Bis(5,5-dimethyl-2-oxo-1,3,2-dioxaphosphorinanyl) oxide

Abstract

Abstract. C10H2007P2, orthorhombic, Pbca, a = 26.88 (2), b = 9.99 (1), c = 11.13 (1) ,~; V = 2988.8 A3; M r = 314.22; D x = 1.39, D m = 1.39 g cm-3; Z = 8; F(000) = 1328.0; 2(Cu Ka) = 1.5418 A; gr(Cu Ktt) ---0.6. The structure was solved by direct methods and refined by least-squares methods with anisotropic temperature factors to an R value of 0. 121 for 1179 observed reflections. The symmetry of the bicyclic molecules is C~. The conformation around the bridge bonds P-O-P is staggered. The two structurally independent dioxaphosphorinane rings have partially flattened chair conformations with the double-bonded O atom in an equatorial and the linking O atom in an axial position. An analysis of the causes of the flattening observed in the 1,3,2-dioxaphosphorinane rings was carried out and the structural results are compared with those for bis(5,5-dimethyl-2-oxo-l,3,2-dioxaphosphorinanyl) sulphide.

Crystal and Molecular Structure and Solid State NMR Studies of Bis(5,5-Dimethyl-2-Oxo-1,3,2-Dioxaphosphorinan-2-Yl) Selenide

“…The "bridge" angles found in literature16 for structures containing oxygen as bridging atom are in the range 129.2-146.1'. [8][9][10][11][12][13] In two structures containing sulfur as bridging atom those angles are 102.2' and 103.3".'4. '5…”

The structure of tetramethyl μ‐monothiopyrophosphate

“…Based on cruickshank's correlation of P-0 bond length with m-bond order [ 151, Bukowska-Strzyzewska and Dobrowolska assigned bond orders to all the P-0 bonds in 3 [7]. The P-0 bonds in the alkoxyl groups are slightly shorter in 3 than in 2 or 1.…”

“…The structure of the analogous ester of pyrophosphate 3 has also been solved by x-ray crystallography [7]. In this article we report the crystal and molecular structure of 1, the tetramethyl ester of pmonothiopyrophosphate.…”

Structure of a racemic compound: the dicyclohexylammonium salt of (2R,4R,2S,4S)-cis-4-methyl-2-oxido-1,3,2-dioxaphosphorinane 2-sulphide, C12H24N+.C4H8O3PS−

“…1. 1,3,2-DOPN ring systems have been extensively investigated during the last decade, but comparatively less information is available on 4-methyl derivatives than on 5,5-dimethyl species (Bukowska-Strzy~ewska & Dobrowolska, 1978). In the title salt the C(4) methyl group is in eis relation to the exocyclic O atom as postulated by Mikotajczyk & Luczak (1972).…”