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Photochemistry of (2,3,9,10-tetramethyl-1,4,8,11-tetraazacyclotetradeca-1,3,8,10-tetraene)copper(II): participation of copper(II) hydrides

Journal Article · · Inorg. Chem.; (United States)
DOI:https://doi.org/10.1021/ic00197a008· OSTI ID:5528643

The photochemistry in acidic methanol and the relevant thermochemistry of (2,3,9,10-tetramethyl-1,4,8,11-tetraazacyclotetradeca-1,3,8,10-tetraene)copper(II) (ligand abbreviations are 2,3,9,10-Me/sub 4/-(14)-1,3,8,10-tetraeneN/sub 4/ or L in this work) have been investigated. UV photolysis results in the rapid formation of a transient identified as Cu(2,3,9,10-Me/sub 4/-(14)-1,3,8,10-tetraeneN/sub 4/)/sup +/. A minor fraction of the transient is produced in t < 10 ns and a major fraction in the microsecond time domain via a second-order process (k = (5.7 +/- 0.3) x 10/sup 7/ M/sup -1/ s/sup -1/) that involves the reaction of solvent radicals (CH/sub 2/OH) with the copper(II) macrocycle. In perchlorate media, (ClO/sub 4//sup -/) > 10/sup -3/ M, a first-order isomerization followed in milliseconds (k = (2.0 +/- 0.3) x 10/sup 3/ s/sup -1/). Cu(2,3,9,10-Me/sub 4/-(14)-1,3,8,10-tetraeneN/sub 4/)/sup 2 +/ then undergoes slow decay by competitive pathways to produce H/sub 2/ and Cu/sub solv//sup +/. The product quantum yields (10/sup -3/ < phi/sub Cu/sup +/solv/ < 10/sup -2/; 10/sup -4/ < phi/sub H/sub 2// < 10/sup -3/) depend on light intensity, acid concentration, and the concentration of the copper(II) macrocycle. The production of hydrogen is postulated to occur via a copper(II) macrocycle in acid solution. The thermal properties relevant to an interpretation of the photochemistry were as follows: (1) There is a dependence on solvent of E/sub 1/2/ for the Cu/sup II/L/Cu/sup I/L couple (varies from -0.02 V in CH/sub 2/Cl/sub 2/ to -0.62 V vs. SCE in H/sub 2/O) and the CuL/sup 2 +/ electronic absorption spectrum. (2) The E/sub 1/2/ value for the ligand reduction at approx.-1.4 V vs. SCE shifts positively in acidic media until it overlaps the metal(II/I) couple. (3) The spectral properties of Cu(2,3,9,10-Me/sub 4/-(14)-1,3,8,10-tetraeneN/sub 4/)/sup +/ generated by coulometric reduction (n = 1.01) at -0.60 V vs. SCE in acetonitrile are lambda/sub max/ = 746 nm with epsilon approx. = 8 x 10/sup 3/ M/sup -1/ s/sup -1/. 24 references.

Research Organization:
Univ. of Notre Dame, IN
OSTI ID:
5528643
Journal Information:
Inorg. Chem.; (United States), Journal Name: Inorg. Chem.; (United States) Vol. 24:3; ISSN INOCA
Country of Publication:
United States
Language:
English

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