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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Phosphite copper(i) trifluoroacetates [((RO)_3P) _mCuO_2CCF_3] (m = 1, 2, 3): Synthesis, solid state structures and their potential use as CVD precursors
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Phosphite copper(i) trifluoroacetates [((RO)_3P) _mCuO_2CCF_3] (m = 1, 2, 3): Synthesis, solid state structures and their potential use as CVD precursors

机译：亚磷酸三氟乙酸亚铜（i）[[（（RO）_3P）_mCuO_2CCF_3]（m = 1，2，3）：合成，固态结构及其作为CVD前体的潜在用途

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摘要

Metal-organics [((RO)_3P)_mCuO_2CCF _3] (R = CH_3: 11a, m = 1; 11b, m = 2; 11c, m = 3. R = CH_2CH_3: 12a, m = 1; 12b, m = 2; 12c, m = 3. R = CH _2CF_3: 13a, m = 1; 13b, m = 2; 13c, m = 3) are either accessible by the reaction of [((RO)_3P)_mCuCl] (R = CH _3: 5a, m = 1; 5b, m = 2; 5c, m = 3. R = CH_2CH_3: 6a, m = 1; 6b, m = 2; 6c, m = 3) with [KO_2CCF_3] (7), or treatment of [Cu_2O] (8) with HO_2CCF_3 (9) and P(OR)_3 (2, R = CH_3; 3, R = CH_2CH_3; 4, R = CH_2CF_3). ~(31)P{~1H} NMR spectra [((CH_3O)_3P)_mCuO_2CCF_3] (m = 1, 1.5, 2, 2.5, 3, 3.5, and 4) have been studied at 25 and -80 °C showing phosphite ligand exchange in solution. The molecular structures of 11a and 13a-13c in the solid state are reported. Complexes 11a and 13a are tetramers featuring μ-η~2(1κO:2κO′)- and μ~3-η~2(1κO:2κO′:3κO′) -(11a) or μ~3-η~2(1κO:2κO′: 3κO′)-bonded O_2CCF_3 ligands (13a) with the Cu(i) ions being part of CuPO_2 and CuPO_3 units (11a), while in 13a solely a CuPO_3 moiety is present. Skeletal isomerism of 11avs.13a is discussed. Compound 13b is dimeric ({CuP_2O _2}_2) with pseudo-tetrahedral Cu environments and μ-η~2(1κO:2κO′)O_2CCF_3 functionalities. In monomeric 13c the O_2CCF_3 ligand is η~1(κO)-bonded to a tetra-coordinated Cu(i) ion. The thermal solid state properties of 11, 12 and 13 were studied by Thermo Gravimetry (TG). These complexes decompose by phosphite elimination, decarboxylation and dealkylation. Hot-wall Chemical Vapour Deposition (CVD) experiments were carried out at 380 °C using 11c as precursor for the deposition of copper onto pieces of TiN-coated oxidized silicon substrates. Copper layers of high purity were obtained with grain sizes between 200-1200 nm.
机译：金属有机物[[（（RO）_3P）_mCuO_2CCF _3]（R = CH_3：11a，m = 1; 11b，m = 2; 11c，m = 3）R = CH_2CH_3：12a，m = 1; 12b，m = 2; 12c，m =3。R = CH _2CF_3：13a，m = 1; 13b，m = 2; 13c，m = 3）均可通过[[（RO）_3P）_mCuCl]的反应得到（R = CH _3：5a，m = 1; 5b，m = 2; 5c，m =3。R= CH_2CH_3：6a，m = 1; 6b，m = 2; 6c，m = 3），带有[KO_2CCF_3]（7） ，或用HO_2CCF_3（9）和P（OR）_3（2，R = CH_3; 3，R = CH_2CH_3; 4，R = CH_2CF_3）处理[Cu_2O]（8）。在25和-80°C下研究了〜（31）P {〜1H} NMR光谱[[（（CH_3O）_3P）_mCuO_2CCF_3]（m = 1、1.5、2、2.5、3、3.5和4），显示亚磷酸盐溶液中的配体交换。报告了固态的11a和13a-13c的分子结构。配合物11a和13a是具有μ-η〜2（1κO：2κO'）-和μ〜3-η〜2（1κO：2κO'：3κO'）-（11a）或μ〜3-η〜2（1κO）的四聚体：2κO'：3κO'）键合的O_2CCF_3配体（13a），其中Cu（i）离子是CuPO_2和CuPO_3单元（11a）的一部分，而在13a中仅存在CuPO_3部分。讨论了11avs.13a的骨架异构现象。化合物13b是具有伪四面体Cu环境和μ-η〜2（1κO：2κO'）O_2CCF_3官能度的二聚体（{CuP_2O _2} _2）。在单体13c中，O_2CCF_3配体通过η〜1（κO）键与四配位的Cu（i）离子键合。通过热重分析（TG）研究了11、12和13的热固态性质。这些配合物通过亚磷酸酯消除，脱羧和脱烷基而分解。热壁化学气相沉积（CVD）实验是在380°C下进行的，使用11c作为前驱体，用于将铜沉积到TiN涂层氧化硅基板上。获得具有200-1200nm之间的晶粒尺寸的高纯度的铜层。

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