THE DIHYDROGENMONOTHIOPHOSPHATE AND TRIHYDROGENDISULFANEDIPHOSPHONATEANIONS - CRYSTAL-STRUCTURES OF KH2SPO3 AND [CO(EN)2CL2]H3S2P2O6

Crystal structures of potassium dihydrogenmonothiophosphate, KH2SPO3 ( 1), and trans-dichlorobis(ethylenediamine)cobalt(III) trihydrogendisul fanediphosphonate, [Co(en)2Cl2]H3S2P2O6 (2), have been determined from X-ray data and refined to R = 0.015 and 0.043 for 476 and 1871 observ ed reflections, respectively. Compound 1 forms monoclinic crystals, sp ace group Cm with Z = 2, and a = 6.549(1), b = 6.317(1), c = 5.894(1) angstrom and beta = 109.13(1)-degrees. Compound 2 forms orthorhombic c rystals, space group P2(1)2(1)2(1) with Z = 4 and a = 8.238(1), b = 10 .295(1), c = 19.383(2) angstrom. In compound 1 the slightly distorted tetrahedral arrangement around phosphorus has the dimensions: S-P = 1. 9681(7), P-O = 1.5244(16)-1.5754(11) angstrom, S-P-O = 112.76(5)-114.4 5(7)-degrees, O-P-O = 102.00(9)-106.96(6)-degrees. The two H atoms are bonded to the two 0 atoms having longest distances from P, with 0-H = 0.78(3) angstrom and P-O-H = 113(2)-degrees. In compound 2 the anion has an unbranched, non-planar phosphorus-sulfur chain in which the P a toms are each bonded to one S atom and 3 O atoms. It has the dimension s: S-S = 2.0561(24) angstrom, S-P = 2.0954(24) and 2.1120(22) P-O = 1. 484(4)-1.540(5) angstrom, S-S-P = 100.04(9) and 102.21(9)-degrees, S-P -O 98.63(23)-110.02(21)-degrees, O-P-O = 107.51(30)-118.83(30)-degrees , O-H = 0.67(6)-0.94(7) angstrom, P-O-H = 118(6)-123(4)-degrees, and t he PSSP torsion angle is - 85.46(11)-degrees.