Poly[[μ(4)-naphthalene-1,4-dicarboxyl-ato-κO:O':O'':O'''-μ(2)-naphthalene-1,4-dicarboxyl-ato-κO,O':O'',O'''-bis-(2-phenyl-1H-1,3,7,8-tetra-azacyclopenta-[l]phenanthrene-κN,N)dimanganese(II)] N,N-dimethyl-formamide solvate].
ABSTRACT One of the two 1,4-dicarboxyl-ate dianions in the title compound, [Mn(2)(C(12)H(6)O(4))(2)(C(19)H(12)N(4))(2)]·C(3)H(7)NO, uses its two carboxyl-ate groups to chelate two N-heterocycle-chelated Mn atoms; the other 1,4-dicarboxyl-ate dianion binds to four such metal centers. The octa-hedrally coordinated Mn atoms are linked through the two dianions into a layer motif; the dimethyl-formamide mol-ecules occupy the spaces between adjacent layers. Ten C atoms and attached H atoms of one dianion are disordered equally over two positions.
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Article: A short history of SHELX.[show abstract] [hide abstract]
ABSTRACT: An account is given of the development of the SHELX system of computer programs from SHELX-76 to the present day. In addition to identifying useful innovations that have come into general use through their implementation in SHELX, a critical analysis is presented of the less-successful features, missed opportunities and desirable improvements for future releases of the software. An attempt is made to understand how a program originally designed for photographic intensity data, punched cards and computers over 10000 times slower than an average modern personal computer has managed to survive for so long. SHELXL is the most widely used program for small-molecule refinement and SHELXS and SHELXD are often employed for structure solution despite the availability of objectively superior programs. SHELXL also finds a niche for the refinement of macromolecules against high-resolution or twinned data; SHELXPRO acts as an interface for macromolecular applications. SHELXC, SHELXD and SHELXE are proving useful for the experimental phasing of macromolecules, especially because they are fast and robust and so are often employed in pipelines for high-throughput phasing. This paper could serve as a general literature citation when one or more of the open-source SHELX programs (and the Bruker AXS version SHELXTL) are employed in the course of a crystal-structure determination.Acta Crystallographica Section A Foundations of Crystallography 02/2008; 64(Pt 1):112-22. · 2.24 Impact Factor
j4O:O0 0 0:O0 0 00 0 0:O0 0 00 0 00 0 0-l2-naphthalene-1,4-
dicarboxylato-j4O,O0 0 0:O0 0 00 0 0,O0 0 00 0 00 0 0-bis(2-
Heng-Da Li,aYang Liu,aMao-Liang Xuband Seik Weng
aDepartment of Chemistry, Jilin Normal University, Siping 136000, People’s
Republic of China,bXi’an Modern Chemistry Research Institute, Xi’an 710065,
People’s Republic of China, andcDepartment of Chemistry, University of Malaya,
50603 Kuala Lumpur, Malaysia
Correspondence e-mail: firstname.lastname@example.org
Received 16 January 2008; accepted 18 April 2008
Key indicators: single-crystal X-ray study; T = 295 K; mean ?(C–C) = 0.011 A ˚;
disorder in main residue; R factor = 0.081; wR factor = 0.262; data-to-parameter
ratio = 11.7.
One of the two 1,4-dicarboxylate dianions in the title
compound, [Mn2(C12H6O4)2(C19H12N4)2]?C3H7NO, uses its
two carboxylate groups to chelate two N-heterocycle-chelated
Mn atoms; the other 1,4-dicarboxylate dianion binds to four
such metal centers. The octahedrally coordinated Mn atoms
are linked through the two dianions into a layer motif; the
dimethylformamide molecules occupy the spaces between
adjacent layers. Ten C atoms and attached H atoms of one
dianion are disordered equally over two positions.
There are several studies of 2-phenyl-1H-1,3,7,8-tetraaza-
cyclopenta[l]phenanthrene-chelated metal compounds; for
the structures of the manganese dicarboxylate adducts, see:
Che (2006); Che & Liu (2006); Wang et al. (2006); Zhang et al.
a = 9.240 (2) A˚
b = 14.852 (5) A˚
c = 21.921 (5) A˚
? = 105.72 (1)?
? = 100.48 (1)?
? = 101.67 (1)?
V = 2745.0 (13) A˚3
Z = 2
Mo K? radiation
? = 0.53 mm?1
T = 295 (2) K
0.26 ? 0.16 ? 0.12 mm
Rigaku R-AXIS RAPID
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
Tmin= 0.760, Tmax= 0.940
21501 measured reflections
9443 independent reflections
4800 reflections with I > 2?(I)
R[F2> 2?(F2)] = 0.080
wR(F2) = 0.262
S = 1.06
H-atom parameters constrained
??max= 1.74 e A˚?3
??min= ?0.48 e A˚?3
Selected bond lengths (A˚).
Symmetry codes: (i) x;y þ 1;z; (ii) x þ 1;y þ 1;z; (iii) x þ 1;y;z.
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement:
RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC,
2002); program(s) used to solve structure: SHELXS97 (Sheldrick,
2008); program(s) used to refine structure: SHELXL97 (Sheldrick,
2008); molecular graphics: X-SEED (Barbour, 2001) and OLEX
(Dolomanov et al., 2003); software used to prepare material for
publication: publCIF (Westrip, 2008).
We thank the Natural Science Foundation of Jilin Province
(No. 20060516), the Doctoral Foundation of Jilin Normal
University (No. 2006006), the Science and Technology Insti-
tute Foundation of Siping City (No. 2005016), the Subject and
Li et al.
