Unique 3D self-penetrating CoII and NiII coordination frameworks with a new (44.610.8) network topology

Article abstract of DOI:10.1039/c0dt00900h

Two unique six-connected self-penetrating coordination polymers with a new (4⁴.6¹⁰.8) network topology, derived from the cross-linking of two 6⁶-dia subnets, were constructed from Ni ^II or Co^II and two types of V-shaped tectons. The Ni ^II complex 1 shows an antiferromagnetic coupling via μ-carboxylate and μ-H₂O pathways, whereas the Co^II complex 2 exhibits the single-ion behavior in 300-34 K and then a ferromagnetic coupling at lower temperatures. The Royal Society of Chemistry 2010.

Full text of DOI:10.1039/c0dt00900h

View Article Online / Journal Homepage / Table of Contents for this issue
COMMUNICATION
www.rsc.org/dalton | Dalton Transactions
Unique 3D self-penetrating CoII and NiII coordination frameworks with a new
(44.610.8) network topology†
Dong-Sheng Li,*a,c Feng Fu,a Jun Zhao,a Ya-Pan Wu,a,c Miao Du,*b Kun Zou,a Wen-Wen Donga,c and
Yao-Yu Wang*c
Received 23rd July 2010, Accepted 5th October 2010
DOI: 10.1039/c0dt00900h
Two unique six-connected self-penetrating coordination
polymers with a new (44.610.8) network topology, derived
from the cross-linking of two 66-dia subnets, were constructed
from NiII or CoII and two types of V-shaped tectons. The
NiII complex 1 shows an antiferromagnetic coupling via l-
carboxylate and l-H2O pathways, whereas the CoII complex
2 exhibits the single-ion behavior in 300–34 K and then a
ferromagnetic coupling at lower temperatures.
most relevance, and numerous such network topologies have been
known.3,4 However, examples for 6-connected self-penetrating nets
are quite rare,7 implying a challenging issue because it is difficult
to predict such target materials prior to synthesis.
As present, a particularly promising approach for the creation
of self-penetrating topologies is to use metal clusters with suitable
geometry and connectivity as the net nodes in virtue of a rational
design of organic ligands.8 In this respect, V-shaped building
blocks can serve as excellent candidates to construct unusual en-
tangled frameworks due to their specific backbones, often flexible.9
Very recently, by using the V-shaped polycarboxylate tectons, we
have successfully obtained the first armed-polyrotaxane 1D array
based on loop chains with side arms, and a unique 3D 8-connected
self-penetrating coordination network based on hexanuclear PbII
clusters.10 As an extension of our work, we combine two types of V-
shaped building blocks, 4,4¢-sulfonyldibenzoic acid (H2sdba) and
4,4¢-dipyridyl-sulfide (dps), into one assembled system to afford
two coordination frameworks {[M(sdba)(dps)(H2O)0.5](H2O)1.2}n
(M = NiII for 1 and CoII for 2). Both complexes show the unique
3D (44.610.8) topological networks with a self-penetrating feature,
which consists of the “warp and weft” interwoven fabric motifs of
the helical subunits.
Since the highly influential books of Wells,1 the network topo-
logical approach, which is a powerful tool for constructing and
analyzing network structures, has received an increasing level of
attention.2 To date, network topologies in coordination polymers
have been discussed in several distinguished reviews,3 and abun-
dant examples, from uninodal networks with 3–12 connectivity,
to mix-connected networks including (3,4)-, (3,6)-, (4,6)- and
(4,8)-connected types, have been reported.4 Undoubtedly, these
significant results extend our understanding and open up new
opportunities for further developing such net-based solid-state
materials.
Meanwhile, particular attention has been devoted to entangled
systems for their undisputed beauty and potential applications as
molecular-based materials. As a result, a variety of novel entangled
systems, such as interpenetrating, polycatenating, polythreading,
and polyknotting, have been discovered thus far.5 Despite the
meaningful progress in this hotspot, there is an unfavorable lack
of systematic and characteristic researches on more sophisticated
entangled architectures, especially cases for the relatively unusual
self-penetrating (or polyknotting) structures. In contrast to in-
terpenetrating networks, self-penetrating nets, as the extended
equivalents of molecular knots, is still in its growing period.3c,6
On the other hand, nodes of 3-, 4-, and 6-connectivity are of
Complexes 1 and 2 were prepared by hydrothermal reaction
of NiII or CoII acetate, H2sdba, dps, and NaOH,11 which were
characterized by IR spectra, elemental analysis, PXRD, and TGA
techniques (see Fig. S1, ESI†).
