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Volumn 46, Issue 19, 2007, Pages 7698-7700

Two new copper azido polymorphs: Structures, magnetic properties, and effects of "noninnocent" reagents in hydrothermal methods

(7) Liu, Fu Chen a Zeng, Yong Fei a Zhao, Jiong Peng a Hu, Bo Wen a Sañudo, E Carolina b Ribas, Joan b Bu, Xian He a

a NANKAI UNIVERSITY (China)

b UNIVERSITY OF BARCELONA (Spain)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 34948905224 PISSN: 00201669 EISSN: None Source Type: Journal
DOI: 10.1021/ic700669c Document Type: Article

Times cited : (60)

References (39)

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- Synthesis of 1. 1 was hydrothermally synthesized under autogenous pressure. A mixture of Cu(NO3)2·6H 2O, NaN3, Hnic, MoO3, and H2O at a ratio of 1:1:1:1:2000 was sealed in a Teflon-lined autoclave, heated to 140°C for 2 days, and cooled to room temperature at 10°C h-1. The black crystals of 1 were obtained in ca. 10% yield based on copper from an unknown powder and solution. Selected IR (KBr, cm-1, 2085, 1603, 1550, 1407. Anal. Calcd for C6H4N 4CuO2 227.41, C, 31.7; H, 1.8; N, 24.6. Found: C, 31.3; H. 1.9; N, 24.1
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35
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- Synthesis of 2. 2 was hydrothermally synthesized under autogenous pressure. A mixture of Cu(NO3)2·6H 2O, NaN3, Hnic, Gd(NO3)3· 6H2O, en, and H2O at a ratio of 1:1:1:1:1:2000 was sealed in a Teflon-lined autoclave, heated to 140°C for 2 days, and cooled to room temperature at 10°C h-1. The black crystals of 2 were obtained in ca. 20% yield based on copper from the reaction solution. Anal. Calcd for C6H4N4CuO2 227.41, C, 31.7; H, 1.8; N, 24.6. Found: C 31.2; H, 1.5: N, 24.3. Caution! Azide complexes are potentially explosive. Only a small amount of the materials should be prepared and handled with care
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36
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- Crystal data for 1: C6H4CuN 4O2, M, 227.41, monoclinic, P21/c, a, 4.8720(14) Å, b, 14.347(4) Å, c, 11.655(3) Å, β, 114.70-(9)°, V, 740.1(4) Å3, Z, 4, Dc, 2.043 Mg m-3, μ, 2.916 mm-1, 1456 [R(int, 0.0187] reflections, of which 118 were assumed as observed [I > 2σ(I, Final R1, 0.0232, wR1, 0.0612 [I > 2σ(I, CCDC 613080, b) Crystal data for 2: C6H4CuN4O2, M, 227.67, orthorhombic, P2(1)2(1)2(1, a, 6.4068(15) Å, b, 9.701(2) Å, c, 12.398(3) Å, V, 770.5(3) Å3, Z, 4, Dc, 1.963 Mg m -3, μ, 2.801 mm-1, 4196 [Rint, 0.0203] reflections, of which 1575
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