(NH 4) 2(C 4O 4), an anhydrous salt of acetylenedicarboxylic acid
Single crystals of anhydrous ammonium acetylenedicarboxylate ((NH 4) 2(C 4O 4), 1) were isolated from a precipitate crystallizing from an aqueous ammonia solution containing acetylenedicarboxylic acid. The crystal structure of 1 ( C 2 / m , Z = 2 ) consists of ordered ammonium cations, which are con...
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| Published in | Solid state sciences Vol. 8; no. 3; pp. 353 - 358 |
|---|---|
| Main Authors | , , |
| Format | Journal Article |
| Language | English |
| Published |
Paris
Elsevier Masson SAS
01.03.2006
Elsevier |
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| Abstract | Single crystals of anhydrous ammonium acetylenedicarboxylate ((NH
4)
2(C
4O
4),
1) were isolated from a precipitate crystallizing from an aqueous ammonia solution containing acetylenedicarboxylic acid. The crystal structure of
1 (
C
2
/
m
,
Z
=
2
) consists of ordered ammonium cations, which are connected via N
H⋯O hydrogen bonds (N
O: 2.826 and 2.947 Å) to four oxygen atoms from four symmetry related acetylenedicarboxylates. The coordination by the bifunctional carboxylates leads to a three-dimensional framework structure. Coupled TGA/DTA/MS measurements show that
1 decomposes completely at about 450 K releasing NH
3, CO
2, and C
2H
2. No order–disorder transition occurs in the temperature range between 20 K and the decomposition temperature. In contrast to Sr(C
4O
4), the other known anhydrous acetylenedicarboxylate, no negative thermal expansion is found below room temperature. |
|---|---|
| AbstractList | Single crystals of anhydrous ammonium acetylenedicarboxylate ((NH
4)
2(C
4O
4),
1) were isolated from a precipitate crystallizing from an aqueous ammonia solution containing acetylenedicarboxylic acid. The crystal structure of
1 (
C
2
/
m
,
Z
=
2
) consists of ordered ammonium cations, which are connected via N
H⋯O hydrogen bonds (N
O: 2.826 and 2.947 Å) to four oxygen atoms from four symmetry related acetylenedicarboxylates. The coordination by the bifunctional carboxylates leads to a three-dimensional framework structure. Coupled TGA/DTA/MS measurements show that
1 decomposes completely at about 450 K releasing NH
3, CO
2, and C
2H
2. No order–disorder transition occurs in the temperature range between 20 K and the decomposition temperature. In contrast to Sr(C
4O
4), the other known anhydrous acetylenedicarboxylate, no negative thermal expansion is found below room temperature. Single crystals of anhydrous ammonium acetylenedicarboxylate ((NH4)2(C4O4), 1) were isolated from a precipitate crystallizing from an aqueous ammonia solution containing acetylenedicarboxylic acid. The crystal structure of 1 (C2/m, Z=2) consists of ordered ammonium cations, which are connected via NHO hydrogen bonds (NO: 2.826 and 2.947 A) to four oxygen atoms from four symmetry related acetylenedicarboxylates. The coordination by the bifunctional carboxylates leads to a three-dimensional framework structure. Coupled TGA/DTA/MS measurements show that 1 decomposes completely at about 450 K releasing NH3, CO2, and C2H2. No order-disorder transition occurs in the temperature range between 20 K and the decomposition temperature. In contrast to Sr(C4O4), the other known anhydrous acetylenedicarboxylate, no negative thermal expansion is found below room temperature. |
| Author | Ruschewitz, Uwe Näther, Christian Stein, Irena |
| Author_xml | – sequence: 1 givenname: Irena surname: Stein fullname: Stein, Irena email: steini@uni-koeln.de organization: Institut für Anorganische Chemie, Universität zu Köln, Greinstraße 6, D-50939 Köln, Germany – sequence: 2 givenname: Christian surname: Näther fullname: Näther, Christian email: cnaether@ac.uni-kiel.de organization: Institut für Anorganische Chemie, Christian-Albrechts-Universität zu Kiel, Olshausenstraße 40, D-24098 Kiel, Germany – sequence: 3 givenname: Uwe surname: Ruschewitz fullname: Ruschewitz, Uwe email: uwe.ruschewitz@uni-koeln.de organization: Institut für Anorganische Chemie, Universität zu Köln, Greinstraße 6, D-50939 Köln, Germany |
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| CitedBy_id | crossref_primary_10_1002_zaac_200900011 crossref_primary_10_1002_zaac_200700133 crossref_primary_10_1002_ange_202011006 crossref_primary_10_1002_zaac_201200006 crossref_primary_10_1002_anie_202011006 crossref_primary_10_1002_ejic_202100965 crossref_primary_10_1002_zaac_200900368 crossref_primary_10_1021_ic1009829 crossref_primary_10_1002_zaac_200900428 crossref_primary_10_1016_j_solidstatesciences_2009_03_008 crossref_primary_10_1016_j_solidstatesciences_2011_01_012 crossref_primary_10_1002_zaac_201000019 |
| Cites_doi | 10.1038/35010088 10.1002/anie.200462786 10.1039/a904297k 10.1524/zkri.220.2.250.59143 10.1107/S0108270199008458 10.1038/nature01650 10.1107/S0567740868002840 10.1002/zaac.19915960120 10.1021/cr9900432 10.1126/science.1067208 10.1021/ic0487373 10.1515/znb-1990-1106 10.1016/S0022-4596(05)80265-8 10.1515/znb-2004-0806 10.1002/1521-3765(20021004)8:19<4536::AID-CHEM4536>3.0.CO;2-I 10.1021/ar0001012 10.1002/ange.200462786 10.1107/S0021889899006020 10.1006/jssc.2000.8723 |
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| Issue | 3 |
| Keywords | Ammonium salts Thermal analysis Acetylenedicarboxylates Coordination polymer Crystal structure Temperature dependence Thermal decomposition Thermogravimetry Mass spectroscopy Differential thermal analysis Carboxylic acids XRD Experimental study Acetylene Monocrystals Anhydrous compound Aqueous solutions Morphology Organic salt Thermal expansion coefficient Organic compounds |
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| Snippet | Single crystals of anhydrous ammonium acetylenedicarboxylate ((NH
4)
2(C
4O
4),
1) were isolated from a precipitate crystallizing from an aqueous ammonia... Single crystals of anhydrous ammonium acetylenedicarboxylate ((NH4)2(C4O4), 1) were isolated from a precipitate crystallizing from an aqueous ammonia solution... |
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| SubjectTerms | Acetylenedicarboxylates Aliphatic, non-condensed and condensed benzenic, and alicyclic compounds Ammonium salts Condensed matter: structure, mechanical and thermal properties Coordination polymer Crystal structure Exact sciences and technology Organic compounds Physics Structure of solids and liquids; crystallography Structure of specific crystalline solids Thermal analysis Thermal expansion; thermomechanical effects Thermal expansion; thermomechanical effects and density Thermal properties of condensed matter Thermal properties of crystalline solids |
| Title | (NH 4) 2(C 4O 4), an anhydrous salt of acetylenedicarboxylic acid |
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