CHEMISTRY OF POLYFUNCTIONAL MOLECULES .11 9. TETRACARBONYL-DICOBALT-TETRAHEDRANE COMPLEXES WITH THE LIGANDS BIS(DIPHENYLPHOSPHANYL)AMINE, 2-BUTIN-1,4-DIOL, AND TERT-BUTYLPHOSPHAACETYLENE - CRYSTAL-STRUCTURE OFTHE PHOSPHAALKYNE DERIVATIVE

Co-2(mu-CO)(2)(CO)(4)(mu-Ph(2)P-NH-PPh(2)-P,P') . 1/2 C6H5CH3 (4 . 1/2 C6H5CH3) reacts with 2-butine-1,4-diol, HOCH2-C=C-CH2OH (5), to the d ark-red tetrahedrane complex 2(CO)(4)(mu-eta(2)-eta(2)-HOCH2-C=C-CH2OH -C-2,C-3) . (mu-Ph(2)P-NH-PPh(2)-P,P') . THF (6 . THF). With t-butyl-p hosphaacetylene, tBu-C=P (7), 4 . THF forms Co-2(CO)(4) . -eta(2),eta( 2))-tBu-C=P)(mu-Ph(2)P-NH-PPh(2)-P,P') (8), which also belongs to the tetrahydrane type. The compounds were characterized by their mass, IR, P-31{H-1} NMR, C-13{H-1} NMR, and H-1 NMR spectra. Crystals suitable for X-ray structure analyses have been obtained for 8 from dioxane. Th e dark red blocks crystallize in the monoclinic P2(1)/c space group wi th the lattice constants a = 1404,1(5), b = 1330,0(7), c = 2578,8(10) pm; beta = 90,82(3)degrees.