TY - JOUR
T1 - Further Studies of the Monooxo-Capped Tritungsten Carboxylate Clusters
AU - Bino, Avi
AU - Albert Cotton, F.
AU - Dori, Zvi
AU - Shaia-Gottlieb, Miriam
AU - Kaponlc, Moshe
PY - 1988/10/1
Y1 - 1988/10/1
N2 - An improved method for the preparation of the [W3O(O2CCH3)6(H2O)3]2+ ion has been found, starting with sodium tungstate, and the compound [W3O(O2CCH3)6(H2O)3]ZnCl4.4H2O (1) has been shown to containthe ion in a completely ordered arrangement. The structure is thus obtained without ambiguity and with more precision than before and has the following principal dimensions (Å): W-W = 2.693 (1), 2.693 (1), 2.712 (1); W-(μ3-0)(av) = 1.98 [1]; W-OH2(av) = 2.17 [2]; W-O(acetate)(av) = 2.078, 2.055 on the capped and uncapped sides, respectively. Compound 1 crystallizes in space group P21/n with a= 14.324 (2) Å, b = 17.081 (2) Å, c = 13.715 (2) Å, β = 90.87 (3)°, and Z = 4. Conversion of the cation in compound 1 to the [W3O(O2CCH3)5(OCH3)(H2O)3]2+ cation has been effected, and this has been isolated and structurally characterized as the compound [W3O(O2CCH3)5(OCH3)(H2O)3]ZnCl4.7H2O (2), which crystallizes in space group P1 with unit cell dimensionst a = 14.063 (7)Å, b = 14.216 (7) Å, c= 9.613 (5) Å, α = 103.78 (5)°,β = 100.91 (5)°, γ = 107.38 (5)°, and Z = 2. The cation in compound 2 (aqueous solution) has a proton NMR spectrum in accord with its solid-state structure, and its UV-visible spectrum shows expected similarities to that of its symmetrical parent.
AB - An improved method for the preparation of the [W3O(O2CCH3)6(H2O)3]2+ ion has been found, starting with sodium tungstate, and the compound [W3O(O2CCH3)6(H2O)3]ZnCl4.4H2O (1) has been shown to containthe ion in a completely ordered arrangement. The structure is thus obtained without ambiguity and with more precision than before and has the following principal dimensions (Å): W-W = 2.693 (1), 2.693 (1), 2.712 (1); W-(μ3-0)(av) = 1.98 [1]; W-OH2(av) = 2.17 [2]; W-O(acetate)(av) = 2.078, 2.055 on the capped and uncapped sides, respectively. Compound 1 crystallizes in space group P21/n with a= 14.324 (2) Å, b = 17.081 (2) Å, c = 13.715 (2) Å, β = 90.87 (3)°, and Z = 4. Conversion of the cation in compound 1 to the [W3O(O2CCH3)5(OCH3)(H2O)3]2+ cation has been effected, and this has been isolated and structurally characterized as the compound [W3O(O2CCH3)5(OCH3)(H2O)3]ZnCl4.7H2O (2), which crystallizes in space group P1 with unit cell dimensionst a = 14.063 (7)Å, b = 14.216 (7) Å, c= 9.613 (5) Å, α = 103.78 (5)°,β = 100.91 (5)°, γ = 107.38 (5)°, and Z = 2. The cation in compound 2 (aqueous solution) has a proton NMR spectrum in accord with its solid-state structure, and its UV-visible spectrum shows expected similarities to that of its symmetrical parent.
UR - http://www.scopus.com/inward/record.url?scp=0011554896&partnerID=8YFLogxK
U2 - 10.1021/ic00293a030
DO - 10.1021/ic00293a030
M3 - ???researchoutput.researchoutputtypes.contributiontojournal.article???
AN - SCOPUS:0011554896
SN - 0020-1669
VL - 27
SP - 3592
EP - 3596
JO - Inorganic Chemistry
JF - Inorganic Chemistry
IS - 20
ER -