5-磺基水杨酸配合物的合成及结构研究
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摘要
本论文研究5—磺基水杨酸(H_3ssal)与中性含氮配体形成的金属配合物的合成、晶体结构及性质。使用的中性配体为2,2'-联吡啶(2,2'-bipy)、4,4'-联吡啶(4,4'-bipy)、1，10-邻菲罗啉(phen)、2-氨基吡啶(2-ampy)、苯并咪唑(BD)和二(4-吡啶)乙烯(bpe)等，研究的金属离子为主族金属Pb以及过渡金属Cu、Co、Zn、Cd和Mn等。总共合成了30个配合物，对所有这些化合物进行了单晶X-射线衍射结构测定及红外光谱分析，并对大部分化合物进行元素分析、热重分析和荧光性质的研究。
对于金属铜配合物研究了不同反应条件(反应物组成及配比、温度、溶剂等)、合成方法及中性配体对配合物拓扑网络结构的影响，共合成了8个配合物，分别为：[Cu(Hssal)(2,2'-bipy)(H_2O)_2]_n(1)，[Cu_4(CH_3COO)_2(ssal)_2(2,2'-bipy)_4(H_2O)_2]·6H_2O(2)，{[Cu(ssal)(2,2'-bipy)][Cu_2(ssal)(2,2'-bipy)_2(H_2O)_2](H_2O)}_n (3)，{[Cu_3(ssal)_2(dpa)_3]·3H_2O}_n (4)，[Cu_2~Ⅱ(ssal)_2(dpa)_2][Cu~Ⅰ(dpa)_2]_2·2H_2O (5)，{[Cu(ssal)(H_2O)](2-ampy)}_n (6)，{[Cu_3(ssal)_2(BD)_6]·8H_2O}_n (7)，[Cu(TTF)(phen)(H_2O)][Cu(TTF)(Hssal)(phen)](8)。配合物1为一维链状结构，并通过氢键作用扩展为三维网络结构；2为四核单元，也通过氢键形成三维网络结构；3为两条阴、阳离子一维链结构，并通过氢键形成二维网络结构。4为二维层状网络结构，而在相似的合成条件下，5却为混合价态Cu配合物，单核结构。6和7都为一维链状网络结构，只是6中还存在游离的2-氨基吡啶阳离子；而8为双核离子缔合物。配合物1和8中H_3ssal只脱去两个氢，保留羟基上的氢；2—7中，全部去质子化。在这8个配合物中，5—磺基水杨酸离子有7种配位方式。
对于主族金属铅配合物研究了不同中性配体(螯合及桥联)对配合物拓扑网络结构的影响，共合成了8个配合物，分别为：[Pb(Hssal)(2,2'-bipy)(DMF)]_n(9)，[Pb(Hssal)(2,2'-bipy)(H_2O)]_n(10)，[Pb(Hssal)(phen)(DMF)]_n(11)，[Pb_3(ssal)_2(phen)_3]_n(12)，{[Pb(Hssal)(2,2'-bipy)](4,4'-bipy)_(0．5)}_n (13)，Pb_2(2,2'-bipy)_2(4,4'-bipy)(Hssal)_2(H_2O)_2] (14)，[Pb(phen)(4,4'-bipy)_(0．5)(Hssal)]_n (15)，[Pb(Hssal)(2,2'-bipy)(bpe)_(0．5)]_n (16)。9和11结构相同，都为一维梯链状结构；10和12为二维网络结构；13也为一维梯链状结构，不过存在4,4'-bipy客体分子；14为双核结构，其中4,4'-bipy配体双齿配位；15也为一维梯链状结构，4,4'-bipy分子单齿配位；16为二维网络结构。除了12，其他7个配合物中，H_3ssal只脱去两个氢，保留羟基上的氢。在这8个配合物中，5—磺基水杨酸离子共存在6种配位模式。在配合物9、11和16中，铅的孤对电子不具有立体化学活性，而在其他5个化合物中都具有立体化学活性，并影响了铅的配位环境。此外，弱的Pb-O键作用和π-π堆积作用也对铅的配位环境有影响。
