CN101024651B - Silver coordination polymer containing azacylo-ligand, its preparing method and use - Google Patents
Silver coordination polymer containing azacylo-ligand, its preparing method and use Download PDFInfo
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- CN101024651B CN101024651B CN200710056819XA CN200710056819A CN101024651B CN 101024651 B CN101024651 B CN 101024651B CN 200710056819X A CN200710056819X A CN 200710056819XA CN 200710056819 A CN200710056819 A CN 200710056819A CN 101024651 B CN101024651 B CN 101024651B
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- methyl
- pyridine
- benzoglyoxaline
- coordinated polymer
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Abstract
The invention supplies a nitrogen heterocyclic ring ligand silver coordination polymer and the producing method and the application. It has double helix structure and the complexes is {[Ag(L)]2(ClO4)2}n, and L is 4-(N- benzimidazole-methyl)- pyridine. The invention has simple structure, high yield, and stable fluorescence.
Description
Technical field
The present invention relates to transition metal complex material field, especially a kind of nitrogen heterocyclic ring part Ag coordinated polymer and preparation method and application thereof, described Ag coordinated polymer is to have double-stranded Ag coordinated polymer, and its photoluminescent property makes it can be used as fluorescent material and is applied.
Background technology
In recent years, to d
10The luminosity research of closedshell transition metal complex increases gradually.Because d
10Family's metal can with part generation metal-ligand charge transfer (MLCT), or part-metal charge transfer (LMCT) perhaps improves the fluorescence efficiency of part.Report [Tao, J. that the photoluminescent property of title complexs such as Zn, Cu, Ag was arranged again in recent years; Shi, J.X.; Tong, M.L.; Zhang, X.X.; Chen, X.M.Inorg.Chem., 2001,40,6328; Omary, M.A.; Rawashdeh-Omary, M.A.; Diyabala-nage, H.V.K.; Dias, H.V.R.Inorg.Chem.Commun.2003,42,8612; Dias, H.V.R.; Diyabalanage, H.V.K.; Rawashdeh-Omary, M.A.; Franzman, M.A.; Omary, M.A.J.Am.Chem.Soc.2003,125,12072; Li, J.; Zhou, J.H.; Li, Y.Z.; Chen, X.T.Wuji Huaxue Xuebao (Chinese J.Inorg.Chem.) 2004,7,841].Since the coordination compound of silver (I) have widely purposes (Wang Xianjiang etc., Wuhan University Of Science and Engineering's journal, Vol.16, No.2,2003,21-25).The Ag coordinated polymer of the fluorescent material that design is synthetic suitable is a very challenging job, up to now, is seen in report less relatively (Mi, the B.X. of document; Gao, Z.Q.; Lee, C.S.; Kwong, H.L.; Wang, N.B.; Lee, S.T.Journal of MaterialsChemistry 2001,11,2244-2247; Tao, X.T.; Miyata, S.; Sasabe, H.; Zhang, G.J.; Wada, T.; Jiang, M.H.Applied Physics Letters 2001,78,279-281).And it is double-stranded more rare.Because Ag
+The 3d track 10 electronics are arranged, have unique photoluminescent property, therefore, also be the new vitality of material science injection for synthetic and explore the type material blaze the trail.
Summary of the invention
The objective of the invention is to disclose a kind of nitrogen heterocyclic ring part silver complex and preparation method and application thereof, this silver complex has double-stranded Ag coordinated polymer, has the stable fluorescence performance under the normal temperature, thereby is the new vitality of material science injection.
Technical scheme of the present invention provides a kind of nitrogen heterocyclic ring part Ag coordinated polymer, it is characterized in that title complex is the compound of the compound of following chemical formula: { [Ag (L)]
2(ClO
4)
2N, and wherein L is 4-(N-benzoglyoxaline-methyl)-pyridine, its molecular formula is as follows:
The preparation method of described Ag coordinated polymer is as follows:
Under the room temperature, with 4-(N-benzoglyoxaline-methyl)-pyridine and AgClO
44CH
3CN stirred 0.5-1 hour in the mixed solvent of methyl alcohol and acetonitrile, filtered, and the normal temperature volatilization obtained colourless bulk-shaped monocrystal in 10～15 days, washing then, drying.
Nitrogen heterocyclic ring part Ag coordinated polymer preparation method technology of the present invention is simple, and yield is higher, has the stable fluorescence performance under the normal temperature, is applied thereby can be used as fluorescent material.
Description of drawings
Fig. 1 { [Ag (L)]
2(ClO
4)
2The unitary crystalline structure figure of n;
Fig. 2 { [Ag (L)]
2(ClO
4)
2The double-spiral structure figure of n;
Fig. 3 { [Ag (L)]
2(ClO
4)
2The solid fluorescence figure of n.