Single-crystal X-ray analysis12 indicates that 1 and 2 are
isomorphous. Therefore, only the structure of 1 will be discussed as
a representative. The asymmetric unit of 1 contains one NiII center,
one sdba anion, one dps linker, half aqua ligand, and lattice water
molecules. Among them, the half aqua ligand has its oxygen atom
on a crystallographic two-fold axis, there are two lattice water
molecules which lie at special positions in the Fddd space group,
but for O2W water oxygen atom, its anisotropic displacement
parameters is very large. In order to give a better reasonable model,
we have tried many times and then gave a final occupancy of only
0.1 for it in the asymmetric unit, even though it is at a site involved
with three two-fold axes. Water O1W lies on a two-fold axis and
its occupancy was normal 0.5. As shown in Fig. 1(a), each NiII
ion takes a distorted octahedral geometry, which is provided by
three carboxylate oxygen atoms of two sdba2- ligands, two pyridyl
nitrogen donors of a pair of dps, and one aqua molecule. In this
structure, each dps and aqua play the bridging role to link the
NiII centers, and as for sdba2-, its two carboxylate groups display
the monodentate and m-O,O¢ coordination modes, respectively,
featuring a m3-linker. In this way, two adjacent NiII centers are
connected by a pair of carboxylate groups and one water bridge to
aCollege of Mechanical & Material Engineering, Hubei Key Laboratory of
Natural Products Research and Development, China Three Gorges Univer-
sity, Yichang, 443002, China. E-mail: lidongsheng1@126.com; Fax: +86-
717-6397516; Tel: +86-717-6397516
bCollege of Chemistry, Tianjin Key Laboratory of Structure and Performance
for Functional Molecule, Tianjin Normal University, Tianjin, 300387,
China. E-mail: dumiao@public.tpt.tj.cn; Fax: +86-22-23766556; Tel: +86-
22-23766556
cKey Laboratory of Synthetic and Natural Functional Molecule Chemistry
of Ministry of Education, Department of Chemistry, Northwest Univer-
sity, Xi’an, 710069, China. E-mail: wyaoyu@nwu.edu.cn; Fax: +86-29-
88303798; Tel: +86-29-88303798
† Electronic supplementary information (ESI) available: Additional ex-
perimental details, a table for bond parameters, structural illustrations,
PXRD patterns and TGA curves for complexes 1 and 2. CCDC reference
numbers 778541 and 778542. For ESI and crystallographic data in CIF or
other electronic format see DOI: 10.1039/c0dt00900h
˚
form a dimeric unit (the adjacent Ni ◊ ◊ ◊ Ni distance = 3.510 A), and
11522 | Dalton Trans., 2010, 39, 11522–11525
This journal is
The Royal Society of Chemistry 2010
©

View Article Online
network based on dia subnets interpenetrated by non-translational
symmetry operation (Class IIa).
As expected, with topological analysis guidance, the compli-
cated structure of 1 can be clearly understood as a combination
of dia subnets and pillars. Each dimeric NiII SBU acts as a
tetrahedral node via the linkage of V-shaped sdba2- connecters
to form a typical dia network. The large diamondoid cages in
each net have the maximum dimensions of 42.96 ¥ 40.06 ¥ 33.86
˚
A (see Fig. S3(a), ESI†), which allows the other selfsame dia
network to penetrate and thus, forms a 2-fold interpenetrating
array (see Fig. 2(a)). Despite interpenetration, the framework of
1 remains open, and contains 1D channels of approximate 13.59
˚
¥ 8.42 A along [100], in which the lattice water molecules are
located. The potential solvent-accessible areas before and after
the exclusion of the water guests are as large as 7025.6 and 7409.3
3
˚
A (35.7% and 37.7% of the unit cell volume), as calculated by
the PLATON software.14 Another fascinating structural feature
of 1 is to form a novel “warp and weft” like interwoven fabric
structure (see Fig. 2(b)). As illustrated in Fig. 2(c), the dimeric NiII
SBUs are bridged by the sdba2- spacers into pairs of heterochiral
Fig. 1 (a) Coordination environment of NiII (symmetry codes: A = -x -
1/2, -y + 1/2, -z + 1; B = x + 1/4, -y + 1/2, z - 1/4; C = -x, y- 1/4, z
- 1/4). (b) Self-penetrating 6-connected network with (44.610.8) topology.
