1，4，5，6-四氢-6-氧-3-哒嗪酸配合物的合成、晶体结构和性质研究
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摘要
利用溶液法和水热法,本文合成了二十个未见报道的1,4,5,6-四氢-6-氧-3-哒嗪酸(Htopca)金属配合物。通过红外光谱、X-射线单晶衍射等手段,较系统地研究了它们的晶体结构,并对配合物(1)、(2)、(3)、(7)、(8)进行了差热分析,在磁场强度为0.5T外加磁场中,在2～300K温度区间内测定了配合物(15)、(16)和(17)的变温磁化率。
所用的配体1,4,5,6-四氢-6-氧-3-哒嗪酸(Htopca)在本论文中出现了以下几种配位方式:
本论文分为以下三部分:
第一章:1,4,5,6-四氢-6-氧-3-哒嗪酸与锌、镉、钴、镍盐直接反应得到结构类似的配合物[Zn(topca)2(H2O)2] (1)、[Zn(topca)2(H2O)2]·2H2O (2)、[Cd(topca)2(H2O)2] (4)、[Co(topca)2(H2O)2]·2H2O (5)、[Ni(topca)2(H2O)2]·2H2O (6),与硝酸锌、2,2’-bipy反应得到配合物[Zn(topca)(2,2’-bipy)](NO3) (3),与不同的锰盐反应得到了中心离子结构类似、抗衡阴离子不同的配合物{[Mn(topca)(H2O)3](topca)·2H2O}n (7)和{[Mn(topca) (H2O)3](ClO4)}n (8),与氯化铜反应,在不同pH值下,得到了中心离子结构类似、结晶水分子数目不同的配合物[Cu(topca)2]·2H2O (9)和[Cu(topca)2]·4H2O (10)。其中(8)属于正交晶系,其余均单斜晶系,(1)～(10)的空间群分别为:P2(1)/n、P2(1)/n、P2(1)/c、P2(1)/n、P2(1)/c、P2(1)/c、Pc、Pna2(1)、P2(1)/c、P2(1)/n。
在(1)、(2)、(4)、(5)、(6)中,中心金属离子M(II)为六配位拉长的八面体结构,配体以(a)形式参与配位。在(3)中,中心金属离子Zn(II)为六配位畸变的八面体结构,Zn(II)与来自(a)形式配体的氧原子、氮原子、2,2’-bipy上两个氮原子以及两个水分子配位。在(7)和(8)中,配体均以(b)形式参与配位,羧基氧原子以双齿桥联的形式参与配位,将相邻的两个Mn(II)离子连接起来形成一维链状结构。在(9)和(10)中,配体均以(a)形式参与配位,中心离子Cu(II)处于四配位的平面四边形配位环境中。分子间氢键将配合物(1)～(9)连成二维网状结构,将配合物(10)连接成三维网络结构。此外,对配合物(1)、(2)、(3)、(7)和(8)分别进行了差热分析。
第二章:1,4,5,6-四氢-6-氧-3-哒嗪酸与钙和铅的氯化物反应得到配合物[Ca(topca)_2(H_2O)_2]n (11)和[Pb(topca)_2(H_2O)_2]_n (12) ,与氧化铋反应得到配合物{[Bi(topca)_3(H_2O)]·H_2O}_n (13)。晶体均属于单斜晶系,空间群均为P2(1)/c。
在配合物(11)中,中心金属离子Ca(II)为八配位的四方反棱柱结构,配体以(c)形式参与配位,在(12)中,中心金属离子Pb(II)为六配位畸变的八面体结构,配体以(d)形式配位,在配合物(11)和(12)中每个配体连接两个中心离子,一个中心离子则连接四个配体形成二维网状结构。在(13)中,中心金属离子Bi(III)为八配位扭曲的四方反棱柱结构,配体以(a)和(b)两种形式配位,配体的2-N原子和两个羧基氧原子以三齿配体的形式与两个Bi(III)离子配位,从而形成一维链状结构。
第三章:1,4,5,6-四氢-6-氧-3-哒嗪酸与镧、镨、钕、钐、铕、钆的氯化物反应,用KOH溶液调至恰好产生浑浊(pH = 5.5),得到配合物{[La(topca)_3(H_2O)_3]·2H_2O}_n (14)、{[Pr(topca)_3(H_2O)_3]·2H_2O}n (15)、[Nd(topca)_3(H_2O)2]n (16)、[Sm(topca)3(H_2O)_2]_n (17),用KOH溶液调至恰好产生浑浊(pH = 3.5),得到配合物[Eu(topca)_3(H_2O)_3]·3H_2O (18)和[Gd(topca)_3(H_2O)_3]·3H_2O (19),与氧化镝直接反应得到配合物[Dy(topca)_3(H_2O)3]·3.5H_2O (20)。晶体均属于单斜晶系,(14)和(15)空间群均为Pc,(16)和(17)空间群均为P2(1)/c (18)～(20)空间群均为P2(1)/n。
在(14)～(20)中,中心金属离子Ln(III)均为九配位的单帽四方反棱柱结构。在(14)和(15)中,配体以(a)、(b)和(e)三种形式配位,在(16)和(17)中,配体以(a)和(b)两种形式配位,由(b)形式的配体将配合物(14)～(17)连接成一维链状结构,在(18)、(19)和(20)中,配体以(a)形式配位,分子间氢键将(14)～(20)连成三维网络结构。磁性数据表明:配合物(15)和(16)的金属离子间存在反铁磁相互作用。
