CN104036910A - Magnetic material HN(C2H5)3 [Co4Na3(heb)6(N3)6] and synthetic method - Google Patents
Magnetic material HN(C2H5)3 [Co4Na3(heb)6(N3)6] and synthetic method Download PDFInfo
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- CN104036910A CN104036910A CN201410292855.6A CN201410292855A CN104036910A CN 104036910 A CN104036910 A CN 104036910A CN 201410292855 A CN201410292855 A CN 201410292855A CN 104036910 A CN104036910 A CN 104036910A
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- heb
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- analytically pure
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- 239000000696 magnetic material Substances 0.000 title claims abstract description 13
- 238000010189 synthetic method Methods 0.000 title claims abstract description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 30
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 15
- 230000005291 magnetic effect Effects 0.000 claims abstract description 15
- PXIPVTKHYLBLMZ-UHFFFAOYSA-N Sodium azide Chemical compound [Na+].[N-]=[N+]=[N-] PXIPVTKHYLBLMZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000005294 ferromagnetic effect Effects 0.000 claims abstract description 7
- 229910001429 cobalt ion Inorganic materials 0.000 claims abstract description 6
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 239000013078 crystal Substances 0.000 claims description 8
- 230000005307 ferromagnetism Effects 0.000 claims description 5
- 235000013495 cobalt Nutrition 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- AIUIJBDEQKTMHT-UHFFFAOYSA-N perchloric acid;hydrate Chemical compound O.OCl(=O)(=O)=O AIUIJBDEQKTMHT-UHFFFAOYSA-N 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 230000005343 Curie-Weiss law Effects 0.000 claims description 3
- 238000000547 structure data Methods 0.000 claims description 3
- 230000005389 magnetism Effects 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- OFQBYHLLIJGMNP-UHFFFAOYSA-N 3-ethoxy-2-hydroxybenzaldehyde Chemical compound CCOC1=CC=CC(C=O)=C1O OFQBYHLLIJGMNP-UHFFFAOYSA-N 0.000 abstract 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract 1
- KPOBHNYTWJSVKF-UHFFFAOYSA-L cobalt(2+);diperchlorate;hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O KPOBHNYTWJSVKF-UHFFFAOYSA-L 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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- Hard Magnetic Materials (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a magnetic material HN(C2H5)3 [Co4Na3(heb)6(N3)6] and a synthetic method. The molecular formula of the magnetic material HN(C2H5)3 [Co4Na3(heb)6(N3)6] is C60H71N19Na3Co4O18, and the molecular weight is 1651.05. The synthetic method includes: dissolving 0.166g of analytically pure 3-ethoxy-2-hydroxy benzaldehyde into a mixed solution of 4-8ml of analytically pure methanol and 4-8ml of analytically pure acetonitrile, then sequentially adding 0.36-0.72g of analytically pure cobalt perchlorate hexahydrate and 0.065-0.13g of analytically pure sodium azide, stirring for 10 minutes prior to adding analytically pure triethylamine to regulate pH (potential of hydrogen) to 5.5, stirring for 20 minutes prior to standing at room temperature, filtering, and washing with the analytically pure methanol. Magnetic properties of the HN(C2H5)3 [Co4Na3(heb)6(N3)6] are shown in that ferromagnetic exchange exist among intramolecular cobalt ions, and the HN(C2H5)3 [Co4Na3(heb)6(N3)6] is integrally ferromagnetic. The magnetic material HN(C2H5)3 [Co4Na3(heb)6(N3)6] and the synthetic method have the advantages of simple technology, low cost, easiness in control of chemical compositions, good repeatability, high productivity and the like.
Description
Technical field
The present invention relates to a kind of magnetic material HN (C
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] (Hheb is 3-ethyoxyl-Benzaldehyde,2-hydroxy) and synthetic method.
Background technology
Modem magnetic materials has been used among our life widely, for example, permanent magnetic material is used as to motor, is applied to the core material in transformer, the magneto optical disk using as memory, computer magnetic recording floppy disk etc.Can say, magnetic material is closely related with the every aspect of informationization, automation, electromechanical integration, national defence, national economy.For having coordination compound magnetic material, explore the mechanism of its magnetic generation and set up the foundation that rational theoretical model is its fast development.From MOLECULE DESIGN, start with, rationally cutting molecular structure, both can economy develop magnetic high-molecular quickly, can carry out modified with functional group to it again and change its magnetic.Along with people's going deep into magnetic theory and macromolecule research, the organic polymer magnetic material more with practical value will be synthesized, and the application of these organic polymer magnetic materials will cause a series of great technological innovations in fields such as space flight, aviation, military project, information, superconductions.
Summary of the invention
Object of the present invention is exactly for designing the functional material of synthetic magnetic property excellence, utilizing normal temperature solwution method synthetic technology to synthesize HN (C
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] (Hheb is 3-ethyoxyl-Benzaldehyde,2-hydroxy).
HN (the C the present invention relates to
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] molecular formula of (Hheb is 3-ethyoxyl-Benzaldehyde,2-hydroxy) is: C
60h
71n
19na
3co
4o
18, molecular weight is: 1651.05.Crystal structure data are in Table one, and bond distance's bond angle data are in Table two.
