CN111471187A - One-dimensional chain Gd-quinoline nitroxide free radical coordination polymer and preparation method thereof - Google Patents
One-dimensional chain Gd-quinoline nitroxide free radical coordination polymer and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a one-dimensional chain Gd-quinoline nitrogen oxygen free radical coordination polymer and a preparation method thereof, relating to the technical field of molecular magnetic material preparation. The method utilizes reaction of gadolinium hexafluoroacetylacetonate and quinoline-substituted nitroxide radical, adjusts the acidity and alkalinity of solution through copper salt of hexafluoroacetylacetonate, and adopts a mode of slowly volatilizing solvent at room temperature to prepare one-dimensional chain Gd-quinoline nitroxide radical complex [ Gd (hfac)3(8‑QNNIT)]nAnd analyzing the complex structure of gadolinium by single crystal X-ray diffraction. Studies of dc magnetic susceptibility show that by gadolinium ions in the system, antiferromagnetic coupling between two radicals dominates. The invention has the advantages that: through the research on the structure and magnetism of one-dimensional Gd-quinoline nitroxide free radical complex, the complex shows antiferromagnetic propertyThe interaction is helpful for understanding the relationship between the structure and the magnetism of the rare earth-free radical complex.
Description
Technical Field
The invention relates to the technical field of molecular magnetic material preparation, in particular to a one-dimensional chain Gd-quinoline nitroxide free radical coordination polymer and a preparation method thereof.
Background
In recent years, molecular-based magnetic materials have received a high degree of attention from researchers in the fields of physics, chemistry, and material science. However, how to improve the performance of magnetic materials and understand the magnetic structure relationship remains a challenging issue in this field. The rare earth gadolinium ion is an isotropic metal ion and has larger ground state spin; the complex is often used for researching the correlation between the structure and the magnetic property. In terms of the selection of organic ligands, nitroxide radicals (nitroxide radial) are widely used in the construction of molecular-based magnetic materials. Nitroxide free radical (nitroxyl nitrate radial) as a bridging ligand, which is stable at room temperature and can be chemically modified by changing the substituent group; when coordinated with rare earth gadolinium ions, it is capable of generating diverse magnetic transfer pathways and efficiently transferring magnetic coupling between spin carriers. This will help to understand the structural and magnetic properties of the nitroxide-gadolinium complex.
Although researchers have reported a large number of rare earth-based molecular magnetic materials, they still have insufficient knowledge on the correlation between the magnetic properties and the structure of gadolinium complexes, the substitution groups of organic ligands, the uncoordinated groups of metal ion co-ligands (β -diketone ligands), the types of metal ions, and the complex spin topology can affect the magnetic transfer pathways in complexes, and the geometrical configuration of rare earth ions and the symmetry of local ligand fields also have an important role in important magnetic properties such as intramolecular and intermolecular interactions of gadolinium complexes.
Disclosure of Invention
The invention provides a one-dimensional chain Gd-quinoline nitrogen oxygen free radical coordination polymer and a preparation method thereof, aiming at solving the problem of preparing a magnetic material by using a gadolinium complex.
The invention is realized by the following technical scheme: the one-dimensional chain Gd-quinoline nitrogen oxygen free radical coordination polymer has a chemical formula of [ Gd (hfac) ]3(8-QNNIT)]nWherein 8-QNNIT represents an 8-quinoline-substituted nitroxide radical, hfac represents hexafluoroacetylacetone, and n represents [ Gd (hfac) ]3(8-QNNIT)]Repeating the arrangement for the elements, and n is at the value103-104Within the range; metal Gd3+The ions adopt an eight-coordinate trigonoedodecahedral geometryD 2dCoordinated to two oxygen atoms of two 8-QNNIT radicals and to the oxygen atoms of three chelating hexafluoroacetylacetonates; in the polymer, 8-QNNIT radical binds to different Gd as bidentate bridging ligand3+Ions, and then form [ rad-Gd ]]A one-dimensional chain structure of repeated arrangement.
