CN101759723B - 1-(4-carboxy phenyl)-5-sulfydryl-1H-tetrazole and 4, 4'-bipyridyl blending cobalt composition and preparation method thereof - Google Patents
1-(4-carboxy phenyl)-5-sulfydryl-1H-tetrazole and 4, 4'-bipyridyl blending cobalt composition and preparation method thereof Download PDFInfo
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- CN101759723B CN101759723B CN2009102274274A CN200910227427A CN101759723B CN 101759723 B CN101759723 B CN 101759723B CN 2009102274274 A CN2009102274274 A CN 2009102274274A CN 200910227427 A CN200910227427 A CN 200910227427A CN 101759723 B CN101759723 B CN 101759723B
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Abstract
The invention relates to a 1-(4-carboxy phenyl)-5-sulfydryl-1H-tetrazole and 4, 4'-bipyridyl blending cobalt composition and a preparation method thereof. The composition has a chemical formula as follows: {[Co(L)(4, 4'-bipy)(H2O)2](H2O)2}, wherein L=1-(4-carboxy phenyl)-5-sulfydryl-1H-tetrazole anion ligand; and 4, 4'-bipy=4, 4'-bipyridyl. The composition is prepared by adopting a diffusion method which is different from synthesizing methods, i.e. a hydrothemal method and the like, of a conventional cobalt metal carboxylic ligand blending composition reported in the traditional literature and overcomes the technical defects of high temperature, pressure and danger, low productivity, difficult purification and separation and poor repeatability; the synthesizing method showed by the invention has moderate condition, high productivity and good repeatability at normal temperature and pressure; and in addition, a magnetism test result of a crystal sample of the composition lays the theoretical foundation for further developing a novel magnetic-function molecular material.
Description
Technical field
The invention belongs to transition metal complex material field, be specifically related to a kind of 1-(4-carboxyphenyl)-5-sulfydryl-1H-tetrazolium and 4,4 '-'-bipyridyl blending cobalt composition and preparation method thereof, described title complex has the two-dimensional network structure, can be used as magneticsubstance by further Application and Development.
Background technology
In recent years, ligand polymer has attracted numerous Chinese scholars to put in the research in this field because of its various topological framework and good character, and such material all shows fabulous application prospect in all many-sides such as host-guest chemistry, magneticsubstance, superconducting material, nonlinear optical material, absorption, catalysis.Up to the present, people have prepared numerous ligand polymer and its performance have been studied.Used part mostly is carboxylic-acid and nitrogen heterocycles.Cobalt metal compounding has received people's very big concern and by a large amount of synthetic and research, has also become one of research focus of coordination chemistry simultaneously owing to having various structure and potential performance all the time.Up to the present, have the carboxylic acid part that enriches coordination mode, particularly fragrance contains two or many carboxyls part of phenyl ring by the extensive and a large amount of research of people.In addition, tetrazolium series part is widely used in the various research fields of coordination chemistry with its various coordination mode, has shown novel structure and potential high-performance.
Compare with above-mentioned carboxylic acid of mentioning that contains phenyl ring separately or independent tetrazolium part, sulfur-bearing tetrazolium carboxylic acid part, the research of its cobalt metal compounding is still seldom.This type of part is compared with the former has more hapto, its multiple bridging mode that has can form abundant coordination chemistry, the sulphur atom that it contained, tetrazyl and carboxyl not only can carry out coordination with metal in every way, and the three belongs to soft hapto and hard hapto respectively, mixed metal complex can also be constructed, thereby the type material of various novel structure function uniquenesses can be accessed with thermostability.Therefore, this type of title complex has wide space aspect the further research and development of structural research and performance.
This class part mixed ligand coordination compound adopts hydro-thermal or solvent thermal synthesis method usually.Hydro-thermal or solvent thermal are synthetic to be meant in enclosed system, utilizes synthetic that the chemical reaction of material in the solvent carries out under certain temperature and pressure.Usually in stainless steel cauldron (inner liner polytetrafluoroethylene), carry out.Hydro-thermal or solvent thermal are synthetic to be to be solvent with water or organic solvent, (100~240 ℃) at a certain temperature, boosting certainly of water strong (under 1~100Mpa) condition, the reaction that original stock carries out.The weak point of this method is, can only see the result generally speaking, is difficult to understand reaction process, and exist High Temperature High Pressure, dangerous big, productive rate is low and the technological deficiency of repeatable difference.