Table one HN (C
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] (CH
3oH) crystallographic parameter
Table two HN (C
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] (CH
3oH) bond distance
and bond angle (°)
| C1-O1 | 1.286(7) | C46-C47 | 1.412(8) | C36-H36 | 0.9300 |
| C1-C2 | 1.410(9) | C46-C51 | 1.424(8) | C37-O13 | 1.293(7) |
| C1-C6 | 1.417(9) | C47-C54 | 1.427(9) | C37-C38 | 1.404(8) |
| C2-C3 | 1.401(10) | C47-C48 | 1.431(9) | C37-C42 | 1.437(8) |
| C2-C9 | 1.431(10) | C48-C49 | 1.351(10) | C38-C45 | 1.414(9) |
| C3-C4 | 1.349(12) | C48-H48 | 0.9300 | C38-C39 | 1.416(9) |
| C3-H3 | 0.9300 | C49-C50 | 1.370(10) | C39-C40 | 1.353(11) |
| C4-C5 | 1.399(11) | C49-H49 | 0.9300 | C39-H39 | 0.9300 |
| C4-H4 | 0.9300 | C50-C51 | 1.388(8) | C40-C41 | 1.375(10) |
| C5-C6 | 1.363(9) | C50-H50 | 0.9300 | C40-H40 | 0.9300 |
| C5-H5 | 0.9300 | C51-O18 | 1.363(7) | Na2-O12 | 2.454(5) |
| C6-O3 | 1.387(7) | C52-O18 | 1.427(7) | C30-C31 | 1.373(11) |
| C7-O3 | 1.445(8) | C52-C53 | 1.490(10) | C57-H57B | 0.9700 |
| C7-C8 | 1.462(11) | C52-H52A | 0.9700 | C14-C15 | 1.376(10) |
| C7-H7A | 0.9700 | C52-H52B | 0.9700 | Na3-O7 | 2.247(4) |
| C7-H7B | 0.9700 | C53-H53A | 0.9600 | Na3-O4 | 2.266(4) |
| C8-H8A | 0.9600 | C53-H53B | 0.9600 | Na3-O9 | 2.390(5) |
| C8-H8B | 0.9600 | C53-H53C | 0.9600 | Na3-O6 | 2.458(6) |
| C8-H8C | 0.9600 | C54-O17 | 1.231(8) | C45-H45 | 0.9300 |
| C9-O2 | 1.222(9) | C54-H54 | 0.9300 | C46-O16 | 1.285(6) |
| C9-H9 | 0.9300 | C55-C56 | 1.40(2) | C41-C42 | 1.371(9) |
| C10-O4 | 1.291(7) | C55-H55A | 0.9600 | C41-H41 | 0.9300 |
| C10-C11 | 1.408(9) | C55-H55B | 0.9600 | C42-O15 | 1.381(7) |
| C10-C15 | 1.417(9) | C55-H55C | 0.9600 | C43-O15 | 1.424(7) |
| C11-C18 | 1.429(11) | C56-N19 | 1.446(18) | C43-C44 | 1.497(10) |
| C11-C12 | 1.438(11) | C56-H56A | 0.9700 | C43-H43A | 0.9700 |
| C12-C13 | 1.328(13) | C56-H56B | 0.9700 | C43-H43B | 0.9700 |
| C12-H12 | 0.9300 | C57-N19 | 1.489(10) | C44-H44A | 0.9600 |
| C13-C14 | 1.391(13) | C57-C58 | 1.563(10) | C44-H44B | 0.9600 |
| C13-H13 | 0.9300 | C57-H57A | 0.9700 | C44-H44C | 0.9600 |
| C14-H14 | 0.9300 | C58-H58A | 0.9600 | Co2-O1 | 2.025(4) |
| C15-O6 | 1.345(8) | C58-H58B | 0.9600 | Co2-O4 | 2.043(4) |
| C16-C17 | 1.352(14) | C58-H58C | 0.9600 | Co2-O2 | 2.097(4) |
| C16-O6 | 1.448(11) | C59-C60 | 1.367(17) | Co2-O5 | 2.106(5) |
| C16-H16A | 0.9700 | C59-N19 | 1.410(16) | Co3-O13 | 2.021(4) |
| C16-H16B | 0.9700 | C59-H59A | 0.9700 | Co3-O16 | 2.025(4) |
| C17-H17A | 0.9600 | C59-H59B | 0.9700 | Co3-O14 | 2.078(4) |
| C17-H17B | 0.9600 | C60-H60A | 0.9600 | Co3-O17 | 2.114(4) |
| C17-H17C | 0.9600 | C60-H60B | 0.9600 | Co4-O10 | 2.029(4) |
| C18-O5 | 1.209(9) | C60-H60C | 0.9600 | C45-O14 | 1.242(8) |
| C18-H18 | 0.9300 | N1-N2 | 1.179(7) | Co4-O7 | 2.040(4) |
| C19-O7 | 1.281(7) | N1-Co2 | 2.143(4) | Co4-O11 | 2.081(4) |
| C19-C20 | 1.412(9) | N1-Co1 | 2.158(4) | Co4-O8 | 2.099(4) |
| C19-C24 | 1.424(9) | N1-Na3 | 2.548(5) | Na2-O13 | 2.260(4) |
| C30-H30 | 0.9300 | N2-N3 | 1.143(8) | Na2-O10 | 2.275(4) |
