CN105367610A - 单核钴配合物及其制备方法 - Google Patents
单核钴配合物及其制备方法 Download PDFInfo
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- CN105367610A CN105367610A CN201510678984.3A CN201510678984A CN105367610A CN 105367610 A CN105367610 A CN 105367610A CN 201510678984 A CN201510678984 A CN 201510678984A CN 105367610 A CN105367610 A CN 105367610A
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- cobalt complex
- monokaryon
- mmole
- pyridyl
- amine
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- 150000004700 cobalt complex Chemical class 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 150000001412 amines Chemical class 0.000 claims abstract description 11
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 125000000339 4-pyridyl group Chemical group N1=C([H])C([H])=C([*])C([H])=C1[H] 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 4
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 229910020647 Co-O Inorganic materials 0.000 claims description 3
- 229910020676 Co—N Inorganic materials 0.000 claims description 3
- 229910020704 Co—O Inorganic materials 0.000 claims description 3
- 125000004429 atom Chemical group 0.000 claims description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 3
- 229910001429 cobalt ion Inorganic materials 0.000 claims description 3
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 125000006850 spacer group Chemical group 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000003446 ligand Substances 0.000 abstract 1
- 229910052708 sodium Inorganic materials 0.000 abstract 1
- 239000011734 sodium Substances 0.000 abstract 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 abstract 1
- 150000003623 transition metal compounds Chemical class 0.000 abstract 1
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical group OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000001455 metallic ions Chemical class 0.000 description 1
- 239000013384 organic framework Substances 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 150000003222 pyridines Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table
- C07F15/06—Cobalt compounds
- C07F15/065—Cobalt compounds without a metal-carbon linkage
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyridine Compounds (AREA)
Abstract
本发明公开了一种单核钴配合物及其制备方法。该钴配合物的结构见说明书附图图1。本发明利用间苯二甲酸-5-磺酸钠、双(4-吡啶基)胺为配体与六水合氯化钴通过水热法获得单核钴配合物，本发明具有工艺简单、成本低廉、重复性好等优点，为合成过渡金属配合物提供了一定的依据。
Description
技术领域
本发明属于配合物制备技术领域，特别涉及一种单核钴配合物及其制备方法。
背景技术
芳香羧酸类配体具有刚性平面，有利于电子转移。它在制备配合物过程中配位稳定不易发生变化，这使得它相较于其他有机配体更容易按照人们的意愿去配位，更容易设计配合物的构型，成功率大大提高。因此，在合成配合物的过程中，芳香羧酸类配体成了人们的首选。另外，含氮杂环类配体中氮原子含有孤对电子易于与金属离子配位，也常常用来做配体。由芳香羧酸类和吡啶类组成的金属有机骨架在配合物这一领域是人们研究的热点。
发明内容
本发明的目的是提供一种单核钴配合物的结构及其制备方法。
