CN102936256A - Dicyandiamide ion contained binuclear copper complex and preparation method thereof - Google Patents

Dicyandiamide ion contained binuclear copper complex and preparation method thereof Download PDF

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CN102936256A
CN102936256A CN 201210454348 CN201210454348A CN102936256A CN 102936256 A CN102936256 A CN 102936256A CN 201210454348 CN201210454348 CN 201210454348 CN 201210454348 A CN201210454348 A CN 201210454348A CN 102936256 A CN102936256 A CN 102936256A
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copper complex
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夏军
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Tianjin Polytechnic University
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Tianjin Polytechnic University
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Abstract

The invention relates to a dicyandiamide ion contained binuclear copper complex and a preparation method thereof. The dicyandiamide ion contained binuclear copper complex has a chemical formula (I) of [Cu2L2] [N (CN) 2]2, wherein L=1, 3-bi(3, 5-dimethyl-1-hydrogen-pyrazolyl)-2-hydroxypropane ligand. The dicyandiamide ion contained binuclear copper complex is of a zero dimension binuclear structure. The preparation method includes subjecting CuCl2*2H2O and the L ligand to reaction in a methanol solution for 2 hours at room temperatures, dissolving an Na [N(CN)2] solid in an aqueous solution, mixing the two solutions, subjecting the two solutions to reaction for 2 hours under the condition of room temperatures, and subjecting the solutions to filtering, standing and volatilizing to obtain the dicyandiamide ion contained binuclear copper complex.

Description

A kind of double-core copper complex that contains the Dyhard RU 100 ion and preparation method thereof
Technical field
The invention belongs to title complex science and technology field, particularly a kind of double-core copper complex that contains the Dyhard RU 100 ion and preparation method thereof.
Technical background
Development along with science and technology, and to the active demand of new forms of energy, novel material, the research of metal complexes has become one of most active field in the current chemical research, and they have potential using value in fields such as catalysis, gas adsorption, chemical separation and ion-exchanges.In all multi-metal complexes, the title complex of metallic copper especially occupies an important position.On Chemical Manufacture, copper complex can be used as catalyzer, and the carrying out of catalyzed chemical reaction promotes the development [D.M.Ma etc., J.Am.Chem.Soc., 120,12459,1998] of green organic synthesis; At life science, metal copper complexes is the important composition composition of many proteolytic enzyme, and vital movement is played vital effect [Sun Ying etc., chemistry circular, 6,495,2009]; At environmental area, utilize the spectrochemical property of copper complex, can effectively repair [Xu Long etc., chemical progress, 17,412,2005] by environmental pollution.In the title complex of metallic copper, the kind of part, the factors such as space structure of title complex all can produce different impacts to its physicochemical property.Therefore, by part regulation and control and molecular self-assembling, the synthetic copper complex with novel space structure and function of design is the common objective that the various countries scientist pursues.In addition, bivalent cupric ion has into single electron, and its title complex often demonstrates beyond thought magnetic property, will produce great effect to the exploration of novel magnetic material and development.
Summary of the invention
The purpose of this invention is to provide a kind of double-core copper complex that contains the Dyhard RU 100 ion and preparation method thereof.This metal copper complexes has the zero dimension dual-core architecture, is with a wide range of applications.
Chemical formula with title complex provided by the invention is [Cu 2L 2] [N (CN) 2] 2, L=1 wherein, 3-two (3,5-dimethyl-1-hydrogen-pyrazolyl)-2-hydroxy propane part.
The structure of copper complex disclosed by the invention as shown in Figure 1, their secondary building unit is: crystal belongs to rhombic system, spacer is Pccn, unit cell parameters is:
Figure BSA00000804894900011
Figure BSA00000804894900012
Figure BSA00000804894900013
α=90.00 °, β=90.00 °, γ=90.00 °; The space structure of this title complex is centered by double-core copper, 1,3-two (3,5-dimethyl-1-hydrogen-pyrazolyl)-2-hydroxy propane and the self-assembly of Dyhard RU 100 ion and the zero-dimension structural that forms; The ligancy of the coordination of Cu ion is 4, is connected with two N atoms with two O atoms in the hydroxyl with the pyrazole ring of L part; These five atoms are substantially coplanar, and its average departure is
Figure BSA00000804894900014
These five atoms have formed a trapezoid, and the corresponding length of side is respectively: O1-O1A,
Figure BSA00000804894900015
O1A-N4A,
Figure BSA00000804894900016
N4A-N1,
Figure BSA00000804894900017
N1-O1,
Figure BSA00000804894900018
Cu1 and its centrosymmetry unit Cu1A and two L parts have consisted of the butterfly-shaped double-core unit of title complex, and Cu1 and Cu1A are connected together by two hydroxyl O bridging, corresponding Cu1 ... the distance of Cu1A is
Figure BSA00000804894900021
Cu1, O1, O1A and four atoms of Cu1A are fully coplanar, and its average departure is zero.These four atoms have formed a parallelogram, and four limits are respectively
Figure BSA00000804894900022
Figure BSA00000804894900023
Corresponding Cu1A-O1-Cu1 angle is 103.9 °.In this dual-core architecture unit, the interfacial angle that forms between neighbouring pyrazole ring is all 62.1 °.
Preparation method of the present invention is as follows:
With CuCl 22H 2O and L part place the beaker that is placed with methanol solution, and reaction is 2 hours under the room temperature condition.With Na[N (CN) 2] in the water-soluble solution of solid.Above-mentioned two kinds of solution are mixed, continue reaction 2 hours under the room temperature condition, with solution filter, filtrate is left standstill in air, is volatilized, and obtains target product after the week.CuCl 22H 2O, L, Na[N (CN) 2] mass ratio be: 1.91: 3.00: 1.
Description of drawings
Fig. 1 [Cu 2L 2] [N (CN) 2] 2Crystalline structure figure.
The crystallographic data of table 1 title complex
Figure BSA00000804894900031
Embodiment
Embodiment 1 Complex synthesis:
0.5mmol CuCl 22H 2O (0.085g) and 0.5mmol L part (0.124g) are dissolved in the 15mL methanol solution, react at ambient temperature 0.5mmol Na[N (CN) 2 hours 2] solid (0.045g) is dissolved in the 8mL water, and two kinds of solution phases are mixed, reacted at ambient temperature 2 hours, with solution filter, filtrate is left standstill in air, is volatilized, and obtains blue bulk crystals after the week, product washs with the 6mL ether, and the productive rate that calculates based on metal Cu is 30%.
The structure determination of embodiment 2 title complexs:
BRUKER SMART 1000X-x ray diffractometer x is adopted in crystal structure determination, uses the Mok alpha-ray through the graphite monochromatization
Figure BSA00000804894900033
Be incident radiation, collect point diffraction with ω-2 θ scan mode, obtain unit cell parameters through least-squares refinement, utilize the SHELXL-97 direct method to solve crystalline structure from the difference Fourier electron density map, and through Lorentz and polarizing effect correction.All H atoms are synthetic and definite through desirable position calculation by difference Fourier.Detailed axonometry data see Table 1.Structure is seen Fig. 1; Fig. 1: [Cu 2L 2] [N (CN) 2] 2Crystalline structure figure.