| C20-C21 | 1.413(9) | C32-C33 | 1.350(9) | Na2-O15 | 2.427(5) |
| C20-C27 | 1.412(10) | N4-N5 | 1.170(6) | C31-C32 | 1.386(11) |
| C21-C22 | 1.347(12) | N4-Co1 | 2.165(4) | N16-N17 | 1.196(6) |
| C21-H21 | 0.9300 | N4-Co3 | 2.186(4) | N16-Co3 | 2.155(4) |
| C22-C23 | 1.375(12) | N4-Na1 | 2.524(4) | N16-Co1 | 2.178(4) |
| C22-H22 | 0.9300 | N5-N6 | 1.144(8) | N16-Na2 | 2.525(4) |
| C23-C24 | 1.389(9) | C36-O11 | 1.233(8) | N17-N18 | 1.132(7) |
| C23-H23 | 0.9300 | N7-N8 | 1.182(6) | N19-H19A | 0.9137 |
| C24-O9 | 1.366(8) | N7-Co4 | 2.158(4) | Na1-O16 | 2.267(4) |
| C25-O9 | 1.431(9) | N7-Co1 | 2.175(4) | Na1-O1 | 2.277(4) |
| C25-C26 | 1.452(12) | N7-Na2 | 2.498(5) | Na1-O18 | 2.402(4) |
| C25-H25A | 0.9700 | N8-N9 | 1.137(8) | Na1-O3 | 2.466(5) |
| C25-H25B | 0.9700 | N10-N11 | 1.195(6) | C32-H32A | 0.9700 |
| C26-H26A | 0.9600 | N10-Co2 | 2.145(4) | C32-H32B | 0.9700 |
| C26-H26B | 0.9600 | N10-Co1 | 2.166(4) | C33-O12 | 1.390(7) |
| C26-H26C | 0.9600 | N10-Na1 | 2.539(5) | C34-O12 | 1.424(7) |
| C27-O8 | 1.249(8) | N11-N12 | 1.141(7) | C34-C35 | 1.506(11) |
| C27-H27 | 0.9300 | N13-N14 | 1.180(6) | C34-H34A | 0.9700 |
| C28-O10 | 1.294(7) | N13-Co1 | 2.142(4) | C34-H34B | 0.9700 |
| C28-C29 | 1.419(8) | N13-Co4 | 2.175(4) | C35-H35A | 0.9600 |
| C28-C33 | 1.422(8) | N13-Na3 | 2.540(5) | C35-H35B | 0.9600 |
| C29-C30 | 1.420(9) | N14-N15 | 1.141(7) | C35-H35C | 0.9600 |
| C29-C36 | 1.421(9) | C31-H31 | 0.9300 | ? | ? |
| O1-C1-C2 | 123.7(6) | O18-Na1-N4 | 140.59(16) | H60A-C60-H60C | 109.5 |
| O1-C1-C6 | 120.4(5) | O3-Na1-N4 | 99.41(16) | H60B-C60-H60C | 109.5 |
| C2-C1-C6 | 115.9(6) | O16-Na1-N10 | 91.88(15) | N2-N1-Co2 | 123.6(4) |
| C3-C2-C1 | 120.9(7) | O1-Na1-N10 | 74.29(15) | N2-N1-Co1 | 131.2(4) |
| C3-C2-C9 | 117.1(7) | O18-Na1-N10 | 97.31(16) | Co2-N1-Co1 | 99.27(17) |
| C1-C2-C9 | 122.0(7) | O3-Na1-N10 | 140.54(16) | N2-N1-Na3 | 102.7(4) |
| C4-C3-C2 | 121.3(8) | N4-Na1-N10 | 75.03(14) | Co2-N1-Na3 | 92.05(17) |
| C4-C3-H3 | 119.3 | O14-C45-C38 | 128.8(6) | Co1-N1-Na3 | 97.26(17) |
| C2-C3-H3 | 119.3 | O18-C52-H52B | 109.9 | N3-N2-N1 | 176.3(8) |
| C3-C4-C5 | 119.2(8) | O18-C52-H52A | 109.9 | O10-Co4-N7 | 87.90(15) |
| C3-C4-H4 | 120.4 | C53-C52-H52A | 109.9 | O7-Co4-N7 | 95.59(16) |
| C5-C4-H4 | 120.4 | C40-C39-H39 | 119.5 | O11-Co4-N7 | 169.56(17) |
| C6-C5-C4 | 120.6(8) | C38-C39-H39 | 119.5 | O8-Co4-N7 | 94.85(17) |
| C6-C5-H5 | 119.7 | O10-Co4-O11 | 86.86(16) | O10-Co4-N13 | 94.37(16) |
| C4-C5-H5 | 119.7 | O7-Co4-O11 | 89.88(17) | O7-Co4-N13 | 87.39(15) |
| C5-C6-O3 | 124.7(7) | O10-Co4-O8 | 92.51(17) | O11-Co4-N13 | 90.71(17) |
| C5-C6-C1 | 122.0(7) | O7-Co4-O8 | 86.02(16) | O8-Co4-N13 | 171.65(18) |
| O3-C6-C1 | 113.3(6) | O11-Co4-O8 | 94.39(18) | N7-Co4-N13 | 80.70(15) |
| O3-C7-C8 | 108.8(7) | N19-C59-H59B | 105.8 | O10-Co4-O7 | 176.31(15) |
| O3-C7-H7A | 109.9 | H59A-C59-H59B | 106.2 | O15-C43-H43A | 110.2 |
| C8-C7-H7A | 109.9 | C59-C60-H60A | 109.5 | C43-C44-H44A | 109.5 |