In this dissertation, twenty new coordination complexes of 1,4,5,6-Tetrahydro-6-oxo-3- pyridazine carboxylic acid have been synthesized by the liquid method or hydrothermal method. They were studied by IR and single crystal X-ray diffraction methods. The thermogravimetric analyses of complexes (1), (2), (3), (7) and (8) were studied, and the magnetic analyses of complex (15), (16) and (17) was also studied.
The ligand we used is 1,4,5,6-Tetrahydro-6-oxo-3-pyridazine carboxylic acid (Htopca), and it has several coordination modes in this dissertation, as follows:
There are three chapters in this dissertation:
Chapter one: The complexes of [Zn(topca)_2(H_2O)_2] (1), [Zn(topca)_2(H_2O)_2]·2H2O (2), [Cd(topca)_2(H_2O)_2] (4), [Co(topca)_2(H_2O)_2]·2H2O (5) and [Ni(topca)_2(H_2O)_2]·2H2O (6) were obtained by the reaction of Htopca and corresponding metallic salts. [Zn(topca)(2,2’-bipy)] (NO3) (3) was obtained by the reaction of Htopca, Zn(NO3)_2·6H2O and 2,2’-bipy. The complexes of {[Mn(topca)(H2O)_3](topca)·2H2O}n (7) and {[Mn(topca)(H2O)_3](ClO4)}n (8) were obtained by reaction of Htopca and different manganic salts. [Cu(topca)_2]·2H2O (9) and [Cu(topca)_2]·4H2O (10) were obtained by the reaction of Htopca and CuCl2·2H2O, while in different pH values. Complex (8) belongs to Orthorhombic, while others belong to monoclinic system, and space groups are P2(1)/n, P2(1)/n, P2(1)/c, P2(1)/n, P2(1)/c, P2(1)/c, Pc, Pna2(1), P2(1)/c, P2(1)/n, respectively.
In complex (1), (2), (4), (5) and (6), M(II) ion is six-coordinated and then formed a distorted octahedron geometry, and ligands coordinate with M(II) ion via (a) in these complexes. In complex (3), Zn(II) is six-coordinated with N3O3 environment, one oxygen atom and one nitrogen atom from the ligand, two nitrogen atoms from 2,2’-bipy, and two oxygen atoms from water molecules. In complex (7) and (8), the ligands coordinate with Mn(II) ions via (b), and Mn(II) ions are connected to 1-D chain structure by bidentate bridging carboxyl O atoms. In complex (9) and (10), Cu(II) ion is four-coordinated and then formed a rectangle geometry. The complex (1)～(9) are assembled to 2-D network structure and (10) is assembled to 3-D network structure by hydrogen bonds. We also have studied thermogravimetric analyses of complex (1), (2), (3), (7) and (8).
Chapter two: Complex [Ca(topca)_2(H_2O)_2]n (11) and [Pb(topca)_2(H_2O)_2]n (12) were obtained by the reaction of Htopca and corresponding metallic chlorides, while {[Bi(topca)_3(H_2O)]·H_2O}n (13) was obtained by the reaction of Htopca and Bi2O3. All the complexes belong to monoclinic system, and space groups are P2(1)/c.