Summary of the invention
The object of the present invention is to provide a kind of 1-(4-carboxyphenyl)-5-sulfydryl-1H-tetrazolium and 4,4 '-'-bipyridyl blending cobalt composition and preparation method thereof.
For achieving the above object, the technical solution used in the present invention is as follows:
1-of the present invention (4-carboxyphenyl)-5-sulfydryl-1H-tetrazolium and 4,4 '-'-bipyridyl blending cobalt composition, this title complex has following chemical formula: [Co (L) (4,4 '-bipy) (H
2O)
2] (H
2O)
2}
∞, L=1-(4-carboxyphenyl)-5-sulfydryl-1H-tetrazolium anion ligand wherein, 4,4 '-bipy=4,4 '-dipyridyl, wherein the structural formula of L and 4,4 '-bipy is as follows respectively:
Described complex crystal belongs to triclinic(crystalline)system, and spacer is P-1, and unit cell parameters is a=6.907 (2), b=11.426 (4), c=13.192 (4)
α=89.135 (4), β=86.520 (4), γ=84.900 (4) °, V=1035.0 (5)
Basic structure is a two-dimensional network, and the free water molecules is connected in the free hole of two-dimensional network by bag.
The synthetic employing diffusion process of title complex: it comprises the steps: under the room temperature, the cobalt metal-salt is placed the test tube bottom, add dissolved in distilled water and form reaction solution A, reaction solution A upper strata adds methyl alcohol and water mixed solution C, the mixed solution C upper strata adds dissolves in 2, the part H of 6-lutidine
2The methyl alcohol reaction solution B of L and 4,4 '-bipy leaves standstill diffusion and obtained red bulk-shaped monocrystal in 20~30 days, with distilled water, methyl alcohol and ether washing, is drying to obtain successively.
Described cobalt metal-salt is any one in nitrate, perchlorate, vitriol or their hydrate.
The concentration of cobalt metal-salt is 0.02~0.04molL among the described reaction solution A
-1
The volume ratio of methyl alcohol and water mixed solution is 1: 1~1: 1.5 in the described mixed solution C.
Part H among the described reaction solution B
2L and part 4,4 '-mol ratio of bipy is 1: 1, part H among the reaction solution B
2The concentration of L is 0.01~0.02molL
-1
Part H among the described reaction solution B
2The volumetric molar concentration of L is 1: 1 with the ratio that reacts the volumetric molar concentration of cobalt metal-salt among the A.
Among the described reaction solution B 2,6-lutidine and part H
2The mol ratio of L is 1: 1~3: 1.
The volume ratio of reaction solution A, mixed solution C, reaction solution B is 1: 2: 1~1: 4: 1.
The synthetic method of title complex provided by the invention adopts Liquid Phase Diffusion method synthetic compound.Reaction solution A and reaction solution B are placed the bottom and the top of test tube respectively, and the middle buffer layer mixed solution C that adds at room temperature leaves standstill test tube then, and reaction solution A and B just have the interface to begin that mutual diffusion mutually is concurrent gives birth to reaction and generate title complex in the process of leaving standstill like this.This synthetic method has overcome its High Temperature High Pressure, danger is big, productive rate is low, be difficult to purifies and separates and repeatable poor technological deficiency.Following at normal temperature and pressure, mild condition, productive rate height, favorable reproducibility.
Description of drawings
Fig. 1 is Co coordination environment figure in the title complex;
Fig. 2 is the two-dimensional network structure iron of title complex;
Fig. 3 is the powdery diffractometry synoptic diagram of title complex;
Fig. 4 is title complex χ under the magnetic field of 5000G
m(Δ) and χ
MThe temperature variant curve of T (zero);
The susceptibility of title complex was with the curve of change of magnetic field strength when Fig. 5 was 2K;
Fig. 6 is the χ of title complex
m -1Temperature variant curve, solid line can better meet according to Curie-Weiss law in (20-300K) high-temperature zone.
