CN103467499A - Copper complex with 2,2'-dipyridyl and preparation method thereof - Google Patents
Copper complex with 2,2'-dipyridyl and preparation method thereof Download PDFInfo
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- CN103467499A CN103467499A CN 201310424590 CN201310424590A CN103467499A CN 103467499 A CN103467499 A CN 103467499A CN 201310424590 CN201310424590 CN 201310424590 CN 201310424590 A CN201310424590 A CN 201310424590A CN 103467499 A CN103467499 A CN 103467499A
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Abstract
The invention relates to a copper complex with 2,2'-dipyridyl and a preparation method thereof. The copper complex is a complex in the chemical formula (I) of [Cu(L)(C2O4)].H2O, wherein L is 2,2'-dipyridyl, and the complex has a one-dimensional chain-shape spatial structure. The preparation method comprises the following steps of: dissolving Cu(CH3COO)2.H2O, pyridine-2,3,5-tricarboxylic acid and 2,2'-dipyridyl in 10mL of water, dripping a droplet of pyridine, and transferring the solution into a stainless steel reaction kettle lined with polytetrafluoroethylene, sealing, and reacting for 3 days at 110 DEG C, and cooling to room temperature; filtering, standing and volatizing the solution to obtain a target product.
Description
Technical field
The invention belongs to title complex science and technology field, particularly with 2, the preparation method of the copper complex of 2 '-dipyridyl.
Technical background
In recent years, the synthetic extensive concern for preparing scientific circles of a metal-organic complex, they are in atmosphere storage, selective separation, catalysis, the fields such as medicament slow release have potential using value.Synthesizing at many metal complexess of copper metal complexes accounts for vital role.At medical field, the metal complexes of copper has anti-tumor activity, becomes the emphasis [Li Xue etc., Guangdong chemical industry, 108 39 2012] of inorganic anticancer complex research; In the applied chemistry field, the copper complex crystal can be used as liquid crystal material, is the emphasis [the chemical journal 331 64 2006 such as Zhao Hongbin] of liquid crystal material research.In the title complex of metallic copper, the kind of part, the factors such as space structure of title complex all can produce different impacts to its physicochemical property.Therefore, by part, regulate and control and molecular self-assembling, the synthetic copper complex with novel space structure and function of design is the common objective that the various countries scientist pursues.
Summary of the invention
The purpose of this invention is to provide and a kind ofly contain 2, the preparation method of the copper complex of 2 '-dipyridyl.This metal copper complexes has the one-dimensional chain space structure, is with a wide range of applications.
The chemical formula of copper complex provided by the invention is [Cu (L) (C
2o
4)] H
2o, L=2 wherein, 2 '-dipyridyl.
As shown in Figure 1, their secondary building unit is: crystal belongs to triclinic(crystalline)system to the structure of copper complex disclosed by the invention, and spacer is P-1, and unit cell parameters is:
α=111.188 (3) °, β=97.329 (4) °, γ=104.965 (4) °; The space structure of this title complex is centered by copper atom, 2, and 2 '-dipyridyl and oxalate denominationby self-assembly and the one-dimensional chain structure that forms; The ligancy of Cu ion is 6, and from one 2, and two N atoms in 2 '-dipyridyl and from four O Atomic coordinates in two oxalates; They form the octahedron of distortion centered by Cu.N1, N2, O1, O3 are on octahedral equatorial plane, and bond distance and the angle of their correspondences are respectively: Cu1-N1,
cu1-N2,
cu1-O1,
cu1-O3,
n1-Cu1-O1,174.197 (74) °, N2-Cu1-O3,175.635 (70) °.O2A, O4A are on octahedral axle, O2A-Cu1-O4A, 158.559 (59) °; Cu1-O2A,
cu1-O4A,
copper atom and oxalate are interconnected to form one-dimensional chain structure (as Fig. 2), with 2 of cupric coordination, and the staggered both sides that appear at chain of 2 '-dipyridyl, and 2, the planes of molecules of 2 '-dipyridyl is vertical with whole chain, and bond angle is: N1-Cu1-O4A, 94.426 °; N2-Cu1-O2A, 94.066 °.
Preparation method of the present invention is as follows:
By Cu (CH
3cOO)
2h
2o, 2,3,5-pyridine three acid and 2,2 '-dipyridyl is dissolved in 10ml water, drips a pyridine, then solution is moved into to have in the teflon-lined stainless steel cauldron to seal, keep temperature be 110 ℃ three days, then with the Speed Reduction temperature of 5 ℃ per hour to room temperature.By solution filter, standing under the filtrate room temperature, an about Zhou Houke obtains blue crystallization.Cu (CH
3cOO)
2h
2o, 2,3,5-pyridine three acid, 2, the mass ratio of 2 '-dipyridyl is 1.92: 1.35: 1.
The accompanying drawing explanation
Fig. 1 [Cu (L) (C
2o
4)] H
2the crystalline structure figure of O;
The one-dimensional chain structure iron of Fig. 2 compound.