In complex (11), the ligand exists in the form of (c), and Ca(II) ion is eight-coordinated, and then formed a distorted square antiprismatic coordination polyhedron. In complex (12), the ligand exists in the form of (d), and Pb(II) ion is six-coordinated, and then formed a distorted octahedron geometry. Both in complex (11) and (12), each ligand links two metal centers and each metal center coordinates four ligands to form a 2-D network. In complex (13), the ligand exists in the forms of (a) and (b), and Bi(III) ion is eight-coordinated, and then formed a distorted square antiprism. The ligand is bridging and chelating tridentate mode in which the coordinated atoms are two carboxyl O atoms and one pyridazinly N atom. By bridging carboxyl O atoms, the complex (13) is connected to 1-D chain structure. Chapter three: Complex {[La(topca)_3(H_2O)_3]·2H_2O}n (14), {[Pr(topca)_3(H_2O)_3]·2H_2O}n (15), [Nd(topca)_3(H_2O)_2]n (16), [Sm(topca)_3(H_2O)_2]n (17), [Eu(topca)_3(H_2O)_3]·3H_2O (18) and [Gd(topca)_3(H_2O)_3]·3H_2O (19) were obtained by the reaction of Htopca and corresponding metallic chlorides. The pH values of the reaction systems of (14)～(17) are 5.5, while (18) and (19) are 3.5. Complex [Dy(topca)_3(H_2O)_3]·3.5H_2O (20) was obtained by the reaction of Htopca and Dy2O3.
Complex (14)～(20) belong to monoclinic system, and space groups of (14) and(15) are Pc, (16) and(17) are P2(1)/c, and (18)～(20) are P2(1)/n. In complex (14)～(20), Ln(III) ion is nine-coordinated and then formed a distorted single-capped square antiprismatic geometry. In complex (14) and (15), the ligands exist in the forms of (a), (b) and (e), and in (16) and (17), the ligands coordinate with Ln(III) ions via (a) and (b). Complex (14)～(17) were connected to 1-D chain structure via the form of (b). In complex (18), (19) and (20), the ligands exist in the form of (a), and intermolecular hydrogen bonds link the complexe of (14)～(20) into 3-D network structures. The magnetic data indicates antiferromagnetic coupling between the metal ions in complex (15) and (16).
所用的配体1,4,5,6-四氢-6-氧-3-哒嗪酸(Htopca)在本论文中出现了以下几种配位方式:
本论文分为以下三部分:
第一章:1,4,5,6-四氢-6-氧-3-哒嗪酸与锌、镉、钴、镍盐直接反应得到结构类似的配合物[Zn(topca)2(H2O)2] (1)、[Zn(topca)2(H2O)2]·2H2O (2)、[Cd(topca)2(H2O)2] (4)、[Co(topca)2(H2O)2]·2H2O (5)、[Ni(topca)2(H2O)2]·2H2O (6),与硝酸锌、2,2’-bipy反应得到配合物[Zn(topca)(2,2’-bipy)](NO3) (3),与不同的锰盐反应得到了中心离子结构类似、抗衡阴离子不同的配合物{[Mn(topca)(H2O)3](topca)·2H2O}n (7)和{[Mn(topca) (H2O)3](ClO4)}n (8),与氯化铜反应,在不同pH值下,得到了中心离子结构类似、结晶水分子数目不同的配合物[Cu(topca)2]·2H2O (9)和[Cu(topca)2]·4H2O (10)。其中(8)属于正交晶系,其余均单斜晶系,(1)～(10)的空间群分别为:P2(1)/n、P2(1)/n、P2(1)/c、P2(1)/n、P2(1)/c、P2(1)/c、Pc、Pna2(1)、P2(1)/c、P2(1)/n。
