CN108191921A - A kind of multi-nuclear metal cluster compound and preparation method based on iminodiacetic acid ligand - Google Patents
A kind of multi-nuclear metal cluster compound and preparation method based on iminodiacetic acid ligand Download PDFInfo
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- CN108191921A CN108191921A CN201711476355.8A CN201711476355A CN108191921A CN 108191921 A CN108191921 A CN 108191921A CN 201711476355 A CN201711476355 A CN 201711476355A CN 108191921 A CN108191921 A CN 108191921A
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- C—CHEMISTRY; METALLURGY
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- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic System
- C07F15/04—Nickel compounds
- C07F15/045—Nickel compounds without a metal-carbon linkage
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/42—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of organic or organo-metallic materials, e.g. graphene
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
Abstract
The present invention relates to a kind of multi-nuclear metal cluster compounds and preparation method based on iminodiacetic acid ligand.The chemical formula of the multi-nuclear metal cluster compound is：Tb26Ni28(ida)28(OH)70](NO3)8·35H2O.The present invention also provides the preparation method of the multi-nuclear metal cluster compound, specially：By Tb (NO3)3·6H2O、Ni(NO3)2·6H2O and iminodiacetic acid are soluble in water, adjust pH value to 3.5~4.5, obtain mixture；At a temperature of the mixture is placed in 160~200 DEG C, reaction 65~72 hours to get.Multi-nuclear metal cluster compound of the present invention is the metal cluster compound containing rare earth ion, there is hydroxyl oxygen bridge in molecular structure so that the shortening of the distance between metal ion interacts between metal and strengthens, show novel magnetism, such as the special magnetic property of unimolecule magnetic, Spin transition.
Description
Technical field
The present invention relates to a kind of cluster compounds and preparation method thereof more particularly to a kind of based on the more of iminodiacetic acid ligand
Core metal cluster compound and preparation method thereof.
Background technology
In recent years, synthesis with zero dimension multinuclear or high core transition metal and lanthanide series metal cluster compound become one it is emerging
Research hotspot.It is not only because this kind of coordination polymer and novel and perfection is shown in structure, it is often more important that this
A little potential using values of the compound in magnetoelectricity field, biochemistry, optical field.Such as Boston Univ USA
Armstrong teaches seminar, the Mn of synthesis4Cluster compound has the function of the photosynthetic work of class, and water turns in being acted on for mimic photosynthesis
Turn to the process of oxygen.For another example, the ferritin known to scientists is exactly a kind of metal cluster compound, research find be due to it
High spin ground state makes them have superparamagnetism and the property of molecule nano magnet.Also some metal cluster compounds are shown as
Spin property and catalytic activity (M.J.Science, 1995,268:77；J.Nature,1996,383:145).
Metal cluster compound shows novelty and uniqueness in configuration aspects, also shows good application in properties
Prospect.Just as mentioned in the introduction, ferromagnetic, antiferromagnetic deeper time has gradually been deep into from traditional for molecular magnetism research.
Wherein, the behaviors such as single molecular magnets, single-stranded magnetic, Spin transition, change magnetic are increasingly becoming the focus of research.In molecular magnetism research
In field, people generally select transition metal either rare earth synthesis three-dimensional or one-dimentional structure, but for linearly aligned mistake
The zero dimension cluster compound for crossing metal and rare earth ion then studies less [6-10], however the cluster compound in relation to Ni+Ln is then less.
Invention content
The purpose of the present invention is to provide a kind of multi-nuclear metal cluster compounds based on iminodiacetic acid ligand；The multinuclear
Metal cluster compound has novel four layers of nested structure, while has excellent molecular magnetism.
The chemical formula of the multi-nuclear metal cluster compound is：Tb26Ni28(ida)28(OH)70](NO3)8·35H2O；
Wherein, ida refers to iminodiacetic acid.