Embodiment
Below by embodiment the present invention is elaborated, but and do not limit the present invention in any way.
With 0.1mmol Co (NO
3)
26H
2O places the test tube bottom, forms reaction solution A with the 5mL dissolved in distilled water; The middle mixed solution C 15ml that adds 1: 1 volume ratio of first alcohol and water; 0.1mmol H
2L and 0.1mmol4,4 '-bipy 5mL dissolve with methanol, add 2,6-lutidine 0.05mL obtains reaction solution B, places the test tube upper strata.Sealing and standing 24 days, the burgundy bulk-shaped monocrystal appears in the place, boundary that connects of solution interface on the test tube wall.Crystal washs with distilled water, methyl alcohol and ether successively, drying, and productive rate is about 50%.
Main infrared absorption peak is: 3447w, 3178w, 1605m, 1546m, 1413m, 1382m, 1363m, 1279m, 1218m, 1130m, 1103w, 1069w, 1040w, 1007m, 950w, 817m, 787m, 732w, 699w, 633m, 599m, 462w.
Embodiment 2
With 0.1mmol Co (ClO
4)
26H
2O places the test tube bottom, forms reaction solution A with the 4mL dissolved in distilled water; The middle mixed solution C 16ml that adds 1: 1.5 volume ratio of first alcohol and water; 0.1mmol H
2L and 0.1mmol 4,4 '-bipy 4mL dissolve with methanol add 2, and 6-lutidine 0.05mL obtains reaction solution B, places the test tube upper strata.Sealing and standing 28 days, the burgundy bulk-shaped monocrystal appears in the place, boundary that connects of solution interface on the test tube wall.Crystal washs with distilled water, methyl alcohol and ether successively, vacuum-drying, and productive rate is 55%.
Main infrared absorption peak is: 3447w, 3178w, 1605m, 1546m, 1413m, 1382m, 1363m, 1279m, 1218m, 1130m, 1103w, 1069w, 1040w, 1007m, 950w, 817m, 787m, 732w, 699w, 633m, 599m, 462w.
With 0.2mmol CoSO
47H
2O places the test tube bottom, forms reaction solution A with the 5mL dissolved in distilled water; The middle mixed solution C 12ml that adds 1: 1.2 volume ratio of first alcohol and water; 0.05mmol H
2L and 0.05mmol 4,4 '-bipy 5mL dissolve with methanol add 2, and 6-lutidine 0.03mL obtains reaction solution B, places the test tube upper strata.Sealing and standing 30 days, the burgundy bulk-shaped monocrystal appears in the place, boundary that connects of solution interface on the test tube wall.Crystal washs with distilled water, methyl alcohol and ether successively, vacuum-drying, and productive rate is 52%.
Main infrared absorption peak is: 3447w, 3178w, 1605m, 1546m, 1413m, 1382m, 1363m, 1279m, 1218m, 1130m, 1103w, 1069w, 1040w, 1007m, 950w, 817m, 787m, 732w, 699w, 633m, 599m, 462w.
Embodiment 4
With 0.15mmol Co (NO
3)
26H
2O places the test tube bottom, forms reaction solution A with the 5mL dissolved in distilled water; The middle mixed solution C 10ml that adds 1: 1.3 volume ratio of first alcohol and water; 0.05mmol H
2L and 0.05mmol 4,4 '-bipy 5mL dissolve with methanol add 2, and 6-lutidine 0.04mL obtains reaction solution B, places the test tube upper strata.Sealing and standing 25 days, the burgundy bulk-shaped monocrystal appears in the place, boundary that connects of solution interface on the test tube wall.Crystal washs with distilled water, methyl alcohol and ether successively, vacuum-drying, and productive rate is 56%.
Main infrared absorption peak is: 3447w, 3178w, 1605m, 1546m, 1413m, 1382m, 1363m, 1279m, 1218m, 1130m, 1103w, 1069w, 1040w, 1007m, 950w, 817m, 787m, 732w, 699w, 633m, 599m, 462w.
