Ionothermal Syntheses and Characterization of Open-framework Manganese Phosphites (NH4)2Mn3(HPO3)4 and Mn(HPO3)†

doi:10.7503/cjcu20140529

Abstract

Abstract:

Two open-framework manganese phosphites, (NH₄)₂Mn₃(HPO₃)₄(1) and Mn(HPO₃)(2), were synthesized under ionothermal conditions and characterized by single crystal X-ray diffraction. The two compounds were synthesized under the same conditions, but the structures were different with the use of diffe-rent ionic liquids. The framework structure of compound 1 is built up from MnO₆ octahedra and phosphite groups, giving rise to a two-dimensional framework with N $H 4 +$ cations filling between the layers; the structure of compound 2 consists of a 3D condensed framework of edge-sharing MnO₆ octahedra linking to [HPO₃] units via oxygens. The compounds were further characterized by scanning electron microscopy(SEM), powder X-ray diffraction(PXRD) and inductively coupled plasma(ICP), and the magnetic measurements results reveal that strong antiferromagnetic interaction exists in compound 1.

Key words: Manganese phosphite, Ionothermal synthesis, Crystal structure, Magnetic property

CLC Number:

O614.7

TrendMD:

HE Yongke, YAN Yan, YANG Fen, WU Junbiao, SONG Xiaowei. Ionothermal Syntheses and Characterization of Open-framework Manganese Phosphites (NH₄)₂Mn₃(HPO₃)₄ and Mn(HPO₃)^†[J]. Chem. J. Chinese Universities, 2014, 35(9): 1859.

Figures/Tables 6

Fig.1 SEM images of compounds 1(A) and 2(B)

Table 1 Crystallographic data for compound 1

Empirical formula	H₁₂Mn₃N₂O₁₂P₄	Z	3
M_r	520.81	D_c/(g·cm^-3)	2.673
T/K	296(2)	μ/mm^-1	3.509
λ/nm	0.071073	F(000)	741
Crystal system	Trigonal	θ range/(°)	1.65—28.37
Space group	R $3 ˉ$ m	Goodness-of-fit on F²	1.021
a/nm	0.54415(3)	Limiting indices	-7≤h≤5, -7≤k≤7, -39≤l≤49
b/nm	0.54415(3)	Reflections collected/unique	2364/358
c/nm	3.7114(4)	Completeness to 28.37°	100.0%
α/(°)	90	Data/restraints/parameters	358/6/31
β/(°)	90	R₁, wR₂[I>2σ(I)]	R₁=0.0326, wR₂=0.0883
γ/(°)	120	R₁, wR₂(all data)	R₁=0.0337, wR₂=0.0889
V/nm³	0.95171(13)

Table 1 Crystallographic data for compound 1

Empirical formula	H₁₂Mn₃N₂O₁₂P₄	Z	3
M_r	520.81	D_c/(g·cm^-3)	2.673
T/K	296(2)	μ/mm^-1	3.509
λ/nm	0.071073	F(000)	741
Crystal system	Trigonal	θ range/(°)	1.65—28.37
Space group	R $3 ˉ$ m	Goodness-of-fit on F²	1.021
a/nm	0.54415(3)	Limiting indices	-7≤h≤5, -7≤k≤7, -39≤l≤49
b/nm	0.54415(3)	Reflections collected/unique	2364/358
c/nm	3.7114(4)	Completeness to 28.37°	100.0%
α/(°)	90	Data/restraints/parameters	358/6/31
β/(°)	90	R₁, wR₂[I>2σ(I)]	R₁=0.0326, wR₂=0.0883
γ/(°)	120	R₁, wR₂(all data)	R₁=0.0337, wR₂=0.0889
V/nm³	0.95171(13)

Fig.2 Experimental(a) and simulated(b) XRD patterns of compounds 1(A) and 2(B)

Fig.3 Thermal ellipsoids given at 50% probability

Fig.4 Views of Mn3 cluster formed by MnO6 octahedra(A), Mn3 cluster linking to six adjacent Mn3 clusters by [HPO3] units along the [001] direction(B), the layer consisted of MnO6 and [HPO3] along the [001] direction(C) and NH4+ ions residing between the layers along the [010] direction(D)

Fig.5 Plots of χmT vs. T(A) and 1/χm vs. T(B) for compound 1 (B) Gray solid line represents Curie-Weiss curve fitting in 300—100 K.

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Ionothermal Syntheses and Characterization of Open-framework Manganese Phosphites (NH₄)₂Mn₃(HPO₃)₄ and Mn(HPO₃)^†

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