The synthesis and charaterization of a series of diborane (4) compounds, such as B2 (1, 2- O2C6H4) 2 (3), B2 (1, 2-S2C6H4) 2 (13), and B2 (OCH2CMe2CH2O) 2 (11), and several ring-substituted derivatives of the catecholate and dithiocatecholate compounds are described along with photoelectron spectroscopic studies on 3, 11, B2 (OCMe2CMe2O) 2 (12), and B2 (NMe2) 4 (1). Several intermediates, impurities, and side reactions have ...