TY - JOUR
T1 - Compounds with M3Se3 (M = Li, Zn) Rings
T2 - Synthesis and Characterization of [Zn(CH2SiMe3)Se-2,4,6-t-Bu3C6H2]3·0.5C6H14 and [Li(THF)Se-2,4,6-t-Bu3C6H2]3·PhMe
AU - Ruhlandt-Senge, Karin
AU - Power, Philip P.
PY - 1993
Y1 - 1993
N2 - The synthesis and structural characterization of two six-membered ring species containing selenium are described. The compound [Zn(CH2SiMe3)SeMes*]3·0.5 C6H14 (Mes* = 2,4,6-t-Bu3C6H2), (1) was synthesized by the reaction Zn(CH2SiMe3)2 with 1 equiv of HSeMes* in hexane whereas [Li(THF)SeMes*]3·PhMe (2) was obtained by the lithiation of HSeMes* with n-BuLi in the presence of 1 equiv of THF. Each molecule has an M3Se3 core (M = Li, Zn) structure. Unlike the corresponding sulfur species, 1 has a nonplanar Zn3Se3 array and represents the first structure of this type for a selenium compound. The nonplanar Li3Se3 core in 2 involves pyramidal coordination at selenium and almost planar lithium coordination. Both species were characterized by 1H NMR and IR spectroscopy and X-ray crystallography. Crystal data with Mo Kα (γ = 0.710 69 Å) at 130 K are as follows: 1, a = 10.355(5) Å, b = 18.850(8) Å, c = 20.885(8) Å, α = 83.67(3)°, β = 86.92(4)°, γ = 77.62(4)°, V = 3956(3) Å3, Z = 2, space group P1̃, 7550 (I > 3σ(I)) data R = 0.077; 2, a = 9.973(5) Å, b = 18.466(7) Å, c = 21.735(9) Å, α = 74.26(3)°, β = 79.45(4)°, γ = 78.21(2), V = 3725(3) Å3, Z = 2, space group P1̃, 5357 (I > 2σ(I)) data, R = 0.069.
AB - The synthesis and structural characterization of two six-membered ring species containing selenium are described. The compound [Zn(CH2SiMe3)SeMes*]3·0.5 C6H14 (Mes* = 2,4,6-t-Bu3C6H2), (1) was synthesized by the reaction Zn(CH2SiMe3)2 with 1 equiv of HSeMes* in hexane whereas [Li(THF)SeMes*]3·PhMe (2) was obtained by the lithiation of HSeMes* with n-BuLi in the presence of 1 equiv of THF. Each molecule has an M3Se3 core (M = Li, Zn) structure. Unlike the corresponding sulfur species, 1 has a nonplanar Zn3Se3 array and represents the first structure of this type for a selenium compound. The nonplanar Li3Se3 core in 2 involves pyramidal coordination at selenium and almost planar lithium coordination. Both species were characterized by 1H NMR and IR spectroscopy and X-ray crystallography. Crystal data with Mo Kα (γ = 0.710 69 Å) at 130 K are as follows: 1, a = 10.355(5) Å, b = 18.850(8) Å, c = 20.885(8) Å, α = 83.67(3)°, β = 86.92(4)°, γ = 77.62(4)°, V = 3956(3) Å3, Z = 2, space group P1̃, 7550 (I > 3σ(I)) data R = 0.077; 2, a = 9.973(5) Å, b = 18.466(7) Å, c = 21.735(9) Å, α = 74.26(3)°, β = 79.45(4)°, γ = 78.21(2), V = 3725(3) Å3, Z = 2, space group P1̃, 5357 (I > 2σ(I)) data, R = 0.069.
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U2 - 10.1021/ic00073a007
DO - 10.1021/ic00073a007
M3 - Article
AN - SCOPUS:0001251285
SN - 0020-1669
VL - 32
SP - 4505
EP - 4508
JO - Inorganic Chemistry
JF - Inorganic Chemistry
IS - 21
ER -