Z. Kristallogr. NCS 224 (2009) 563-564 / DOI 10.1524/ncrs.2009.0246
563
© by Oldenbourg Wissenschaftsverlag, München
Crystal structure of diaqua-(2,4-dinitroimidazolato)strontium(II),
Sr(H2O)2(C3HN4O4)
Fa-You TangI, Mei-Yu CaiI and Ping Li*,I,II
I
II
Shaanxi Normal University, School of Chemistry and Materials Science, Xi’an, 710062, P. R. China
Jining Teachers College, Department of Chemistry, Wulanchabu, Inner Mongolia, 012000, P. R. China
Received July 12, 2009, accepted and available on-line September 8, 2009; CCDC no. 1267/2713
Abstract
C6H10N8O12Sr, monoclinic, C12/c1 (no. 15), a = 16.778(6) Å,
b = 6.395(2) Å, c = 15.241(5) Å, * = 110.879(3)°,
V = 1527.9 Å3, Z = 4, Rgt(F) = 0.024, wRref(F2) = 0.059,
T = 296 K.
Source of material
40 ml aqueous mixture containing 2,4-dinitroimidazolate (2,4DNI, 0.47.g) was stirred 10 minuates at 50 °C. Then 0.236.g strontium hydroxide (Sr(OH)2.·.8H2O) was added and reaction continue for 1 hour. The solution was refluxed for 3 hours at 120 °C.
After filtration, the filtrate was evaporated to dryness, and
recrystallized with ethanol. After one week yellow block-like
crystals were collected and washed by distilled water (yield,
61.6.%, m.p. 290 °C). Elemental analysis — found: C, 15.41 %;
H, 2.16 %; N, 23.81 %; calculated for C6H10N8O12Sr: C, 15.20 %;
H, 2.11 %; N, 23.64 %. IR data are available in the CIF.
Discussion
In modern ordnance, there is a need to have an explosive molecule, which is highly stable to thermal heating, substantially insensitive to impact, and highly powerful upon explosion. Many
kinds of sensitivities such as heat, friction, impact, shock and
electrostatic charges have been identified in terms of nature of
stimuli causing detonation. High-energy (HE) materials have
been shown to have several well-established characteristics:
strained rings and cages, high nitrogen content, and high density.
The search of energetic materials is best carried out presently using thermodynamics and molecular engineering approaches.
Polynitro compounds have long been the focal point for energetic
potential. Stability of polynitro compounds is necessary to avoid
undesirable decomposition. The presence of nitro groups tends to
decrease heat of formation, but contributes markedly to the overall energetic performance. However, to the best of our knowledge, the literature contains a few report on nitroimi- dazole
compounds. We have reported the nitropyridino group as a part of
ligand coordinating the metal and organic cation [1,2]. This work
presents a new polynitro compound expected be applied in explosives and propellants.
The crystal structure of the title compound is composed of (2,4dinitroimidazolate anion, Sr2+ cations and water molecules. The
metal cation is ten-coordinated with four oxygen atoms from nitro groups, two N ligands from imidazole and other four oxygen
atoms from water. The Sr—N bond distance is 2.741(2) Å, and
the Sr—O bond lengths vary from 2.629(2) Å to 3.249(2) Å. The
four ligands around the metal cation in (010) nearly be coplanar,
whereas the angles O5–Sr1–N1 and O6–Sr1–N1 are 76.87(6)°
and 79.40(6)°, respectively. In the crystal structure, O–H bonds
of the coordination water are connected by hydrogen bond, and
the hydrogen bonds distances are in the reasonable range.
Table 1. Data collection and handling.
Crystal:
Wavelength:
.:
Diffractometer, scan mode:
2,max:
N(hkl)measured, N(hkl)unique:
Criterion for Iobs, N(hkl)gt:
N(param)refined:
Programs:
yellow block, size 0.25 × 0.32 × 0.37 mm
Mo K+ radiation (0.71073 Å)
36.19 cm−1
Bruker SMART CCD, #/%
50.98°
5529, 1416
Iobs > 2 )(Iobs), 1326
123
SHELX-90 [4], SHELXS-97 [5],
SHELXL-97 [6], SHELXTL [7]
Table 2. Atomic coordinates and displacement parameters (in Å2).
Atom
Site
x
y
H(1W)
H(2W)
H(3W)
H(4W)
H(2)
8f
8f
8f
8f
8f
0.3857
0.3981
0.5521
0.5006
0.2859
−0.0144
−0.0478
0.6482
0.7511
0.5512
z
Uiso
0.1061
0.1986
0.1187
0.1568
0.2449
0.044
0.044
0.050
0.050
0.030
_____________
* Correspondence author (e-mail: [email protected])
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564
Sr(H2O)2(C3HN4O4)
Table 3. Atomic coordinates and displacement parameters (in Å2).
