Whole-mol-ecule disorder of the heterometallic complex di-aqua-1κ(2) O-di-chlorido-2κ(2) Cl-(μ-2-formyl-6-meth-oxy-phenolato-1κ(2) O (1),O (2):2κO (6)){μ-2-meth-oxy-6-[(methyl-imino)-meth-yl]phenolato-1κ(2) N,O (1):2κO (6)}lead(II)nickel(II).

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作者:Vassilyeva Olga Yu, Kokozay Vladimir N, Goreshnik Evgeny
The new mol-ecular complex [NiPb(C(9)H(10)NO(2))(C(8)H(7)NO(3))Cl(2)(H(2)O)(2)] with the Schiff base 2-meth-oxy-6-[(methyl-imino)-meth-yl]phenol and ortho-vanillin ligands, both deprotonated, crystallizes in the monoclinic space group P2(1)/c with one mol-ecule per asymmetric unit. The heterometallic mol-ecule exhibits a whole-mol-ecule orientational disorder [occupancy ratio 0.711†(6): 0.289†(6)] about a pseudo-twofold rotation axis that roughly bis-ects the mol-ecule along the Ni-Pb axis. The Ni centre coordination is distorted octa-hedral [Ni-N/O(eq) = 1.996†(8)-2.021†(7)†à , major component] with two water mol-ecules in the apexes [2.088†(6) and 2.090†(5)†à ]. The Pb atom is six-coordinate in a highly distorted tetra-gonal-bipyramidal geometry. Two phenolato and two methoxo O atoms from the deprotonated ligand moieties are nearly coplanar with the metal centre [Pb-O 2.301†(8)-2.740†(10)†à , major component], while the two chlorides are located on opposite sides of the plane [Pb-Cl = 2.821†(5) and 2.868†(5)†à ]. The Ni-Pb pair of metals is bridged by two phenolato O atoms enabling a metal-metal separation of 3.441†(3)/3.477†(7)†à . Two intra-molecular O-H⋯Cl hydrogen bonds between coordinated aqua and chloride ligands appear to be a reason for the Cl-Pb-Cl and O-Ni-O angles being far from 180°. In the solid state, the well-separated heterometallic mol-ecules are inter-linked by π-π stacking and weak O-H⋯Cl and C-H⋯Cl/O hydrogen bonds. The mol-ecules show no significant inter-molecular inter-actions: the minimal M⋯M distance in the crystal is about 7.65†à (Ni⋯Pb).

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