Although phase transition materials (PTMs) under external stimuli are of great research interest duo to their rich potential applications, it is still challenging to explore multi-responsive PTMs. Herein, two different phases of organic-inorganic hybrid copper-based halides, α-and β-Gua 3 Cu 2 I 5 (Gua + = CN 3 H 6 + ), were synthesized by solvent evaporation method, which they crystalize in the noncentrosymmetric space group Fdd2 with zero-dimensional structure and centrosymmetric space group C2/c with one-dimensional metal-halogen framework, respectively. Interestingly, it is firstly demonstrated that Gua 3 Cu 2 I 5 simultaneously possesses reversible PL conversion and NLO switching properties in response to thermal stimulus. Strikingly, apart from heat, its structural phase transition can also be triggered by crystalline-phase-recognition (CPR) and mechanical force. These new findings may pave a path for future exploration of PTMs with multiple physical properties.

A series of pentanary chalcogenoborates (A 3 X)-[InB 12 (InQ 4 ) 3 ] (A = K, Rb, Cs; X = Cl, Br, I; Q = S, Se) were obtained by high-temperature solid-state reactions. These saltinclusion chalcogenides crystallize in the hexagonal space group P6 3 22, a type of Kleinman-forbidden noncentrosymmetric structure. Their structures feature a [InB 12 (InQ 4 ) 3 ] open framework built by InQ 6 octahedra and InQ 4 tetrahedra consolidated B 12 cluster, which accomodates octahedral cavities for XA 6 units. They are second-harmonic generation active, and their optical properties were studied experimentally and theoretically. This work can evoke more interest in chalcogenoborate-based second-order nonlinear optical materials.

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Although phase transition materials (PTMs) under external stimuli are of great research interest duo to their rich potential applications, it is still challenging to explore multi‐responsive PTMs. Herein, two different phases of organic–inorganic hybrid copper‐based halides, α‐ and β‐Gua3Cu2I5 (Gua+=CN3H6+), were synthesized by solvent evaporation method, which they crystalize in the noncentrosymmetric space group Fdd2 with zero‐dimensional structure and centrosymmetric space group C2/c with one‐dimensional metal‐halogen framework, respectively. Interestingly, it is firstly demonstrated that Gua3Cu2I5 simultaneously possesses reversible PL conversion and NLO switching properties in response to thermal stimulus. Strikingly, apart from heat, its structural phase transition can also be triggered by crystalline‐phase‐recognition (CPR) and mechanical force. These new findings may pave a path for future exploration of PTMs with multiple physical properties.