A preparation method of a one-dimensional chain Gd-quinoline nitrogen oxygen free radical coordination polymer selects 8-QNNIT as an organic ligand, hexafluoroacetylacetone salt of gadolinium as a rare earth salt, the acid-base property of the solution is adjusted by copper salt of hexafluoroacetylacetone, a reaction solvent is a mixed solvent of n-heptane and dichloromethane, and the specific steps are as follows:
(1) preparation of quinoline-substituted nitroxide radical 8-QNNIT, gadolinium hexafluoroacetylacetonato salt hydrate Gd (hfac) by adopting free radical synthesis method and beta-diketone metal salt synthesis method3×2H2Hexafluoroacetylacetonato hydrate of O and copper Cu (hfac)2×2H2O；
(2) Gd (hfac) is added into the experimental container in a molar ratio of 2:13×2H2O and Cu (hfac)2×2H2Mixed metal salt of O, wherein Cu (hfac)2×2H2O is an acid-base regulator; then adding an n-heptane solvent into the mixed metal salt, stirring, heating and refluxing for 5 hours at the temperature of 100-110 ℃; then, adding dichloromethane solution dissolved with nitroxide free radical 8-QNNIT, continuously heating and reacting for 25 minutes to obtain pink solution, then cooling the solution to room temperature, and filtering the obtained pink solution at normal temperature after a large amount of needle crystals are separated out;
(3) filtering the solution into another container, sealing the container with a preservative film, standing, gradually volatilizing the solvent at room temperature, and obtaining a pink product which is the one-dimensional chain Gd-quinoline nitrogen-oxygen free radical coordination polymer after three days. Because the preservative film also has certain air permeability, the preservative film sealing can also volatilize the solvent, and only the volatilization is slow, so that the experimental requirements are just met.
Preferably, if the solvent evaporation speed is slightly increased, in the step (3), a plurality of holes with large needle tips can be punched on the preservative film.
Compared with the prior art, the invention has the following beneficial effects: the one-dimensional chain Gd-quinoline nitroxide free radical coordination polymer and the preparation method thereof provided by the invention assemble one example of the one-dimensional chain Gd-quinoline nitroxide free radical coordination polymer with larger chain spacing by a simple chemical synthesis mode. Magnetic studies also show that the complexes exhibit antiferromagnetic interactions. The research on the magnetic material is helpful for understanding the relationship between the structure and magnetism of the rare earth-radical complex.
Drawings
FIG. 1 is a one-dimensional chain structure diagram of Gd-rad complex.
FIGS. 2 and 3 are two independent Gd3+SHAPE analysis of the ions.
FIG. 4 is a spatial stacking diagram of Gd-rad one dimensional complexes.
FIGS. 5 and 6 are DC test charts of one-dimensional complexes: wherein, FIG. 5 is a temperature-changing direct-current magnetic susceptibility (cT-T) detection diagram of the complex; FIG. 6 is a diagram showing isothermal variable field magnetization (M-H) test of the complex.
Detailed Description
The present invention is further illustrated by the following specific examples.
The one-dimensional chain Gd-quinoline nitrogen oxygen free radical coordination polymer has a chemical formula of [ Gd (hfac) ]3(8-QNNIT)]nWherein 8-QNNIT represents an 8-quinoline-substituted nitroxide radical, hfac represents hexafluoroacetylacetone, and n represents [ Gd (hfac) ]3(8-QNNIT)]Repeating the arrangement for the elements, and n is 103-104Within the range; metal Gd3+The ions adopt an eight-coordinate trigonoedodecahedral geometryD 2dCoordinated to two oxygen atoms of two 8-QNNIT radicals and to the oxygen atoms of three chelating hexafluoroacetylacetonates; in the polymer, 8-QNNIT radical binds to different Gd as bidentate bridging ligand3+Ions, and then form [ rad-Gd ]]One-dimensional chain of repeated arrangementAnd (5) structure.
A preparation method of a one-dimensional chain Gd-quinoline nitrogen oxygen free radical coordination polymer selects 8-QNNIT as an organic ligand, hexafluoroacetylacetone salt of gadolinium as a rare earth salt, the acid-base property of the solution is adjusted by copper salt of hexafluoroacetylacetone, a reaction solvent is a mixed solvent of n-heptane and dichloromethane, and the specific steps are as follows:
(1) synthesis of nitroxide radical 8-QNNIT:
under ice bath conditions, 1.48g (10mmol) of a mixed solution of ethanol and water of 2, 3-dimethyl-2, 3-dihydroxyaminobutane (25 ml, volume ratio 1: 1) was added to a 50ml round-bottom flask, then 5ml of an ethanol solvent in which 1.57g (10mmol) of 8-quinolinecarboxaldehyde was dissolved was slowly added, and stirred in ice bath for 72 hours to obtain a yellow turbid liquid, which was filtered with suction to obtain a pale yellow precipitate. Adding the light yellow precipitate into 75ml of dichloromethane solution, and stirring for 3 minutes under the ice bath condition; subsequently, 5ml of an aqueous solution containing 2g of sodium periodate was slowly added dropwise thereto with a rubber-tipped dropper, and stirred rapidly for 10 minutes, after which the solvent was removed by liquid separation, washing, drying, and reduced pressure, purple powder of 8-QNNIT nitroxide was obtained with a yield of 52%.