Claims (5)

1. double-core copper complex that contains the Dyhard RU 100 ion, this coordination chemistry formula is [Cu 2L 2] [N (CN) 2] 2, L=1 wherein, 3-two (3,5-dimethyl-1-hydrogen-pyrazolyl)-2-hydroxy propane part.
2. the double-core copper complex that contains the Dyhard RU 100 ion according to claim 1 is characterized in that its secondary building unit is:
Crystal belongs to rhombic system, and spacer is Pccn, and unit cell parameters is:
Figure FSA00000804894800011
Figure FSA00000804894800012
Figure FSA00000804894800013
α=90.00 °, β=90.00 °, γ=90.00 °; The space structure of this title complex is centered by double-core copper, 1,3-two (3,5-dimethyl-1-hydrogen-pyrazolyl)-2-hydroxy propane and the self-assembly of Dyhard RU 100 ion and the zero-dimension structural that forms; The ligancy of the coordination of Cu ion is 4, is connected with two N atoms with two O atoms in the hydroxyl with the pyrazole ring of L part; These five atoms are substantially coplanar, and its average departure is 0.0023
Figure FSA00000804894800015
These five atoms have formed a trapezoid, and the corresponding length of side is respectively: O1-O1A, O1A-N4A,
Figure FSA00000804894800017
N4A-N1, N1-O1,
Figure FSA00000804894800019
Cu1 and its centrosymmetry unit Cu1A and two L parts have consisted of the butterfly-shaped double-core unit of title complex, and Cu1 and Cu1A are connected together by two hydroxyl O bridging, corresponding Cu1 ... the distance of Cu1A is
Figure FSA000008048948000110
3. the preparation method who contains the double-core copper complex of Dyhard RU 100 ion according to claim 1 is characterized in that it comprises the steps:
1) by measuring CuCl 22H 2O and L part are dissolved in the methanol solution, react at ambient temperature 2 hours;
2) take by weighing a certain amount of Na[N (CN) 2] solid, be dissolved in the 8mL aqueous solution;
3) above-mentioned two kinds of solution phases are mixed, and at ambient temperature, continue reaction 2 hours;
4) with the gained solution filter, clear filtrate leaves standstill in air, volatilizees, and obtains target product after the week.
4. the preparation method who contains the double-core copper complex of Dyhard RU 100 ion according to claim 3 is characterized in that described CuCl 22H 2O, L, Na[N (CN) 2] mass ratio be: 1.91: 3.00: 1.
5. the preparation method of multi-ligand hybridized dinuclear copper compound according to claim 3 is characterized in that described reaction conditions is at room temperature, utilizes magnetic agitation.
CN 201210454348 2012-11-14 2012-11-14 Dicyandiamide ion contained binuclear copper complex and preparation method thereof Pending CN102936256A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103193802A (en) * 2013-04-11 2013-07-10 山西大学 Double-kernel copper complex and preparation method thereof
CN106680356A (en) * 2017-02-27 2017-05-17 福州大学 Method for rapidly detecting metal copper ions

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103193802A (en) * 2013-04-11 2013-07-10 山西大学 Double-kernel copper complex and preparation method thereof
CN103193802B (en) * 2013-04-11 2015-09-30 山西大学 A kind of dicopper complex4-amino-3 and preparation method thereof
CN106680356A (en) * 2017-02-27 2017-05-17 福州大学 Method for rapidly detecting metal copper ions

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