对于过渡金属Co和Zn，得到了两离子缔合物[Co(phen)_2(H_2O)_2](Hssal)·4H_2O(17)和[Zn(phen)_2(H_2O)_2](Hssal)·4H_2O(19)，并以它们为原料进行次级合成，得到了两个混金属配合物{[Co(phen)(H_2O)_4][Cu_2(phen)_2(ssal)_2]·5H_2O (18)和[Zn_2(μ-OH)_2(phen)_2(H_2O)_2][Cu_2(phen)_2(ssal)_2]·3H_2O(20)。17和19结构相似，Hssal~(2-)都未参与配位，只是作为抗衡离子存在；而在18和20中，Hssal~(2-)继续去质子化，并参与配位。
水热条件下的原位反应，到目前为止大部分机理还不甚清楚，这是近年来广大化学工作者关注的一个焦点。我们在5—磺基水杨酸功能化合物的设计合成过程中发现水热下的三种原位反应：Cu(Ⅱ)的还原反应、脱羧反应及水解反应，并合成了8个配合物，分别为{[Cu~ⅠCu~Ⅱ(ssal)(2,2'-bipy)(4,4'-bippy)]·2H_2O}_n (21)，{[Cu~Ⅱ(ssal)_2][Cu_4~Ⅰ(4,4'-bipy)_4(H_2O)]·5H_2O}_n (22)，[Cu(2,2'-bipy)_2Cl]·(4-HBS)·2H_2O(23)，[Cu(2,2'-bipy)_2Cl]·(4-HBS)·(1,4-dp)_(0．5)·H_2O (24)，{[Cd_3(CH_3COO)_4(4,4'-bipy)_4](HBS)_2·10H_2O}_n (25)，[Cd(4,4'-bipy)_2(H_2O)_4](HBS)_2·4H_2O(26)，[Mn(4，4'-bipy)_2(H_2O)_4](HBS)_2·4H_2O (27)，{[Co(4,4'-bipy)(H_2O)_4](HBS)_2·3H_2O}_n (28)。21和22为铜混合价态配合物，21为二维网络结构，22为一维链状结构。23中有脱羧产物，对羟基苯磺酸离子，但不参与配位，只作为抗衡离子存在。24中既有脱羧产物，还有水解产物，不过它们都没参与配位，分别作为抗衡离子和客体分子存在。25—28中只存在脱羧产物，对羟基苯磺酸离子，也没有参加配位。25为二维网络结构；26和27结构相同，都为单核结构；28为一维链状结构。
DMF在加热回流下发生水解反应，其产物甲酸根也会与金属配位，得到两个配合物{[M(COO)(H_2O)_2(4，4’-bipy)]_2[M(4，4’-bipy)(Hssal)_2(H_2O)_2]}_n(M=Cd，29；Mn，30)。这两配合物结构相似，都为一维链状结构，并通过氢键作用扩展为三维网络结构。
In this presentation, we report the syntheses, crystal structures and properties of the metal coordination complexes constructed from 5-sulfosalicylate (H_3ssal). In the procedures of syntheses, we chose 2,2'-bipyridine (2,2'-bipy), 4,4'-bipyridine (4,4'-bipy), 1,10-phenanthroline (1,10-phen), 2-aminopyridine (2-ampy), benzimidazole (BD) and trans-1,2-bis(4-pyridyl)ethylene (bpe) as neutral ligands, and Pb, Cu, Co, Zn, Cd and Mn as metal ions in our research. Totally thirty compounds were synthesized, and have been characterized by X-ray single crystal diffraction, IR spectrum, element analysis, TG and photoluminescent.
