Trinuclear Co(II) and Ni(II) complexes with tridentate fluorine, [M-3(mu(3)-F)(CF3COO)(6)(CF3COOH)(3)](-): Synthesis and crystal structureстатья
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Аннотация:The first trinuclear carboxylates of divalent metals containing a planar coordinated tridentate fluorine atom, NO[M-3( mu(3)-F)(CF3COO)(6)(CF3COOH)(3)], where M = Ni (1), Co (11), and K[Ni-3(mu(3)-F)(CF3COO)(6)(CF3COOH)(3)] (III), were synthesized and studied by X-ray diffraction. Compounds I-III were obtained by crystallization from solutions of Ni(NO3)(2) (1), Co(NO3)(2) (11), or Ni(NO3)(2) and KHF2 (111) in trifluoroacetic acid in the presence of fluoride ions, anhydrous nitric acid, and phosphoric anhydride as the drying agent. As shown by X-ray diffraction, the isotypical compounds I and 11 crystallize in the orthorhombic system, space group Pbca, Z = 8, with the following parameters: for 1, a = 27.812(6) Angstrom, b = 17.750(3) A, c = 15.719(3) Angstrom, V = 7760(3) Angstrom(3), R-1 = 0.0443; for II, a = 27.855(7) Angstrom, b = 18.023(4) Angstrom, c = 15.736(3) Angstrom, V = 7900(3) Angstrom(3), R-1 = 0.0533. The crystals of III are monoclinic, space group P2(1)/c, a = 13.578(3) Angstrom, b = 14.371(2) Angstrom, c = 20.754(5) Angstrom, beta = 104.32(2)degrees, V = 3923.9(14) Angstrom(3), Z = 4, R-1 = 0.0408. The structural units in 1, 11, and III are NO+ (K+) cations and trinuclear [M-4(mu(3)-F)(CF3COO)(6)(CF3COOH)(3)](-) anions constructed similarly to trinuclear 3d-metal oxocarboxylates. The M atoms form a nearly regular M3F triangle centered by the fluorine atom, which coordinates the metal atoms at average Ni-F distances of 1.999 (1) and 1.989 (111) and a Co-F distance of 2.033 Angstrom (11). Each side of the M3F triangle plane bears three bridging bidentate trifluoroacetate groups, which connect the metal atoms in pairs at average (MM)-M-... distances of 3.46, 3.52, and 3.44 Angstrom in structures 1, 11 and III, respectively. Each metal atom coordinates the carbonyl O atom of a CF3COOH molecule trans to the mu(3)-fluorine atom, thus completing the coordination environment to a distorted octahedron.