A variety of tetrasubstituted alkynediols react with (cdt)Ni (cdt = 1.5.9-cyclododecatriene) to give the homoleptic (alkyne)nickel complexes (HOR1R2CC⋮CCR1R2OH)2Ni as yellow crystals that are stable in the solid state at room temperature (R1 = R2 = Et, 1; R1 = Me, R2 = Et, 2; R1 = Me, R2 = Pr, 3; R1 = R2 = −(CH2)5−, 4; R1 = Me, R2 = i-Bu, 5). The 13C-NMR spectra show resonances for the coordinated alkyne carbon nuclei in the 133.5−135.2 ppm region. Only one resonance was found for 1−4 indicating a symmetrical structure. More than one resonance was found for 5 as well as for its platinum analog, compound 8, indicating the presence of different isomeric bis(alkyne)metal complexes. The structure of 1 has been established by single-crystal X-ray diffraction. The central atom is tetrahedrally coordinated to the four carbon atoms of two terminal alkynes. The network of hydrogen bonding between the four OH groups of neighboring molecules, which consists exclusively of intermolecular hydrogen bonds, stabilizes th...