For copper complexes, we focused on the effect of the reaction conditions (reactants, the molar ratio, temperature and solvent), and neutral ligands on the structures. We discussed eight copper complexes: [Cu(Hssal)(2,2'-bipy)(H_2O)_2]_n(1), [Cu_4(CH_3COO)_2(ssal)_2(2,2'-bipy)_4(H_2O)_2]·6H_2O (2),{[Cu(ssal)(2,2'-bipy)][Cu_2(ssal)(2,2'-bipy)_2(H_2O)_2](H_2O)}_n (3),{[Cu_3(ssal)_2(dpa)_3]·3H_2O}_n (4), [Cu_2~Ⅱ(ssal)_2(dpa)_2][Cu~Ⅰ(dpa)_2]_2·2H_2O (5), {[Cu(ssal)(H_2O)](2-ampy)}_n (6), {[Cu_3(ssal)_2(BD)_6]·8H_2O}_n (7),[Cu(TTF)(phen)(H_2O)][Cu(TTF)(Hssal)(phen)] (8). The framework is one-dimensional chain in 1, tetraneutral in 2, two one-dimensional cationic-anionic chains in 3; all of which are extended to three-dimensional network by hydrogen bonding. 4 has two-dimensional layer network, however, in the similar synthesis condition, 5 is a mixed-valence copper complex. Both 6 and 7 are one-dimensional structures. 8 is a cationic-anionic complex. In complexes 1 and 8, H_3ssal ligands are doubly deprotonated and remain phenol protons; while in the other six compounds, they are fully deprotonated. There are seven coordination modes of 5-sulfosalicylates in the eight complexes.
For lead complexes, we focused on the effect of neutral ligands (chelating and bridging) on the structures. There are eight complexes synthesized and characterized: [Pb(Hssal)(2,2'-bipy)(DMF)]_n (9), [Pb(Hssal)(2,2'-bipy)(H_2O)]_n (10), [Pb(Hssal)(phenXDMF)]_n (11), [Pb_3(ssal)_2(phen)_3]_n (12),{[Pb(Hssal)(2,2'-bipy)](4,4'-bipy)_(0.5)}_n (13), Pb_2(2,2'-bipy)_2(4,4'-bipy)(Hssal)_2(H_2O)_2] (14), [Pb(phen)(4,4'-bipy)_(0.5)(Hssal)]_n (15), [Pb(Hssal)(2,2'-bipy)(bpe)_(0.5)]_n (16). Complexes 9 and 11 are isostructural, consisting of one-dimensional ladder-like chains. 10 is a two-dimensional double-layer architecture, while 12 is a two-dimensional layer network. The structure of complex 13 possesses a one-dimensional ladder-like chain with guest 4,4'-bipy molecules, while the molecular structure of complex 14 is a dimeric species with a coordinating 4,4'-bipy ligand. Complex 15 consists of a one-dimensional ladder-like chain with monodentate 4,4'-bipyridine but somewhat different from that of complex 13. Complex 16 is a two-dimensional layer structure. The coordination spheres of Pb~Ⅱions in 9-16 are controlled by three factors: the activity of a lone pair of electrons, weak Pb-0 interactions, andπ-πstacking interactions. The Pb~Ⅱlone pairs in 9,11 and 16 are inactive, whereas in the other five complexes, they are stereochemically active. Except in 12, H_3ssal is fully deprotonated, while in the other seven complexes, it only loses two protons. 5-Sulfosalicylate anions have six coordination modes in the eight complexes.
For transition metal Co and Zn, we have synthesized two cationic-anionic complexes: [Co(phen)_2(H_2O)_2](Hssal)·4H_2O (17) and [Zn(phen)_2(H_2O)_2](Hssal)·4H_2O (19), which act as the reactants for the secondary synthsis, and two mixed-metal complexes have been gotten: {[Co(phen)(H_2O_)4][Cu_2(phen)_2(ssal)_2]·5H_2O (18) and [Zn_2(μ-OH)_2(phen)_2(H_2O)_2][Cu_2(phen)_2(ssal)_2]·3H_2O (20). 17 and 19 are isostructure, where Hssal~(2-) ions are free ligands and act as counter ions. In 18 and 20, Hssal~(2-) ligands are further deprotonated and coordinated to metal ions.
