Two subvalent, redox-active diborane(4) anions, [3]4? and [3]2?, carrying exceptionally high negative charge densities are reported: Reduction of 9-methoxy-9-borafluorene with Li granules without stirring leads to the crystallization B(sp3)?B(sp2) diborane(5) anion salt Li[5]. [5]? contains a 2,2?-biphenyldiyl-bridged B?B core, chelating 2,2?-biphenyldiyl moiety, MeO substituent. Li[5] Na metal...