Cl5 exhibits a metallic black/grey colour, allowing it to be separated from white/yellow PbCl2 crystals. Due to the incongruent nature of the compound, the pure bulk InPb2Cl5 was not obtained. The black/grey InPb2Cl5 crystals were characterized by powder and single-crystal X-ray diffraction. InPbCl3 was also explored, however the growth was unsuccessful.

2.
ACS Appl Mater Interfaces ; 13(47): 56296-56301, 2021 Dec 01.
Article in English | MEDLINE | ID: mdl-34787392

ABSTRACT

Bismuth thiophosphate, BiPS4, is a promising nontoxic, high-density ternary chalcogenide semiconductor. Polycrystalline BiPS4 was synthesized from the stoichiometric melt of Bi, P, and S. Phosphorus was purified via an in-situ sublimation method. Single crystals of BiPS4 were grown using a modified vertical Bridgman method with a thermal gradient of 18 °C/cm. The material exhibits an electrical resistivity of 2 × 109 Ω·cm. The Knoop hardness of the single crystals is 128 ± 0.8 kg mm-2. A blocking contact behavior was observed with asymmetric contacts of Ga/BiPS4/Ag. A clear photocurrent response was observed from a BiPS4 crystal under an electric field as low as 1.14 V mm-1. Using a tungsten X-ray source, an X-ray sensitivity of 52 µ Gy-1 cm-2 was measured under an electric field of 80 V mm-1. When a single-crystal BiPS4 radiation detector device was used in a pulse-height radiation detection system, a clear charge collection response was observed under a 241Am α-particle radiation source.

3.
Inorg Chem ; 59(10): 7049-7055, 2020 May 18.
Article in English | MEDLINE | ID: mdl-32369351

ABSTRACT

The investigations of bismuth halide chemistry in DMSO/MeOH solutions led to the discovery of a new solvent-stabilized compound with a chemical formula of Cs3BiBr6·3DMSO. In addition, a new phase of Cs3BiBr6 was generated as a result of a crystal-to-crystal transition driven by the change in the solvent composition. The solvent stabilized Cs3BiBr6·3DMSO adopts an orthorhombic P212121 type crystal structure with unit cell dimension of a = 13.6160(6) Å, b = 14.4359(8) Å, and c = 14.6487(7) Å. Bulk single crystals of Cs3BiBr6·3DMSO with average size of 4.5 × 3.5 × 3.5 mm3 were grown by the antisolvent crystal growth method. With the change of the solvent composition from 2:1 DMSO: MeOH to 1:1 DMSO: MeOH, the single crystals of Cs3BiBr6·3DMSO underwent a crystal-to-crystal transition yielding another structurally distinct Cs3BiBr6 phase, with a tetragonal P42/m type structure and unit cell dimensions of a = 9.8394(5) Å, b = 9.8394(5) Å, and c = 8.0950(6) Å. Both compounds exhibit isolated BiBr6 octahedral resembling the structures of the zero-dimensional (0D) perovskites.

4.
Dalton Trans ; 48(33): 12512-12521, 2019 Sep 07.
Article in English | MEDLINE | ID: mdl-31363732

ABSTRACT

Phosphaamidine metal complexes Rh2Cl2[Ph2PC(Ph)[double bond, length as m-dash]NPh]2µ-CO (1), RuCl2[Ph2PC(Ph)[double bond, length as m-dash]N(Ph)]2 (2), [Rh{iPr2PC(Ph)[double bond, length as m-dash]NiPr}(COD)]BF4 (3), and RuCl2[iPr2PC(Ph)[double bond, length as m-dash]NiPr](DMSO)2 (4) are prepared by combining phosphaamidines Ph2P-C(Ph)[double bond, length as m-dash]NPh and iPr2P-C(Ph)[double bond, length as m-dash]NiPr (1,3-P,N) with their corresponding metal ions. Complexes 1 and 2 are stable in air while 3 and 4 are stable under inert conditions. For further comparison of structure and stability, a Ru(ii) phosphaguanidine complex, RuCl2[Me2NC(PPh2)[double bond, length as m-dash]NiPr](DMSO)2 (6) was prepared. Complex 6 is stable in air and in the presence of water. The structures of the phosphaamidine and phosphaguanidine complexes, determined using single crystal X-ray diffraction, revealed P,N bidentate coordination. While all five complexes have some activity as precatalysts, complex 6 was the most active.

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