Hydrothermal in situ ligand synthesis has been rapidly developed over the past several years due to its effectiveness, simplicity and environmental friendliness. However, up to now, most of the mechanisms of the in situ ligand syntheses have not been very clear. We have discovered three hydrothermal in-situ reactions in the process of synthesizing 5-sulfosalicylate complexes: the redox of Cu(Ⅱ), decarboxylation and hydrolysis. Eight products of in-situ reactions have been obtained and characterized: {[Cu~ⅠCu~Ⅱ(ssal)(2,2'-bipy)(4,4'-bippy)]·2H_2O}_n (21),{[Cu~Ⅱ(ssal)_2][Cu_4~Ⅰ(4,4'-bipy)_4(H_2O)]·5H_2O}_n (22), [Cu(2,2'-bipy)_2Cl]·(4-HBS)·2H_2O (23),[Cu(2,2'-bipy)_2Cl]·(4-HBS)·(1 ,4-dp)_(0.5)·H_2O (24),{[Cd_3(CH_3COO)_4(4,4'-bipy)_4](HBS)_2·10H_2O}_n (25),[Cd(4,4'-bipy)_2(H_2O)_4](HBS)_2·4H_2O (26), [Mn(4,4'-bipy)_2(H_2O)_4](HBS)_2·4H_2O (27), {[Co(4,4'-bipy)(H_2O)_4](HBS)_2·3H_2O}_n (28). Both 21 and 22 are mixed-valenced copper complexes, and 21 is a two-dimensional network, while 22 consists of one-dimensional chain. 23 only contains the decarboxylation product, 4-hydroxybenzenesulfonate ion is free ligand and acts as counter ion. However,24 contains both decarboxylation and hydrolysis products, both of which are free ligands, acting as counter ions or guest molecules. Complexes 25-28 only exist the products of decarboxylation, which are also free ligands. 25 is two-dimensional layer network, while 28 consists of one-dimensional chain. 26 and 27 are isostructural, mononeutral.
DMF can take hydrolysis reaction under reflux or hydrothermal conditions, and the product, formate, can coordinate to metal ions. Two complexes containing the hydrolysis products of DMF have been synthesized and characterized: {[M(COO)(H_2O)_2(4,4'-bipy)]_2[M(4,4'-bipy)(Hssal)_2(H_2O)_2]}_n (M=Cd, 29; Mn, 30). These two complexes are isostructural and consist of one-dimensional chains, further extended into three-dimensional network by hydrogen bonding.
对于金属铜配合物研究了不同反应条件(反应物组成及配比、温度、溶剂等)、合成方法及中性配体对配合物拓扑网络结构的影响，共合成了8个配合物，分别为：[Cu(Hssal)(2,2'-bipy)(H_2O)_2]_n(1)，[Cu_4(CH_3COO)_2(ssal)_2(2,2'-bipy)_4(H_2O)_2]·6H_2O(2)，{[Cu(ssal)(2,2'-bipy)][Cu_2(ssal)(2,2'-bipy)_2(H_2O)_2](H_2O)}_n (3)，{[Cu_3(ssal)_2(dpa)_3]·3H_2O}_n (4)，[Cu_2~Ⅱ(ssal)_2(dpa)_2][Cu~Ⅰ(dpa)_2]_2·2H_2O (5)，{[Cu(ssal)(H_2O)](2-ampy)}_n (6)，{[Cu_3(ssal)_2(BD)_6]·8H_2O}_n (7)，[Cu(TTF)(phen)(H_2O)][Cu(TTF)(Hssal)(phen)](8)。配合物1为一维链状结构，并通过氢键作用扩展为三维网络结构；2为四核单元，也通过氢键形成三维网络结构；3为两条阴、阳离子一维链结构，并通过氢键形成二维网络结构。4为二维层状网络结构，而在相似的合成条件下，5却为混合价态Cu配合物，单核结构。6和7都为一维链状网络结构，只是6中还存在游离的2-氨基吡啶阳离子；而8为双核离子缔合物。配合物1和8中H_3ssal只脱去两个氢，保留羟基上的氢；2—7中，全部去质子化。在这8个配合物中，5—磺基水杨酸离子有7种配位方式。