| O3-C7-H7B | 109.9 | C59-C60-H60B | 109.5 | N5-N4-Co1 | 130.6(4) |
| C8-C7-H7B | 109.9 | H60A-C60-H60B | 109.5 | N5-N4-Co3 | 123.0(4) |
| H7A-C7-H7B | 108.3 | C57-C58-H58A | 109.5 | Co1-N4-Co3 | 98.60(16) |
| C7-C8-H8A | 109.5 | C57-C58-H58B | 109.5 | N5-N4-Na1 | 105.0(4) |
| C7-C8-H8B | 109.5 | H58A-C58-H58B | 109.5 | Co1-N4-Na1 | 97.33(16) |
| H8A-C8-H8B | 109.5 | C57-C58-H58C | 109.5 | Co3-N4-Na1 | 93.07(14) |
| C7-C8-H8C | 109.5 | H58A-C58-H58C | 109.5 | N6-N5-N4 | 176.3(7) |
| H8A-C8-H8C | 109.5 | H58B-C58-H58C | 109.5 | O15-C42-C37 | 113.4(5) |
| H8B-C8-H8C | 109.5 | C60-C59-N19 | 125.9(16) | O14-Co3-O17 | 92.12(18) |
| O2-C9-C2 | 130.6(7) | C60-C59-H59A | 105.8 | O13-Co3-N16 | 87.04(15) |
| O2-C9-H9 | 114.7 | N19-C59-H59A | 105.8 | O16-Co3-N16 | 94.39(16) |
| C2-C9-H9 | 114.7 | C60-C59-H59B | 105.8 | O14-Co3-N16 | 171.28(16) |
| O4-C10-C11 | 123.1(6) | C58-C57-H57A | 107.1 | O17-Co3-N16 | 94.70(17) |
| O4-C10-C15 | 118.5(6) | N19-C57-H57B | 107.1 | O13-Co3-N4 | 93.79(16) |
| C11-C10-C15 | 118.4(6) | C58-C57-H57B | 107.1 | O16-Co3-N4 | 86.80(15) |
| C10-C11-C18 | 122.5(7) | H57A-C57-H57B | 106.8 | O14-Co3-N4 | 92.73(17) |
| C10-C11-C12 | 118.7(8) | O13-Na2-O10 | 165.56(17) | O17-Co3-N4 | 171.80(17) |
| C18-C11-C12 | 118.8(7) | O13-Na2-O15 | 67.32(14) | N16-Co3-N4 | 81.15(15) |
| C13-C12-C11 | 121.7(9) | O10-Na2-O15 | 123.91(16) | O15-C43-C44 | 107.4(6) |
| C13-C12-H12 | 119.2 | O13-Na2-O12 | 120.08(16) | N8-N7-Co4 | 124.7(4) |
| C11-C12-H12 | 119.2 | O10-Na2-O12 | 67.31(14) | N8-N7-Co1 | 126.9(4) |
| C12-C13-C14 | 119.6(9) | O15-Na2-O12 | 108.69(17) | Co4-N7-Co1 | 98.88(17) |
| C12-C13-H13 | 120.2 | O13-Na2-N7 | 94.67(16) | N8-N7-Na2 | 109.1(4) |
| C14-C13-H13 | 120.2 | O10-Na2-N7 | 74.88(15) | Co4-N7-Na2 | 93.25(16) |
| C15-C14-C13 | 121.8(9) | O15-Na2-N7 | 101.38(16) | Co1-N7-Na2 | 95.48(15) |
| C15-C14-H14 | 119.1 | O12-Na2-N7 | 140.52(16) | N9-N8-N7 | 179.1(9) |
| C13-C14-H14 | 119.1 | O13-Na2-N16 | 73.69(15) | N11-N10-Co2 | 122.7(4) |
| O6-C15-C14 | 125.3(8) | O10-Na2-N16 | 94.03(15) | N11-N10-Co1 | 131.2(4) |
| O6-C15-C10 | 114.9(6) | O15-Na2-N16 | 140.80(16) | N10-Co1-N16 | 94.73(16) |
| C14-C15-C10 | 119.8(8) | O12-Na2-N16 | 93.91(15) | N7-Co1-N16 | 92.44(15) |
| C17-C16-O6 | 112.0(10) | N7-Na2-N16 | 77.45(14) | C1-O1-Co2 | 130.6(4) |
| C17-C16-H16A | 109.2 | O16-Co3-O14 | 91.45(16) | C1-O1-Na1 | 122.4(4) |
| O6-C16-H16A | 109.2 | O13-Co3-O17 | 93.05(17) | Co2-O1-Na1 | 104.30(17) |
| C17-C16-H16B | 109.2 | O16-Co3-O17 | 86.47(16) | C9-O2-Co2 | 124.9(5) |
| O6-C16-H16B | 109.2 | O13-Co3-O16 | 178.52(16) | C6-O3-C7 | 116.8(6) |
| H16A-C16-H16B | 107.9 | O13-Co3-O14 | 87.18(15) | C6-O3-Na1 | 115.6(4) |
| C16-C17-H17A | 109.5 | C55-C56-H56B | 108.9 | C7-O3-Na1 | 125.4(4) |
| C16-C17-H17B | 109.5 | N19-C56-H56B | 108.9 | C10-O4-Co2 | 130.6(4) |
| H17A-C17-H17B | 109.5 | H56A-C56-H56B | 107.7 | C10-O4-Na3 | 122.6(4) |
| C16-C17-H17C | 109.5 | N19-C57-C58 | 121.0(11) | Co2-O4-Na3 | 103.52(18) |
| H17A-C17-H17C | 109.5 | N19-C57-H57A | 107.1 | Co2-N10-Co1 | 98.92(17) |
