TY - JOUR
T1 - Formation of separated versus contact ion triplets in magnesium thiolates. Synthesis and cCharacterization of [Mg(15-crown-5)(SCPh3)2] and [Mg(15-crown-5)(THF)2][S-2,4,6-tBu3C6H 2]2
AU - Chadwick, Scott
AU - Englich, Ulrich
AU - Ruhlandt-Senge, Karin
PY - 1999
Y1 - 1999
N2 - The synthesis and structural characterization of two magnesium thiolate complexes are described. Both compounds were prepared by analogous reactions routes, namely, alkane elimination and transamination, but using differently sized ligands. Utilization of the smaller HSCPh3, resulted in the formation of [Mg(15-crown-5)(SCPh3)2], 1, displaying a seven-coordinate magnesium center with two magnesium-sulfur bonds. Employment of the sterically more encumbered HS-2,4,6-tBu3C6H2 yielded a separated cation and anions as displayed in [Mg(15-crown-5)-(THF)2][S-2,4,6-tBu3C6H 2]2, 2. Compound 2 exhibits a seven-coordinate cation, completing its coordination environment with five metal - crown-ether interactions in addition to two tetrahydrofuran (THF) contacts. The compounds were characterized by IR and NMR spectroscopy in addition to X-ray crystallography. Crystal data with Mo Kα (λ = 0.71073 Å) are as follows: 1, C48H50MgO5S2, a = 8.4785(4) Å, b = 9.3595(5) Å, c = 13.8306(6) Å, a = 87.332(1)°, β= 85.929(1)°, y = 68.733(1)°, Z = 1, triclinic; 2, C54H94MgO7S2, a = 13.6755-(2) Å, b = 12.8045(6) Å, c = 32.7127(12) Å, β= 97.87(1)°, Z = 4, monoclinic.
AB - The synthesis and structural characterization of two magnesium thiolate complexes are described. Both compounds were prepared by analogous reactions routes, namely, alkane elimination and transamination, but using differently sized ligands. Utilization of the smaller HSCPh3, resulted in the formation of [Mg(15-crown-5)(SCPh3)2], 1, displaying a seven-coordinate magnesium center with two magnesium-sulfur bonds. Employment of the sterically more encumbered HS-2,4,6-tBu3C6H2 yielded a separated cation and anions as displayed in [Mg(15-crown-5)-(THF)2][S-2,4,6-tBu3C6H 2]2, 2. Compound 2 exhibits a seven-coordinate cation, completing its coordination environment with five metal - crown-ether interactions in addition to two tetrahydrofuran (THF) contacts. The compounds were characterized by IR and NMR spectroscopy in addition to X-ray crystallography. Crystal data with Mo Kα (λ = 0.71073 Å) are as follows: 1, C48H50MgO5S2, a = 8.4785(4) Å, b = 9.3595(5) Å, c = 13.8306(6) Å, a = 87.332(1)°, β= 85.929(1)°, y = 68.733(1)°, Z = 1, triclinic; 2, C54H94MgO7S2, a = 13.6755-(2) Å, b = 12.8045(6) Å, c = 32.7127(12) Å, β= 97.87(1)°, Z = 4, monoclinic.
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U2 - 10.1021/ic990814k
DO - 10.1021/ic990814k
M3 - Article
AN - SCOPUS:0001552283
SN - 0020-1669
VL - 38
SP - 6289
EP - 6293
JO - Inorganic Chemistry
JF - Inorganic Chemistry
IS - 26
ER -