对于主族金属铅配合物研究了不同中性配体(螯合及桥联)对配合物拓扑网络结构的影响，共合成了8个配合物，分别为：[Pb(Hssal)(2,2'-bipy)(DMF)]_n(9)，[Pb(Hssal)(2,2'-bipy)(H_2O)]_n(10)，[Pb(Hssal)(phen)(DMF)]_n(11)，[Pb_3(ssal)_2(phen)_3]_n(12)，{[Pb(Hssal)(2,2'-bipy)](4,4'-bipy)_(0．5)}_n (13)，Pb_2(2,2'-bipy)_2(4,4'-bipy)(Hssal)_2(H_2O)_2] (14)，[Pb(phen)(4,4'-bipy)_(0．5)(Hssal)]_n (15)，[Pb(Hssal)(2,2'-bipy)(bpe)_(0．5)]_n (16)。9和11结构相同，都为一维梯链状结构；10和12为二维网络结构；13也为一维梯链状结构，不过存在4,4'-bipy客体分子；14为双核结构，其中4,4'-bipy配体双齿配位；15也为一维梯链状结构，4,4'-bipy分子单齿配位；16为二维网络结构。除了12，其他7个配合物中，H_3ssal只脱去两个氢，保留羟基上的氢。在这8个配合物中，5—磺基水杨酸离子共存在6种配位模式。在配合物9、11和16中，铅的孤对电子不具有立体化学活性，而在其他5个化合物中都具有立体化学活性，并影响了铅的配位环境。此外，弱的Pb-O键作用和π-π堆积作用也对铅的配位环境有影响。
对于过渡金属Co和Zn，得到了两离子缔合物[Co(phen)_2(H_2O)_2](Hssal)·4H_2O(17)和[Zn(phen)_2(H_2O)_2](Hssal)·4H_2O(19)，并以它们为原料进行次级合成，得到了两个混金属配合物{[Co(phen)(H_2O)_4][Cu_2(phen)_2(ssal)_2]·5H_2O (18)和[Zn_2(μ-OH)_2(phen)_2(H_2O)_2][Cu_2(phen)_2(ssal)_2]·3H_2O(20)。17和19结构相似，Hssal~(2-)都未参与配位，只是作为抗衡离子存在；而在18和20中，Hssal~(2-)继续去质子化，并参与配位。
水热条件下的原位反应，到目前为止大部分机理还不甚清楚，这是近年来广大化学工作者关注的一个焦点。我们在5—磺基水杨酸功能化合物的设计合成过程中发现水热下的三种原位反应：Cu(Ⅱ)的还原反应、脱羧反应及水解反应，并合成了8个配合物，分别为{[Cu~ⅠCu~Ⅱ(ssal)(2,2'-bipy)(4,4'-bippy)]·2H_2O}_n (21)，{[Cu~Ⅱ(ssal)_2][Cu_4~Ⅰ(4,4'-bipy)_4(H_2O)]·5H_2O}_n (22)，[Cu(2,2'-bipy)_2Cl]·(4-HBS)·2H_2O(23)，[Cu(2,2'-bipy)_2Cl]·(4-HBS)·(1,4-dp)_(0．5)·H_2O (24)，{[Cd_3(CH_3COO)_4(4,4'-bipy)_4](HBS)_2·10H_2O}_n (25)，[Cd(4,4'-bipy)_2(H_2O)_4](HBS)_2·4H_2O(26)，[Mn(4，4'-bipy)_2(H_2O)_4](HBS)_2·4H_2O (27)，{[Co(4,4'-bipy)(H_2O)_4](HBS)_2·3H_2O}_n (28)。21和22为铜混合价态配合物，21为二维网络结构，22为一维链状结构。23中有脱羧产物，对羟基苯磺酸离子，但不参与配位，只作为抗衡离子存在。24中既有脱羧产物，还有水解产物，不过它们都没参与配位，分别作为抗衡离子和客体分子存在。25—28中只存在脱羧产物，对羟基苯磺酸离子，也没有参加配位。25为二维网络结构；26和27结构相同，都为单核结构；28为一维链状结构。
DMF在加热回流下发生水解反应，其产物甲酸根也会与金属配位，得到两个配合物{[M(COO)(H_2O)_2(4，4’-bipy)]_2[M(4，4’-bipy)(Hssal)_2(H_2O)_2]}_n(M=Cd，29；Mn，30)。这两配合物结构相似，都为一维链状结构，并通过氢键作用扩展为三维网络结构。
In this presentation, we report the syntheses, crystal structures and properties of the metal coordination complexes constructed from 5-sulfosalicylate (H_3ssal). In the procedures of syntheses, we chose 2,2'-bipyridine (2,2'-bipy), 4,4'-bipyridine (4,4'-bipy), 1,10-phenanthroline (1,10-phen), 2-aminopyridine (2-ampy), benzimidazole (BD) and trans-1,2-bis(4-pyridyl)ethylene (bpe) as neutral ligands, and Pb, Cu, Co, Zn, Cd and Mn as metal ions in our research. Totally thirty compounds were synthesized, and have been characterized by X-ray single crystal diffraction, IR spectrum, element analysis, TG and photoluminescent.
