Synthesis, Structures and Photochemical Properties of Two New Cd(II) Metal-organic Frameworks Isolated from the Same Reaction System†

doi:10.7503/cjcu20150471

Abstract

Abstract:

The solvothermal reactions of Cd(NO₃)₂ with 4,4'-(phenylazanediyl)dibenzoic acid(H₂L) and 1,4-bis(pyridin-4-ylmethl)piperazine(bpmp) gave rise to a mixture of colorless sheet-like crystals {[CdL(bpmp)(H₂O)]·H₂O·DMF}_n(1) and yellowish bulk crystals {[Cd₂L₂(bpmp)₂]·3H₂O·2DMF}_n(2), which were mechanically separated. Both compounds were structurally determined by single-crystal X-ray diffraction. Compounds 1 and 2 were also characterized by FTIR spectroscopy, elemental analyses, thermal analysis, and powder X-ray diffraction(PXRD). Compound 1 exhibits a 4-fold interpenetrating 3D framework with a {6⁵·8} topology. Compound 2 consists of 1D [Cd₂L₂]_n helical chains linked by bpmp ligands to form a 2D network with a {3⁶·4⁶·5³} topology.

Key words: 4,4'-(Phenylazanediyl)dibenzoic acid, 1,4-Bis(pyridin-4-ylmethl)piperazine, Metal-organic framework, Solvothermal synthesis

CLC Number:

O614.24

TrendMD:

ZHAO Lun, ZHANG Min, SUN Erjun, WANG Xiaofeng, WANG Zichen. Synthesis, Structures and Photochemical Properties of Two New Cd(II) Metal-organic Frameworks Isolated from the Same Reaction System^†[J]. Chem. J. Chinese Universities, 2015, 36(12): 2380.

Figures/Tables 7

Table 1 Crystal data and structure refinement of compounds 1 and 2

Compound	1	2	β/(°)	99.502	80.4340(10)
CCDC No.	1405252	1405253	γ/(°)	90.00	87.1420(10)
Molecular formula	C₃₉H₃₈CdN₆O₇	C₇₈H₇₈Cd₂N₁₂O₁₃	V/nm³	3.9333(3)	3.9015(4)
F_w	815.17	1616.32	Z	4	2
Crystal system	Monoclinic	Triclinic	D_c/(g·cm^-3)	1.371	1.376
Space group	P2₁/c	P $1 ˉ$	F(000)	1600	1660
a/nm	1. 01080(5)	0.99134(6)	GOF on F²	1.047	1.048
b/nm	1.36695(7)	1. 49303(9)	R₁, wR₂[I>2σ(I)]	0.0456, 0.1173	0.0418, 0.1094
c/nm	2. 88626(14)	2. 67860(16)	R₁, wR₂(all data)	0.0915, 0.1564	0.0697, 0.1316
α/(°)	90.00	87.2570(10)

Table 1 Crystal data and structure refinement of compounds 1 and 2

Compound	1	2	β/(°)	99.502	80.4340(10)
CCDC No.	1405252	1405253	γ/(°)	90.00	87.1420(10)
Molecular formula	C₃₉H₃₈CdN₆O₇	C₇₈H₇₈Cd₂N₁₂O₁₃	V/nm³	3.9333(3)	3.9015(4)
F_w	815.17	1616.32	Z	4	2
Crystal system	Monoclinic	Triclinic	D_c/(g·cm^-3)	1.371	1.376
Space group	P2₁/c	P $1 ˉ$	F(000)	1600	1660
a/nm	1. 01080(5)	0.99134(6)	GOF on F²	1.047	1.048
b/nm	1.36695(7)	1. 49303(9)	R₁, wR₂[I>2σ(I)]	0.0456, 0.1173	0.0418, 0.1094
c/nm	2. 88626(14)	2. 67860(16)	R₁, wR₂(all data)	0.0915, 0.1564	0.0697, 0.1316
α/(°)	90.00	87.2570(10)

Fig.1 Coordination environment of the Cd(II) ions(A), views of 1D chain(B), 3D framework(C), { 65·8} topology net(D) and 4-fold interpenetrating architecture(E) in compound 1 Hydrogen atoms are omitted for clarity. Symmetry codes: #1: x, 0.5-y, z-0.5; #2: x-1, y+1, z; #3: x+1, y-1, z; #4: x, -y+0.5, z+0.5.

Fig.2 Coordination environment of the Cd(II) ions(A), views of 1D chain(B), 2D framework(C), {36·46·53} topology net(D) and helical chains(E) in compound 2 Hydrogen atoms are omitted for clarity. Symmetry codes: #1: x-1, y-1, z; #2: -x, - y-1, -z+1; #3: x+1, y+1, z; #4: -x+1, -y, -z+2, #5: -x-1, -y-2, -z+1; #6: -x+2, -y+1, -z +2; #7: -x+2, -y, -z+2.

Fig.3 Experimental(a) and simulated(b) PXRD patterns of compound 1(A) and compound 2(B)

Fig.4 TG curves of compounds 1(a) and 2(b)

Fig.5 Solid-state emission spectra of compounds and ligands at room temperature

Fig.6 Decay curves of compounds 1(A) and 2(B)

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