(c) Two parallel dia subnets. (d) Schematic view of the self-penetrating
structure.
˚
helical chains, with the pitch of 20.828 A. Interestingly, pairs of
homochiral side-by-side double helix from two individual dia nets
are laid one over the other alternately, which leads to the “warp
and weft” type 2D nets along the ab plane (see Fig. 2(b)). In
this condition, two dia networks are composed of pairs of such
“warp and weft” type 2D networks in an alternate fashion (see Fig.
S3(b), ESI†). Although several “warp and weft” type coordination
polymers based on 1D tectons have been reported,15 such helical
interwoven fabric structural motif in 1 is unique. Further, the V-
shaped dps ligands serve as pillars to join the neighboring dimeric
NiII SBUs to 1D quadrate loops (see Fig. S3(c), ESI†), which
interlink the two dia networks to produce the final self-penetrating
pattern (see Fig. 1(d) and 2(d), Fig. S3(d), ESI†).
such dimeric secondary building units (SBUs) are further extended
by the sdba2- ligands to afford a very complicated 3D network (see
Fig. S2, ESI†). In addition, strong O–H ◊ ◊ ◊ O H-bonds between
water ligands (O7) and uncoordinated carboxylate groups (O2)
(O ◊ ◊ ◊ O: 2.574, 159.34◦) also stabilize the whole structure.
In order to clearly understand such a 3D architecture, the
topological method is used to simplify the structure. Topologically,
by regarding each Ni2-SBU as a network node, the overall 3D
net can be rationalized as a uninodal 6-connected framework
with the point symbol of (44.610.8) (Fig. 1(b), vertex symbol:
[4.4.4.4.63.63.65.65.65.65.66.66.66.66. 89], named as net B). Further
analysis of this structure indicates that it consists of two interpen-
etrating 4-connected diamonds (dia) of Class IIa (related by an
inversion center) nets with dimeric NiII nodes (see Fig. 1(c)) and
sdba2- connectors, which are interconnected by the dps pillars.
Within this network, the 6-membered circuits mutually interweave
into a novel self-penetrating motif (see Fig. 1(d)).
Notably, 6-connected self-penetrating networks are quite rare,
and there is an interesting relationship between the current
net B and other reported 6-connected self-penetrating types:
(44.610.8) (mab),7a–d (44.610.8) (roa),7b,e,f (48.66.8) (rob),7b,g (44.611),7h
and (48.67).7i Following the topological approach proposed for
the analysis of high connectivity materials,3b all above-mentioned
6-connected nets are based on square layers (44-sql). Notably,
the most difference between our net B and other 6-connected
self-penetrating nets is the presence of unusual parallel inter-
penetration of two identical dia subnets, and an analysis of the
interpenetrating topology with the TOPOS program13 suggests
that it belongs to class IIa, that is, the individual nets are related
by means of a full interpenetration symmetry element. In addition,
net B is closely related to, but different from those of mab and roa.
In the latter three cases, the similar 6-connected self-penetrating
nets have the same Schla¨fli symbol (44.610.8), but with different
vertex symbols for mab of 4.4.4.4.64.64.65.65.65.65.611.611.611.611.*,
and for roa 4.4.4.4. 62.62.65.65.65.65.65.65.65.65.*. In this sense,
net B can be classified as the first six-connected self-penetrating
Fig. 2 (a) Two fold interpenetrating dia network. (b) The “warp and
weft” interwoven fabric structure along the ab plane constructed by
pairs of homochiral (blue/yellow for left- or teal/purple for right-hand)
side-by-side double helix from two individual dia nets. (c) The dia subnet
constructed by heterochiral helical chains. (d) 3D coordination network
with 1D quadrate loops and dia subnets.