| H17B-C17-H17C | 109.5 | C56-C55-H55C | 109.5 | N11-N10-Na1 | 104.7(4) |
| O5-C18-C11 | 130.0(7) | H55A-C55-H55C | 109.5 | Co2-N10-Na1 | 92.70(16) |
| O5-C18-H18 | 115.0 | H55B-C55-H55C | 109.5 | Co1-N10-Na1 | 96.87(17) |
| C11-C18-H18 | 115.0 | C55-C56-N19 | 113.4(16) | N12-N11-N10 | 177.7(7) |
| O7-C19-C20 | 124.3(6) | C55-C56-H56A | 108.9 | N14-N13-Co1 | 129.9(4) |
| O7-C19-C24 | 118.3(6) | N19-C56-H56A | 108.9 | N14-N13-Co4 | 124.0(4) |
| C20-C19-C24 | 117.4(6) | N13-Co1-N10 | 94.26(16) | Co1-N13-Co4 | 99.36(17) |
| O15-C43-H43B | 110.2 | N1-Co1-N10 | 80.50(17) | N14-N13-Na3 | 103.5(4) |
| C44-C43-H43B | 110.2 | N4-Co1-N10 | 90.76(16) | Co1-N13-Na3 | 97.92(17) |
| H43A-C43-H43B | 108.5 | N13-Co1-N7 | 81.06(16) | Co4-N13-Na3 | 92.41(15) |
| C19-C20-C21 | 120.7(7) | N1-Co1-N7 | 92.73(16) | N15-N14-N13 | 176.0(7) |
| C19-C20-C27 | 122.2(6) | O7-Na3-O4 | 164.91(17) | C18-O5-Co2 | 125.7(5) |
| C21-C20-C27 | 117.2(7) | O7-Na3-O9 | 68.12(16) | C15-O6-C16 | 116.6(7) |
| C22-C21-C20 | 120.5(8) | O4-Na3-O9 | 122.44(18) | C15-O6-Na3 | 115.7(4) |
| C22-C21-H21 | 119.8 | O7-Na3-O6 | 123.4(18) | C16-O6-Na3 | 125.8(5) |
| C20-C21-H21 | 119.8 | O4-Na3-O6 | 66.65(17) | C19-O7-Co4 | 131.1(4) |
| C21-C22-C23 | 120.1(7) | O9-Na3-O6 | 105.18(19) | C19-O7-Na3 | 122.4(4) |
| C21-C22-H22 | 119.9 | O7-Na3-N13 | 74.72(14) | Co4-O7-Na3 | 105.42(16) |
| C23-C22-H22 | 119.9 | O4-Na3-N13 | 93.26(15) | C27-O8-Co4 | 126.1(5) |
| C22-C23-C24 | 122.0(8) | O9-Na3-N13 | 142.51(18) | C24-O9-C25 | 119.4(6) |
| C22-C23-H23 | 119.0 | O6-Na3-N13 | 99.03(18) | C24-O9-Na3 | 116.0(4) |
| C24-C23-H23 | 119.0 | O7-Na3-N1 | 92.58(16) | O14-C45-H45 | 115.6 |
| O9-C24-C23 | 126.3(7) | O4-Na3-N1 | 75.06(16) | C38-C45-H45 | 115.6 |
| O9-C24-C19 | 114.4(5) | O9-Na3-N1 | 102.45(18) | N17-N16-Co3 | 121.6(4) |
| C23-C24-C19 | 119.3(7) | O6-Na3-N1 | 140.69(17) | N17-N16-Co1 | 127.5(4) |
| O9-C25-C26 | 110.0(7) | N13-Na3-N1 | 74.00(15) | Co3-N16-Co1 | 99.16(17) |
| O9-C25-H25A | 109.7 | C42-C41-C40 | 120.5(7) | N17-N16-Na2 | 112.6(3) |
| C26-C25-H25A | 109.7 | C42-C41-H41 | 119.7 | Co3-N16-Na2 | 93.46(16) |
| O9-C25-H25B | 109.7 | C40-C41-H41 | 119.7 | Co1-N16-Na2 | 94.63(15) |
| C26-C25-H25B | 109.7 | C59-C60-H60C | 109.5 | N18-N17-N16 | 176.5(7) |
| H25A-C25-H25B | 108.2 | O16-C46-C47 | 124.7(5) | C59-N19-C56 | 111.4(12) |
| C25-C26-H26A | 109.5 | O16-C46-C51 | 118.2(5) | C25-O9-Na3 | 124.5(5) |
| C25-C26-H26B | 109.5 | C44-C43-H43A | 110.2 | C28-O10-Co4 | 129.0(4) |
| H26A-C26-H26B | 109.5 | C53-C52-H52B | 109.9 | C28-O10-Na2 | 121.4(3) |
| C25-C26-H26C | 109.5 | C41-C42-O15 | 125.7(6) | Co4-O10-Na2 | 103.92(17) |
| H26A-C26-H26C | 109.5 | C41-C42-C37 | 120.9(6) | C36-O11-Co4 | 126.4(4) |
| H26B-C26-H26C | 109.5 | C39-C40-C41 | 120.6(8) | C33-O12-C34 | 117.3(5) |
| O8-C27-C20 | 129.6(6) | C39-C40-H40 | 119.7 | C33-O12-Na2 | 115.3(3) |
| O8-C27-H27 | 115.2 | C41-C40-H40 | 119.7 | C34-O12-Na2 | 124.1(4) |
| C20-C27-H27 | 115.2 | N4-Co1-N7 | 94.37(16) | C37-O13-Co3 | 130.0(4) |
