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Based on chiral polyfunctional ligand coordination polymers Synthesis, Characterization and Properties

Author: OuYangXiang
Tutor: JiaZuo
School: Fudan University
Course: Organic Chemistry
Keywords: Chiral Coordination Polymers Chiral ligands Solvothermal Diffusion method Fluorescence
CLC: TB383.4
Type: Master's thesis
Year: 2008
Downloads: 141
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Abstract


Coordination polymer is defined by the metal ion or metal ion clusters and small organic polyfunctional ligand formed by self-assembly process network structure with periodic crystalline porous materials. Compared with conventional inorganic porous material, with a polymer having a more moderate reaction conditions, modification of pore size and structure of the more advantages and can be used to form the chiral ligand chirality. Chiral coordination polymers combine two kinds of chiral porous nature of the design and synthesis of such crystalline materials have become a challenging task. In this paper, we designed and synthesized three eight hydrogenated BINOL chiral polyfunctional ligands (expressed as H 2 Lx 1 ~ HLx 3 ). The one of the chiral ligand (R) -5,5 ', 6,6', 7,7 ', 8,8' - octahydro-2, 2'- dimethoxy-1, 1'- - binaphthyl 3,3 '- dicarboxylic acid (H 2 Lx 1 ) and transition metal salts by hydrothermal and solvothermal method has been six chiral coordination polymer (expressed as FDCX-n), respectively: [Cu (Lx 1 ) (Py) 3 ] (FDCX-1), [ Cd (Lx 1 ) (Py) 3 ] (FDCX-2), [Zn (Lx 1 )) (Py) 2 ] (FDCX-3), {Na [Cd (Lx 1 ) (HLx 1 )] · 2.5H 2 O} (FDCX-4), {[NH 2 (CH 3 ) 2 ] [Cd (Lx 1 ') 2 ] · DMF · H 2 O} (FDCX-5) and [Zn 4 (Lx 1 < / sub>) 4 ] (FDCX-6); synthesized via diffusion method, a chiral coordination polymer, expressed as: {[NH 2 (CH 3 ) 2 ] 2 [Cd 3 O (Lx 1 ) 3 (H 2 O) 3 ] 2 · 6H 2 O} (FDCX- 7). All chiral coordination polymers were characterized by X-ray diffraction analysis of the structure by X-ray powder diffraction technique (XRD) characterize the phase purity, and then conducted a thermal gravimetric analysis (TGA), elemental analysis, solid fluorescence and infrared and other related tests. X-ray diffraction analysis showed that, FDCX-1 and FDCX-2 is allomerism structures are single metal ions as nodes, Lx 1 2 - for the formation of a one-dimensional helical linker chain structure; FDCX-3 with a single metal ion as nodes, Lx 1 2 - to connect the body to form a one-dimensional linear chain structure . FDCX-4 with four attached single Cd 2 ions as nodes, chiral ligand Lx 1 2 - and HLx 1 - is connected to the body, forming a two-dimensional lattice structure of carboxylic acid cadmium [Cd (Lx 1 ) (HLx 1 ) ] - ; cadmium in acid skeleton structure plays a balancing role in the charge Na ions and six oxygen atoms, adjacent Na ion By sharing two carboxyl oxygen and a water molecule to form Na 2 O 6 clusters, the clusters of sodium oxide carboxylic further connecting adjacent two-dimensional lattice of cadmium, resulting in a Two-dimensional layer structure, the layers form a space between the stacked arrangement of staggered. FDCX-6 in the chiral ligand Lx 1 2 - to connect the five dual-core secondary structural elements \2 ) 3 (RCO 2 ) 2 \1 2 - and then in another way a ligand-dimensional chain structure connected together to form a two-dimensional layered structure ABAB taken between layers staggered stacked to form a spatial arrangement. FDCX-7 to connect three relatively rare six-core secondary structural elements \2 ) 3 (H 2 O) 3 \> 2 - to connect the body to form a two-dimensional hexagonal pore layered structure. In FDCX-5 configuration, the chiral ligand H 2 Lx 1 of the two-situ hydrolysis of methoxy two phenolic hydroxyl groups to form a ligand Lx 1 ' 2 - . FDCX-5 with eight ligand dodecahedron coordination geometry of the single Cd 2 is the junction point, Lx 1 ' 2 - for the connection body along the a-axis and c-axis of a two-dimensional mesh layer structure, taken between the layers staggered ABCDABCD accumulation. TGA showed FDCX-4 can be stabilized to 330 ℃, FDCX-6 can be stabilized to 350 ℃. So far, few chiral polymer stable to such high temperatures. Solid at room temperature fluorescence emission spectra show FDCX-2 ~ 4 with violet photoluminescence properties. FDCX-1 after activation by heating under reduced pressure, the racemic 2 - butanol have a certain adsorption capacity.

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