TGA curves of complexes 1 and 2 are similar, probably because
of their isostructural nature (see Fig. S4, ESI†). Complex 1 is used
This journal is
The Royal Society of Chemistry 2010
Dalton Trans., 2010, 39, 11522–11525 | 11523
©

View Article Online
as an example. The first weight loss of 3.8% corresponds to the
removal of 2.25 water molecules per formula unit (calc. 3.35%).
From ca. 250 ◦C the expulsion of organic components occurs. The
final residue seems to be NiO (observed: 13.9% and calculated:
13.07%), which has also been further confirmed by temperature-
variable PXRD patterns of 1 (see Fig. S1(b), ESI†).
For 2, spin-orbital coupling of the CoII ion gives rise to a cMT
value of 4.5 cm3 K mol-1 at room temperature, which is much
higher than that of two non-interacting CoII ions (3.75 cm3 K
mol-1 assuming g = 2.0). The cMT decreases as cooling and has
a minimum of 3.15 cm3 K mol-1 (see Fig. 3(b)). In the region of
300–34 K, complex 2 mainly shows the single-ion behavior of CoII.
Below 34 K, a ferromagnetic coupling between CoII overcomes the
effect of spin-orbital coupling and thus, compensates the decrease
of cMT, leading a sharp increase of cMT to a maximal value of
4.6 cm3 K mol-1 at 14.9 K, which however, cannot give a ground
state spin of ST = 3. Temperature dependence of the reciprocal
The magnetic susceptibilities (cM) of 1 and 2 were measured in
2–300 K (see Fig. 3). For 1, the cMT value at room temperature
is 1.55 cm3 K mol-1, which falls in the normal range of two non-
coupled NiII ions. As the temperature is lowered, the cMT decreases
slowly until ca. 50 K, and then sharply to 0.53 cm3 K mol-1 upon
cooling to 2 K, indicating a dominant antiferromagnetic coupling.
In order to quantitatively evaluate the magnetic interactions, the
susceptibility (cM-1) above 50 K follows the Curie–Weiss law (cM
=
C/(T - q)) with a Weiss constant q = -4.65 K and a Curie constant
C = 4.40 cm3 K mol-1. This contribution of spin-orbital interaction
diminishes the ferromagnetic exchange, resulting in a negative
Weiss constant.
following equation for a dinuclear NiII model is derived from the
16
ˆ
Hamiltonian H = JS1S2, where J is the intradimer exchange
constant. A least-squares fit of the magnetic susceptibilities data
led to J = -1.15 cm-1, g = 2.49, and R = 3.02 ¥ 10-4. The negative J
value indicates a weak antiferromagnetic interaction between the
adjacent NiII ions.
2
2
2
ˆ
ˆ ˆ
ˆ
ˆ
H = −2JS1S2 = −J (ST −
S )
∑
i=1
Ng2b2 84e12J / kT + 30e6J / kT +6e2J / kT
Ng2b2 A
cM
=
×
3kT
7e12J / kT + 5e6J / kT + 3e2J / kT +1
14e12J / kT + 5e6J / kT +e2J / kT
cM
=
KT
B
2Ng2b2
=
×
⎡
⎤
⎡
⎤
J
3J
kT
7e12J / kT + 5e6J / kT + 3e2J / kT +1
A = 2exp
+10exp
⎢
⎣
⎥
⎦
⎢
⎣
⎥
⎦
KT
KT
⎡
⎤
⎡
⎤
J
3J
B = 1+ 3exp
+ 5exp
⎢
⎣
⎥
⎢
⎣
⎥
⎦
In summary, we have prepared two unique six-connected self-
penetrating 3D coordination frameworks, which can interestingly
be regarded as the cross-linking of two interpenetrating dia sub-
nets. This unique structural example will enrich our knowledge of
network topologies and suggest the great potential of constructing
unusual entangled networks from the V-shaped tectons, which are
under way in our lab.