在(1)、(2)、(4)、(5)、(6)中,中心金属离子M(II)为六配位拉长的八面体结构,配体以(a)形式参与配位。在(3)中,中心金属离子Zn(II)为六配位畸变的八面体结构,Zn(II)与来自(a)形式配体的氧原子、氮原子、2,2’-bipy上两个氮原子以及两个水分子配位。在(7)和(8)中,配体均以(b)形式参与配位,羧基氧原子以双齿桥联的形式参与配位,将相邻的两个Mn(II)离子连接起来形成一维链状结构。在(9)和(10)中,配体均以(a)形式参与配位,中心离子Cu(II)处于四配位的平面四边形配位环境中。分子间氢键将配合物(1)～(9)连成二维网状结构,将配合物(10)连接成三维网络结构。此外,对配合物(1)、(2)、(3)、(7)和(8)分别进行了差热分析。
第二章:1,4,5,6-四氢-6-氧-3-哒嗪酸与钙和铅的氯化物反应得到配合物[Ca(topca)_2(H_2O)_2]n (11)和[Pb(topca)_2(H_2O)_2]_n (12) ,与氧化铋反应得到配合物{[Bi(topca)_3(H_2O)]·H_2O}_n (13)。晶体均属于单斜晶系,空间群均为P2(1)/c。
在配合物(11)中,中心金属离子Ca(II)为八配位的四方反棱柱结构,配体以(c)形式参与配位,在(12)中,中心金属离子Pb(II)为六配位畸变的八面体结构,配体以(d)形式配位,在配合物(11)和(12)中每个配体连接两个中心离子,一个中心离子则连接四个配体形成二维网状结构。在(13)中,中心金属离子Bi(III)为八配位扭曲的四方反棱柱结构,配体以(a)和(b)两种形式配位,配体的2-N原子和两个羧基氧原子以三齿配体的形式与两个Bi(III)离子配位,从而形成一维链状结构。
第三章:1,4,5,6-四氢-6-氧-3-哒嗪酸与镧、镨、钕、钐、铕、钆的氯化物反应,用KOH溶液调至恰好产生浑浊(pH = 5.5),得到配合物{[La(topca)_3(H_2O)_3]·2H_2O}_n (14)、{[Pr(topca)_3(H_2O)_3]·2H_2O}n (15)、[Nd(topca)_3(H_2O)2]n (16)、[Sm(topca)3(H_2O)_2]_n (17),用KOH溶液调至恰好产生浑浊(pH = 3.5),得到配合物[Eu(topca)_3(H_2O)_3]·3H_2O (18)和[Gd(topca)_3(H_2O)_3]·3H_2O (19),与氧化镝直接反应得到配合物[Dy(topca)_3(H_2O)3]·3.5H_2O (20)。晶体均属于单斜晶系,(14)和(15)空间群均为Pc,(16)和(17)空间群均为P2(1)/c (18)～(20)空间群均为P2(1)/n。
在(14)～(20)中,中心金属离子Ln(III)均为九配位的单帽四方反棱柱结构。在(14)和(15)中,配体以(a)、(b)和(e)三种形式配位,在(16)和(17)中,配体以(a)和(b)两种形式配位,由(b)形式的配体将配合物(14)～(17)连接成一维链状结构,在(18)、(19)和(20)中,配体以(a)形式配位,分子间氢键将(14)～(20)连成三维网络结构。磁性数据表明:配合物(15)和(16)的金属离子间存在反铁磁相互作用。
In this dissertation, twenty new coordination complexes of 1,4,5,6-Tetrahydro-6-oxo-3- pyridazine carboxylic acid have been synthesized by the liquid method or hydrothermal method. They were studied by IR and single crystal X-ray diffraction methods. The thermogravimetric analyses of complexes (1), (2), (3), (7) and (8) were studied, and the magnetic analyses of complex (15), (16) and (17) was also studied.
The ligand we used is 1,4,5,6-Tetrahydro-6-oxo-3-pyridazine carboxylic acid (Htopca), and it has several coordination modes in this dissertation, as follows:
There are three chapters in this dissertation:
Chapter one: The complexes of [Zn(topca)_2(H_2O)_2] (1), [Zn(topca)_2(H_2O)_2]·2H2O (2), [Cd(topca)_2(H_2O)_2] (4), [Co(topca)_2(H_2O)_2]·2H2O (5) and [Ni(topca)_2(H_2O)_2]·2H2O (6) were obtained by the reaction of Htopca and corresponding metallic salts. [Zn(topca)(2,2’-bipy)] (NO3) (3) was obtained by the reaction of Htopca, Zn(NO3)_2·6H2O and 2,2’-bipy. The complexes of {[Mn(topca)(H2O)_3](topca)·2H2O}n (7) and {[Mn(topca)(H2O)_3](ClO4)}n (8) were obtained by reaction of Htopca and different manganic salts. [Cu(topca)_2]·2H2O (9) and [Cu(topca)_2]·4H2O (10) were obtained by the reaction of Htopca and CuCl2·2H2O, while in different pH values. Complex (8) belongs to Orthorhombic, while others belong to monoclinic system, and space groups are P2(1)/n, P2(1)/n, P2(1)/c, P2(1)/n, P2(1)/c, P2(1)/c, Pc, Pna2(1), P2(1)/c, P2(1)/n, respectively.
