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The crystal and molecular structure of 10-phenoxarsine sulfide, (Ci2H8OAs)2S, has been determined by single-crystal X-ray diffraction methods. The unit cell is triclinic: a = 9.033 (1) Á, b = 11.435 (2) Á, c = 14.114 (3) A, a -127.83 (3)°, ß = 112.10 (2)°, and y = 84.36 (1)°. The Delauney cell has a = 9.033 (1) A, b = 11.435 (2) Á, c = 13.597 (3) Á, a -124.85 (3)°, ß = 105439 (2)°, r = 95.64 (1)°, with ámeas<¡ = 1.61 (1) g cm"3 and ¿cai"d (for Z = 2) = 1.640 (3) g cm"3. The space group is PI (G1; No. 2), and there are two molecules per unit cell. Manual diffractometer methods (Mo radiation, 0.71069 A) were used to obtain 1412 observed (/ > 3 (/)) reflections at 23°. Refinement of the structure by fullmatrix least-squares methods, utilizing anisotropic thermal parameters for the As and S atoms and assigned positions and thermal parameters for the H atoms, gave a final R index of 0.033. The molecule has nearly planar phenoxarsine (Ci2H8OAs) moieties. The three planes which include all of the atoms of the structure (the two phenoxarsine planes and the As-S-As plane) are very nearly mutually perpendicular. The As-S distances are 2.267 (3) and 2.282 (3) A, the AsSAs angle is 99.87 (6)°, and all of the bond angles at the arsenic atoms are 94.4-99.8°. Atoms Dist, Á Atoms Angles, deg As(l)-S 2,267 (3) As(l)-S-As(2) 99.87 (6) As(2)-S 2.282 (3) S-As(l)-C(l) 99.5 (3) As(l)-C(l) 1.95 (1) S-As(l)-C(7) 99.8 (3) As(l)-C(7) 1.95 (1) S-As(2)-C(13) 99.3 (3) As(2)-C(I3) 1.93 (1) S-As(2)-C(19) 99.8 (3) As(2)-C(19) 1.93 (1) S-As-C (av) 99.6 (2)a As-C (av) 1.94 (l)a As(l)-C(l)-C(6) 124.3 (6) 0(1)-C(6) 1.34 (1) As(l)-C(7)-C(12) 123.7 (6) 0(1)-C(12) 1.38 (1) As(2)-C(I3)-C(I8) 123.9 (7) 0(2)-C(I8) 1.36 (1) As(2)-C(19)-C(24) 123.8 (7) 0(2)-C (24) 1.40 (I) As-C(av) 123.9 (2)° -C (av) 1.38 (2)a C(l)-As(l)-C(7) 94.4 (4) C(l)-C(2) 1.40 (1) C(13)-As(2)-C(19) 95.2 (4) C(2)-C(3) 1.41 (2) C(6)-0(l)-C(12) 125.6 (6) C(3)-C(4) 1.35 (2)

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The crystal and molecular structure of triethylammonium phenylthioarsenate, (C2H5)3NH +(C6H5)AsSO(OH)-, was determined from three-dimensional X-ray data collected with a manual diffractometer using Mo Ka ( 0.71069 k) radiation.The compound crystallizes in the triclinic space group PI, with a = 11.807 (1) Á, b = 10.558 (1) Á, c = 8.788 (1) A, a - 116.21 (2)°, ß = 98.95 (1)°, 7 = 117.91 (1)°, Z = 2, dmeosd = 1.40 (1) g cm"1 23, and d"i=d = 1.373 (3) g cm-3, at 23°. The structure was determined by Patterson and Fourier methods and refined with 362 observed reflections by full-matrix least squares to an R of 0.051. In the final refinement the phenyl ring was constrained as a rigid group, and the As and S atoms were refined with anisotropic thermal parameters. The anion of the structure consists of an arsenic atom tetrahedrally bonded to a phenyl group, two oxygen atoms, and a sulfur atom at distances of 1.90 (2), 1.65 (2), 1.75 (3), and 2.08 (2) Á, respectively. Hydrogen bonding holds pairs of anions together and one cation to each anion. This is the first monothioarsenate structure to be reported, and the As-S bond length is one of the shortest values reported for that bond.