Crystal and molecular structure of (2,2,2-crypt)potassium telluridoplumbate, (2,2,2-crypt-K+)2Pb2Te32-

Abstract

Inorg. Chem. 1991,solve as the solution is neutralized carefully to pH = 7.0. Evaporation in a rotary evaporator at aspirator vacuum and temperature less than 30 OC left a solid that was then pumped under high vacuum for several hours to remove traces of water. The solid was extracted with chloroform and the solvent removed under high-vacuum pumping to leave a semisolid. Stirring with a few drops of water caused crystallization to white crystals that were then dried under high vacuum, giving 1.20 g (80%) of Me2NCH2BH2NMe2CH2BHCONH2 (4). A sublimed sample (65-70 OC/high vacuum) melted sharply at 158-1 59 OC as opposed to a melting range beginning at 127 OC for the product as obtained, even though the infrared spectra were identical. NMR data: 'H NMe2 2.85, 2.69, 2.65, 2.61; NH2 broad doublet 5.5 and 5.4; CHI broad ca. 1:3:3:1 quartet 2.42, broad ca. I :2: 1 triplet I .90; "B unsymmetrical and shouldered triplet -8.4, -9.4, -10.0 decouples to a singlet -8.9. GC/MS data: one major GC peak and one minor one; m/e 184 (21%) and 183 (11%) parent -1 with 11B2 and 1°B1lB isotopic composition; 141 (100%) and 140 (52%) parent -1 for 1. Infrared data (cm-I) : N H 3435, 3282, 3166 s; BH 2343/2313 s with multiple shoulders; amide carbonyl 1621, 1575 s; 1306 w with shoulders, 1235 w, 1175 w, 1330-1320 m doublet, 1070 m multiplet, 1030-IOIO m doublet, 966 m, 930 m, 889 w, 852 m, 830 w, 734 m. If the basic hydrolysis solution is treated with 1 M HCI to approximately 0.15 M H+, the carboxylate derivative Me,NCH,BH,CH,NMe,BHCO?H (3) settles slowly from the solution Contribution from the

Organic Cation and Complex Cation‐Stabilized (Poly‐)Selenides, [Cation]x(Sey)z: Diversity in Structures and Properties

“…[Mn(en) 3 ](Se 2 Te) [39] (c) that is isostructural to its (Se 3 ) [27] (NBu 4 ) 2 (Se 3 SSe 2 ) (c), [63] [ 4 ]·en (c) were reported, though the latter suffered from disorder and the co-crystallization of an anion of the same composition but with trigonal pyramidal structure (b). [64] The latter structural arrangement would again be a metalate-type one, whereas those mentioned before all belong to the group of organic cation selenides.…”

“…[21] Oxidation can be achieved with H 2 O 2 , elemental iodine or via electrolysis. Reducing agents range from borohydrides and N 2 H 4 to elemental alkali metals.…”

“…Björgvinsson and Schrobilgen started a compilation of various homo-and hetero-(poly)chalcogenides in en and/or liquid NH 3 [21] and on the (HSe) -anion in the solid state, [30] which were complemented by Cusick and Dance in other solvents. [75] Both groups could not observe an (Se 2 ) 2-in solution, which seems to disproportionate.…”

Synthesis and Crystal Structure of Manganese-tris(1,2-ethanediamine)tetratelluride [Mn(en)3]Te4 Exhibiting Intermolecular Interactions between the Tetratelluride Anions

“…In total seven Te±Te interchain separations between 316.2 and 350.4 pm were reported [13]. found in (2,2,2-crypt-K) 2 TeSe 2´e n (341±356 pm) and (2,2,2-crypt-K) 2 TeSe 3´e n (332±354 pm) [26], and a Te´´´H distance of 284.7 pm with an angle Te´´´H±N of 172.2°was observed in [Mn(en) 3 ]TeSe 2 [16].…”

Li2TeS3 and Li2TeSe3: Preparation, Crystal Structure and Impedance Spectroscopic Characterization

“…Knowledge about the homologous selenidotellurates is small to date. Only a few compounds are known, i. e., Na 2 TeSe 3 and K 2 TeSe 3 [18] or (2, 2, 2-crypt-K) 2 TeSe 3 · en [19]. All these materials have [TeQ 3 ] 2Ϫ -units in common.…”