TY - JOUR
T1 - Synthesis of [Tl4Se16]4-
T2 - a novel tetranuclear Tl3+ polyselenide
AU - Dhingra, Sandeep
AU - Liu, Fei
AU - Kanatzidis, Mercouri G.
N1 - Funding Information:
Financial support from the Center for Fundamental Materials Research (CFMR) and the Donors of the Petroleum ResearchF und, administeredb y the American Chemical Society, is gratefully acknowledged. M.G.K. is an A.P. Sloan FoundationF ellow 1991-1993.
PY - 1993/8/15
Y1 - 1993/8/15
N2 - (Ph4P)4[Tl4Se16] was prepared hydrothermally in a sealed pyrex tube by the reaction of TlCl, K2Se4 and Ph4PCl in a 1:1:1 molar ratio at 110 °C for one day. The red crystals were obtained in 50% yield. Crystals of (Ph4P)4[Tl4Se16]: triclinic P1 (No. 2), Z=1, a=12.054(9), b=19.450(10), c=11.799(6) Å, α=104.63(4), β=98.86(6), γ=101.99(6)° and V=2555(3) Å3 at 23 °C, 2θmax=40.0°, μ=120.7 cm-1, Dcalc=2.23. The structure was solved by direct methods. Number of data collected: 5206. Number of unique data having Fo2>3σ(Fo2): 1723. Final R=0.075 and Rw=0.089. [Tl4Se16]4- consists of four, almost already linearly arranged, tetrahedral thallium centers which are coordinated by two chelating Se42-, two bridging Se22- and four bridging Se2- ligands. [Tl4Se16]4- sits on an inversion center and possesses a central {Tl2Se2}2+ planar core. The Tl(1)-Tl(1)′ distance in this core is 3.583(6) Å. These two thallium atoms are then each linked to two cyclic Tl(Se4) fragments via bridging Se22- and Se2- ligands forming Tl2Se(Se2) five-membered rings.
AB - (Ph4P)4[Tl4Se16] was prepared hydrothermally in a sealed pyrex tube by the reaction of TlCl, K2Se4 and Ph4PCl in a 1:1:1 molar ratio at 110 °C for one day. The red crystals were obtained in 50% yield. Crystals of (Ph4P)4[Tl4Se16]: triclinic P1 (No. 2), Z=1, a=12.054(9), b=19.450(10), c=11.799(6) Å, α=104.63(4), β=98.86(6), γ=101.99(6)° and V=2555(3) Å3 at 23 °C, 2θmax=40.0°, μ=120.7 cm-1, Dcalc=2.23. The structure was solved by direct methods. Number of data collected: 5206. Number of unique data having Fo2>3σ(Fo2): 1723. Final R=0.075 and Rw=0.089. [Tl4Se16]4- consists of four, almost already linearly arranged, tetrahedral thallium centers which are coordinated by two chelating Se42-, two bridging Se22- and four bridging Se2- ligands. [Tl4Se16]4- sits on an inversion center and possesses a central {Tl2Se2}2+ planar core. The Tl(1)-Tl(1)′ distance in this core is 3.583(6) Å. These two thallium atoms are then each linked to two cyclic Tl(Se4) fragments via bridging Se22- and Se2- ligands forming Tl2Se(Se2) five-membered rings.
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U2 - 10.1016/S0020-1693(00)83333-2
DO - 10.1016/S0020-1693(00)83333-2
M3 - Article
AN - SCOPUS:0006129094
VL - 210
SP - 237
EP - 239
JO - Inorganica Chimica Acta
JF - Inorganica Chimica Acta
SN - 0020-1693
IS - 2
ER -