本實驗室以雙氮基脒為配基合成出低配位低價數之雙鉻金屬五重鍵錯合物Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2 (1)。將錯合物1與一當量炔類分子如三甲基矽乙炔、叔丁基乙炔與苯乙炔進行反應，則分別得到(μ-κ2-(CH3)3SiCCH)Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2 (2)、(μ-κ2-(CH3)3CCCH)Cr2[μ
-κ2-HC(N-2,6-iPr2C6H3)2]2 (3)及(μ-κ2-(C6H5)CCH)Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2 (4)等三轉軸雙鉻四重鍵錯合物；另外僅在錯合物1與三甲基矽乙炔的反應中，我們發現三當量的三甲基矽乙炔與錯合物1反應後能夠形成[μ-η6:η6-(1,3,5-(SiMe3)3C6H3)]Cr2[κ2-HC(N-2,6-iPr2C6H3)2]2 (5)反三明治結構的雙鉻錯合物，且我們發現將錯合物5溶於四氫呋喃中或是與2,4,6-三甲基苯甲腈反應，會再次形成雙鉻五重鍵錯合物1。若將錯合物1或5與腈類分子如苯甲腈、2-甲基苯甲腈、4-甲基苯甲腈及3-甲基-4-甲氧基苯甲腈反應，皆可得到相同結構的產物，分別為(μ-κ1C:κ2N-PhCN)2(κ1-PhCN)2Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2 (6)、(μ-κ1C:κ2N-o-tolylCN)2(κ1-o-tolylCN)2Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2 (7)、(μ-κ1C:κ2N-p-tolyl-CN)2(κ1-p-tolylCN)2Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2 (8)及(μ-κ1C:κ2N-2-methoxy-m-tolylCN)2(κ1-2-methoxy-m-tolylCN)2Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2 (9)。我們也嘗試錯合物5與三甲基矽乙炔、1-戊炔與苯乙炔的反應，研究其催化三聚合環化反應的進行。最後，我們也嘗試將錯合物1與吡啶硼烷反應，發現其進行了碳-氫鍵活化反應，並得到Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2(μ-H)(μ-κ2-C5H4BH3) (10)。
另外我們以β-二酮亞胺配基合成出反三明治雙鉻錯合物(μ-η6:η6-C7H8)[Cr(Nacnac)]2 (11) (Nacnac = HC((CMe)NC6H3-iPr2)2)並與腈類分子進行反應，當錯合物11與2-甲基苯甲腈反應，得到Cr(Nacnac)(o-tolylCN)[NH(3-(o-tolyl)isoquinoline)] (12)；當11與2,4,6-三甲基苯甲腈反應，則得到Cr(Nacnac)[κ2-HN(C-2,4,6-Me3C6H2)2NH] (13)。兩個反應皆有碳-碳鍵偶合的發生。
最後我們嘗試了以鉻單核錯合物Cr[κ2-HC(N-2,6-iPr2C6H3)2]2 (14)與二氯亞鈷反應，得到了異核雙核金屬錯合物Co[κ1-HC(N-2,6-iPr2C6H3)2][μ-κ2-HC(N-2,6
-iPr2C6H3)2]Cr[κ2-HC(N-2,6-iPr2C6H3)2] (15)。

Our group have reported the synthesis of low-coordinate and low-valent quintuply-bonded dichromium complex Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2 (1). Treatment of 1 with alkynes afforded a family of alkyne-complexed compounds (μ-κ2-(CH3)3SiCCH)Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2 (2), (μ-κ2-(CH3)3CCCH)Cr2[μ-
