Synthesis and characterization of palladium complexes containing tridentate ligands with PXP (X = C, N, O, S, As) donor sets and their evaluation as electrochemical CO[sub 2] reduction catalysts

Journal Article · Thu Dec 01 04:00:00 EST 1994 · Organometallics; (United States)

DOI:https://doi.org/10.1021/om00024a030· OSTI ID:6736244

Steffey, B D; Miedaner, A; Maciejewski-Farmer, M L; Bernatis, P R; Herring, A M; DuBois, D L ^[1]; Allured, V S; Carperos, V ^[2]

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1. National Renewable Energy Lab., Golden, CO (United States)
2. Univ. of Colorado, Boulder, CO (United States)

Square-planar palladium complexes containing tridentate ligands with PXP (X = C, N, O, S, and As) donor sets have been prepared. For [Pd(POP-R)(CH[sub 3]CN)[sub 2]](BF[sub 4])[sub 2] complexes (where POP-R is bis((diethylphosphino)ethyl) ether, bis((diphenylphosphino)ethyl) ether, or bis((dicyclohexylphosphino)ethyl) ether), the POP-R ligands function as bidentate ligands. For all other complexes, the PXP ligands function as tridentate ligands. The complex [Pd(PCP)(PEt[sub 3])](BF[sub 4]) (where PCP is 2,6-bis(diphenylphosphino)methyl)phenyl crystallizes in the triclinic space group P[bar 1] with a = 10.276(2) angstroms, b = 10.978(2) angstroms, c = 18.807(3) angstroms, [alpha] = 84.820(10)[degrees], [beta] = 76.910(10)[degrees], [gamma] = 63.870(10)[degrees], V = 1855.2(6) angstroms[sup 3], and Z = 2. The structure was refined to R = 0.0335 and R[sub w] = 0.0442 for 7570 independent reflections with F > 4.0[sigma](F). [Pd(PNP)(PEt[sub 3])](BF[sub 4])[sub 2] (where PNP is 2,6-bis(disphenylphosphino)methyl)pyridine crystallizes in the monoclinic space group C2/c with a = 13.246(2) angstroms, b = 14.299(2) angstroms, c = 20.847(4) angstroms, [beta] = 100.96(2)[degrees], V = 3876.5(11)angstroms[sup 3], and Z = 4. 40 refs., 6 figs., 4 tabs.

• OSTI ID: 6736244
• Journal Information: Organometallics; (United States), Journal Name: Organometallics; (United States) Vol. 13:12; ISSN ORGND7; ISSN 0276-7333
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400102 -- Chemical & Spectral Procedures
400201* -- Chemical & Physicochemical Properties
400400 -- Electrochemistry
ACETONITRILE
AMPEROMETRY
CARBON COMPOUNDS
CARBON DIOXIDE
CARBON MONOXIDE
CARBON OXIDES
CATALYSIS
CHALCOGENIDES
CHEMICAL BONDS
CHEMICAL REACTIONS
COHERENT SCATTERING
COMPILED DATA
COMPLEXES
CRYSTALLOGRAPHY
DATA
DIFFRACTION
INFORMATION
LIGANDS
MAGNETIC RESONANCE
NITRILES
NUCLEAR MAGNETIC RESONANCE
NUMERICAL DATA
ORGANIC COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
OXIDES
OXYGEN COMPOUNDS
PALLADIUM COMPLEXES
REDUCTION
RESONANCE
SCATTERING
SYNTHESIS
TITRATION
TRANSITION ELEMENT COMPLEXES
VOLTAMETRY
X-RAY DIFFRACTION