Three organometallic complexes [C6H4-p-(CO2CH2C2H-mu (2)] [Co-2(CO) (6)] (2)(l), [C6H4-p-(CO2CH2C2H) (2)] [RuCO2(CO) (9)] (2) (2) and [(HC2CH2OCO) C6H4-p-(CO2CH2C2H-mu)] [Mo2CP2 (CO) (4)] (3) have been prepared from the reactions of dipropargyl terephthalate with CO2 (CO) (8), Mo2Cp2 (CO) (4) and RuCo2 (CO) (11). From their H-1 NMR spectra, it is found that the deshielding effect of metal species on terminal alkyne follows RuCo2 (CO) (9) > Co-2 (CO) (6) > Mo-2 (CO) 4CP2. The single-crystal diffraction of compound 1 was undertaken with the data: triclinic, P (1) over bar, a = 8.139(2) Angstrom, b = 8.808(3) Angstrom, c = 11.343(3) Angstrom, beta = 96.260(6)degrees , V = 773.4(4) Angstrom (3), Z = 1, Dc = 1.748g (.) cm(-3), R = 0.0513, w R = 0.1266.