（2）[Gd(hfac)3(8-QNNIT)]nThe synthesis of (2):
into a 50ml round bottom flask, 0.0081g of Gd (hfac)3×2H2O and 0.0049g of Cu (hfac)2×2H2Adding 15ml of dry n-heptane solvent into the O solid mixture, and stirring, heating and refluxing the solution for 5 hours at 105 ℃; subsequently, 4ml of a dichloromethane solution containing 0.0037g of nitroxide radical 8-QNNIT was added, heating was continued for 25 minutes, the solution was cooled to room temperature, and after a large amount of needle crystals were precipitated, filtration was performed at room temperature.
(3) Filtering the solution into a small beaker of 25ml, sealing the beaker by using a preservative film, (if the volatilization speed is increased, a small hole with a large needle point can be pricked on the preservative film), standing, slowly volatilizing the solvent at room temperature, and obtaining pink blocky crystals after three days, wherein the yield is 30%.
Wherein Gd (hfac)3×2H2O、Cu(hfac)2×2H2Substances of O and 8-QNNITThe ratio of the amounts of (A) to (B) is 1:0.5: 1; the hexafluoroacetylacetonato hydrate of copper (Cu (hfac)2×2H2O) is used for adjusting the pH value of the solution.
Single crystal structure test and structure description of one-dimensional chain Gd-quinoline nitrogen oxygen free radical coordination polymer:
pick the pink patches 0.21X 0.19X 0.18 mm3The crystal of (1) is obtained by using Rigaku Saturn type CCD X-ray single crystal diffractometer, Mo-Ka ray (l = 0.71073 Å) monochromized by graphite, collecting 84130 pink single crystal diffraction points by using an omega-phi scanning mode at low temperature of 150K, calculating by using programs of SHE L XS-2014 and SHE L X L-2014, and carrying out appropriate correction on disordered atoms by using commands of ISOR, SIMU, DE L U and the like3(8-QNNIT)]nThe crystal structure belongs to a monoclinic system, and the space group isP21/cThe unit cell parameter isa= 22.871(5) Å，b= 16.724(3) Å，c= 22.870(5) Å，a=g= 90°，ßUnit cell volume of = 117.06(3) °V= 7790(3) Å3，ZAnd = 4. Crystallographic data of single crystal X-ray diffraction of the complex are shown in Table 1; a single crystal structure, as shown in fig. 1 to 4, wherein fig. 1 is a one-dimensional chain structure diagram of Gd-rad complex; FIGS. 2 and 3 are two independent Gd3+SHAPE analysis of the ions; FIG. 4 is a spatial stacking diagram of the one-dimensional Gd-rad complex. In this complex, the center Gd3+The ions adopt an eight-coordinate trigonoedodecahedral geometryD 2dCoordinated to two oxygen atoms of two 8-QNNIT radicals and to the oxygen atoms of three chelating hexafluoroacetylacetonates; 8-QNNIT radical as bidentate bridging ligand binding to different Gd3+Ions, and then form [ rad-Gd ]]A one-dimensional chain structure of repeated arrangement.
TABLE 1 crystallographic data for one-dimensional Gd-rad complexes
The magnetic test of the one-dimensional chain Gd-quinoline nitrogen oxygen free radical coordination polymer comprises the following steps:
magnetic measurement is carried out by adopting Quantum Design SQUID MPMS-7, and Pascal's constant is used for diamagnetic correction of magnetic data of the one-dimensional chain Gd-quinoline nitroxide free radical complex. During measurement, a pink monocrystal sample is ground into powder, 15mg of the powder is weighed and filled into a U-shaped test capsule, and a Quantum Design SQUID MPMS-7 device is used for measuring the direct current magnetic susceptibility.
FIGS. 5 and 6 are DC test plots of one-dimensional Gd-rad complexes. Wherein, FIG. 5 shows the variable temperature direct current magnetic susceptibility of Gd-rad complex: (cT-T) Detecting the map; at the time of the room temperature, the temperature of the mixture,χ M Thas a value of 8.036 cm3Kmol–1Slightly lower than the uncoupled one GdIIISum of spins alone of ion and one radical of 8.255 cm3Kmol–1. As the temperature is lowered, the temperature of the reaction solution is lowered,χ M Tgradually decreases to 1.225 cm at 2K3Kmol–1. This phenomenon illustrates that by gadolinium ions, the antiferromagnetic coupling between two radicals dominates. FIG. 6 shows isothermal varying field magnetization of Gd-rad complex: (M-H) And (6) testing the graph. The test results show that the value of the magnetization with increasing field strength (M) And also rapidly increases. At a field strength of 70 kOe, of the complexMThe value reached 8.76N β, but was slightly below the theoretical saturation magnetization value of 7.53N β, indicating that antiferromagnetic coupling was present in the one-dimensional complex.
