含Tp基团Mo(W)/Cu/S簇的合成及组装
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摘要
Mo(W)/Cu/S簇合物由于其结构的多样性以及在工业催化和光学材料等方面具有广阔的应用前景,一直是化学和材料科学研究的热点领域之一。在以前报道的Mo(W)/Cu/S簇合物中,大部分由起始物[ME_xS_(4-x)]~(2-),[Cp~*MS_3]~-(M=Mo,W;E=O,S;x=0-3)和Cu(Ⅰ)化合物反应得到。本论文以[Et_4N][Tp~*WS_3](1a),[Et_4N][TpMoSS_4](1b)(Tp~*=三(3,5-二甲基吡唑)氢合硼酸根;Tp=三吡唑氢合硼酸根)为起始物和Cu(Ⅰ)化合物反应,得到15个簇合物。并以得到的立方烷型和蝶型簇合物为前驱体和含磷,含氮有机配体反应,得到12个簇合物。其中有6个为超分子簇合物。主要结果简述如下:
一、起始物1a和CuBr,CuCN,CuNCS进行逐步加成反应,获得了10个逐步加成产物:[Et_4N][Tp~*W(μ-S)_2S(CuBr)](2),[Et_4N][Tp~*W(μ-S)_2(μ_3-S)(CuBr)_2](3),[Et_4N][Tp~*W(μ_3-S)_3(CuBr)_3](4),[Et_4N][(Tp~*W(μ-S)_2OCu)_2(μ-CN)]·CH_3CN(5·CH_3CN),[Tp~*W(μ-S)_2(μ_3-S)(CuCN)_2·ClCH_2CH_2Cl]_n(6·ClCH_2CH_2Cl),[Et_4N][Tp~*W(μ-S)_2(μ_3-S)(CuCN)_2]·CHCl_3(7·CHCl_3),[Et_4N][Tp~*WS(μ-S)_2(CuNCS)]·0.5CH_2Cl_2(8·0.5CH_2Cl_2),[Et_4N][Tp~*W(μ_3-S)(μ-S)_2(CuNCS)_2]·ClCH_2CH_2Cl(9·ClCH_2CH_2Cl),[Et_4N]_2[Tp~*W(μ_3-S)_3(CuNCS)_3(μ_3-Br)·1.5ani(10·1.5ani),{[Et_4N][Tp~*W(μ_3-S)_3(Cu-μ-SCN)_3(Cu-μ_3-NCS)]}_n(11)。对化合物8-11进行了三阶非线性光学测试,研究发现随着簇核的增大,化合物8-11的三阶非线性也随着增强。
二、开口立方烷前驱体[Et_4N][Tp~*W(μ_3-S)_3(CuBr)_3](4)和六种不同类型的含N配体(包括两个单齿配体吡啶和苯胺,两个双齿刚性配体4,4'-bipy和bpee,两个双齿柔性配体bpe和bpp)反应,分离得到了6个新的化合物:[Tp~*W(μ_3-S)_3Cu_3(py)_3(μ_3-Br)](PF_6)(12),[{Tp~*W(μ_3-S)_3(CuBr)_3}(μ_6-Br){Tp~*W(μ_3-S)_3Cu_3(ani)_3}]·4ani·0.5Et_2O(13·4ani·0.5Et_2O),{[Tp~*W(μ_3-S)_3Cu_3(4,4'-bipy)3(μ_3-Br)](PF_6)·H_2O}_n(14),[{Tp~*W(μ_3-S)_3Cu_3Br_2}_2(bpee)]·0.5CH_2Cl_2(15·0.5CH_2Cl_2),{[{Tp~*W(μ_3-S)_3Cu_3(μ_3-Br)}_2(bpe)_3](PF_6)_2·MeCN}_n(16),([Tp~*W(μ_3-S)_3Cu_3Br(μ_3-Br)(bpp)]·DMF}_n(17)。其中,14为二维网格含簇超分子化合物;16和17分别为一维锯齿状和一维螺旋状含簇超分子化合物。并对12-17进行了电喷雾质谱和三阶非线性光学测试。
三、以蝶型前驱体[Et_4N][Tp~*W(μ_3-S)(μ-S)_2(CuSCN)_2](9)和三种不同类型含氮配体py,4,4'-bipy,bpp反应,得到三个中性簇合物[Tp~*W(μ_3-S)(μ-S)_2Cu_2(SCN)(py)_2](18),[{Tp~*W(μ_3-S)(μ-S)_2Cu_2(SCN)}_2(4,4'-bipy)]·3.5H_2O(19·3.5H_2O)和[Tp~*W(μ_3-S)(μ-S)_2Cu_2(SCN)(bpp)]_2(20)。测试了化合物18-20的三阶非线性光学性质。
