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Solid–Solid Phase Transitions in [trans-Pt(PMe3)2(C≡CC6H4R)2]-Containing Materials (R = O(CH2)nH; n = 6, 9, 12, and 15)
Organometallics ( IF 2.5 ) Pub Date : 2018-07-17 , DOI: 10.1021/acs.organomet.8b00304 Gabriel Marineau Plante 1 , Daniel Fortin 1 , Armand Soldera 1 , Pierre D. Harvey 1
Organometallics ( IF 2.5 ) Pub Date : 2018-07-17 , DOI: 10.1021/acs.organomet.8b00304 Gabriel Marineau Plante 1 , Daniel Fortin 1 , Armand Soldera 1 , Pierre D. Harvey 1
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The title complexes were prepared in Hagihara conditions and were investigated by single crystal X-ray crystallography (n = 6, [Pt]C6; n = 12, [Pt]C12), X-ray powder diffraction (powder XRD), differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA, [Pt]C12), and steady-state and time-resolved solid state UV–vis and emission spectroscopy at 298 and 77 K. [Pt]C6 complex exhibits no phase change with the temperature. Concurrently, [Pt]C9 (n = 9) and [Pt]C12 complexes exhibit an irreversible Tendo values of 104 and 119 °C, respectively, associated with a thermal annealing. Finally, [Pt]C15 (n = 15) complex exhibit a reversible thermal processes with a large hysteresis (Tendo = 126 °C, Texo = 140 °C) followed by a glass transition (Tendo = 146 °C, Texo = 69 °C) as depicted by DSC. These phase changes are accompanied by a decrease in triplet excited state lifetimes upon cycling the sample temperature over and under the transition temperatures. These various thermal processes induce a significant decrease in emission lifetimes, strongly suggesting the presence of a reorganization of the complexes in the solid state favoring more chain-chromophore contacts, thus promoting nonradiative “knocking” processes.
中文翻译：
固-固相变的[反式-Pt（PME 3）2（C≡CC 6 ħ 4 R）2 ]含材料（R = O（CH 2）Ñ H; Ñ = 6，9，12，和15 ）
在Ha原条件下制备标题配合物，并通过单晶X射线晶体学（n = 6，[Pt] C 6；n = 12，[Pt] C 12），X射线粉末衍射（粉末XRD），差示扫描量热法（DSC），热重分析（TGA，[Pt] C 12）以及在298和77 K时的稳态和时间分辨固态紫外可见光谱和发射光谱。[Pt] C 6络合物没有表现出相随温度变化。同时，[Pt] C 9（n = 9）和[Pt] C 12配合物表现出不可逆的T内热值分别为104和119°C，与热退火有关。最后，[Pt] C 15（n = 15）配合物表现出可逆的热过程，并具有较大的磁滞（T end = 126°C，T exo = 140°C），随后发生玻璃化转变（T end = 146°C，Ť外= 69°C），如DSC所述。当样品温度在转变温度之上和之下循环时，这些相变伴随着三重态激发态寿命的减少。这些不同的热过程导致发射寿命的显着减少，强烈表明固态复合物的重组有利于更多的链发色团接触，从而促进了非辐射的“敲除”过程。
更新日期：2018-07-18
中文翻译：
固-固相变的[反式-Pt（PME 3）2（C≡CC 6 ħ 4 R）2 ]含材料（R = O（CH 2）Ñ H; Ñ = 6，9，12，和15 ）
在Ha原条件下制备标题配合物，并通过单晶X射线晶体学（n = 6，[Pt] C 6；n = 12，[Pt] C 12），X射线粉末衍射（粉末XRD），差示扫描量热法（DSC），热重分析（TGA，[Pt] C 12）以及在298和77 K时的稳态和时间分辨固态紫外可见光谱和发射光谱。[Pt] C 6络合物没有表现出相随温度变化。同时，[Pt] C 9（n = 9）和[Pt] C 12配合物表现出不可逆的T内热值分别为104和119°C，与热退火有关。最后，[Pt] C 15（n = 15）配合物表现出可逆的热过程，并具有较大的磁滞（T end = 126°C，T exo = 140°C），随后发生玻璃化转变（T end = 146°C，Ť外= 69°C），如DSC所述。当样品温度在转变温度之上和之下循环时，这些相变伴随着三重态激发态寿命的减少。这些不同的热过程导致发射寿命的显着减少，强烈表明固态复合物的重组有利于更多的链发色团接触，从而促进了非辐射的“敲除”过程。
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