The relevant characterization of title complex
(1) crystal 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 through the Mo-K of graphite monochromator monochromatization alpha-ray (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 the hydrogen atom position is determined by theoretical mode computation.Detailed axonometry data see Table 1; Important bond distance and bond angle data see Table 2.Crystalline structure is seen Fig. 1 and Fig. 2.
Fig. 1: the Co coordination environment figure of title complex; Fig. 2: the two-dimensional network structure iron of title complex.
(2) the XPRD phase purity of title complex characterizes
The XPRD of title complex characterizes and shows that it has reliable phase purity, for its further research as magneticsubstance provides assurance.See Fig. 3.(instrument model: Bruker/D8Advance).
(3) magnetic property of title complex research
(cooperation unit: Unitat de Mesures Magnetiques of Universitat deBarcelona) is finished in the magnetic test of title complex (adopting crystal prototype, about 30mg) on SQUID MPMS-XL magnetometer.Magneticstrength 5T, the temperature range of alternating temperature susceptibility test is 2~300K (0-5T is at interval); Diamagnetic part is proofreaied and correct with the Pascal constant.Test result such as Fig. 4, Fig. 5 and shown in Figure 6.Fig. 4 has provided the χ of this title complex
mAnd χ
MT is temperature variant trend in the 2-300K scope.Under 5000G magnetic field during 300K, χ
MT=3.31cm
3K mol
-1When temperature is reduced to 2K, χ
MT also descends up to 1.39cm thereupon
3K mol
-1In temperature is 2K, when magneticstrength is 5T, and the specific magnetising moment (M/N μ
B) reached saturation value 2.40 (shown in Figure 5).The magnetic result that experiment obtains is consistent with Co (II) the ionic magnetic behavior of octahedral coordination environment.High-temperature zone alternating temperature susceptibility between 20K-300K meets Curie-Weiss law: C=3.49cm
3Mol
-1, θ=-15.57K (r=0.998).Along with magneticstrength is reduced to 500G, the susceptibility of title complex does not have the presentation dependency.When the magneticstrength position is 50G, there are not zero-fieldcool-field cool (ZFC-FC) hysteresis and long-range magnetic disorder.Fig. 6 is the χ of title complex
m -1Temperature variant curve, solid line can better meet according to Curie-Weiss law in (20-300K) high-temperature zone.Relevant test result has been established theoretical basis for further developing this type of novel magnetic functional molecule material.
The main crystallographic data of table 1 title complex
aR=∑(||F
0|-|F
C||)/∑|F
0|;
bwR=[∑w(|F
0|
2-|F
C|
2)
2/∑w(F
0 2)
2]
1/2.
The main bond distance of table 2 title complex
And bond angle [°]
*
*Symmetry code: #1x, y+1, z #2x-1, y, z
Claims (9)
- A 1-(4-carboxyphenyl)-5-sulfydryl-1H-tetrazolium and 4,4 '-'-bipyridyl blending cobalt composition, it is characterized in that: this title complex has following chemical formula: [Co (L) (4,4 '-bipy) (H 2O) 2] (H 2O) 2} ∞, L=1-(4-carboxyphenyl)-5-sulfydryl-1H-tetrazolium anion ligand wherein, 4,4 '-bipy=4,4 '-dipyridyl;Described complex crystal belongs to triclinic(crystalline)system, and spacer is P-1, and unit cell parameters is a=6.907 (2) b=11.426 (4) c=13.192 (4) α=89.135 (4) °, β=86.520 (4) °, γ=84.900 (4) °, V=1035.0 (5) Basic structure is a two-dimensional network, and the free water molecules is connected in the free hole of two-dimensional network by bag.
- 2. the described 1-of claim 1 (4-carboxyphenyl)-5-sulfydryl-1H-tetrazolium and 4,4 '-preparation method of '-bipyridyl blending cobalt composition, it is characterized in that: it comprises the steps: under the room temperature, the cobalt metal-salt is placed the test tube bottom, add dissolved in distilled water and form reaction solution A, reaction solution A upper strata adds methyl alcohol and water mixed solution C, and the mixed solution C upper strata adds dissolves in 2, the part H of 6-lutidine 2The methyl alcohol reaction solution B of L and 4,4 '-bipy leaves standstill diffusion and obtained red bulk-shaped monocrystal in 20~30 days, with distilled water, methyl alcohol and ether washing, is drying to obtain successively.