κ2-HC(N-2,6-iPr2C6H3)2]2 (3) and (μ-κ2-(C6H5)CCH)Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2 (4), which all feature a Cr-Cr quadruple bond. When treatment of 1 with three equivalents of ethynyltrimethylsilane, we obtain an inverted-sandwich compound [μ-η6:η6-(1,3,5-(SiMe3)3C6H3)]Cr2[κ2-HC(N-2,6-iPr2C6H3)2]2 (5). This result is only observed in the reaction with 1 and ethynyltrimethylsilane. Surprisingly, after 5 dissolved in tetrahydrofuran or reacts with 2,4,6-trimethylbenzonitrile, 5 turns back to 1. Treatment of 1 or 5 with a series of benzonitrile, they show identical reacitivity and afforded compounds with same structure (μ-κ1C:κ2N-PhCN)2(κ1-PhCN)2Cr2[μ-κ2-HC(
-N-2,6-iPr2C6H3)2]2 (6), (μ-κ1C:κ2N-o-tolylCN)2(κ1-o-tolylCN)2Cr2[μ-κ2-HC(N-2,6-iP
-r2C6H3)2]2 (7), (μ-κ1C:κ2N-p-tolyl-CN)2(κ1-p-tolylCN)2Cr2[μ-κ2-HC(N-2,6-iPr2C6H3
-)2]2 (8) and (μ-κ1C:κ2N-2-methoxy-m-tolylCN)2(κ1-2-methoxy-m-tolylCN)2Cr2[μ-κ2-
-HC(N-2,6-iPr2C6H3)2]2 (9). 5 show excellent yield and regioselectivity in the cyclotrimerization with alkynes. Last, treatment of 1 with pyridine-borane generated Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2(μ-H)(μ-κ2-C5H4BH3) (10) during C-H bond activation.
(μ-η6:η6-C7H8)[Cr(Nacnac)]2 (11) (Nacnac = HC((CMe)NC6H3-iPr2)2), an inverted-sandwich dichromium compelex is prepared. Treatment 11 with 2-methylbenzonitrile and 2,4,6-trimethylbenzonitrile afforded Cr(Nacnac)(o-tolylCN)
-[NH(3-(o-tolyl)isoquinoline)] (12) and Cr(Nacnac)[κ2-HN(C-2,4,6-Me3C6H2)2NH] (13). Both reactions involve C-C coupling.
Treatment mononuclear chromium complex Cr[κ2-HC(N-2,6-iPr2C6H3)2]2 (14) with CoCl¬2 obtained hetero-dinuclear complex Co[κ1-HC(N-2,6-iPr2C6H3)2][μ-κ2-HC(
-N-2,6-iPr2C6H3)2]Cr[κ2-HC(N-2,6-iPr2C6H3)2] (15).

摘要 Ⅰ
Abstract Ⅲ
謝誌 Ⅴ
目錄 Ⅵ
圖目錄 Ⅸ
流程圖目錄 Ⅹ
表目錄 ⅩⅠ
第一章 緒論 1
1-1 金屬多重鍵 1
1-2 反三明治(Inverted-Sandwich)錯合物 6
1-3 金屬多重鍵與反三明治錯合物之差異 7
1-4 研究方向 8
1-4-1 金屬多重鍵 8
1-4-2 反三明治金屬錯合物 8
1-4-3 異核金屬多重鍵 9
第二章 雙鉻五重鍵反應性研究 11
2-1 雙鉻五重鍵錯合物之[2+2]環化加成反應 11
2-1-1 前言 11
2-1-2 錯合物(μ-κ2-(CH3)3SiCCH)Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2 (2)、(μ-κ2-(C
-H3)3CCCH)Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2 (3)與(μ-κ2-(C6H5)CCH)Cr2[μ-κ2-H
-C(N-2,6-iPr2C6H3)2]2 (4)的合成與鑑定 13
2-2 雙鉻五重鍵之可逆斷裂與形成 15
2-2-1 前言 15
2-2-2 錯合物[μ-η6:η6-(1,3,5-(SiMe3)3C6H3)]Cr2[κ2-HC(N-2,6-iPr2C6H3)2]2 (5)的合成與鑑定 16