四、利用起始物1b中富余的S原子和CuX中的卤素离子来合成多核Mo/Cu/S簇合物。以MeCN作溶剂,得单立方烷和双立方烷型簇合物[Et_4N][TpMo(μ_3-S)_3Cu_3Cl_2(μ_3-Cl)(MeCN)]·MeCN(21·MeCN),[Et_4N]_2[TpMo(μ_3-S)_3(CuBr)_3(μ_3-Br)]·0.75MeCN·0.125MeOH(22·0.75MeCN·0.125MeOH),[Et_4N][{TpMo(μ_3-S)_3Cu_3Br}_2(μ_4-Br)(μ-Br)_2]·4H_2O(23·4H_2O),[Et_4N]_2[{TpMo(μ3-S)_3Cu_3I(μ_4-I)}_2Cu(μ-I)_3]·3.5MeCN(24·3.5MeCN)。而以吡啶作溶剂时,得到一系列结构相似的四立方烷型多核簇合物(PyH){[{TpMo(μ_3-S)_3Cu_3}_4(μ_3-S)_4](μ_(12)-X)}·Et_2O(X=Cl,25a·Et_2O;Br,25b·Et_2O;I,25c·Et_2O)。在生成25a-25c时,1b中富余的S原子和Cu原子上的卤素原子同时起桥联作用进而将单立方烷簇核连接成四立方烷簇合作用。
五、尝试以Mo的闭口立方烷簇合物[Et_4N]_2[TpMo(μ_3-S)_3(CuBr)_3(μ_3-Br](22)为前驱体与含磷配体PPh_3,单齿含氮配体苯胺,及双齿柔性含氮配体bpp的反应,得到闭口立方烷簇骨架保持的三个化合物[Et_4N][TpMo(μ_3-S)_3(CuBr)_3(PPh_3)]·CH_2Cl_2(26·CH_2Cl_2),[Et_4N][TpMo(μ_3-S)_3(CuBr)_3(ani)]·2ani(27·2ani),和{[TpMoCu_3Br_2(bpp)(μ_3-S)_3](DMSO)_2(H_2O)_2(CH_3OH)_(0.5)}_n(28)。其中28为一维锯齿状含簇超分子化合物。
六、双核前驱体[Et_4N]_2[(edt)_2Mo_2S_2(μ-S)_2]和CuBr在吡啶和dppm下反应获得两个对称和两个不对称的产物[Et_4N]_2[(edt)_2Mo_2(μ-S)_3(μ_3-S)Cu]_2·2CH_2Cl_2(29·2CH_2Cl_2),[Mo_2O_2(μ-S)_2(edt)_2Cu_2(dppm)_2](30),[(edt)_2Mo_2O(μ_3-S)(μ-S)_2Cu_2(Py)_4](31),[Mo_2(μ-S)_2(μ_3-S)_2(edt)_2Cu_2(dppm)(Py)]·Py(32·Py)。这其中,30和31具有内部镜面对称和假镜面对称;29和32为不对称产物,但由于它们在晶体中存在各自的对映异构体,它们只是外消旋化合物。
In the past decades, reactions of thiometallate anions [ME_xS_(4-x)]~(2-) [Cp~*MS_3]~- (M = Mo, W; E =O,S; x = 0-3) with copper(Ⅰ) complexes have been extensively investigated. This is because the resulting Mo(W)/Cu/S clusters possess interesting structural chemistry and various potential applications in biological systems and optoelectronic materials. In this thesis, the third family of synthons [Et_4N][Tp~*WS_3] (1a) and [Et_4N][TpMoSS_4] (1b) (Tp~* = Hydridotris(3,5-dimethylpyrazol-1-yl)borate; Tp = Hydridotris(pyrazol-1-yl)borate) were used to react with Cu(Ⅰ) complexes, and fifteen clusters were isolated therefore. Furthermore, the obtained cubane like core and butterfly-shaped core precursors were chose to react with P- and N-donor ligands to afford another twelve clusters. Among them, six compounds were cluster-based supramolecular assemblies. The main results were briefly summarized as follows:
1.Stepwise reactions of [Et_4N][Tp~*WS_3] (1a) with CuBr, CuCN, and CuNCS afforded ten addition products:[Et_4N][Tp~*W(μ-S)_2S(CuBr)](2), [Et_4N][Tp~*W(μ-S)_2(μ_3-S)(CuBr)_2](3), [Et_4N][Tp~*W(μ_3-S)_3(CuBr)_3](4), [Et_4N][(Tp~*W(μ-S)_2OCu)_2(μ-CN)]·CH_3CN(5·CH_3CN), [Tp~*W(μ-S)_2(μ_3-S)(CuCN)_2·ClCH_2CH_2Cl]_n(6·ClCH_2CH_2Cl), [Et_4N][Tp~*W(μ-S)_2(μ_3-S)(CuCN)_2]·CHCl_3(7·CHCl_3), [Et_4N][Tp~*WS(μ-S)_2(CuNCS)]·0.5CH_2Cl_2(8·0.5CH_2Cl_2), [Et_4N][Tp~*W(μ_3-S)(μ-S)_2(CuNCS)_2]·ClCH_2CH_2Cl(9·ClCH_2CH_2Cl), [Et_4N]_2[Tp~*W(μ_3-S)_3(CuNCS)_3(μ_3-Br)·1.5ani(10·1.5ani), {[Et_4N][Tp~*W(μ_3-S)_3(Cu-μ-SCN)_3(Cu-μ_3-NCS)]}_n(11).From this synthetic strategy, the third-order NLO performances of 8-11, relative to those of 1a, were improved. In addition, 8-11 were observed to show enhanced NLO performances with increasing the number of copper atoms in their frameworks.
2. A new set of monomeric, dimeric and polymeric W/Cu/S clusters from a precursor cluster [Et_4N][Tp~*W(μ_3-S)_3(CuBr)_3] (4) and various N-donor ligands was reported: [Tp~*W(μ_3-S)_3Cu_3(py)_3(μ_3-Br)](PF_6)(12),[{Tp~*W(μ_3-S)_3(CuBr)_3}(μ_6-Br){Tp~*W(μ_3-S)_3Cu_3(ani)_3}]·4ani·0.5Et_2O(13·4ani·0.5Et_2O), {[Tp~*W(μ_3-S)_3Cu_3(4,4'-bipy)3(μ_3-Br)](PF_6)·H_2O}_n(14),[{Tp~*W(μ_3-S)_3Cu_3Br_2}_2(bpee)]·0.5CH_2Cl_2(15·0.5CH_2Cl_2), {[{Tp~*W(μ_3-S)_3Cu_3(μ_3-Br)}_2(bpe)_3](PF_6)_2·MeCN}_n(16), ([Tp~*W(μ_3-S)_3Cu_3Br(μ_3-Br)(bpp)]·DMF}_n(17). Among them, 14 is a 2D (6,3) cationic network; and 16,17 are 1D zigzag cationic chain and 1D spiral chain, respectively. The NLO performances and electrospary mass spectroscopy of 12-17 were also investigated.
3.Reactions of the preformed butterfly cluster [Et_4N][Tp~*W(μ_3-S)(μ-S)_2(CuSCN)_2](9) with three kinds of N-donor ligand (py, 4,4'-bipy or bpp) led to the formation of three neutral [Tp~*W(μ_3-S)(μ-S)_2Cu_2]-based compounds [Tp~*W(μ_3-S)(μ-S)_2Cu_2(SCN)(py)_2](18), [{Tp~*W(μ_3-S)(μ-S)_2Cu_2(SCN)}_2(4,4'-bipy)]·3.5H_2O(19·3.5H_2O), and [Tp~*W(μ_3-S)(μ--S)_2Cu_2(SCN)(bpp)]_2(20), respectively. The NLO performances of 18-20 were also studied.