The metal cluster compound is anorthic system, and space group isContain 26 independences in the multi-nuclear metal cluster compound
Tb (III) ion, 28 independent Ni (II) ions and 28 independent ida ligand ions and 70 hydroxyl ions.
The complete structure of the multi-nuclear metal cluster compound is four layers of nested structure, as shown in Fig. 2,3A~D, the multinuclear gold
Belong to cluster compound structure from inside to outside, specifically：
First layer includes 8 Ni (II) ions, and eight ions are closely connected together by μ 3-OH as bridge, becomes nested
The core of structure, each Ni (II) ion is hexa-coordinate, deforms octoploids structure；
The second layer includes 20 Tb (III) ions, wherein 8 ions form cubical vertex, remaining Tb (III) ions position
In the midpoint of cube each edge, 20 Tb (III) ions are linked to be cubical 12 sides, μ 3-OH are simultaneously by μ 3-OH as bridge
As bridge, Tb (III) ions in the second layer and first layer Ni (II) ion are connected；
Third layer includes 32 Tb (III) ions, wherein having 3 μ 3- on Tb (III) ion in cube each edge
OH groups, one to Tb (III) ion adjacent in the bridging second layer, Ni (II) ion of the 4th layer of another pair bridging；
4th layer includes 48 Ni (II) ions, and similar to the cube on no vertex, each vertex position is this layer of structure
Three Ni (II) ions of rounded projections arranged, the geometry shape of entire molecule is similar to cube, positioned at cube apex
Ni (II) ions are by the N in ida ligands and O atom complexing (two carboxyls from ida), at the same time, O atom and third layer
Two independent Tb (III) ion complexations.The another two O atom of the ida carboxyls and adjacent Ni (II) ion coordination.
Wherein, all Ni (II) ions are hexa-coordinate environment, to deform octoploids structure；
There are two types of coordination modes for Tb (III) ion, and Tb (III) ion of the second layer is seven coordination modes, to add hat trigone
Column geometric configuration, Tb (III) ion of third layer is nine coordination modes, forms three cap trigone column configurations.
The spacing of adjacent metal ion The spacing is in normal range (NR).
The second object of the present invention is to provide a kind of preparation method of above-mentioned metal cluster compound.
Preferably, preparation method provided by the present invention includes at least：
By Tb (NO3)3·6H2O、Ni(NO3)2·6H2O and iminodiacetic acid are soluble in water, adjust pH value to 3.5-
4.5 obtain mixture；By the mixture in 10~20h, 175~185 DEG C are at the uniform velocity warming up to, maintains 35~70h of the temperature
Afterwards, 6~for 24 hours after, be at the uniform velocity cooled to room temperature to get.
Above-mentioned reaction carries out preferably in Muffle furnace.
Present invention adjusting pH value can be used usual manner and be adjusted；It is preferred that using sodium hydroxide solution；The hydroxide
A concentration of 0.8~1.2mol/L of sodium.
In the method for the invention, Tb (NO3)3·6H2O can be prepared by commercially available or this field conventional method
It arrives, present invention preferably employs following preparation methods to be made：
Tb (the NO3)3·6H2O is made with the following method：By Tb4O7With mass fraction be 65%~70% nitric acid,
After reacting 25~35min at a temperature of 90~110 DEG C, adjustment pH value for 3.4~4 to get.
Preparation method of the present invention, it is preferable that the Tb (NO3)3·6H2The O and Ni (NO3)2·6H2O's rubs
You are at ratio：1.4~1.9:1, preferably 1.65~1.72:1；
Ni (the NO3)2·6H2The molar ratio of O and the iminodiacetic acid is 1:1.6~2.4, preferably 1:1.9~
2.1。
Preferably, per water described in 1mL in molten 0.2~0.25mol the Tb (NO3)3·6H2O。
The condition of the preparation method can be more preferably by the mixture in 14~16h, to be at the uniform velocity warming up to
155~165 DEG C, then in 4.5~5.5h, continuation is at the uniform velocity warming up to 175~185 DEG C, after maintaining 36~38h of the temperature,
At the uniform velocity be cooled in 14~16h room temperature to get.