- 3. 1-according to claim 2 (4-carboxyphenyl)-5-sulfydryl-1H-tetrazolium and 4,4 '-preparation method of '-bipyridyl blending cobalt composition, it is characterized in that: described cobalt metal-salt is any one in nitrate, perchlorate, vitriol or their hydrate.
- According to claim 2 or 3 described 1-(4-carboxyphenyl)-5-sulfydryl-1H-tetrazolium and 4,4 '-preparation method of '-bipyridyl blending cobalt composition, it is characterized in that: the concentration of cobalt metal-salt is 0.02~0.04molL among the reaction solution A -1
- 5. the preparation method of 1-according to claim 2 (4-carboxyphenyl)-5-sulfydryl-1H-tetrazolium and 4,4 '-'-bipyridyl blending cobalt composition is characterized in that: the volume ratio of methyl alcohol and water mixed solution is 1: 1~1: 1.5 in the mixed solution C.
- 6. the preparation method of 1-according to claim 2 (4-carboxyphenyl)-5-sulfydryl-1H-tetrazolium and 4,4 '-'-bipyridyl blending cobalt composition is characterized in that: part H among the reaction solution B 2L and part 4,4 '-mol ratio of bipy is 1: 1, part H among the reaction solution B 2The concentration of L is 0.01~0.02molL -1
- According to claim 2 or 6 described 1-(4-carboxyphenyl)-5-sulfydryl-1H-tetrazolium and 4,4 '-preparation method of '-bipyridyl blending cobalt composition, it is characterized in that: part H among the reaction solution B 2The ratio of the volumetric molar concentration of cobalt metal-salt is 1: 1 among the volumetric molar concentration of L and the reaction solution A; Among the reaction solution B 2,6-lutidine and part H 2The mol ratio of L is 1: 1~3: 1.
- 8. the preparation method of 1-according to claim 2 (4-carboxyphenyl)-5-sulfydryl-1H-tetrazolium and 4,4 '-'-bipyridyl blending cobalt composition is characterized in that: the volume ratio of reaction solution A, mixed solution C, reaction solution B is 1: 2: 1~1: 4: 1.
- The described 1-of claim 1 (4-carboxyphenyl)-5-sulfydryl-1H-tetrazolium and 4,4 '-'-bipyridyl blending cobalt composition is as the application of magneticsubstance.
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CN102382145B (en) * | 2011-08-27 | 2013-09-25 | 南昌航空大学 | Cobalt coordination compound containing 5-(3-pyridyl)-isophthalic acid organic ligands and preparation method for same |
CN102584866B (en) * | 2012-01-18 | 2014-06-18 | 郑州轻工业学院 | 1,2-naphthalene diacid containing cadmium coordination complex and preparation method thereof |
CN102603779B (en) * | 2012-01-18 | 2014-08-27 | 郑州轻工业学院 | Cadmium 3,4-bis(4'-carboxyphenyl) benzoate coordination compound and preparation method thereof |
CN102690296B (en) * | 2012-06-26 | 2014-07-30 | 天津师范大学 | 5-methyl-1H-tetrazole cobalt (II) complex magnetic material, and preparation method and application thereof |
CN102942596B (en) * | 2012-12-06 | 2015-05-20 | 河南大学 | One-dimensional coordination polymer magnetic material constructed by Co(II)-carboxyl and preparation method thereof |
CN104628790B (en) * | 2015-01-26 | 2017-09-22 | 郑州轻工业学院 | Selective absorption microporous cobalt metal-organic framework materials and preparation method thereof |
CN108727251B (en) * | 2018-05-17 | 2021-03-02 | 商丘师范学院 | Magnetic cobalt (II) complex based on 4, 4' -bipyridyl-itaconic acid derivative ligand and preparation method thereof |
CN110437465B (en) * | 2019-08-30 | 2020-09-01 | 武汉大学 | Cobalt complex, preparation method thereof and application of cobalt complex as proton conducting material |
CN110394161B (en) * | 2019-09-06 | 2020-09-08 | 武汉大学 | Application of cobalt complex as greenhouse gas adsorption material |
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