4.Utilization of the redundant sulfur atoms of 1b itself and halide atom in CuX to synthesis the high nuclearity Mo/Cu/S clusters. Treatment of 1b with three equiv. of CuX in MeCN gave rise to four compounds [Et_4N][TpMo(μ_3-S)_3Cu_3Cl_2(μ_3-Cl)(MeCN)]·MeCN(21·MeCN), [Et_4N]_2[TpMo(μ_3-S)_3(CuBr)_3(μ_3-Br)]·0.75MeCN·0.125MeOH(22·0.75MeCN·0.125MeOH), [Et_4N][{TpMo(μ_3-S)_3Cu_3Br}_2(μ_4-Br)(μ-Br)_2]·4H_2O(23·4H_2O),[Et_4N]_2[{TpMo(μ3-S)_3Cu_3I(μ_4 -I)}_2Cu(μ-I)_3]·3.5MeCN(24·3.5MeCN). The analogous reactions performed in pyridine afforded three tetracubane-type clusters (PyH){[{TpMo(μ_3-S)_3Cu_3}_4(μ_3- S)_4](μ_(12)-X)}·Et_2O(X=Cl, 25a·Et_2O;Br,25b·Et_2O;I,25c·Et_2O). In the cases of 25a-c, the redundant sulfide atoms of 1b and halide in CuX worked together to bond the basic cluster fragments into tetracubane-like clusters.
5.Reactions of the preformed complete cubane core cluster [Et_4N]_2[TpMo(μ_3-S)_3(CuBr)_3(μ_3-Br] (22) with PPh_3, aniline, and bpp afforded three compounds [Et_4N][TpMo(μ_3-S)_3(CuBr)_3(PPh_3)]·CH_2Cl_2(26·CH_2Cl_2),[Et_4N][TpMo(μ_3-S)_3(CuBr)_3(ani)]·2ani (27·2ani), and {[TpMoCu_3Br_2(bpp)(μ_3-S)_3](DMSO)_2(H_2O)_2(CH_3OH)_(0.5)}_n(28). Among them, 28 is a 1D zigzag supramolecular compound.
6.Treatment of dinuclear precursor [Et_4N]_2[(edt)_2Mo_2S_2(μ-S)_2] with CuBr in the presence of py and dppm afforded two symmetric and two asymmetric clusters [Et_4N]_2[(edt)_2Mo_2(μ-S)_3(μ_3-S)Cu]_2·2CH_2Cl_2(29·2CH_2Cl_2),[Mo_2O_2(μ-S)_2(edt)_2Cu_2(dppm)_2](30), [(edt)_2Mo_2O(μ_3-S)(μ-S)_2Cu_2(Py)_4](31), and [Mo_2(μ-S)_2(μ_3-S)_2(edt)_2Cu_2(dppm)(Py)]·Py(32·Py). Among these obtained clusters, 30 and 31 have internal mirror symmetry or pseudo mirror symmetry; 29 and 32 are asymmetric clusters with racemic formations.
一、起始物1a和CuBr,CuCN,CuNCS进行逐步加成反应,获得了10个逐步加成产物:[Et_4N][Tp~*W(μ-S)_2S(CuBr)](2),[Et_4N][Tp~*W(μ-S)_2(μ_3-S)(CuBr)_2](3),[Et_4N][Tp~*W(μ_3-S)_3(CuBr)_3](4),[Et_4N][(Tp~*W(μ-S)_2OCu)_2(μ-CN)]·CH_3CN(5·CH_3CN),[Tp~*W(μ-S)_2(μ_3-S)(CuCN)_2·ClCH_2CH_2Cl]_n(6·ClCH_2CH_2Cl),[Et_4N][Tp~*W(μ-S)_2(μ_3-S)(CuCN)_2]·CHCl_3(7·CHCl_3),[Et_4N][Tp~*WS(μ-S)_2(CuNCS)]·0.5CH_2Cl_2(8·0.5CH_2Cl_2),[Et_4N][Tp~*W(μ_3-S)(μ-S)_2(CuNCS)_2]·ClCH_2CH_2Cl(9·ClCH_2CH_2Cl),[Et_4N]_2[Tp~*W(μ_3-S)_3(CuNCS)_3(μ_3-Br)·1.5ani(10·1.5ani),{[Et_4N][Tp~*W(μ_3-S)_3(Cu-μ-SCN)_3(Cu-μ_3-NCS)]}_n(11)。对化合物8-11进行了三阶非线性光学测试,研究发现随着簇核的增大,化合物8-11的三阶非线性也随着增强。