KT
KT
⎦
Acknowledgements
This work was financially supported by the NSF of China
(21073106, 20773104), NCET (NCET-06-0891), MOE (208143),
IPHPEO (Z20091301,Q20101203), and the NSF of Hubei
Province (2008CDB030). M. D. also thanks the support from
Tianjin Normal University.
References
1 (a) A. F. Wells, Structural Inorganic Chemistry, Oxford University Press,
Oxford, 5th ed., 1984; (b) A. F. Wells, Three-dimensional Nets and
Polyhedra, Wiley, New York, 1977; (c) A. F. Wells, Further Studies of
Three-dimensional Nets, ACA monograph 8, 1979.
2 (a) D. J. Tranchemontagne, J. L. Mendoza-Cortes, M. O’Keeffe and
O. M. Yaghi, Chem. Soc. Rev., 2009, 38, 1257; (b) X. L. Wang, C. Qin,
S. X. Wu, K. Z. Shao, Y. Q. Lan, S. Wang, D. X. Zhu, Z. M. Su and
E. B. Wang, Angew. Chem., Int. Ed., 2009, 48, 5291; (c) M. L. Tong,
X. L. Chen and S. R. Batten, J. Am. Chem. Soc., 2003, 125, 16170;
(d) M. Du, Z. H. Zhang, L. F. Tang, X. G. Wang, X. J. Zhao and S. R.
Batten, Chem.–Eur. J., 2007, 13, 2578; (e) J. Y. Lu, Coord. Chem. Rev.,
2003, 246, 327.
3 (a) S. R. Batten and R. Robson, Angew. Chem., Int. Ed., 1998, 37, 1460;
(b) R. J. Hill, D. L. Long, N. R. Champness, P. Hubberstey and M.
Schro¨der, Acc. Chem. Res., 2005, 38, 335; (c) B. Moulton and M. J.
Zaworotko, Chem. Rev., 2001, 101, 1629; (d) L. Carlucci, G. Ciani and
D. M. Proserpio, Coord. Chem. Rev., 2003, 246, 247; (e) N. W. Ockwig,
O. Ddelgado- Friedrichs, M. O’Keeffe and O. M. Yaghi, Acc. Chem.
Res., 2005, 38, 176; (f) V. A. Blatov, L. Carlucci, G. Ciani and D. M.
Proserpio, CrystEngComm, 2004, 6, 378; (g) V. A. Blatov, M. O’Keeffe
and D. M. Proserpio, CrystEngComm, 2010, 12, 44; (h) I. A. Baburin,
Fig. 3 Temperature dependence of cMT and cM for 1 (a) and 2 (b). Open
points are the experimental data, and the solid line represents the best fit
obtained from the Hamiltonian given in the text.
11524 | Dalton Trans., 2010, 39, 11522–11525
This journal is
The Royal Society of Chemistry 2010
©

View Article Online
V. A. Blatov, L. Carlucci, G. Ciani and D. M. Proserpio, J. Solid State
Chem., 2005, 178, 2452; (i) I. A. Baburin, V. A. Blatov, L. Carlucci, G.
Ciani and D. M. Proserpio, Cryst. Growth Des., 2008, 8, 519; (j) M.
O’Keeffe, M. A. Peskov, S. J. Ramsden and O. M. Yaghi, Acc. Chem.
Res., 2008, 41, 1782.
4 (a) M. O’Keeffe, O. M. Yaghi and S. Ramsden, Reticular Chem-
istry Structure Resource, http://rcsr.anu.edu.au; (b) S. Ramsden, V.
Robins, S. T. Hyde and S. Hungerford, EPINET: Euclidean Patterns
in Non-Euclidean Tilings, http://epinet.anu.edu.au; (c) V. A. Blatov,
http://www.topos.ssu.samara.ru; (d) S. R. Batten, http://www.chem.
monash.edu.au/staff/sbatten/interpen/index.html.
J. M. Zheng, Cryst. Growth Des., 2009, 9, 2756; (c) D. R. Xiao, Y. G.
Li, E. B. Wang, L. L. Fan, H. Y. An, Z. M. Su and L. Xu, Inorg. Chem.,
2007, 46, 4158; (d) E. Shyu, R. M. Supkowski and R. L. LaDuca,
Inorg. Chem., 2009, 48, 2723; (e) H. J. Jiang, B. Liu and Q. Xu, Cryst.