2-2-3 雙鉻五重鍵及反三明治雙鉻錯合物與腈類分子(nitrile)之反應性 22
2-2-4 錯合物(μ-κ1C:κ2N-PhCN)2(κ1-PhCN)2Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2 (6)的合成與鑑定 23
2-2-5 錯合物(μ-κ1C:κ2N-o-tolylCN)2(κ1-o-tolylCN)2Cr2[μ-κ2-HC(N-2,6-iPr2C6
-H3)2]2 (7)、(μ-κ1C:κ2N-p-tolylCN)2(κ1-p-tolylCN)2Cr2[μ-κ2-HC(N-2,6-iPr2C6H3
)2]2 (8)與(μ-κ1C:κ2N-2-methoxy-m-tolylCN)2(κ1-3-methoxy-m-tolylCN)2Cr2[μ-
-κ2-HC(N-2,6-iPr2C6H3)2]2 (9)的合成與鑑定 24
2-3 三聚合環化反應 27
2-4 雙鉻金屬五重鍵錯合物與硼烷之反應 29
2-4-1 前言 29
2-4-2 Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2(μ-H)(μ-κ2-C5H4BH3) (10)的合成與鑑定 30
2-5 結論 33
第三章 反三明治雙鉻錯合物與腈類之反應性研究 34
3-1 前言 34
3-2 錯合物Cr(Nacnac)(o-tolylCN)[NH(3-(o-tolyl)isoquinoline)] (12)的合成與鑑定 35
3-3 錯合物Cr(Nacnac)[κ2-HN(C-2,4,6-Me3C6H2)2NH] (13)的合成與鑑定 37
3-4 結論 39
第四章 其他嘗試 41
4-1 異核雙金屬多重鍵錯合物之嘗試 41
4-1-1 前言 41
4-1-2 錯合物Co[κ1-HC(N-2,6-iPr2C6H3)2 ][μ-κ2-HC(N-2,6-iPr2C6H3)2]Cr[κ2-H
-C(N-2,6-iPr2C6H3)2] (15)的合成與鑑定 42
第五章 實驗步驟 44
5-1 實驗儀器與溶劑 44
5-1-1 一般操作 44
5-1-2 實驗使用儀器 44
5-1-3 使用溶劑及藥品 .45
5-2 實驗步驟 47
5-2-1 (μ-κ2-(CH3)3SiCCH)Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2 (2)的合成 47
5-2-2 (μ-κ2-(CH3)3CCCH)Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2 (3)的合成 48
5-2-3 (μ-κ2-(C6H5)CCH)Cr2[μ-κ+-HC(N-2,6-iPr2C6H3)2]2 (4)的合成 48
5-2-4 [μ-η6:η6-(1,3,5-(SiMe3)3C6H3)]Cr2[κ2-HC(N-2,6-iPr2C6H3)2]2 (5)的合成 49
5-2-5 (μ-κ1C:κ2N-PhCN)2(κ1-PhCN)2Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2 (6)的合成 49
5-2-6 (μ-κ1C:κ2N-o-tolylCN)2(κ1-o-tolylCN)2Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2 (7)的合成 50
5-2-7 (μ-κ1C:κ2N-p-tolylCN)2(κ1-p-tolylCN)2Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2 (8)的合成 51
5-2-8 (μ-κ1C:κ2N-2-methoxy-m-tolylCN)2(κ1-3-methoxy-m-tolylCN)2Cr2[μ-κ2-H
-C(N-2,6-iPr2C6H3)2]2 (9)的合成 52
5-2-9 三聚合環化反應 53
5-2-10 Cr2[μ-κ2-HC(N-2,6-iPr2C6H3)2]2(μ-H)(μ-κ2-C5H4BH3) (10)的合成 53
5-2-11 Cr(Nacnac)(o-tolylCN)[NH(3-(o-tolyl)isoquinoline)] (12)的合成 54
5-2-12 Cr(Nacnac)[κ2-HN(C-2,4,6-Me3C6H2)2NH] (13)的合成 54
5-2-13 Co[κ1-HC(N-2,6-iPr2C6H3)2][μ-κ2-HC(N-2,6-iPr2C6H3)2]Cr[κ2-HC(N-2,6-
-iPr2C6H3)2] (15)的合成 55
5-3 晶體結構資料表 56
參考文獻 63

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