二、开口立方烷前驱体[Et_4N][Tp~*W(μ_3-S)_3(CuBr)_3](4)和六种不同类型的含N配体(包括两个单齿配体吡啶和苯胺,两个双齿刚性配体4,4'-bipy和bpee,两个双齿柔性配体bpe和bpp)反应,分离得到了6个新的化合物:[Tp~*W(μ_3-S)_3Cu_3(py)_3(μ_3-Br)](PF_6)(12),[{Tp~*W(μ_3-S)_3(CuBr)_3}(μ_6-Br){Tp~*W(μ_3-S)_3Cu_3(ani)_3}]·4ani·0.5Et_2O(13·4ani·0.5Et_2O),{[Tp~*W(μ_3-S)_3Cu_3(4,4'-bipy)3(μ_3-Br)](PF_6)·H_2O}_n(14),[{Tp~*W(μ_3-S)_3Cu_3Br_2}_2(bpee)]·0.5CH_2Cl_2(15·0.5CH_2Cl_2),{[{Tp~*W(μ_3-S)_3Cu_3(μ_3-Br)}_2(bpe)_3](PF_6)_2·MeCN}_n(16),([Tp~*W(μ_3-S)_3Cu_3Br(μ_3-Br)(bpp)]·DMF}_n(17)。其中,14为二维网格含簇超分子化合物;16和17分别为一维锯齿状和一维螺旋状含簇超分子化合物。并对12-17进行了电喷雾质谱和三阶非线性光学测试。
三、以蝶型前驱体[Et_4N][Tp~*W(μ_3-S)(μ-S)_2(CuSCN)_2](9)和三种不同类型含氮配体py,4,4'-bipy,bpp反应,得到三个中性簇合物[Tp~*W(μ_3-S)(μ-S)_2Cu_2(SCN)(py)_2](18),[{Tp~*W(μ_3-S)(μ-S)_2Cu_2(SCN)}_2(4,4'-bipy)]·3.5H_2O(19·3.5H_2O)和[Tp~*W(μ_3-S)(μ-S)_2Cu_2(SCN)(bpp)]_2(20)。测试了化合物18-20的三阶非线性光学性质。
四、利用起始物1b中富余的S原子和CuX中的卤素离子来合成多核Mo/Cu/S簇合物。以MeCN作溶剂,得单立方烷和双立方烷型簇合物[Et_4N][TpMo(μ_3-S)_3Cu_3Cl_2(μ_3-Cl)(MeCN)]·MeCN(21·MeCN),[Et_4N]_2[TpMo(μ_3-S)_3(CuBr)_3(μ_3-Br)]·0.75MeCN·0.125MeOH(22·0.75MeCN·0.125MeOH),[Et_4N][{TpMo(μ_3-S)_3Cu_3Br}_2(μ_4-Br)(μ-Br)_2]·4H_2O(23·4H_2O),[Et_4N]_2[{TpMo(μ3-S)_3Cu_3I(μ_4-I)}_2Cu(μ-I)_3]·3.5MeCN(24·3.5MeCN)。而以吡啶作溶剂时,得到一系列结构相似的四立方烷型多核簇合物(PyH){[{TpMo(μ_3-S)_3Cu_3}_4(μ_3-S)_4](μ_(12)-X)}·Et_2O(X=Cl,25a·Et_2O;Br,25b·Et_2O;I,25c·Et_2O)。在生成25a-25c时,1b中富余的S原子和Cu原子上的卤素原子同时起桥联作用进而将单立方烷簇核连接成四立方烷簇合作用。
五、尝试以Mo的闭口立方烷簇合物[Et_4N]_2[TpMo(μ_3-S)_3(CuBr)_3(μ_3-Br](22)为前驱体与含磷配体PPh_3,单齿含氮配体苯胺,及双齿柔性含氮配体bpp的反应,得到闭口立方烷簇骨架保持的三个化合物[Et_4N][TpMo(μ_3-S)_3(CuBr)_3(PPh_3)]·CH_2Cl_2(26·CH_2Cl_2),[Et_4N][TpMo(μ_3-S)_3(CuBr)_3(ani)]·2ani(27·2ani),和{[TpMoCu_3Br_2(bpp)(μ_3-S)_3](DMSO)_2(H_2O)_2(CH_3OH)_(0.5)}_n(28)。其中28为一维锯齿状含簇超分子化合物。
六、双核前驱体[Et_4N]_2[(edt)_2Mo_2S_2(μ-S)_2]和CuBr在吡啶和dppm下反应获得两个对称和两个不对称的产物[Et_4N]_2[(edt)_2Mo_2(μ-S)_3(μ_3-S)Cu]_2·2CH_2Cl_2(29·2CH_2Cl_2),[Mo_2O_2(μ-S)_2(edt)_2Cu_2(dppm)_2](30),[(edt)_2Mo_2O(μ_3-S)(μ-S)_2Cu_2(Py)_4](31),[Mo_2(μ-S)_2(μ_3-S)_2(edt)_2Cu_2(dppm)(Py)]·Py(32·Py)。这其中,30和31具有内部镜面对称和假镜面对称;29和32为不对称产物,但由于它们在晶体中存在各自的对映异构体,它们只是外消旋化合物。