Most preferably, by the mixture in 15h, 160 DEG C are at the uniform velocity warming up to, then in 5h, continuation at the uniform velocity heats up
To 180 DEG C, after maintaining temperature 37h, be at the uniform velocity cooled in 15h room temperature to get.
The present invention provides a kind of preferred embodiment, and the preparation method of the multi-nuclear metal cluster compound is specifically, by Tb (NO3)3·
6H2O、Ni(NO3)2·6H2O and iminodiacetic acid are soluble in water, adjust pH value to 3.5~4.5, obtain mixture；By described in
Mixture is at the uniform velocity warming up to 175~185 DEG C in 8~12h, after maintaining 45~55h of temperature, is at the uniform velocity cooled in 6~12h
Room temperature, filtering, it is dry to get；
Wherein, the Tb (NO3)3·6H2The O and Ni (NO3)2·6H2The molar ratio of O is 1.65~1.72:1；It is described
Ni(NO3)2·6H2O is 1 in molar ratio with the iminodiacetic acid:1.9~2.1.
Another object of the present invention be above-mentioned multi-nuclear metal cluster compound molecular magnetic materials, more metal multi-iron materials and
Application on molecular memory Material Field.
Multi-nuclear metal cluster compound of the present invention is the metal cluster compound containing rare earth ion, has hydroxyl oxygen in molecular structure
Bridge so that the shortening of the distance between metal ion interacts between metal and strengthens, shows novel magnetism, such as unimolecule
The special magnetic property such as magnetic, Spin transition.
Preferably, the multi-nuclear metal cluster compound is in low-temperature nano temperature control magnetic switch, nano-magnetic controller field
Application.
Description of the drawings
Figure 1A is the variable temperature magnetic susceptibility curve graph of multi-nuclear metal cluster compound made from embodiment 1；
Figure 1B is the variable field magnetisation curve of multi-nuclear metal cluster compound made from embodiment 1；
Fig. 2 is the structure diagram of multi-nuclear metal cluster compound made from embodiment 1；
Fig. 3 A are the first layer structure diagram of multi-nuclear metal cluster compound made from embodiment 1；
Fig. 3 B are the second layer structure diagram of multi-nuclear metal cluster compound made from embodiment 1；
Fig. 3 C are the third layer structure diagram of multi-nuclear metal cluster compound made from embodiment 1；
Fig. 3 D are the four-layer structure schematic diagram of multi-nuclear metal cluster compound made from embodiment 1；
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Tb (NO in following examples3)3·6H2O is made with the following method：By Tb4O7With mass fraction for 65%~
70% nitric acid, after reacting 30min at a temperature of 100 DEG C, using the extra unreacted raw material of alkali neutralization, adjustment pH value is
3.5~4.5 to get.
Embodiment 1
By 1.69mmol Tb (NO3)3·6H2O、1mmol Ni(NO3)2·6H2O and 2mmol ida are added in 8mL water, are adopted
PH value is adjusted to 3.5~4.5 with the NaOH of 1mol/L, after stirring evenly, obtains mixture；It is even by the mixture in 15h
Speed is warming up to 160 DEG C, and then in 5h, continuation is at the uniform velocity warming up to 180 DEG C, after maintaining temperature 37h, at the uniform velocity cools down in 15h
To room temperature to get.
Multi-nuclear metal cluster compound obtained by the present embodiment is green bulk crystals, yield 62%.
Elemental analysis result C112H150N36Ni28Tb26O251 (%)：C 11.48, H1.26, N 4.29.IR(KBr,
cm-1)：3259(s),2969(vs),2934(vs),1641(m),1585(m),1397(m),1221(m),798(m).
