Inorganic Chemistry, Vol.33, No.19, 4351-4359, 1994
Simultaneous First-Sphere and 2nd-Sphere Coordination - Organopalladium Crown-Ether Complexes as Metalloreceptors for O-Aminopyridine Derivatives
The complexes [Pd(L)(CH3CN)][BF4] (L = 2, 14-dithia[15]-m-cyclophane (L(o)), 5-oxa-2,8-dithia[9]-m-cyclophane (L(1)), 5,8,11-trioxa-2,14-dithia[15]-m-cyclophane (L(3))) were prepared by palladation of the respective thiacyclophane employing [Pd(CH3CN)(4)][BF4](2). For studies involving L(1), [Pd(L(1))(CH3CN)][CF3SO3] was also prepared in an analogous manner from [Pd(CH3CN)(4)][CF3SO3]. [Pd(L(0))(CH3CN)][BF4].CH3CN crystallized in the space group C2/c with a = 13.237(4) Angstrom A, b = 19.206(2) Angstrom A, c = 20.232(2) Angstrom A, V = 5168(3) Angstrom A(3), and Z = 8. The structure refined to R = 5.62% and R(w) = 4.76% for 3112 reflections with F-o(2) > 3 sigma(F-o(2)). [Pd(L(1))(CH3CN)][CF3SO3] crystallized in the space group P2(1)/c with a = 8.639(2) Angstrom A, b = 17.165(2) Angstrom A, c = 13.099(2) Angstrom A, beta = 91.85(2)degrees, V = 1941.3(5) Angstrom A(3), and Z = 4.
Keywords:RAY CRYSTAL-STRUCTURE;CATIONIC RHODIUM COMPLEXES;MOLECULAR RECOGNITION;2ND-SPHERE COORDINATION;2-POINT FIXATION;THIOETHER LIGAND;HYDROGEN-BONDS;18-CROWN-6;RECEPTORS;(Y(OH2)8)CL3.(15-CROWN-5)