The muon decay parameter ξ 00 has been determined in a measurement of the longitudinal polarization of positrons emitted from polarized and depolarized muons. The result, ξ 00 ¼ 0.981 AE 0.045 stat AE 0.003 syst , is consistent with the Standard Model prediction of unity, and provides an order of magnitude improvement in the relative precision of this parameter. This value sets new constraints on exotic couplings beyond the dominant V-A description of the leptonic weak interaction.