CRYSTAL AND MOLECULAR STRUCTURE OF 4-TERT-BUTYLPHOSPHORINANE 1-SULFIDE DERIVATIVES

Abstract Three derivatives of the parent 4-tert-butylphosphorinane sulfide were prepared and investigated by single crystal X-ray diffraction: trans-4-tert-butyl-1-phenoxyphosphorinane sulfide (2a) and the cis and trans isomers of 4-tert-butyl-1-phenylphosphorinane sulfide (3b and 3a, respectively). Crystallographic data for 2a: space group P21/n (No. 14) with a = 6.1670(6) A, b = 10.999(1) A, c = 23.275(2) A, β = 94.978(7)°, V = 1572.7(5) A3, and Dcalc = 1.193 g cm−3 for Z = 4, R = 0.040; for 3a: space group C2/c (No. 15) with a = 25.826(3) A, b = 6.427(1) A, c = 20.050(3) A, β = 111.57(1)°, V = 3094(1) A3, and Dcalc = 1.143 g cm−3 for Z = 8, R = 0.043; for 3b: space group P21/c (No. 14) with a = 6.2914(7) A, b = 11.632(1) A, c = 21.088(1) A, β = 96.892(7)°, V = 1532.1(4) A3, and Dcalc = 1.155 g cm−3 for Z = 4, R = 0.048. In every structure the phosphorinane ring adopts a chair conformation with tert-butyl group in an equatorial position. The relative spatial arrangement of the latter and the phenoxy or ...