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A new magnesium antimony tartrate perchlorate [Mg 2 Sb 2 (C 4 H 2 O 6 ) 2 (H 2 O) 8 ](ClO 4 ) 2 ·5H 2 O,  1 , was synthesized in single crystal form by slowly evaporating an aqueous solution of potassium antimony tartrate and magnesium perchlorate. In the temperature interval 298 K–123 K, the compound undergoes two reversible structural phase transitions. The transition from phase I to phase II at ca. 236 K is second order and the transition from phase II to phase III at ca. 144 K is first order. Phase I has an orthorhombic structure,  P 2 1 2 1 2, a=11.8658(4) Å, b=16.464(1) Å, c=8.3895(4) Å at 298 K, containing infinite chains of antimony tartrate dimeric clusters bridged by MgO 2 (H 2 O) 4  octahedra. The ClO 4  −  anions occupying the interchain space show pronounced dynamic disorder. Phase II is monoclinic,  P 2 1 , a=8.3813(8) Å, b=11.760(1) Å, c=16.289(2) Å, β=92.442(2)° at 153 K. Phase III has an orthorhombic unit cell with quadrupled cell volume,  P 2 1 2 1 2 1 , a=11.6914(8) Å, b=16.176(1) Å, c=33.426(2) Å at 123 K. While the infinite chains in phases II and III are closely similar to those in phase I, the ClO 4  −  anions show different orientations and gradual disappearance of dynamic disorder as the temperature is lowered.

Synthesis and structural phase transitions of [Mg 2 Sb 2 (C 4 H 2 O 6 ) 2 (H 2 O) 8 ](ClO 4 ) 2 ·5H 2 O with complex homochiral chains