Growth Des., 2010, 10, 806; (f) G. A. Fernandez, P. K. Thallapally, R. K.
Motkuri, S. K. Nune, J. C. Sumrak, J. Tian and J. Liu, Cryst. Growth
Des., 2010, 10, 1037.
10 (a) X. M. Gao, D. S. Li, J. J. Wang, F. Fu, Y. P. Wu, H. M. Hu and J. W.
Wang, CrystEngComm, 2008, 10, 479; (b) D. S. Li, Y. P. Wu, P. Zhang,
M. Du, J. Zhao, C. P. Li and Y. Y. Wang, Cryst. Growth Des., 2010, 10,
2037.
5 (a) H. L. Jiang, Y. Tatsu, Z. H. Lu and Q. Xu, J. Am. Chem. Soc.,
2010, 132, 5586; (b) L. Carlucci, G. Ciani, M. Moret, D. M. Proserpio
and S. Rizzato, Angew. Chem., Int. Ed., 2000, 39, 1506; (c) X. J. Luan,
Y. Y. Wang, D. S. Li, P. Liu, H. M. Hu, Q. Z. Shi and S. M. Peng,
Angew. Chem., Int. Ed., 2005, 44, 3864; (d) S. N. Wang, Y. Yang, J. F.
Bai, Y. Z. Li, M. Scheer, Y. Pan and X. Z. You, Chem. Commun., 2007,
4416; (e) X. Kuang, X. Wu, R. Yu, J. P. Donahue, J. Huang and C. Z.
Lu, Nat. Chem., 2010, 2, 461; (f) L. F. Ma, L. Y. Wang, M. Du and
S. R. Batten, Inorg. Chem., 2010, 49, 365; (g) J. Fan, H. F. Zhu, T. A.
Okamura, W. Y. Sun, W. X. Tang and N. Ueyama, Inorg. Chem., 2003,
42, 158.
11 Preparation of 1. A mixture of Ni(OAc)2·4H2O (24.9 mg, 0.1 mmol),
H2sdba (30.6 mg, 0.1 mmol), dps (18.8 mg, 0.1 mmol) and NaOH
(8 mg, 0.2 mmol) in H2O (10 mL) was placed in a Parr Teflon-lined
stainless steel (25 mL) autoclave, and heated to 160 ◦C for 5 days. Green
block crystals of 1 were obtained in 58% yield (based on NiII). Anal.
calcd for C48H36.4N4O14.2S4Ni2: C, 50.48; H, 3.21; N, 4.91%. Found: C,
50.23; H, 3.23; N,4.87%. IR (KBr, cm-1): 3435 m, 2995 s, 1593 s, 1552 s,
1432 s, 1386 m, 1299 m, 1216 m, 1141 m, 1066 s, 922 w, 819 s, 761 w,
733 m, 630 s, 472 w. Preparation of 2. An identical procedure to that
of 1 was used except Ni(OAc)2·4H2O was replaced by Co(OAc)2·4H2O
(24.9 mg, 0.1 mmol). Pink block crystals of 2 were obtained in 50%
yield (based on CoII). Anal. calcd for C48H36.4N4O14.2S4Co2: C, 50.46;
H, 3.21; N, 4.91%. Found: C, 50.20; H, 3.21; N, 4.86%. IR (KBr, cm-1):
3438 m, 2987 s, 1588 s, 1559 s, 1436 s, 1380 m, 1291 m, 1221 m, 1148
m, 1069 s, 918 w, 822 s, 766 w, 738 m, 638 s, 477 w.
6 S. R. Batten, S. M. Neville and D. R. Turner, Coordination Polymers
Design, Analysis and Application, Published by the Royal Society of
Chemistry, 2009.
7 (a) H. L. Sun, S. Gao, B. Q. Ma and S. R. Batten, CrystEngComm,
2004, 6, 579; (b) J. Zhang, Y. G. Yao and X. Bu, Chem. Mater., 2007,
19, 5083; (c) D. P. Maryin, R. M. Supkowski and R. L. LaDuca, Cryst.