For copper complexes, we focused on the effect of the reaction conditions (reactants, the molar ratio, temperature and solvent), and neutral ligands on the structures. We discussed eight copper complexes: [Cu(Hssal)(2,2'-bipy)(H_2O)_2]_n(1), [Cu_4(CH_3COO)_2(ssal)_2(2,2'-bipy)_4(H_2O)_2]·6H_2O (2),{[Cu(ssal)(2,2'-bipy)][Cu_2(ssal)(2,2'-bipy)_2(H_2O)_2](H_2O)}_n (3),{[Cu_3(ssal)_2(dpa)_3]·3H_2O}_n (4), [Cu_2~Ⅱ(ssal)_2(dpa)_2][Cu~Ⅰ(dpa)_2]_2·2H_2O (5), {[Cu(ssal)(H_2O)](2-ampy)}_n (6), {[Cu_3(ssal)_2(BD)_6]·8H_2O}_n (7),[Cu(TTF)(phen)(H_2O)][Cu(TTF)(Hssal)(phen)] (8). The framework is one-dimensional chain in 1, tetraneutral in 2, two one-dimensional cationic-anionic chains in 3; all of which are extended to three-dimensional network by hydrogen bonding. 4 has two-dimensional layer network, however, in the similar synthesis condition, 5 is a mixed-valence copper complex. Both 6 and 7 are one-dimensional structures. 8 is a cationic-anionic complex. In complexes 1 and 8, H_3ssal ligands are doubly deprotonated and remain phenol protons; while in the other six compounds, they are fully deprotonated. There are seven coordination modes of 5-sulfosalicylates in the eight complexes.
For lead complexes, we focused on the effect of neutral ligands (chelating and bridging) on the structures. There are eight complexes synthesized and characterized: [Pb(Hssal)(2,2'-bipy)(DMF)]_n (9), [Pb(Hssal)(2,2'-bipy)(H_2O)]_n (10), [Pb(Hssal)(phenXDMF)]_n (11), [Pb_3(ssal)_2(phen)_3]_n (12),{[Pb(Hssal)(2,2'-bipy)](4,4'-bipy)_(0.5)}_n (13), Pb_2(2,2'-bipy)_2(4,4'-bipy)(Hssal)_2(H_2O)_2] (14), [Pb(phen)(4,4'-bipy)_(0.5)(Hssal)]_n (15), [Pb(Hssal)(2,2'-bipy)(bpe)_(0.5)]_n (16). Complexes 9 and 11 are isostructural, consisting of one-dimensional ladder-like chains. 10 is a two-dimensional double-layer architecture, while 12 is a two-dimensional layer network. The structure of complex 13 possesses a one-dimensional ladder-like chain with guest 4,4'-bipy molecules, while the molecular structure of complex 14 is a dimeric species with a coordinating 4,4'-bipy ligand. Complex 15 consists of a one-dimensional ladder-like chain with monodentate 4,4'-bipyridine but somewhat different from that of complex 13. Complex 16 is a two-dimensional layer structure. The coordination spheres of Pb~Ⅱions in 9-16 are controlled by three factors: the activity of a lone pair of electrons, weak Pb-0 interactions, andπ-πstacking interactions. The Pb~Ⅱlone pairs in 9,11 and 16 are inactive, whereas in the other five complexes, they are stereochemically active. Except in 12, H_3ssal is fully deprotonated, while in the other seven complexes, it only loses two protons. 5-Sulfosalicylate anions have six coordination modes in the eight complexes.