本发明的思路：利用间苯二甲酸-5-磺酸钠、双(4-吡啶基)胺为配体与六水合氯化钴通过水热法获得单核钴配合物。
所述钴配合物属于单斜晶系，空间群为P21。该配合物是一个单核的四元配合物，每个结构单元中包含一个Co(II)离子，一个间苯二甲酸-5-磺酸阴离子，一个双(4-吡啶基)胺，四个配位的水分子以及两个游离的水分子。间苯二甲酸-5-磺酸阴离子的磺酸基是质子化的，通过一个羧基的一个氧原子与钴离子配位。Co1与来自一个间苯二甲酸-5-磺酸阴离子的氧原子O2，一个双(4-吡啶基)胺的氮原子N1，四个水分子的氧原子O8、O9、O10、O11配位。配位数为六，六个配位原子在Co(II)离子周围以畸形八面体形式排布。Co-O键长在2.0358?-2.1466?之间，Co-N键长为2.1435?。
上述钴配合物的制备方法为：
(1)称量0.1~0.5毫摩尔间苯二甲酸-5-磺酸钠溶解于5~10毫升蒸馏水中，将溶液移入容积为25毫升的密封反应釜中。
(2)在步骤（1）所得溶液中加入0.2~1毫摩尔氢氧化钠和0.1~0.5毫摩尔的双(4-吡啶基)胺。
(3)称量0.1~1毫摩尔六水合氯化钴溶于5~10毫升的蒸馏水中。
(4)将步骤（3）所得溶液加入到步骤（2）所得溶液中，将反应釜密封，在120℃下恒温3天，然后缓慢冷却至室温，过滤，收集滤液，静置保存，20天后得到红色块状晶体，即为单核钴配合物。
本发明具有工艺简单、成本低廉、重复性好等优点，成功的合成了单核钴配合物，为合成钴配合物提供了一定的依据。
附图说明
图1是本发明的钴配合物的结构图。
具体实施方式
实施例：
(1)称量0.1毫摩尔(0.0268g)间苯二甲酸-5-磺酸钠溶解于5毫升蒸馏水中，将溶液移入容积为25毫升的密封反应釜中。
(2)在步骤（1）所得溶液中加入0.2毫摩尔(0.008g)氢氧化钠和0.1毫摩尔(0.0171g)的双(4-吡啶基)胺。
(3)称量0.1毫摩尔(0.0237g)六水合氯化钴溶于5毫升的蒸馏水中。
(4)将步骤（3）所得溶液加入到步骤（2）所得溶液中，将反应釜密封，在120℃下恒温3天，然后缓慢冷却至室温，过滤，收集滤液，静置保存，20天后得到红色块状晶体，即为单核钴配合物。
制得的单核钴配合物的结构见图1，单核钴配合物属于单斜晶系，空间群为P21。该配合物是一个单核的四元配合物，每个结构单元中包含一个Co(II)离子，一个间苯二甲酸-5-磺酸阴离子，一个双(4-吡啶基)胺，四个配位的水分子以及两个游离的水分子。间苯二甲酸-5-磺酸阴离子的磺酸基是质子化的，通过一个羧基的一个氧原子与钴离子配位。Co1与来自一个间苯二甲酸-5-磺酸阴离子的氧原子O2，一个双(4-吡啶基)胺的氮原子N1，四个水分子的氧原子O8、O9、O10、O11配位。配位数为六，六个配位原子在Co(II)离子周围以畸形八面体形式排布。Co-O键长在2.0358?-2.1466?之间，Co-N键长为2.1435?。
Claims (2)
1.一种单核钴配合物，其特征在于单核钴配合物的结构见说明书附图图1；
所述单核钴配合物属于单斜晶系，空间群为P21；该配合物是一个单核的四元配合物，每个结构单元中包含一个Co(II)离子，一个间苯二甲酸-5-磺酸阴离子，一个双(4-吡啶基)胺，四个配位的水分子以及两个游离的水分子；间苯二甲酸-5-磺酸阴离子的磺酸基是质子化的，通过一个羧基的一个氧原子与钴离子配位；Co1与来自一个间苯二甲酸-5-磺酸阴离子的氧原子O2，一个双(4-吡啶基)胺的氮原子N1，四个水分子的氧原子O8、O9、O10、O11配位；配位数为六，六个配位原子在Co(II)离子周围以畸形八面体形式排布；Co-O键长在之间，Co-N键长为
2.根据权利要求1所述的单核钴配合物的制备方法，其特征在于具体步骤为：
(1)称量0.1～0.5毫摩尔间苯二甲酸-5-磺酸钠溶解于5～10毫升蒸馏水中，将溶液移入容积为25毫升的密封反应釜中；
(2)在步骤(1)所得溶液中加入0.2～1毫摩尔氢氧化钠和0.1～0.5毫摩尔的双(4-吡啶基)胺；
(3)称量0.1～1毫摩尔六水合氯化钴溶于5～10毫升的蒸馏水中；
(4)将步骤(3)所得溶液加入到步骤(2)所得溶液中，将反应釜密封，在120℃下恒温3天，然后缓慢冷却至室温，过滤，收集滤液，静置保存，20天后得到红色块状晶体，即为单核钴配合物。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106496285A (zh) * | 2016-09-12 | 2017-03-15 | 桂林理工大学 | 间苯二甲酸钴配位聚合物及其制备方法 |
| CN111362987A (zh) * | 2020-03-23 | 2020-07-03 | 桂林理工大学 | 一种钴配合物的晶体结构及其磁性质 |
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- 2015-10-19 CN CN201510678984.3A patent/CN105367610A/zh active Pending
Non-Patent Citations (1)
| Title |
|---|
| JACQUELINE S. LUCAS等,: "Substituent dependent dimensionalities in cobalt isophthalate supramolecular complexes and coordination polymers containing dipyridylamine ligands", 《INORGANICA CHIMICA ACTA》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106496285A (zh) * | 2016-09-12 | 2017-03-15 | 桂林理工大学 | 间苯二甲酸钴配位聚合物及其制备方法 |
| CN111362987A (zh) * | 2020-03-23 | 2020-07-03 | 桂林理工大学 | 一种钴配合物的晶体结构及其磁性质 |
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Application publication date: 20160302 |