Atom
Site
x
Sr(1)
O(1)
O(2)
O(3)
O(4)
O(5)
O(6)
N(1)
N(2)
N(3)
N(4)
C(1)
C(2)
C(3)
4e
8f
8f
8f
8f
8f
8f
8f
8f
8f
8f
8f
8f
8f
½
0.4128(1)
0.2980(1)
0.1175(1)
0.0657(1)
0.4205(1)
0.5365(1)
0.3393(1)
0.2146(1)
0.3382(1)
0.1238(1)
0.2961(1)
0.2786(2)
0.2040(1)
y
0.33374(4)
0.3654(3)
0.4447(3)
0.6631(3)
0.6662(3)
−0.0124(3)
0.6572(3)
0.4746(3)
0.5294(3)
0.4252(3)
0.6340(3)
0.4766(3)
0.5341(4)
0.5647(4)
z
¼
0.0229(2)
−0.0940(1)
0.1852(1)
0.0334(2)
0.1607(1)
0.1647(1)
0.1479(1)
0.0235(1)
−0.0098(1)
0.1072(2)
0.0548(2)
0.1819(2)
0.1064(2)
U11
U22
U33
U12
0.0121(2)
0.024(1)
0.049(1)
0.035(1)
0.023(1)
0.030(1)
0.033(1)
0.017(1)
0.016(1)
0.025(1)
0.020(1)
0.018(1)
0.021(1)
0.017(1)
0.0198(2)
0.043(1)
0.043(1)
0.046(1)
0.086(2)
0.036(1)
0.038(1)
0.034(1)
0.020(1)
0.020(1)
0.024(1)
0.018(1)
0.037(1)
0.020(1)
0.0226(2)
0.056(1)
0.022(1)
0.037(1)
0.038(1)
0.0202(9)
0.031(1)
0.017(1)
0.0182(9)
0.031(1)
0.030(1)
0.020(1)
0.016(1)
0.022(1)
0
0.0050(8)
0.0000(9)
0.0049(9)
0.023(1)
−0.0009(8)
0.0074(8)
0.0048(8)
0.0017(8)
−0.0011(8)
0.0015(8)
0.0003(9)
0.005(1)
0.0013(9)
U13
0.0062(1)
0.023(1)
0.0191(9)
0.0241(9)
0.0041(9)
0.0046(7)
0.0133(8)
0.0029(8)
0.0060(8)
0.0165(9)
0.0114(9)
0.0083(9)
0.006(1)
0.0095(9)
U23
0
−0.0053(9)
−0.0012(8)
−0.0051(9)
0.004(1)
−0.0029(7)
0.0089(8)
0.0004(8)
−0.0004(7)
−0.0024(9)
−0.0011(8)
−0.0007(9)
−0.000(1)
−0.0010(9)
Acknowledgment. The authors acknowledge the scientific research projects
(NJ09204 and NJzy08217) of Higher Education of Inner Mongolia.
References
1. Tang, F. Y.; She, J. B.; Li, J. Z.; Zhang, G. F.; Zahn, G.: Crystal structure of
4 -o x o -3 , 5 -d i n i t rop y r i d i n e - N - h y d r o x i d e
m o nohydr a t e ,
C5NH2(NO2)2O(OH) · H2O. Z. Kristallogr. NCS 221 (2006) 539-540.
2. Bracuti, A. J.: Crystal structure of 2,4-dinitroimidazole (24DNI). J. Chem.
Crystallogr. 25 (1995) 625-627.
3. Zhou, Q. P.; Zhang, G. F.; She, J. B.: Syntheses, crystal structures and
thermoanalyses of alkaline earth metal complexes derived from dinitropyridone. J. Coord. Chem. 61 (2008) 2601-2614.
4. Sheldrick, G. M.: Phase Annealing in SHELX-90: Direct Methods for
Larger Structures. Acta Crystallogr. A46 (1990) 467-473.
5. Sheldrick, G. M.: SHELXS-97. Program for the Solution of Crystal Structures. University of Göttingen, Germany 1997.
6. Sheldrick, G. M.: SHELXL-97. Program for the Refinement of Crystal
Structures. University of Göttingen, Germany 1997.
7. Sheldrick, G. M.: SHELXTL. Structure Determination Software Suite.
Version 6.14. Bruker AXS, Madison, Wisconsin, USA 2000.
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