Embodiment
Complex crystal of the present invention belongs to rhombic system, and spacer is Fdd2, and unit cell parameters is: a=19.882
B=27.867
, c=9.902
, β=90 °; Based on the L part of two coordinate silver ionss head and the tail bridging, this part forms has double-stranded three-dimensional supramolecule network; Each part respectively with two silver ions coordinations, and each silver ions connects two parts respectively, and and ClO
4 -Between the weak effect of Ag-O is arranged.
In the preparation method of Ag coordinated polymer of the present invention, 4-(N-benzoglyoxaline-methyl)-pyridine and AgClO
44CH
3The mol ratio of CN is 1: 1, the volume ratio of methyl alcohol and acetonitrile: 1: 1～1: 1.2; 4-(N-benzoglyoxaline-methyl)-pyridine and AgC1O
44CH
3The concentration of CN in the mixed solution of methyl alcohol and acetonitrile is 0.04～0.05molL
-1
Synthesizing of embodiment 1 title complex:
1mmol 4-(N-benzoglyoxaline-methyl)-pyridine (0.209g), 1mmol AgClO
44CH
3The mixture of CN (0.540g) and 20mL methyl alcohol and acetonitrile (volume ratio is 1: 1) at room temperature stirs 0.5 hour after-filtration, and the room temperature volatilization obtained colourless bulk-shaped monocrystal after 10 days, washing, drying.Productive rate is 50%.
The main infrared absorption peak of title complex is: 3527cm
-1, 3112cm
-1, 2361cm
-1, 1610cm
-1, 1562cm
-1, 1509cm
-1, 1465cm
-1, 1427cm
-1, 1385cm
-1, 1297cm
-1, 1269cm
-1, 1226cm
-1, 1185cm
-1, 1117cm
-1, 1090cm
-1, 870cm
-1, 817cm
-1, 777cm
-1, 763cm
-1, 749cm
-1, 720cm
-1, 624cm
-1, 584cm
-1, 544cm
-1, 498cm
-1, 471cm
-1, 428cm
-1
Synthesizing of embodiment 2 title complexs:
0.8mmol 4-(N-benzoglyoxaline-methyl)-pyridine (0.167g), 0.8mmol AgClO
44CH
3The mixture of CN (0.432g) and 20mL methyl alcohol and acetonitrile (volume ratio is 1: 1.2) at room temperature stirs 0.5 hour after-filtration, and the room temperature volatilization obtained colourless bulk-shaped monocrystal after 12 days, washing, drying.Productive rate is 55%.
The main infrared absorption peak of title complex is: 3527cm
-1, 3112cm
-1, 2361cm
-1, 1610cm
-1, 1562cm
-1, 1509cm
-1, 1465cm
-1, 1427cm
-1, 1385cm
-1, 1297cm
-1, 1269cm
-1, 1226cm
-1, 1185cm
-1, 1117cm
-1, 1090cm
-1, 870cm
-1, 817cm
-1, 777cm
-1, 763cm
-1, 749cm
-1, 720cm
-1, 624cm
-1, 584cm
-1, 544cm
-1, 498cm
-1, 471cm
-1, 428cm
-1
Synthesizing of embodiment 3 title complexs:
1mmol 4-(N-benzoglyoxaline-methyl)-pyridine (0.209g), 1mmol AgClO
44CH
3The mixture of CN (0.540g) and 20mL methyl alcohol and acetonitrile (volume ratio is 1: 1.2) at room temperature stirs 1 hour after-filtration, and the room temperature volatilization obtained colourless bulk-shaped monocrystal after 10 days, washing, drying.Productive rate is 52%.
The main infrared absorption peak of title complex is: 3527cm
-1, 3112cm
-1, 2361cm
-1, 1610cm
-1, 1562cm
-1, 1509cm
-1, 1465cm
-1, 1427cm
-1, 1385cm
-1, 1297cm
-1, 1269cm
-1, 1226cm
-1, 1185cm
-1, 1117cm
-1, 1090cm
-1, 870cm
-1, 817cm
-1, 777cm
-1, 763cm
-1, 749cm
-1, 720cm
-1, 624cm
-1, 584cm
-1, 544cm
-1, 498cm
-1, 471cm
-1, 428cm
-1
The sign of embodiment 2 title complexs:
(1) structure determination of title complex
The monocrystalline of choosing suitable size at microscopically at room temperature carries out the X-ray diffraction experiment.On BrukerSmart 1000 CCD diffractometers, use Mo-K through the graphite monochromator monochromatization
αRay (λ=0.71073
), with
Mode is collected diffraction data.Carry out reduction of data with Bruker SAINT program.The diffraction data of part-structure carries out absorption correction with the SADABS program.Crystalline structure is solved in conjunction with difference Fourier is synthetic by direct method.All non-hydrogen atom coordinate and anisotropic parameters carry out the complete matrix least-squares refinement, and C-H and N-H atom site are determined by theoretical mode computation.Detailed axonometry data see Table 1.Structure is seen Fig. 1, Fig. 2; Fig. 1: { [Ag (L)]
2(ClO
4)
2N crystalline structure figure.Fig. 2: { [Ag (L)]
2(ClO
4)
2N double-spiral structure figure.