Characterization experiment is carried out to multi-nuclear metal cluster compound made from embodiment 1.The crystal of size 0.1mm or so is selected,
Single crystal diffraction experiment is carried out using Rigaku R-axis Rapid IP surface detectors under room temperature or low temperature.WithRay, collects the diffraction data of cluster compound with ω -2 θ scan modes, testing result,
The crystallographic parameters of cluster compound are as shown in the table：
The crystallographic parameters of 1 cluster compound of table
A R1=Σ | | Fo |-| Fc | |/| Fo |, wR2=[2/ Σ w (Fo2) 2 of Σ w (Fo2-Fc2)] 1/2.
Within the temperature range of 2-300K, using the external magnetic field of 1000Oe embodiment 1 is made multi-nuclear metal cluster compound into
Variable temperature magnetic susceptibility test is gone.
During room temperature 300K, χ mT values are 451.5cm3K mol–1, slightly below 56 independences do not couple the Ni of ground state2+With 52
It is independent not couple ground state Tb3+Sum it up (468.76cm3Kmol–1).It is reduced with temperature, χ mT values also slowly decline therewith, are opened in 50K
Beginning rapid decrease reaches minimum value 400.0cm in 2K3K mol–1, the trend of curve shows before 2K, Ni2+、Tb3+Ion
Between interaction for antiferromagnetic coupling, as shown in Figure 1A.
In the temperature of 2K-300K, above test data is fitted using Curie-Weiss laws, is obtained
Curie constants C=458.7cm3K mol–1, Weiss constants θ=- 1.29K, negative Weiss constants have further demonstrated that cluster compound
It is weak antiferromagnetic interaction between intermediate ion.Isothermal magnetization rate curve in 2K is weak between can also proving each ion
Antiferromagnetic interaction, increased rapidly with the increase M values of field strength, be slowly increased after 2T, reach 482N when 7T
μBClose to theory saturation value 476N μB, as shown in Figure 1B.
Embodiment 2
By 1.69mmol Tb (NO3)3·6H2O、1mmol Ni(NO3)2·6H2O and 2mmol ida are added in 8mL water, are adopted
PH value is adjusted to 3.5~4.5 with the NaOH of 1mol/L, after stirring evenly, obtains mixture；It is even by the mixture in 10h
Speed is warming up to 180 DEG C, after maintaining temperature 70h, 12~it is interior for 24 hours be at the uniform velocity cooled to room temperature, filtering is spontaneously dried to get multinuclear
Metal cluster compound.
Multi-nuclear metal cluster compound obtained by the present embodiment is green bulk crystals, yield 82%.
Elemental analysis result C112H150N36Ni28Tb26O251 (%)：C 11.48, H1.26, N 4.29.IR(KBr,
cm-1)：3268(s),2998(vs),3010(vs),1680(m),1545(m),1354(m),1288(m),787(m)；
By analysis result it is recognized that while the yield of metal cluster compound is higher, but meet the crystal of 1 crystallographic parameters of table compared with
It is few.
Although above having used general explanation, specific embodiment and experiment, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (10)
1. a kind of multi-nuclear metal cluster compound based on iminodiacetic acid ligand, chemical formula are：Tb26Ni28(ida)28(OH)70]
(NO3)8·35H2O；Wherein ida refers to iminodiacetic acid.
2. multi-nuclear metal cluster compound according to claim 1, which is characterized in that the metal cluster compound is anorthic system,
Space group isCell parameter α=
69.38 (3) °, β=69.42 (3) °, γ=69.49 (3) °.