| O10-C28-C29 | 123.0(5) | N10-Co1-N7 | 171.75(16) | C37-O13-Na2 | 123.9(3) |
| O10-C28-C33 | 120.1(5) | N13-Co1-N16 | 94.92(16) | O1-Na1-N4 | 93.01(15) |
| C29-C28-C33 | 116.9(6) | N1-Co1-N16 | 172.83(16) | C59-N19-C57 | 121.5(12) |
| C28-C29-C30 | 119.7(6) | N4-Co1-N16 | 81.10(15) | C56-N19-C57 | 106.1(12) |
| C28-C29-C36 | 123.6(6) | O2-Co2-O5 | 97.26(19) | C59-N19-H19A | 104.8 |
| C30-C29-C36 | 116.7(7) | O1-Co2-N1 | 95.31(17) | C56-N19-H19A | 114.3 |
| C31-C30-C29 | 120.5(8) | O4-Co2-N1 | 89.26(16) | C57-N19-H19A | 98.4 |
| C31-C30-H30 | 119.8 | O2-Co2-N1 | 90.63(18) | O16-Na1-O1 | 163.36(16) |
| C29-C30-H30 | 119.8 | O5-Co2-N1 | 170.63(19) | O16-Na1-O18 | 67.44(14) |
| C30-C31-C32 | 119.8(8) | O1-Co2-N10 | 88.66(16) | O1-Na1-O18 | 122.62(17) |
| C30-C31-H31 | 120.1 | O4-Co2-N10 | 95.13(17) | O16-Na1-O3 | 124.77(17) |
| C32-C31-H31 | 120.1 | O2-Co2-N10 | 170.44(19) | O1-Na1-O3 | 66.94(16) |
| C33-C32-C31 | 121.1(7) | O5-Co2-N10 | 91.24(17) | Co3-O13-Na2 | 105.80(17) |
| C33-C32-H32A | 107.1 | N1-Co2-N10 | 81.32(17) | C45-O14-Co3 | 126.6(4) |
| C31-C32-H32A | 107.1 | O1-Co2-O4 | 174.47(16) | C42-O15-C43 | 115.8(5) |
| C33-C32-H32B | 107.1 | O1-Co2-O2 | 86.97(18) | C42-O15-Na2 | 117.0(3) |
| C31-C32-H32B | 107.1 | O4-Co2-O2 | 89.87(18) | C43-O15-Na2 | 126.7(4) |
| H32A-C32-H32B | 106.8 | O1-Co2-O5 | 90.17(19) | C46-O16-Co3 | 130.6(4) |
| C32-C33-O12 | 124.7(6) | O4-Co2-O5 | 85.73(18) | C46-O16-Na1 | 123.0(4) |
| C32-C33-C28 | 122.0(7) | O1-Co2-O4 | 174.47(16) | Co3-O16-Na1 | 105.80(15) |
| O12-C33-C28 | 113.2(5) | N13-Co1-N1 | 90.80(17) | C54-O17-Co3 | 126.6(4) |
| O12-C34-C35 | 108.4(7) | N13-Co1-N4 | 173.84(16) | C51-O18-C52 | 117.9(5) |
| O12-C34-H34A | 110.0 | N1-Co1-N4 | 93.54(16) | C51-O18-Na1 | 117.0(3) |
| C35-C34-H34A | 110.0 | C56-C55-H55A | 109.5 | C52-O18-Na1 | 125.1(4) |
| O12-C34-H34B | 110.0 | C56-C55-H55B | 109.5 | O18-Na1-O3 | 109.27(17) |
| C35-C34-H34B | 110.0 | H55A-C55-H55B | 109.5 | O16-Na1-N4 | 74.15(14) |
| H34A-C34-H34B | 108.4 | H52A-C52-H52B | 108.3 | C47-C46-C51 | 117.2(5) |
| C34-C35-H35A | 109.5 | C52-C53-H53A | 109.5 | C46-C47-C54 | 122.6(6) |
| C34-C35-H35B | 109.5 | C52-C53-H53B | 109.5 | C46-C47-C48 | 120.0(6) |
| H35A-C35-H35B | 109.5 | H53A-C53-H53B | 109.5 | C54-C47-C48 | 117.4(6) |
| C34-C35-H35C | 109.5 | C52-C53-H53C | 109.5 | C49-C48-C47 | 120.6(7) |
| H35A-C35-H35C | 109.5 | H53A-C53-H53C | 109.5 | C49-C48-H48 | 119.7 |
| H35B-C35-H35C | 109.5 | H53B-C53-H53C | 109.5 | C47-C48-H48 | 119.7 |
| O11-C36-C29 | 128.0(7) | O17-C54-C47 | 128.5(6) | C48-C49-C50 | 120.4(6) |
| O11-C36-H36 | 116.0 | O17-C54-H54 | 115.8 | C48-C49-H49 | 119.8 |
| C29-C36-H36 | 116.0 | C47-C54-H54 | 115.8 | C50-C49-H49 | 119.8 |
| O13-C37-C38 | 124.7(5) | C49-C50-H50 | 119.3 | C49-C50-C51 | 121.4(7) |
| O13-C37-C42 | 118.2(5) | C51-C50-H50 | 119.3 | C43-C44-H44B | 109.5 |
| C38-C37-C42 | 117.1(6) | O18-C51-C50 | 125.2(6) | H44A-C44-H44B | 109.5 |
| C37-C38-C45 | 122.6(6) | O18-C51-C46 | 114.3(5) | C43-C44-H44C | 109.5 |
