X-ray crystal structures of [ Et3NH][{(CO)(5) Mo( P( OCH2CMe2CH2O)O)}(2)H], 3, and ( CO)(5)Mo{mu-Ph2POPPh2} Mo( CO) 5, 2, are reported. Crystallization of 3 occurs in P-1 space group with a = 9.6944( 19) angstrom, b = 10.814( 2) angstrom, c = 19.730( 4) angstrom, alpha = 94.24( 3)degrees, beta = 92.23( 3)degrees, gamma = 113.47( 3)degrees, Z = 4. Crystallization of 2 occurs in C2/c space group with a = 10.357( 2) angstrom, b = 20.149( 4) angstrom, c = 17.155( 3) angstrom, alpha = 90 degrees, beta = 97.28(3)degrees, gamma = 90 degrees, Z = 8. Compound 2 is a bimetallic complex with a P-O-P bridging group containing bond distances similar to that of other complexes in which two metal centers are bridged by a single R2POPR2 ligand. Compound 3 contains intermolecular hydrogen bonded P-O-H-O-P linkages with bond distances comparable to those seen in similar structures with intramolecular hydrogen bonding suggesting that the distance is a function of the nature of the bond and not affected by the cis arrangement of the ligands about the metal center.