For transition metal Co and Zn, we have synthesized two cationic-anionic complexes: [Co(phen)_2(H_2O)_2](Hssal)·4H_2O (17) and [Zn(phen)_2(H_2O)_2](Hssal)·4H_2O (19), which act as the reactants for the secondary synthsis, and two mixed-metal complexes have been gotten: {[Co(phen)(H_2O_)4][Cu_2(phen)_2(ssal)_2]·5H_2O (18) and [Zn_2(μ-OH)_2(phen)_2(H_2O)_2][Cu_2(phen)_2(ssal)_2]·3H_2O (20). 17 and 19 are isostructure, where Hssal~(2-) ions are free ligands and act as counter ions. In 18 and 20, Hssal~(2-) ligands are further deprotonated and coordinated to metal ions.
Hydrothermal in situ ligand synthesis has been rapidly developed over the past several years due to its effectiveness, simplicity and environmental friendliness. However, up to now, most of the mechanisms of the in situ ligand syntheses have not been very clear. We have discovered three hydrothermal in-situ reactions in the process of synthesizing 5-sulfosalicylate complexes: the redox of Cu(Ⅱ), decarboxylation and hydrolysis. Eight products of in-situ reactions have been obtained and characterized: {[Cu~ⅠCu~Ⅱ(ssal)(2,2'-bipy)(4,4'-bippy)]·2H_2O}_n (21),{[Cu~Ⅱ(ssal)_2][Cu_4~Ⅰ(4,4'-bipy)_4(H_2O)]·5H_2O}_n (22), [Cu(2,2'-bipy)_2Cl]·(4-HBS)·2H_2O (23),[Cu(2,2'-bipy)_2Cl]·(4-HBS)·(1 ,4-dp)_(0.5)·H_2O (24),{[Cd_3(CH_3COO)_4(4,4'-bipy)_4](HBS)_2·10H_2O}_n (25),[Cd(4,4'-bipy)_2(H_2O)_4](HBS)_2·4H_2O (26), [Mn(4,4'-bipy)_2(H_2O)_4](HBS)_2·4H_2O (27), {[Co(4,4'-bipy)(H_2O)_4](HBS)_2·3H_2O}_n (28). Both 21 and 22 are mixed-valenced copper complexes, and 21 is a two-dimensional network, while 22 consists of one-dimensional chain. 23 only contains the decarboxylation product, 4-hydroxybenzenesulfonate ion is free ligand and acts as counter ion. However,24 contains both decarboxylation and hydrolysis products, both of which are free ligands, acting as counter ions or guest molecules. Complexes 25-28 only exist the products of decarboxylation, which are also free ligands. 25 is two-dimensional layer network, while 28 consists of one-dimensional chain. 26 and 27 are isostructural, mononeutral.
DMF can take hydrolysis reaction under reflux or hydrothermal conditions, and the product, formate, can coordinate to metal ions. Two complexes containing the hydrolysis products of DMF have been synthesized and characterized: {[M(COO)(H_2O)_2(4,4'-bipy)]_2[M(4,4'-bipy)(Hssal)_2(H_2O)_2]}_n (M=Cd, 29; Mn, 30). These two complexes are isostructural and consist of one-dimensional chains, further extended into three-dimensional network by hydrogen bonding.
引文
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