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. 2022 Aug 18;78(Pt 9):926-931.
doi: 10.1107/S2056989022007964. eCollection 2022 Sep 1.

Crystal structure of an indium-salicyl-hydroximate complex cation: [In4(H2shi)8(H2O)6](NO3)4·8.57H2O

Ozha A Aziz  1 , Matthias Zeller  2 , Curtis M Zaleski  1
Affiliations

Crystal structure of an indium-salicyl-hydroximate complex cation: [In4(H2shi)8(H2O)6](NO3)4·8.57H2O

Ozha A Aziz et al. Acta Crystallogr E Crystallogr Commun. .

Abstract

The synthesis and crystal structure for the title compound, hexa-aqua-hexa-kis(μ-2-hy-droxy-benzene-carbo-hydrox-a-mato)bis-(2-hy-droxy-benzene-carbo-hydrox-a-m-ato)tetra-indium(III) tetra-nitrate 8.57-hydrate + unknown solvent, [In4(H2shi)8(H2O)6](NO3)4·8.57H2O·solvent, where H2shi- is salicylhydrox-imate (C7H5NO3), are reported. The complex cation of the structure, [In4(H2shi)8(H2O)6]4+, is a dimer with a step-like topology and possesses an inversion center that relates each [In2(H2shi)4(H2O)3]2+ side of the complex cation. Each InIII ion is seven-coordinate with a penta-gonal-bipyramidal geometry, and the salicyl-hydroximate ligands have a 1- charge as only the oxime oxygen of the ligand is deprotonated. Four inter-stitial nitrate anions maintain the charge balance of the compound. One of the nitrate anions (and its symmetry equivalent) is disordered over two different orientations with an occupancy ratio of 0.557 (7) to 0.443 (7). The inter-stitial solvent water mol-ecules show substantial disorder. Approximately 8.57 water mol-ecules per formula unit were refined as disordered and partially occupied, while a suitable model could not be devised for the other extensively disordered solvent mol-ecules (water and possibly methanol as this was the synthesis solvent). Thus, these latter solvent mol-ecules were instead treated with the SQUEEZE routine [Spek (2015). Acta Cryst. C71, 9-18.] as implemented in the program PLATON, and the procedure corrected for 151 electrons within solvent-accessible voids of 367 Å3.

Keywords: crystal structure; indium; salicyl­hydroxamic acid.

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Figures

Figure 1
Figure 1
The single-crystal X-ray structure of [In4(H2shi)8(H2O)6](NO3)4·8.57H2O·solvent, 1, with displacement ellipsoids at the 50% probability level [symmetry code: (i) −x + 1, −y + 1, −z + 1]. (a) top view with only the metal ions and heteroatoms labeled for clarity and (b) side view with only the metal ions and axial heteroatoms labeled. In addition, hydrogen atoms, inter­stitial nitrate anions, inter­stitial water mol­ecules, and disorder have been omitted for clarity. Color scheme: green – In, red – oxygen, dark blue – nitro­gen, and gray – carbon. All figures were generated with the program Mercury (Macrae et al., 2020 ▸).
Figure 2
Figure 2
Top view of a [In2(H2shi)4(H2O)3]2+ unit of 1 with displacement ellipsoids at the 50% probability level [symmetry code: (i) −x + 1, −y + 1, −z + 1]. In addition, the intra­molecular hydrogen bonding in 1 between the hydrogen atoms (white) of the oxime nitro­gen atoms and the phenol oxygen atoms and between the hydrogen atoms of the oxime nitro­gen atoms and the carbonyl oxygen atoms are displayed. See Fig. 1 ▸ for additional display details.
Figure 3
Figure 3
Inter­molecular hydrogen bonding in 1 between the hydrogen atom (white) of the water mol­ecule associated with O13 (coordinated to In1) and the oxime oxygen atom (O1) of a neighboring complex cation of 1 [symmetry code: (iv) −x + 1, −y + 1, −z]. The hydrogen bonding results in a one-dimensional chain. For clarity only the oxygen atoms involved in the hydrogen bonding have been labeled. See Fig. 1 ▸ for additional display details.
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