In the past decades, reactions of thiometallate anions [ME_xS_(4-x)]~(2-) [Cp~*MS_3]~- (M = Mo, W; E =O,S; x = 0-3) with copper(Ⅰ) complexes have been extensively investigated. This is because the resulting Mo(W)/Cu/S clusters possess interesting structural chemistry and various potential applications in biological systems and optoelectronic materials. In this thesis, the third family of synthons [Et_4N][Tp~*WS_3] (1a) and [Et_4N][TpMoSS_4] (1b) (Tp~* = Hydridotris(3,5-dimethylpyrazol-1-yl)borate; Tp = Hydridotris(pyrazol-1-yl)borate) were used to react with Cu(Ⅰ) complexes, and fifteen clusters were isolated therefore. Furthermore, the obtained cubane like core and butterfly-shaped core precursors were chose to react with P- and N-donor ligands to afford another twelve clusters. Among them, six compounds were cluster-based supramolecular assemblies. The main results were briefly summarized as follows:
1.Stepwise reactions of [Et_4N][Tp~*WS_3] (1a) with CuBr, CuCN, and CuNCS afforded ten addition products:[Et_4N][Tp~*W(μ-S)_2S(CuBr)](2), [Et_4N][Tp~*W(μ-S)_2(μ_3-S)(CuBr)_2](3), [Et_4N][Tp~*W(μ_3-S)_3(CuBr)_3](4), [Et_4N][(Tp~*W(μ-S)_2OCu)_2(μ-CN)]·CH_3CN(5·CH_3CN), [Tp~*W(μ-S)_2(μ_3-S)(CuCN)_2·ClCH_2CH_2Cl]_n(6·ClCH_2CH_2Cl), [Et_4N][Tp~*W(μ-S)_2(μ_3-S)(CuCN)_2]·CHCl_3(7·CHCl_3), [Et_4N][Tp~*WS(μ-S)_2(CuNCS)]·0.5CH_2Cl_2(8·0.5CH_2Cl_2), [Et_4N][Tp~*W(μ_3-S)(μ-S)_2(CuNCS)_2]·ClCH_2CH_2Cl(9·ClCH_2CH_2Cl), [Et_4N]_2[Tp~*W(μ_3-S)_3(CuNCS)_3(μ_3-Br)·1.5ani(10·1.5ani), {[Et_4N][Tp~*W(μ_3-S)_3(Cu-μ-SCN)_3(Cu-μ_3-NCS)]}_n(11).From this synthetic strategy, the third-order NLO performances of 8-11, relative to those of 1a, were improved. In addition, 8-11 were observed to show enhanced NLO performances with increasing the number of copper atoms in their frameworks.
2. A new set of monomeric, dimeric and polymeric W/Cu/S clusters from a precursor cluster [Et_4N][Tp~*W(μ_3-S)_3(CuBr)_3] (4) and various N-donor ligands was reported: [Tp~*W(μ_3-S)_3Cu_3(py)_3(μ_3-Br)](PF_6)(12),[{Tp~*W(μ_3-S)_3(CuBr)_3}(μ_6-Br){Tp~*W(μ_3-S)_3Cu_3(ani)_3}]·4ani·0.5Et_2O(13·4ani·0.5Et_2O), {[Tp~*W(μ_3-S)_3Cu_3(4,4'-bipy)3(μ_3-Br)](PF_6)·H_2O}_n(14),[{Tp~*W(μ_3-S)_3Cu_3Br_2}_2(bpee)]·0.5CH_2Cl_2(15·0.5CH_2Cl_2), {[{Tp~*W(μ_3-S)_3Cu_3(μ_3-Br)}_2(bpe)_3](PF_6)_2·MeCN}_n(16), ([Tp~*W(μ_3-S)_3Cu_3Br(μ_3-Br)(bpp)]·DMF}_n(17). Among them, 14 is a 2D (6,3) cationic network; and 16,17 are 1D zigzag cationic chain and 1D spiral chain, respectively. The NLO performances and electrospary mass spectroscopy of 12-17 were also investigated.