The scope of the invention is not limited to the above embodiments, and various modifications and changes may be made by those skilled in the art, and any modifications, improvements and equivalents within the spirit and principle of the invention should be included in the scope of the invention.
Claims (5)
1. The one-dimensional chain Gd-quinoline nitrogen oxygen free radical coordination polymer is characterized in that: the chemical formula of the polymer is [ Gd (hfac) ]3(8-QNNIT)]nWherein 8-QNNIT represents an 8-quinoline-substituted nitroxide radical, hfac represents hexafluoroacetylacetone, and n represents [ Gd (hfac) ]3(8-QNNIT)]Is a baseThe elements are arranged repeatedly, and n is 103-104Within the range; metal Gd3+The ions adopt an eight-coordinate trigonoedodecahedral geometryD 2dCoordinated to two oxygen atoms of two 8-QNNIT radicals and to the oxygen atoms of three chelating hexafluoroacetylacetonates; in the polymer, 8-QNNIT radical binds to different Gd as bidentate bridging ligand3+Ions, and then form [ rad-Gd ]]A one-dimensional chain structure of repeated arrangement.
2. The preparation method of the one-dimensional chain Gd-quinoline nitrogen oxygen free radical coordination polymer is characterized in that: selecting 8-QNNIT as an organic ligand, taking hexafluoroacetylacetone salt of gadolinium as a rare earth salt, adjusting the acid-base property of the solution through copper salt of hexafluoroacetylacetone, and using a reaction solvent as a mixed solvent of n-heptane and dichloromethane, wherein the specific steps are as follows:
(1) preparation of quinoline-substituted nitroxide radical 8-QNNIT, gadolinium hexafluoroacetylacetonato salt hydrate Gd (hfac) by adopting free radical synthesis method and beta-diketone metal salt synthesis method3×2H2Hexafluoroacetylacetonato hydrate of O and copper Cu (hfac)2×2H2O；
(2) Gd (hfac) is added into the experimental container in a molar ratio of 2:13×2H2O and Cu (hfac)2×2H2Mixed metal salt of O, wherein Cu (hfac)2×2H2O is an acid-base regulator; then adding an n-heptane solvent into the mixed metal salt, stirring, heating and refluxing for 5 hours at the temperature of 100-110 ℃; then, adding dichloromethane solution dissolved with nitroxide free radical 8-QNNIT, continuously heating and reacting for 25 minutes to obtain pink solution, then cooling the solution to room temperature, and filtering the obtained pink solution at normal temperature after a large amount of needle crystals are separated out;
(3) filtering the solution into another container, sealing the container with a preservative film, standing, gradually volatilizing the solvent at room temperature, and obtaining a pink product which is the one-dimensional chain Gd-quinoline nitrogen-oxygen free radical coordination polymer after three days.
3. According toThe method for preparing a one-dimensional chain Gd-quinoline nitroxide radical coordination polymer according to claim 2, characterized in that: in the step (2), gadolinium hexafluoroacetylacetonate hydrate Gd (hfac)3×2H2The mass of O was 0.0081g, the mass of nitroxide radical 8-QNNIT was 0.0037g, the volume of n-heptane solvent was 15ml, and the volume of dichloromethane solvent was 4 ml.
4. The method for preparing a one-dimensional chain-like Gd-quinoline nitroxide radical coordination polymer according to claim 2, characterized in that: said Gd (hfac)3×2H2O、Cu(hfac)2×2H2The ratio of the amounts of O and 8-QNNIT is 1:0.5: 1.
5. The method for preparing a one-dimensional chain-like Gd-quinoline nitroxide radical coordination polymer according to claim 2, characterized in that: in the step (3), a plurality of holes with large needle tips can be punched on the preservative film.
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| CN102360674A (en) * | 2011-09-09 | 2012-02-22 | 南开大学 | Metal-radical one-dimensional coordination polymer magnetic material as well as preparation method and application thereof |
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| CN108358954A (en) * | 2018-01-17 | 2018-08-03 | 南开大学 | A kind of chirality rare earth-NO free radical single-chain magnets and preparation method thereof |
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| CN102360674A (en) * | 2011-09-09 | 2012-02-22 | 南开大学 | Metal-radical one-dimensional coordination polymer magnetic material as well as preparation method and application thereof |
| CN104402915A (en) * | 2014-10-31 | 2015-03-11 | 天津工业大学 | Tm(III)-nitroxide radical complex and preparation method thereof |
| CN108358954A (en) * | 2018-01-17 | 2018-08-03 | 南开大学 | A kind of chirality rare earth-NO free radical single-chain magnets and preparation method thereof |
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