On the sequence of three related phases of [Ni(H2O)2(15-crown-5)](HSO4)2 in the temperature range 110-295 K

Acta Crystallographica. Section B, Structural Science
Maxime A Siegler, Eli Stavitski

Abstract

Attempts to prepare the compound [Ni(H(2)O)(2)(15-crown-5)](X)(2) were eventually successful with X = NO(3)(-) provided that a synthetic route aimed at restricting water was followed. Application of this method was extended to make the analogous compound with X = HSO(4)(-), for which three symmetry-related phases were isolated between 295 and 110 K: a room-temperature phase with Z' = (1/2) [phase (I)], an intermediate-temperature phase with Z' = 1 [phase (II)] and a low-temperature phase with Z' = 2 [phase (III)]. The phases are related by two reversible solid-solid phase transitions, and both transitions take place without a significant loss of crystallinity. In the phase sequence (I) <--> (II) <--> (III) (Z': (1/2) <--> 1 <--> 2), the crystal packing remains remarkably similar but the degree of order in the crystal changes significantly; the structure is very disordered at room and intermediate temperatures but is ordered at 110 K. The compound [Ni(H(2)O)(2)(15-crown-5)](HSO(4))(2) has a complicated hydrogen-bonding network, which contains O-H...O bonds between the counterions. Structural changes are largest along some face-diagonal directions in the sequence (I) <--> (II) <--> (III).

References

Apr 1, 1990·Acta Crystallographica. Section B, Structural Science·M C EtterJ Bernstein
Jul 1, 1994·Ophthalmic & Physiological Optics : the Journal of the British College of Ophthalmic Opticians (Optometrists)·M BonackerW Jaschinski
Aug 16, 2000·Acta Crystallographica. Section B, Structural Science·T Steiner
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Nov 25, 2005·Acta Crystallographica. Section B, Structural Science·Xiang HaoCarolyn Pratt Brock
Dec 25, 2007·Acta Crystallographica. Section A, Foundations of Crystallography·George M Sheldrick
Nov 26, 2008·Acta Crystallographica. Section B, Structural Science·Maxime A SieglerCarolyn Pratt Brock
Nov 26, 2008·Acta Crystallographica. Section B, Structural Science·Maxime A SieglerCarolyn Pratt Brock
Mar 23, 2010·Acta Crystallographica. Section B, Structural Science·Maxime A SieglerCarolyn Pratt Brock

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Citations

Jul 5, 2019·Acta Crystallographica. Section C, Structural Chemistry·Ricardo Baggio

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