CLAIRE WILSON AND JUDITH A. K. HOWARD 547
Triclinic
PT
a = 7.0543 (7) ,A
o
b = 8.8125 (9) A
c = 15.016 (1) A
a = 72.980 (3) °
= 77.562 (3) °
7 = 69.707 (3) °
V 830.4(1) A 3
Z=2
Dx = 1.592 Mg m -3
D,, not measured
Data collection
Siemens SMART CCD
diffractometer
to rotation scans with narrow
frames
Absorption correction:
empirical via ~b scans
(SHELXTL; Sheldrick,
1994)
Train = 0.65, Tmax = 0.89
Refinement
Refinement on F 2
R[F 2 > 20.(F2)] = 0.039
wR(F 2) = 0.099
S - 1.118
2554 reflections
266 parameters
Only coordinates of H atoms
refined
w = 1/[0.2(F2) + (0.0414P) 2
+ 1.0763P]
where P = (F 2 + 2F~)/3
Cell parameters from 510
reflections
0 = 7.0-24.1 °
# = 0.711 mm -~
T = 150 (2) K
Rectangular
0.50 x 0.42 x 0.16 mm
Colourless
3487 measured reflections
2560 independent reflections
2429 reflections with
I > 20(/)
Rint = 0.032
0max = 25.14 °
h = - 8 ----~ 7
k= -10 ---~ 7
1 = - 17 ~ 17
(m/o')max -- 0.001
Apmax = 0.295 e ~-3
Apmin = -0.390 e ~-3
Extinction correction:
SHELXL
Extinction coefficient:
0.072 (5)
Scattering factors from
International Tables for
Crystallography (Vol. C)
References
Geich, H., Grimme, W. & Proske, K. (1992). J. Am. Chem. Soc. 114,
1492-1493.
Hagenbuch, J.-P., Stampfli, B. & Vogel, P. (1981). J. Am. Chem. Sac.
103, 3934-3935.
Mackenzie, K., Howard, J. A. K., Mason, S. A., Gravett, E. C., Astin,
K. B., Shi-Xiong, L., Batsanov, A. B., Vlaovic, D., Maher, J. P.,
Murray, M., Kendrew, D., Wilson, C., Johnson, R. E., PreiB, T. &
Gregory, R. J. (1993). J. Chem. Sac. Perkin Trans. 2, pp. 1211-
1228.
Mackenzie, K., Howard, J. A. K., Siedlecka, R., Astin, K. B., Gravett,
E. C., Wilson, C., Cole, J., Gregory, R. G. & Tomlins, A. S. (1996).
J. Chem. Soc. Perkin Trans. 2, pp. 1749-1760.
Mackenzie, K., Proctor, G. & Woodnutt, D. J. (1987). Tetrahedron,
43, 5981-5993.
Molecular Structure Corporation (1991). MSCIAFC Diffractometer
Control Software. MSC, 3200 Research Forest Drive, The Wood-
lands, TX 77381, USA.
Molecular Structure Corporation (1992). TEXSAN. TEXRAY Structure
Analysis Package. MSC, 3200 Research Forest Drive, The Wood-
lands, TX 77381, USA.
O'Doherty, G. A., Rogers, R. D. & Paquette, L. A. (1994). J. Am.
Chem. Soc. 116, 10883-10894.
Paquette, L. A., Kesselmayer, M. A. & Rogers, R. D. (1990). J. Am.
Chem. Soc. 112, 284-291.
Paquette, L. A., O'Doherty, G. A. & Rogers, R. D. (1991). J. Am.
Chem. Soc. 113, 7761-7762.
Sheldrick, G. M. (1994). SHELXTL. Structure Determination Pro-
grams. Version 5.03. Siemens Analytical X-ray Instruments Inc.,
Madison, Wisconsin, USA.
Siemens (1995). SMART and SAINT. Area Detector Control and
Integration Software. Siemens Analytical X-ray Instruments Inc.,
Madison, Wisconsin, USA.
Wilson, C. (1995). PhD thesis, University of Durham, England.
Table 2. Selected bond lengths (,~)for (2D)
c2--c7 1.395 (3) Cl2--Cll 1.530 (4)
Data collection: MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1991) for (1D); SMART
(Siemens, 1995) for (2D). Cell refinement: TEXSAN (Molec-
ular Structure Corporation, 1992) for (1D); SMART for (2D).
Data reduction: TEXSAN for (1D); SA/NT (Siemens, 1995) for
(2D). For both compounds, program(s) used to solve struc-
tures: SHELXTL (Sheldrick, 1994); program(s) used to refine
structures: SHELXTL; molecular graphics: SHELXTL; software
used to prepare material for publication: SHELXTL.
We thank Dr K. Mackenzie who conceived the
research programme, executed preparative and kinetic
work, and provided excellent quality crystals. Dr R.
Siedlecka is thanked for the preparation of compound
(2D). CW thanks the Institut Laue-Langevin for a
studentship.
Supplementary data for this paper are available from the IUCr
electronic archives (Reference: CF1209). Services for accessing these
data are described at the back of the journal.
Acta Cryst. (1998). C54, 547-550
Two New Structures of 5-Nitrouracil
ALAN R. KENNEDY, /~AURICE O. OKOTH,t DAVID B.
SHEEN, JOHN N. SHERWOOD AND RANKO M. VRCELJ
Department of Pure and Applied Chemistry, University
of Strathclyde, Glasgow G1 1XL Scotland. E-mail:
a. r. kennedy @ ccsun, strath, ac. uk
(Received 17 July 1997; accepted 12 November 1997)
Abstract
The structure of monoclinic anhydrous 5-nitrouracil,
C4H3N304, and of the solvate 5-nitrouracil dimethyl
sulfoxide, C4H3N304.C2H6OS, are presented and com-
pared with the previously known structures of the
orthorhombic anhydrous form and the monohydrate.
f Present address: Department of Chemistry, Moi University, PO Box
1125, Eldoret, Kenya.
© 1998 Intemational Union of Crystallography
Printed in Great Britain - all fights reserved
Acta Crystallographica Section C
ISSN 0108-2701 ©1998