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Journal ArticleDOI

CRYSTAL STRUCTURE OF T-BUTYL PERTHIOPHOSPHONIC ANHYDRIDE, (t-C4H9PS2)2, AND ITS SELENIUM ANALOG (t-C4H9PSe2)2

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TLDR
In this paper, it was shown that the sulfur compound is orthorhombic, Cmca, with a = 9.872 (1), b=9.724 (1) A, V=1479.0 (4) A3, Z=4, and Dc = 2.21 g cm−2.
Abstract
Crystals of the title sulfur compound are orthorhombic, Cmca, with a=9.872 (1), b=9.594 (1), and c=15.488 (1) A, V=1467.0 (4) A3, Z=4, and Dc =1.38 g cm−2. The final refinement using 537 observed reflections for 57 variable gave R=0.025. The non-isomorphous crystals of the selenium analog are also orthorhombic, Cmca, with a=9.300 (1), b=19.724 (1), c=8.064 (1) A, V=1479.1 (4) A, Z=4, and Dc =2.21 g cm−2. Refinement with 48 variables using 447 observed reflections gives R=0.041. In both structures the molecules have 2/m symmetry imposed by the lattice symmetry; the S (or Se) atoms of the central 4-membered ring are located on the rotation axis, and the P, exo S (or Se), and two carbon atoms of the t-butyl group lie on the mirror plane. The central rings are not readily hydrolyzed or oxidized by exposure to air, apparently as a result of steric protection provided by the t-butyl groups.

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Citations
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Journal ArticleDOI

A New Synthesis of (PhPSe2)2 (Woollins Reagent) and Its Use in the Synthesis of Novel P–Se Heterocycles

TL;DR: Four novel phosphorus-selenium heterocycles, including a spirocyclic heterocycle exhibiting a four-membered P2SeC ring, were obtained from the reaction of WR with two reactive substrates (diphenylcyclopropenone and methyl phenylpropiolate).
Journal ArticleDOI

Formation and Reactivity of Phosphorus–Selenium Rings

TL;DR: Phosphorus-selenium ring chemistry has developed to include the synthesis of some exciting new motifs and provided organic chemists with a new reagent, [PhPSe(2)](2), which has become known as Woollins' reagent.
Journal ArticleDOI

Heterocycle formation using [PhP(Se)(μ-Se)]2. The crystal structures of [PhP(Se)(μ-Se)]2, PhP(Se)Se2(C7H10) and PhP(Se)(μ-Se)(μ-NPh)P(Se)Ph

TL;DR: An X-ray crystallographic study of [PhP(Se)(μ-Se)]21, the oxidation product of the homocycle (PhP)5 with ten equivalents of selenium, revealed that the molecule is centrosymmetric with a planar central P2(μ)-Se)2 core and trans disposition of exocyclic PSe bonds as mentioned in this paper.
Journal ArticleDOI

Synthesis and Structural Studies of Pyridine‐2‐selenolates − Reactions with Electrophilic Phosphorus(III) Compounds and Related Complex Chemistry

TL;DR: In this article, the reaction intermediates in the synthesis of 2,2′-bis(pyridyl) diselenide (2, 2′-Py2Se2) have been determined.
References
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Journal ArticleDOI

N, N-Dimethylamido-trithiophosphorsäure-anhydrid†

TL;DR: In this paper, the results of an X-ray analysis of tetraphosphorustrisulfide and bis(dimethylamino)sulfane were reported and discussed.
Journal ArticleDOI

Über 3,6-Dihydro-2H-1,2-thiaphosphorin-2-sulfide

TL;DR: In this paper, a 3,6-Dihydro-2H-1,2-thiaphosphorin-sulfide was Metallierung mit Alkylierungsmitteln in die entsprechenden Dithiophosphinsaureester ubergefuhrt werden konnen.
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