| Abstract: | Bis(1,2‐diselenosquarato) Metalates A series of 1,2‐diselenosquarato metalates [M(dssq)2]2– (M = Pd2+, Pt2+, Cu2+, Ni2+, Zn2+, Cd2+, Pb2+, VO2+) was available by direct synthesis from the appropriate metal salt with dipotassium 1,2‐diselenosquarate in deoxygenized water under an argon athmosphere. The copper(II)complex, [Cu(dssq)2]2–, and the oxovanadium(IV)complex, [VO(dssq)2]2–, were identified in solution by EPR spectroscopy (parameters: [Cu(dssq)2]2–: g0 = 2.073; a = –76.0 · 10–4 cm–1, a = 47.0 · 10–4 cm–1; [VO(dssq)2]2–: g0 = 1.986; a = 74.9 · 10–4 cm–1). The complexes bis(tetraphenylphosphonium)[bis(1,2‐diselenosquarato)nickelate(II)], (Ph4P)2[Ni(dssq)2], and bis(tetraphenylphosphonium)[bis(1,2‐diselenosquarato)zincate(II)], (Ph4P)2[Zn(dssq)2], were characterized by X‐ray structure analysis. The square‐planar NiII complex (Ph4P)2[Ni(dssq)2] crystallizes in the monoclinic spacegroup P21/n with the unit cell parameters a = 11.1472(8) Å, b = 15.331(1) Å, c = 14.783(1) Å, β = 94.441(1)° and Z = 2. The ZnII‐complex (Ph4P)2[Zn(dssq)2] is tetrahedral coordinated and crystallizes in the monoclinic spacegroup P21/c with the unit cell parameters a = 9.4238(1) Å, b = 18.5823(3) Å, c = 29.5309(5) Å, β = 96.763(1)° and Z = 4. |
