TY - JOUR
T1 - Synthesis and Characterization of the Strontium Thiolate Sr(SMes*)2(THF)4•2THF (Mes* = 2,4,6-tBu3C6H2) and Selenolate Sr(SeMes*)2(THF)4•2THF. Structural Investigation of SrI2(THF)5
AU - Ruhlandt-Senge, Karin
AU - Davis, Kelly
AU - Dalai, Sona
AU - Englich, Ulrich
AU - Senge, Mathias O.
PY - 1995/5/1
Y1 - 1995/5/1
N2 - The syntheses and structural characterization of the strontium thiolate Sr(SMes*)2(THF)4•2THF, 1 (Mes* = 2,4,6-tBu3C6H2), and selenolate Sr(SeMes*)2(THF)4•2THF, 2, are described. We also report the synthesis and structural characterization of SrI2(THF)5,3, the apparent starting material for the synthesis of 1 and 2. 3 exhibits pentagonal bipyramidal geometry at the strontium atom. 3 can be prepared by dissolving SrI2 in THF, while the treatment of 3 with 2 equiv of the sterically demanding potassium thiolate and selenolate in THF affords 1 and 2 in good yields. 1 and 2 exhibit distorted octahedral environments at the metal center, with the degree of distortion much more significant for the thiolato derivative. 1 and 2 were characterized by 1H NMR and IR spectroscopy, elemental analysis, and X-ray crystallography; 3 was characterized by single-crystal structure analysis. Crystal data with Mo Kα (λ = 0.710 73 (Å) at 213 K are as follows. 1: a = 18.535(4) Å, b = 19.222(4) Å, c = 18.775(4) Å, β = 107.30(3)°, V = 6387(2) Å3, Z = 4, monoclinic, space group I2la, 2254 (I > 3σ(I)) data, R = 0.071. 2: a = 18.330(4) Å, b = 19.498(4) Å, c = 18.608(4) Å, β = 105.52(3)°, V = 6408(3) Å3, Z = 4, monoclinic, space group I2la, 2331 (I > 3σ(I)) data, R = 0.057. 3: a = 8.851(1) Å, c = 35.353(7) Å, V = 2770(1) Å3, Z = 4, tetragonal, space group P43212 939 (I > 3σ(I)) data, R = 0.069.
AB - The syntheses and structural characterization of the strontium thiolate Sr(SMes*)2(THF)4•2THF, 1 (Mes* = 2,4,6-tBu3C6H2), and selenolate Sr(SeMes*)2(THF)4•2THF, 2, are described. We also report the synthesis and structural characterization of SrI2(THF)5,3, the apparent starting material for the synthesis of 1 and 2. 3 exhibits pentagonal bipyramidal geometry at the strontium atom. 3 can be prepared by dissolving SrI2 in THF, while the treatment of 3 with 2 equiv of the sterically demanding potassium thiolate and selenolate in THF affords 1 and 2 in good yields. 1 and 2 exhibit distorted octahedral environments at the metal center, with the degree of distortion much more significant for the thiolato derivative. 1 and 2 were characterized by 1H NMR and IR spectroscopy, elemental analysis, and X-ray crystallography; 3 was characterized by single-crystal structure analysis. Crystal data with Mo Kα (λ = 0.710 73 (Å) at 213 K are as follows. 1: a = 18.535(4) Å, b = 19.222(4) Å, c = 18.775(4) Å, β = 107.30(3)°, V = 6387(2) Å3, Z = 4, monoclinic, space group I2la, 2254 (I > 3σ(I)) data, R = 0.071. 2: a = 18.330(4) Å, b = 19.498(4) Å, c = 18.608(4) Å, β = 105.52(3)°, V = 6408(3) Å3, Z = 4, monoclinic, space group I2la, 2331 (I > 3σ(I)) data, R = 0.057. 3: a = 8.851(1) Å, c = 35.353(7) Å, V = 2770(1) Å3, Z = 4, tetragonal, space group P43212 939 (I > 3σ(I)) data, R = 0.069.
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U2 - 10.1021/ic00114a016
DO - 10.1021/ic00114a016
M3 - Article
AN - SCOPUS:0000074957
SN - 0020-1669
VL - 34
SP - 2587
EP - 2592
JO - Inorganic Chemistry
JF - Inorganic Chemistry
IS - 10
ER -