Acta Cryst. (2008). E64, m704–m705
Acta Crystallographica Section E
Base Construction Foundation of Jilin Normal University (No.
2006041), and the University of Malaya for supporting this
Supplementary data and figures for this paper are available from the
IUCr electronic archives (Reference: RZ2195).
Barbour, L. J. (2001). J. Supramol. Chem. 1, 189–191.
Che, G.-B. (2006). Acta Cryst. E62, m1244–m1246.
Che, G.-B. & Liu, C.-B. (2006). Acta Cryst. E62, m1453–m1455.
Dolomanov, O. V., Blake, A. J., Champness, N. R. & Schro ¨der, M. (2003). J.
Appl. Cryst. 36, 1283–1284.
Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
Rigaku (1998). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.
Rigaku/MSC (2002). CrystalStructure. Rigaku/MSC, The Woodlands, Texas,
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.
Wang, L., Che, G.-B. & Liu, C.-B. (2006). Acta Cryst. E62, m2406–m2408.
Westrip, S. P. (2008). publCIF. In preparation.
Zhang, S.-C., Sun, J., Yu, Z.-X. & Zhao, X.-H. (2006). Acta Cryst. E62, m2893–
Acta Cryst. (2008). E64, m704–m705Li et al.
Acta Cryst. (2008). E64, m704-m705 [ doi:10.1107/S1600536808010787 ]
Poly[[ 4-naphthalene-1,4-dicarboxylato-4O:O':O'':O'''- 2-naphthalene-1,4-dicarboxylato-
2N7,N8)dimanganese(II)] N,N-dimethylformamide solvate]
H.-D. Li, Y. Liu, M.-L. Xu and S. W. Ng
There are several studies of metal complexes of 2-phenyl-1H-1,3,7,8-tetraazacyclopenta[l]phenanthrene. Among these are
several manganese complexes, the manganese succinate (Zhang et al., 2006), manganese adipate (Wang et al., 2006), man-
ganese isophthalate (Che & Liu, 2006) and manganese terephthalate (Che, 2006) adducts, all of which feature carboxylate-
bridged chain motifs. The title naphthalene-1,4-dicarboxylate adduct adopts a layer motif instead.
One of the two 1,4-dicarboxylate dianions in Mn2(C19H12N4)2(C12H6O4)2.DMF uses its two carboxyl –CO2 groups
to chelate to two N-heterocycle-chelated manganese atoms; the other 1,4-dicarboxylate dianion binds to four such metal
centers. The octahedrally coordinated manganese atoms are linked through the two dianions into a layer motif; the DMF
molecules occupy the spaces between adjacent layers.
Manganese dichloride dihydrate (0.1 mmol), naphthalene-1,4-dicarboxylic acid (0.1 mmol), 2-phenyl-1H-1,3,7,8-
tetraazacyclopenta[l]phenanthrene (0.1 mmol), water (8 ml) and DMF (4 ml) were heated in a 23 ml, Teflon-lined, stain-
less-steel Parr bomb at 408 K for 2 days. Crystals were obtained in 40% yield.
The naphthalene-1,4-dicarboxylate dianion that is involved in µ4-bridging is disordered over two positions in the fused-ring
portion. This was refined as two rigid naphthalene groups of 1.39 Å sides; the occupancy was arbitrarily set as 0.5 as this
could not be refined. The C1–C11 and C1'–C11 distances were restrained to within 0.01 Å of each other, as were the C4–C12
and C4'–C12 pair of distances. The anisotropic displacement factors of the two fused-rings were restrained to be nearly
The carbon-bound H atoms were placed in calculated positions [C–H 0.93, N–H 0.86 Å and Uiso(H) 1.2Ueq(C,N)], and
were included in the refinement in the riding-model approximation.
The final difference Fourier map had a large peak at 2.8 Å from O7, but this could not be modeled as a water molecule.
Fig. 1. Thermal ellipsoid plot of Mn2(C19H12N4)2(C12H6O4)2.DMF; displacement ellipsoids
are drawn at the 50% probability level, and H atoms as spheres of arbitrary radius. The dis-
order in one of the naphthalene-1,4-dicarboxylate dianions is not shown. Symmetry codes are
given in Table 1.
Fig. 2. Layer structure of the manganese-naphthalene-1,4-dicarboxylate network as illustrated
by OLEX (Dolomanov et al., 2003).
Poly[[µ4-naphthalene-1,4-dicarboxylato- κ4O:O':O'':O'''- µ2-naphthalene-1,4-dicarboxylato- κ4O,O':O'',O'''-
bis(2-phenyl-1H-1,3,7,8-tetraazacyclopenta[l]phenanthrene- κ2N7,N8)dimanganese(II)] N,N-dimethylformam-
Mr = 1203.96
Z = 2
F000 = 1236
Dx = 1.457 Mg m−3
Mo Kα radiation
λ = 0.71073 Å
Cell parameters from 15789 reflections
θ = 3.0–27.5º
µ = 0.53 mm−1
T = 295 (2) K
0.26 × 0.16 × 0.12 mm
Hall symbol: -P 1
a = 9.240 (2) Å
b = 14.852 (5) Å
c = 21.921 (5) Å
α = 105.72 (1)º
β = 100.48 (1)º
γ = 101.67 (1)º
V = 2745.0 (13) Å3
Rigaku R-AXIS RAPID
Radiation source: fine-focus sealed tube
Detector resolution: 10 pixels mm-1
T = 295(2) K
Absorption correction: Multi-scan
(ABSCOR; Higashi, 1995)
9443 independent reflections
4800 reflections with I > 2σ(I)
Rint = 0.084
θmax = 25.0º
θmin = 3.0º
h = −10→10
k = −17→17