In complex (1), (2), (4), (5) and (6), M(II) ion is six-coordinated and then formed a distorted octahedron geometry, and ligands coordinate with M(II) ion via (a) in these complexes. In complex (3), Zn(II) is six-coordinated with N3O3 environment, one oxygen atom and one nitrogen atom from the ligand, two nitrogen atoms from 2,2’-bipy, and two oxygen atoms from water molecules. In complex (7) and (8), the ligands coordinate with Mn(II) ions via (b), and Mn(II) ions are connected to 1-D chain structure by bidentate bridging carboxyl O atoms. In complex (9) and (10), Cu(II) ion is four-coordinated and then formed a rectangle geometry. The complex (1)～(9) are assembled to 2-D network structure and (10) is assembled to 3-D network structure by hydrogen bonds. We also have studied thermogravimetric analyses of complex (1), (2), (3), (7) and (8).
Chapter two: Complex [Ca(topca)_2(H_2O)_2]n (11) and [Pb(topca)_2(H_2O)_2]n (12) were obtained by the reaction of Htopca and corresponding metallic chlorides, while {[Bi(topca)_3(H_2O)]·H_2O}n (13) was obtained by the reaction of Htopca and Bi2O3. All the complexes belong to monoclinic system, and space groups are P2(1)/c.
In complex (11), the ligand exists in the form of (c), and Ca(II) ion is eight-coordinated, and then formed a distorted square antiprismatic coordination polyhedron. In complex (12), the ligand exists in the form of (d), and Pb(II) ion is six-coordinated, and then formed a distorted octahedron geometry. Both in complex (11) and (12), each ligand links two metal centers and each metal center coordinates four ligands to form a 2-D network. In complex (13), the ligand exists in the forms of (a) and (b), and Bi(III) ion is eight-coordinated, and then formed a distorted square antiprism. The ligand is bridging and chelating tridentate mode in which the coordinated atoms are two carboxyl O atoms and one pyridazinly N atom. By bridging carboxyl O atoms, the complex (13) is connected to 1-D chain structure. Chapter three: Complex {[La(topca)_3(H_2O)_3]·2H_2O}n (14), {[Pr(topca)_3(H_2O)_3]·2H_2O}n (15), [Nd(topca)_3(H_2O)_2]n (16), [Sm(topca)_3(H_2O)_2]n (17), [Eu(topca)_3(H_2O)_3]·3H_2O (18) and [Gd(topca)_3(H_2O)_3]·3H_2O (19) were obtained by the reaction of Htopca and corresponding metallic chlorides. The pH values of the reaction systems of (14)～(17) are 5.5, while (18) and (19) are 3.5. Complex [Dy(topca)_3(H_2O)_3]·3.5H_2O (20) was obtained by the reaction of Htopca and Dy2O3.
Complex (14)～(20) belong to monoclinic system, and space groups of (14) and(15) are Pc, (16) and(17) are P2(1)/c, and (18)～(20) are P2(1)/n. In complex (14)～(20), Ln(III) ion is nine-coordinated and then formed a distorted single-capped square antiprismatic geometry. In complex (14) and (15), the ligands exist in the forms of (a), (b) and (e), and in (16) and (17), the ligands coordinate with Ln(III) ions via (a) and (b). Complex (14)～(17) were connected to 1-D chain structure via the form of (b). In complex (18), (19) and (20), the ligands exist in the form of (a), and intermolecular hydrogen bonds link the complexe of (14)～(20) into 3-D network structures. The magnetic data indicates antiferromagnetic coupling between the metal ions in complex (15) and (16).
引文
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