Template-directed Synthesis of a Novel Two-dimensional Dy(Ⅲ) Complex Containing Helical Chains Using [PMo12O40y2

doi:10.7503/cjcu20160141

Abstract

Abstract:

A new two-dimensional(2D) Dy(Ⅲ) complex, [Dy(BMBCP)(H₂O)₄][PMo₁₂O₄₀]·2.75H₂O{H₂BMBCP=1,1'-[1,4-phenylene-bis(methylene)]-bis(pyridine-4-carboxylicaicd)}, denoted as HNU-7, was hydrothermally synthesized using [PMo₁₂O₄₀]^3- as template, and characterized by single crystal X-ray diffraction, Infrared spectroscopy(IR), X-ray diffraction(XRD), inductively coupled plasa(ICP) and luminescent techniques. Interestingly, due to the electrostatic attraction between the guest ions [PMo₁₂O₄₀]^3- and N⁺ of BMBCP ligands in the host sheets, pairs of helical -Dy₂ cluster-BMBCP-Dy₂ cluster-BMBCP- chains were formed by the alternation of Dy₂ clusters and the BMBCP ligands. The left- and right-handed helical chains are linked together via Dy₂ clusters to from the infinite sheet structure with 4,4-net.

Key words: Template, Hydrothermal synthesis, Host-guest system, Helical structure

CLC Number:

O613
O643

TrendMD:

LIU Xiaojing, TANG Weidong, ZHOU Sihui, WANG Fuxiang, LIU Ying, XIANG Mingyue, PAN Qinhe. Template-directed Synthesis of a Novel Two-dimensional Dy(Ⅲ) Complex Containing Helical Chains Using [PMo₁₂O₄₀ $y 2$ [J]. Chem. J. Chinese Universities, 2016, 37(6): 1025.

Figures/Tables 6

Table 1 Crystal data and structure refinement for HNU-7

Empirical formula	C₂₀ $] n 3 n +$ DyMo₁₂N₂O_50.75P
M_r	2454.71
Temperature/K	273(2)
λ/nm	0.071073
Crystal system, space group	Monoclinic, P2₁/n
a, b, c/nm	1.4589(2), 1.37252(19), 2.8535(4)
α, β, γ/(°)	90, 90.556(3), 90
V/nm³	5.7135(14)
Z, calculated density/(Mg·m^-3)	4, 2.845
F(000)	4618
Crystal size	0.3 mm×0.2 mm×0.15 mm
θ range for data collection	1.43°—26.40°
Limiting indices	-18≤h≤16, -17≤k≤17, -19≤l≤35
Reflections collected/unique[R_int=0.0969]	33731/11693
Completeness to θ=28.48°	99.8%
Refinement method	Full-matrix least-squares on F²
Data/restraints/parameters	11693/30/811
Goodness-of-fit on F²	0.963
Final R indices[I>2σ(I)]	R₁=0.0664, wR₂=0.1845
R indices(all data)	R₁=0.1428, wR₂=0.1989
Largest diff. peak and hole(e·nm^-3)	2508, -1125

Table 1 Crystal data and structure refinement for HNU-7

Empirical formula	C₂₀ $] n 3 n +$ DyMo₁₂N₂O_50.75P
M_r	2454.71
Temperature/K	273(2)
λ/nm	0.071073
Crystal system, space group	Monoclinic, P2₁/n
a, b, c/nm	1.4589(2), 1.37252(19), 2.8535(4)
α, β, γ/(°)	90, 90.556(3), 90
V/nm³	5.7135(14)
Z, calculated density/(Mg·m^-3)	4, 2.845
F(000)	4618
Crystal size	0.3 mm×0.2 mm×0.15 mm
θ range for data collection	1.43°—26.40°
Limiting indices	-18≤h≤16, -17≤k≤17, -19≤l≤35
Reflections collected/unique[R_int=0.0969]	33731/11693
Completeness to θ=28.48°	99.8%
Refinement method	Full-matrix least-squares on F²
Data/restraints/parameters	11693/30/811
Goodness-of-fit on F²	0.963
Final R indices[I>2σ(I)]	R₁=0.0664, wR₂=0.1845
R indices(all data)	R₁=0.1428, wR₂=0.1989
Largest diff. peak and hole(e·nm^-3)	2508, -1125

Fig.1 XRD patterns of HNU-7

Fig.2 TG curves of HNU-7

Fig.3 Structure of HNU-7 viewed along [010] direction(A), two-dimensional sheet viewed from the [101] direction(B), binuclear Dy2 cluster, which could be regarded as four-connected building unit(C) and left-handed and right-handed infinite -Dy2 cluster-BMBCP-Dy2 cluster- helical chains exist in sheet(D)

Fig.4 Illustration of the formation of helical chains(A) [PMo12O40]3- anions, which could be regarded as a node; (B) left-handed helical chains accommodated and supported with two [PMo12O40]3- anions; (C) left-handed helical chains surrounded by [PMo12O40]3- anions from adjacent sheets.

Fig.5 Solid state excitation(A) and emission(B) spectra of HNU-7

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Template-directed Synthesis of a Novel Two-dimensional Dy(Ⅲ) Complex Containing Helical Chains Using [PMo₁₂O₄₀ $y 2$

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