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Title: Synthesis and characterization of water-soluble 1,2-bis(bis(hydroxyalkyl)phosphino)ethane ligands and their nickel(II), ruthenium(III), and rhodium(I) complexes

Journal Article · · Inorganic Chemistry
DOI:https://doi.org/10.1021/ic960766t· OSTI ID:420973
; ;  [1]
  1. Univ. of Oregon, Eugene, OR (United States); and others

The syntheses of the water-soluble, chelating phosphines 1,2-bis(bis(hydroxybutyl)phosphino)ethane (1, n = 3; DHBuPE) and 1,2-bis(bis(hydroxypentyl)phosphino)ethane (1, n = 4; DHPePE) are reported. These ligands (and, in general, other 1,2-bis(bis(hydroxyalkyl)phosphino)ethane ligands) can be used to impact water solubility of metal complexes. As examples of this, the [Ni(DHPrPE){sub 2}Cl]Cl (2), [Rh(DHPrPE){sub 2}][Cl] (3), and [Ru-(DHBuPE){sub 2}Cl{sub 2}][Cl] (4) complexes were synthesized; they are indeed soluble in water (>0.5 M). Crystals of DHPrPE (1, n = 2) are monoclinic, space group P2{sub 1/c}, with a = 9.5935(8) {angstrom}, b = 9.353(2) {angstrom}, c = 10.655(2) {angstrom}, {alpha} = 90{degrees}, {beta} = 100.03(1){degrees}, {gamma} = 90, V = 941.5(5) {angstrom}{sup 3}, R = 0.051, and Z = 2. Crystals of [Ni(DHPrPE){sub 2}Cl]Cl (2) are monoclinic, space group I2, with a = 15.951(3) {angstrom}, b = 11.454(2) {angstrom}, c = 20.843(3) {angstrom}, {alpha} = 90{degrees}, {beta} = 91.24(2){degrees}, {gamma} = 90{degrees}, V = 3807(2) {angstrom}{sup 3}, R = 0.062, and Z = 4. Crystals of [Rh(DHPrPE){sub 2}][Cl] (3) are triclinic, space group P1, with a = 13.900(2) {angstrom}, b = 15.378(2) {angstrom}, c = 18.058(2) {angstrom}, {alpha} = 87.71(1){degrees}, {beta} = 75.03(1){degrees}, {gamma} = 85.24(1), V = 3715(2) {angstrom}{sup 3}, R = 0.044, and Z = 4. Crystals of [Ru(DHBuPE){sub 2}Cl{sub 2}][Cl] (4) are monoclinic, space group C2/c, with a = 14.310(2) {angstrom}, b = 21.630(2) {angstrom}, c = 15.459(3) {angstrom}, {alpha} = 90{degrees}, {beta} = 99.83(1){degrees}, {gamma} = 90, V = 4715(1) {angstrom}{sup 3}, R = 0.056, and Z = 4.

OSTI ID:
420973
Journal Information:
Inorganic Chemistry, Vol. 35, Issue 23; Other Information: PBD: 6 Nov 1996
Country of Publication:
United States
Language:
English