3.Reactions of the preformed butterfly cluster [Et_4N][Tp~*W(μ_3-S)(μ-S)_2(CuSCN)_2](9) with three kinds of N-donor ligand (py, 4,4'-bipy or bpp) led to the formation of three neutral [Tp~*W(μ_3-S)(μ-S)_2Cu_2]-based compounds [Tp~*W(μ_3-S)(μ-S)_2Cu_2(SCN)(py)_2](18), [{Tp~*W(μ_3-S)(μ-S)_2Cu_2(SCN)}_2(4,4'-bipy)]·3.5H_2O(19·3.5H_2O), and [Tp~*W(μ_3-S)(μ--S)_2Cu_2(SCN)(bpp)]_2(20), respectively. The NLO performances of 18-20 were also studied.
4.Utilization of the redundant sulfur atoms of 1b itself and halide atom in CuX to synthesis the high nuclearity Mo/Cu/S clusters. Treatment of 1b with three equiv. of CuX in MeCN gave rise to four compounds [Et_4N][TpMo(μ_3-S)_3Cu_3Cl_2(μ_3-Cl)(MeCN)]·MeCN(21·MeCN), [Et_4N]_2[TpMo(μ_3-S)_3(CuBr)_3(μ_3-Br)]·0.75MeCN·0.125MeOH(22·0.75MeCN·0.125MeOH), [Et_4N][{TpMo(μ_3-S)_3Cu_3Br}_2(μ_4-Br)(μ-Br)_2]·4H_2O(23·4H_2O),[Et_4N]_2[{TpMo(μ3-S)_3Cu_3I(μ_4 -I)}_2Cu(μ-I)_3]·3.5MeCN(24·3.5MeCN). The analogous reactions performed in pyridine afforded three tetracubane-type clusters (PyH){[{TpMo(μ_3-S)_3Cu_3}_4(μ_3- S)_4](μ_(12)-X)}·Et_2O(X=Cl, 25a·Et_2O;Br,25b·Et_2O;I,25c·Et_2O). In the cases of 25a-c, the redundant sulfide atoms of 1b and halide in CuX worked together to bond the basic cluster fragments into tetracubane-like clusters.
5.Reactions of the preformed complete cubane core cluster [Et_4N]_2[TpMo(μ_3-S)_3(CuBr)_3(μ_3-Br] (22) with PPh_3, aniline, and bpp afforded three compounds [Et_4N][TpMo(μ_3-S)_3(CuBr)_3(PPh_3)]·CH_2Cl_2(26·CH_2Cl_2),[Et_4N][TpMo(μ_3-S)_3(CuBr)_3(ani)]·2ani (27·2ani), and {[TpMoCu_3Br_2(bpp)(μ_3-S)_3](DMSO)_2(H_2O)_2(CH_3OH)_(0.5)}_n(28). Among them, 28 is a 1D zigzag supramolecular compound.
6.Treatment of dinuclear precursor [Et_4N]_2[(edt)_2Mo_2S_2(μ-S)_2] with CuBr in the presence of py and dppm afforded two symmetric and two asymmetric clusters [Et_4N]_2[(edt)_2Mo_2(μ-S)_3(μ_3-S)Cu]_2·2CH_2Cl_2(29·2CH_2Cl_2),[Mo_2O_2(μ-S)_2(edt)_2Cu_2(dppm)_2](30), [(edt)_2Mo_2O(μ_3-S)(μ-S)_2Cu_2(Py)_4](31), and [Mo_2(μ-S)_2(μ_3-S)_2(edt)_2Cu_2(dppm)(Py)]·Py(32·Py). Among these obtained clusters, 30 and 31 have internal mirror symmetry or pseudo mirror symmetry; 29 and 32 are asymmetric clusters with racemic formations.
引文
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