3. multi-nuclear metal cluster compound according to claim 1 or 2, which is characterized in that the knot of the multi-nuclear metal cluster compound
Structure is four layers of nested structure；
Preferably, the structure of the multi-nuclear metal cluster compound is specially from the inside to the outside：
First layer includes 8 Ni ions, Ni ions described in μ 3-OH bridgings；
The second layer includes 20 Tb ions, wherein 8 Tb ions form cubical vertex, it is every that remaining Tb ion is located at cube
20 Tb ions are linked to be cubical 12 sides by the midpoint on side, μ 3-OH, and by the Tb ions in the second layer and first layer
Ni ions connect；
Third layer includes 32 Tb ions, wherein have 3 μ 3-OH groups on the Tb ions in cube each edge, one
To Tb ions adjacent in the bridging second layer, the Ni ions that the 4th layer of another pair bridging；
4th layer includes 48 Ni ions, cube of this layer of structure for no vertex, and each vertex is three of rounded projections arranged
Ni, the Ni ions positioned at cube apex are complexed by the N in ida ligands and O atom, meanwhile, O atom and two independences of third layer
Tb ion complexations；The another two O atom of the ida carboxyls and adjacent Ni ion coordinations；
Wherein, the Ni ions are hexa-coordinate environment, to deform octoploids structure；
There are two types of coordination modes for the Tb ions, and the Tb ions of the second layer are seven coordination modes, to add hat triangular prism geometry structure
Type；Equal nine coordination mode of Tb ions of third layer forms three cap trigone column configurations；
It is highly preferred that the spacing of adjacent metal ion
4. the preparation method of any multi-nuclear metal cluster compound of claims 1 to 3, which is characterized in that by Tb (NO3)3·
6H2O、Ni(NO3)2·6H2O and iminodiacetic acid are soluble in water, adjust pH value to 3.5~4.5, obtain mixture；By described in
Mixture is at the uniform velocity warming up to 175~185 DEG C in 10~20h, after maintaining 35~70h of the temperature, 6~for 24 hours after, at the uniform velocity drop
Warm to room temperature to get.
5. preparation method according to claim 4, which is characterized in that the Tb (NO3)3·6H2The O and Ni (NO3)2·
6H2The molar ratio of O is：1.4~1.9:1, preferably 1.65~1.72:1.
6. preparation method according to claim 4 or 5, which is characterized in that the Ni (NO3)2·6H2O and the imino group
The molar ratio of oxalic acid is 1:1.6~2.4, preferably 1:1.9~2.1.
7. according to any preparation method of claim 4~6, which is characterized in that molten 0.2 in water described in per 1mL~
Tb (the NO of 0.25mol3)3·6H2O。
8. according to any preparation method of claim 4~7, which is characterized in that even by the mixture in 14~16h
Speed is warming up to 155~165 DEG C, then in 4.5~5.5h, continuation be at the uniform velocity warming up to 175~185 DEG C, maintain the temperature 36~
After 38h, be at the uniform velocity cooled in 14~16h room temperature to get；
Preferably, by the mixture in 15h, 160 DEG C are at the uniform velocity warming up to, then in 5h, continuation is at the uniform velocity warming up to 180
DEG C, after maintaining temperature 37h, be at the uniform velocity cooled in 15h room temperature to get.
9. preparation method according to claim 4, which is characterized in that by Tb (NO3)3·6H2O、Ni(NO3)2·6H2O and
Iminodiacetic acid is soluble in water, adjusts pH value to 3.5~4.5, obtains mixture；It is even by the mixture in 8~12h
Speed is warming up to 175~185 DEG C, and after maintaining 45~55h of the temperature, room temperature is at the uniform velocity cooled in 6~12h, filters, dry, i.e.,
；
Wherein, the Tb (NO3)3·6H2The O and Ni (NO3)2·6H2The molar ratio of O is 1.65~1.72:1；The Ni
(NO3)2·6H2O is 1 in molar ratio with the iminodiacetic acid:1.9~2.1；Molten 0.2~0.25mol in water described in per 1mL
The Tb (NO3)3·6H2O。
10. any multi-nuclear metal cluster compound of claims 1 to 3 or any preparation method of claim 4~9 are made
Application of the multi-nuclear metal cluster compound obtained in molecular magnetic materials, more metal multi-iron materials and molecular memory Material Field；
Preferably, the multi-nuclear metal cluster compound answering in low-temperature nano temperature control magnetic switch, nano-magnetic controller field
With.
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