Complex crystal belongs to rhombic system, and spacer is Fdd2, and unit cell parameters is: a=19.882
, b=27.867
, c=9.902
, β=90 °; Based on the L part of two coordinate silver ionss head and the tail bridging, this part forms has double-stranded three-dimensional supramolecule network; Each part respectively with two silver ions coordinations, and each silver ions connects two parts respectively, and and ClO
4 -Between the weak effect of Ag-O is arranged.
(2) photoluminescent property of title complex
Exsiccant carries out fluorometric investigation after milled processed, excite at the 375nm place, all obtains emission peak at the 431nm place.Solid fluorescence figure sees Fig. 3.
The crystallographic data of table 1 title complex
Claims (4)
1. nitrogen heterocyclic ring part Ag coordinated polymer is characterized in that it is the compound of following chemical formula:
{ [Ag (L)]
2(ClO
4)
2N, and wherein L is 4-(N-benzoglyoxaline-methyl)-pyridine, its molecular formula is:
Complex crystal belongs to rhombic system, and spacer is Fdd2, and unit cell parameters is: a=19.882
B=27.867
C=9.902
β=90 °; Based on the L part of two coordinate silver ionss head and the tail bridging, this part forms has double-stranded three-dimensional supramolecule network; Each part respectively with two silver ions coordinations, and each silver ions connects two parts respectively, and and ClO
4 -Between the weak effect of Ag-O is arranged.
2. the preparation method of the described nitrogen heterocyclic ring part of claim 1 Ag coordinated polymer is characterized in that it comprises the steps: under the room temperature, with 4-(N-benzoglyoxaline-methyl)-pyridine and AgClO
44CH
3The mixed solvent that CN puts into methyl alcohol and acetonitrile stirred 0.5～1 hour, filtered, and the normal temperature volatilization obtained colourless bulk-shaped monocrystal in 10～15 days, washing then, and drying obtains; The preparation method of described Ag coordinated polymer is characterized in that the volume ratio of described methyl alcohol and acetonitrile: 1: 1～1: 1.2; The preparation method of described Ag coordinated polymer is characterized in that described 4-(N-benzoglyoxaline-methyl)-pyridine and AgClO
44CH
3The mol ratio of CN: 1: 1.
3. according to the preparation method of the described Ag coordinated polymer of claim 2, it is characterized in that described 4-(N-benzoglyoxaline-methyl)-pyridine and AgClO
44CH
3The concentration of CN in the mixed solution of methyl alcohol and acetonitrile is 0.04～0.05molL
-1
The described nitrogen heterocyclic ring part of claim 1 Ag coordinated polymer aspect material as the application of fluorescent material.
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| CN101406826B (en) * | 2008-11-17 | 2010-06-09 | 南开大学 | Coordination polymer having solvent selectivity reversible adsorption and preparation method thereof |
| CN102516984B (en) * | 2011-11-09 | 2015-09-16 | 中国科学院福建物质结构研究所 | A kind of orange red phosphor crystal material and its production and use |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005255773A (en) * | 2004-03-10 | 2005-09-22 | Shinobu Ito | Metal complex phosphor |
| CN1730509A (en) * | 2005-09-01 | 2006-02-08 | 南开大学 | Ag coordinated polymer and preparation method and uses |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005255773A (en) * | 2004-03-10 | 2005-09-22 | Shinobu Ito | Metal complex phosphor |
| CN1730509A (en) * | 2005-09-01 | 2006-02-08 | 南开大学 | Ag coordinated polymer and preparation method and uses |
Non-Patent Citations (4)
| Title |
|---|
| 张同来等.{[Ag{ATO}2]ClO4}n的制备和分子结构.化学学报58 5.2000,58(5),533-537. |
| 张同来等.{[Ag{ATO}2]ClO4}n的制备和分子结构.化学学报58 5.2000,58(5),533-537. * |
| 朱惠芳等.二维网状银配合物的合成、结构与性质研究.高等学校化学学报26 1.2005,26(1),19-21. |
| 朱惠芳等.二维网状银配合物的合成、结构与性质研究.高等学校化学学报26 1.2005,26(1),19-21. * |
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