| C37-C38-C39 | 119.6(6) | C50-C51-C46 | 120.4(6) | H44A-C44-H44C | 109.5 |
| C45-C38-C39 | 117.7(6) | O18-C52-C53 | 109.0(6) | H44B-C44-H44C | 109.5 |
HN (C
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] the synthetic method concrete steps of (Hheb is 3-ethyoxyl-Benzaldehyde,2-hydroxy) are:
0.166 gram of analytically pure 3-ethyoxyl-Benzaldehyde,2-hydroxy is dissolved in to 4-8 milliliter to be analyzed pure methyl alcohol 4-8 milliliter and analyzes in the mixed solution of pure acetonitrile, add successively again 0.36-0.72g to analyze pure six perchloric acid hydrate cobalts and 0.065-0.13g analyzes pure sodium azide, and stir to add after solution being mixed in 10 minutes and analyze pure triethylamine and be adjusted to pH=5.5, continue to stir after 20 minutes, prepared mixed liquor is statically placed under room temperature, after 30 minutes, obtain red strip crystal, filter, and clean with analyzing pure methanol wash, after drying, obtain product HN (C in air
2h
5)
3[Co
4na
3(heb)
6(N
3)
6].
HN (C
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] magnetic property: between cobalt ions, have ferromagnetic exchange in molecule, its general performance is ferromagnetism.
The present invention has that technique is simple, with low cost, chemical constituent is easy to control, reproducible and output advantages of higher.
Accompanying drawing explanation
Fig. 1 is HN (C of the present invention
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] structure chart.
Fig. 2 is HN (C of the present invention
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] χ
m-T, χ
mt-T curve chart.
Fig. 3 is HN (C of the present invention
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] χ
m – 1-T curve chart.
Embodiment
Embodiment 1:
HN (the C the present invention relates to
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] molecular formula be:
C
60h
71n
19na
3co
4o
18molecular weight is: 1651.05.
HN (C
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] synthetic method concrete steps be:
(1) by 0.166 gram, analyzing pure 3-ethyoxyl-Benzaldehyde,2-hydroxy is dissolved in the mixed solution of 4 milliliters of analytically pure acetonitriles of 4 milliliters of analytically pure methyl alcohol, add successively the more analytically pure six perchloric acid hydrate cobalts of 0.36g, the analytically pure sodium azide of 0.065g, and stir to add after solution being mixed in 10 minutes and analyze pure triethylamine and be adjusted to pH=5.5, continue to stir after 20 minutes, prepared mixed liquor is statically placed under room temperature, after 30 minutes, obtain red strip crystal, filter, and clean with analyzing pure methanol wash, after drying, obtain product HN (C in air
2h
5)
3[Co
4na
3(heb)
6(N
3)
6].Output: 142mg, productive rate: 51.60%, and it measures HN (C by single crystal diffraction
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] structure, crystal structure data are in Table one, bond distance's bond angle data are in Table two.