The crystallographic data of table 1 title complex
Embodiment
Synthesizing of embodiment 1 title complex:
Cu (CH by 0.15mmol
3cOO)
2h
22 of O (0.030g), 0.1mmol, 3,2 of 5-pyridine three acid (0.0212g) and 0.1mmol, 2 '-dipyridyl (0.0156g) is dissolved in 10ml water, drip a pyridine, then solution is moved into to having in the teflon-lined stainless steel cauldron of 15mL and seals, keep temperature be 110 ℃ three days, then with the Speed Reduction temperature of 5 ℃ per hour to room temperature.By solution filter, standing under the filtrate room temperature, an about Zhou Houke obtains blue crystallization.Calculating productive rate based on metallic copper is 30%.
The structure determination of embodiment 2 title complexs:
Crystal structure determination adopts BRUKER SMART1000X-x ray diffractometer x, the Mok alpha-ray of use process graphite monochromatization (
) be incident radiation, collect point diffraction with ω-2 θ scan mode, obtain unit cell parameters through least-squares refinement, from the difference Fourier electron density map, utilize the SHELXL-97 direct method to solve crystalline structure, and through Lorentz and polarizing effect correction.All H atoms are synthetic and definite through desirable position calculation by difference Fourier.Detailed axonometry data are in Table 1.Structure is shown in Fig. 1, Fig. 2; Fig. 1: [Cu (L) (C
2o
4)] H
2the crystalline structure figure of O, Fig. 2: the one-dimensional chain structure iron of compound.
Claims (5)
1. with 2, the copper complex of 2 '-dipyridyl, the chemical formula of this compound is [Cu (L) (C
2o
4)] H
2o, L=2 wherein, 2 '-dipyridyl.
2. according to claim 1 with 2, the copper complex of 2 '-dipyridyl is characterized in that its secondary building unit is:
Crystal belongs to triclinic(crystalline)system, and spacer is P-1, and unit cell parameters is:
α=111.188 (3) °, β=97.329 (4) °, γ=104.965 (4) °; The space structure of this title complex is centered by copper atom, 2, and 2 '-dipyridyl and oxalate denominationby self-assembly and the one-dimensional chain structure that forms; The ligancy of Cu ion is 6, and from one 2, and two N atoms in 2 '-dipyridyl and from four O Atomic coordinates in two oxalates; They form the octahedron of distortion centered by Cu.N1, N2, O1, O3 are on octahedral equatorial plane, and bond distance and the angle of their correspondences are respectively: Cu1-N1,
cu1-N2,
cu1-O1,
cu1-O3,
n1-Cu1-O1,174.197 (74) °, N2-Cu1-O3,175.635 (70) °.O2A, O4A are on octahedral axle, O2A-Cu1-O4A, 158.559 (59) °; Cu1-O2A,
cu1-O4A,
copper atom and oxalate are interconnected to form the one-dimensional chain structure, with 2 of cupric coordination, and the staggered both sides that appear at chain of 2 '-dipyridyl, and 2, the planes of molecules of 2 '-dipyridyl is vertical with whole chain, and bond angle is: N1-Cu1-O4A, 94.426 °; N2-Cu1-O2A, 94.066 °.
3. according to claim 1 with 2, the preparation method of the copper complex of 2 '-dipyridyl, is characterized in that it comprises the steps:
1) by measuring ratio Cu (CH
3cOO)
2h
2o, 2,3,5-pyridine three acid, 2,2 '-dipyridyl is dissolved in 8mL water;
2) drip a pyridine in solution and regulate pH value;
3) solution moved into to have in the teflon-lined stainless steel cauldron seal, react three days, then with the Speed Reduction temperature of 5 ℃ per hour to room temperature;
4), by solution filter, standing under the filtrate room temperature, an about Zhou Houke obtains target product.
4. according to claim 3 with 2, the preparation method of 2 '-Bipyridine-copper Complex, is characterized in that described Cu (CH
3cOO)
2h
2o, 2,3,5-pyridine three acid, 2, the mass ratio of 2 '-dipyridyl is 1.92: 1.35: 1.
5. according to claim 3 with 2, the preparation method of 2 '-Bipyridine-copper Complex, is characterized in that described reaction method is the hydro-thermal reaction method, and temperature of reaction is 110 ℃
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864823A (en) * | 2014-03-14 | 2014-06-18 | 洛阳师范学院 | Cu (I) coordination polymer green light emitting material and synthesis method thereof |
| CN105646549A (en) * | 2016-01-13 | 2016-06-08 | 山西大学 | Double-terminal-group pyridine copper complex and preparation method thereof |
| CN106397786A (en) * | 2016-09-12 | 2017-02-15 | 广西师范大学 | 3-carboxyl-5-thioketone-1,2,4-triazole copper coordination polymer and in-situ synthesis method thereof |
-
2013
- 2013-09-13 CN CN 201310424590 patent/CN103467499A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864823A (en) * | 2014-03-14 | 2014-06-18 | 洛阳师范学院 | Cu (I) coordination polymer green light emitting material and synthesis method thereof |
| CN103864823B (en) * | 2014-03-14 | 2016-08-24 | 洛阳师范学院 | A kind of Cu (I) coordination polymer green luminescent material and synthetic method thereof |
| CN105646549A (en) * | 2016-01-13 | 2016-06-08 | 山西大学 | Double-terminal-group pyridine copper complex and preparation method thereof |
| CN106397786A (en) * | 2016-09-12 | 2017-02-15 | 广西师范大学 | 3-carboxyl-5-thioketone-1,2,4-triazole copper coordination polymer and in-situ synthesis method thereof |
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Application publication date: 20131225 |