A. Paulo et al., COORDINATION OF TETRAKIS(PYRAZOLYL)BORATE IN RHENIUM COMPLEXES CONTAINING THE [RE-V=0](3+) CORE, Inorganic chemistry, 35(7), 1996, pp. 1798-1807
The complex [Re{eta(3)-B(pz)(4)}(OMe)(2)] (1) reacts with potentially
bidentate protic substrates yielding several monomeric and dimeric oxo
rhenium compounds in which the tetrakis(pyrazolyl)borate presents diff
erent coordination modes: [ReO(acac){eta(2)-B(pz)(4)}(OMe)] (3), [ReO(
acac){eta(2)-B(pz)(4)}](2)(mu-O) (4), [ReO(eta(2)-B(pz)(4)}-(quinolin-
8-olate)(OMe)] (5), [ReO{eta(2)-B(pz)(4)}(OMe)(pz)(pz*H)](pz* = pz (6
) or 3,5-Me(2)pz (7)), [ReO{eta(2)-B(pz)(4)}(mu-pz)](2)(mu-O) (pz* =
pz (9) or 3,5-Me(2)pz (10)), [ReO(HNCH2CH2NH){eta(3)-B(pz)(4)}] (14),
and [ReO(m-nitrophenyl-o-diaminate){eta(3)-B(pz)(4)}] (15). Using the
analogous alkoxide [ReO{eta(3)-B(pz)(4)}(OEt)(2)] (2), the compound [R
eO{eta(2)-B(pz)(4)}(OEt)(pz)(pzH)] (8) has also been obtained. Compoun
ds 3 and 5 react with trimethylsilyl chloride providing the monochlori
des [ReO(acac){eta(2)-B(pz)(4)}Cl] (12) and [ReO{eta(2)-B(pz)(4)}(quin
olin-8-olate)Cl] (13), respectively. Compounds 9, 10, and 14 were also
prepared by reacting [ReO{mu-O){B(pz)(4)}](2) (11) with the respectiv
e substrates. The new compounds 3-10 and 12-15 were characterized by e
lemental analysis and IR and H-1 NMR spectroscopies. Compounds 3, 4, a
nd 9 have also been characterized by X-ray crystallography. Compounds
3 and 4 both crystallize in the monoclinic space group P2(1)/c, with a
= 7.862(1) Angstrom, b = 14.152(2) Angstrom, c = 19.975(3) Angstrom,
beta = 91.79(1)degrees, V = 2221(1) Angstrom(3) and Z = 4 (3) and a =
13.547(2) Angstrom, b = 9.959(1) Angstrom, c = 15.878(2) Angstrom, bet
a = 102.00(1)degrees, V = 2095(1) Angstrom(3) and Z = 2 (4). Compound
9 crystallizes in the monoclinic space group P2(1), with cell paramete
rs a = 11.086(2) Angstrom, b = 15.269(1) Angstrom, c = 12.133(1) Angst
rom, beta 93.51(1)degrees, V = 2050(1) Angstrom(3) and Z = 2.