(2) after the product 0.0247 gram of step (1) being obtained pulverizes, on magnetic tester device, carry out magnetic test, obtain magnetic test curve as accompanying drawing 2,3, HN (C
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] χ at room temperature
mt is 12.53cm
3kmol
-1, along with temperature reduces, χ
mt raises gradually, reaches maximum 20.08cm to 14K
3kmol
-1, be sharply down to subsequently 8.38cm
3kmol
-1.And χ
m – 1-T curve is deferred to Curie-Weiss law, and it is 5.00K that its matching is obtained to Wei Si constant, and Curie constant is 12.56cm
3kmol
– 1.Large and positive Wei Si constant and χ
mt-T curvilinear trend all implies in molecule and has ferromagnetic exchange between cobalt ions, and its general performance is ferromagnetism.
Embodiment 2:
HN (the C the present invention relates to
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] (CH
3oH) molecular formula is:
C
60h
71n
19na
3co
4o
18molecular weight is: 1651.05.
HN (C
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] synthetic method concrete steps be:
(1) by 0.166 gram, analyzing pure 3-ethyoxyl-Benzaldehyde,2-hydroxy is dissolved in 8 milliliters of pure acetonitriles of analysis and 8 milliliters of pure methyl alcohol mixed solutions of analysis, add successively again 0.72g to analyze pure six perchloric acid hydrate cobalts and 0.13g analyzes pure sodium azide, and stir to add after solution being mixed in 10 minutes and analyze pure triethylamine and be adjusted to pH=5.5, continue to stir after 20 minutes, prepared mixed liquor is statically placed under room temperature, after 30 minutes, obtain red strip crystal, filter, and clean with analyzing pure methanol wash, after drying, obtain product HN (C in air
2h
5)
3[Co
4na
3(heb)
6(N
3)
6].
(2) the product HN (C 0.0247 gram of step (1) being obtained
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] on magnetic tester device, carry out magnetic test after pulverizing, obtain magnetic test curve as accompanying drawing 2,3, HN (C
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] χ at room temperature
mt is 12.53cm
3kmol
-1, along with temperature reduces, χ
mt raises gradually, reaches maximum 20.08cm to 14K
3kmol
-1, be sharply down to subsequently 8.38cm
3kmol
-1.And χ
m – 1-T curve is deferred to Curie-Weiss law, and it is 5.00K that its matching is obtained to Wei Si constant, and Curie constant is 12.56cm
3kmol
– 1.Large and positive Wei Si constant and χ
mt-T curvilinear trend all implies in molecule and has ferromagnetic exchange between cobalt ions, and its general performance is ferromagnetism.
Claims (1)
1. a magnetic material HN (C
2h
5)
3[Co
4na
3(heb)
6(N
3)
6], it is characterized in that HN (C
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] thering is good magnetism characteristic, its molecular formula is: C
60h
71n
19na
3co
4o
18, molecular weight is: 1651.05, and wherein Hheb is 3-ethyoxyl-Benzaldehyde,2-hydroxy, and crystal structure data are in Table one, and bond distance's bond angle data are in Table two; HN (C
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] magnetic property: between cobalt ions, have ferromagnetic exchange in (1) molecule, its general performance is ferromagnetism; (2) HN (C
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] χ at room temperature
mt is 12.53cm
3kmol
-1, along with temperature reduces, χ
mt raises gradually, reaches maximum 20.08cm to 14K
3kmol
-1, the 8.38cm while being sharply down to 2K subsequently
3kmol-
1; And χ
m – 1-T curve is deferred to Curie-Weiss law, and it is 5.00K that its matching is obtained to Wei Si constant, and Curie constant is 12.56cm
3kmol
– 1; Large and positive Wei Si constant and χ
mt-T curvilinear trend all implies in molecule and has ferromagnetic exchange between cobalt ions, and its general performance is ferromagnetism;
Described HN (C
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] synthetic method concrete steps be:
By 0.166 gram, analyzing pure 3-ethyoxyl-Benzaldehyde,2-hydroxy is dissolved in 4-8 milliliter and analyzes pure methyl alcohol 4-8 milliliter and analyze in the mixed solution of pure acetonitrile, add successively again 0.36-0.72g to analyze pure six perchloric acid hydrate cobalts and 0.065-0.13g analyzes pure sodium azide, and stir to add after solution being mixed in 10 minutes and analyze pure triethylamine and be adjusted to pH=5.5, continue to stir after 20 minutes, prepared mixed liquor is statically placed under room temperature, after 30 minutes, obtain red strip crystal, filter, and clean with analyzing pure methanol wash, after drying, obtain product HN (C in air
2h
5)
3[Co
4na
3(heb)
6(N
3)
6];
Table one HN (C
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] (CH
3oH) crystallographic parameter
Table two HN (C
2h
5)
3[Co
4na
3(heb)
6(N
3)
6] (CH
3oH) bond distance
and bond angle (°)
。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106220687A (en) * | 2016-09-13 | 2016-12-14 | 桂林理工大学 | { [Co3k (emimp)4(DCA)2] ClO4}6(H2and synthetic method O) |
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