Growth Des., 2008, 8, 3518; (d) X. H. Zhou, X. D. Du, G. N. Li, J. L. Zuo
and X. Z. You, Cryst. Growth Des., 2009, 9, 4487; (e) B. F. Abrahams,
M. J. Hardie, B. F. Hoskins, R. Robson and E. E Sutherland, J. Chem.
Soc., Chem. Commun., 1994, 1049; (f) Y. Zhang, M. K. Saha and I.
Bernal, CrystEngComm, 2003, 5, 34; (g) D. L. Long, R. J. Hill, A. J.
Blake, N. R. Champness, P. Hubberstey, C. Wilson and M. Schro¨der,
Chem.–Eur. J., 2005, 11, 1384; (h) J. Yang, J. F. Ma, Y. Y. Liu and S. R.
Batten, CrystEngComm, 2009, 11, 151; (i) L. Carlucci, G. Ciani, D. M.
Proserpio and L. Spadacini, CrystEngComm, 2004, 6, 96.
8 (a) Y. Q. Lan, X. L. Wang, S. L. Li, Z. M. Su, K. Z. Shao and E. B.
Wang, Chem. Commun., 2007, 4863; (b) P. K. Chen, S. R. Batten, Y.
Qi and J. M. Zheng, Cryst. Growth Des., 2009, 9, 2756; (c) Y. Q. Wang,
J. Y. Zhang, Q. X. Jia, E. Q. Gao and C. M. Liu, Inorg. Chem., 2009, 48,
789; (d) L. F. Ma, L. Y. Wang, Y. Y. Wang, S. R. Batten and J. G. Wang,
Inorg. Chem., 2009, 48, 915; (e) S. R. Zheng, Q. Y. Yang, R. Yang, M.
Pan, R. Cao and C. Y. Su, Cryst. Growth Des., 2009, 9, 2341.
9 (a) X. L. Wang, C. Qin, E. B. Wang, Z. M. Su, L. Xu and S. R. Batten,
Chem. Commun., 2005, 4789; (b) P. K. Chen, S. R. Batten, Y. Qi and
12 Crystallographic data for 1 (CCDC: 778541): C48H36.4N4O14.2S4Ni2,
Mr = 1142.07, orthorhombic, Fddd, a = 11.466(1), b = 39.891(3),
3
c = 43.067(4) A, V = 19699(3) A , Z = 16, rc = 1.54 g cm-3, m =
1.006 mm-1, S = 0.81, Rint = 0.0373 (for 4575 unique reflections),
R1 = 0.0708 and wR2 = 0.1730. Crystallographic data for 2 (CCDC:
˚
˚
778542): C48H36.4N4O14.2S4Co2, Mr = 1142.55, orthorhombic, Fddd, a =
3
˚
˚
11.418(1), b = 40.061(4), c = 42.963(4) A, V = 19653(3) A , Z = 16, rc =
1.544 g cm-3, m = 0.917 mm-1, S = 1.053, Rint = 0.0718 (for 4574 unique
reflections), R1 = 0.0412 and wR2 = 0.0865.
13 V. A. Blatov, A. P. Shevchenko and V. N. Serezhkin, J. Appl. Crystallogr.,
2000, 33, 1193.
14 A. L. Spek, PLATON, A multipurpose crystallographic tool, Untrecht
University, 2003.
15 (a) P. M. V. Calcar, M. M. Olmsteed and A. L. Balch, Chem. Commun.,
1995, 1773; (b) A. M. P. Peedikakkal and J. J. Vittal, Cryst. Growth
Des., 2008, 8, 375; (c) Y. H. Li, C. Y. Su, A. M. Goforth, K. D. Shimizu,
K. D. Gray, M. D. Smith and H. C. Zur Loye, Chem. Commun., 2003,
1630.
16 S. K. Dey, M. S. El Fallah, J. Ribas, T. Matsushita, V. Gramlich and S.
Mitra, Inorg. Chim. Acta, 2004, 357, 1517.
This journal is
The Royal Society of Chemistry 2010
Dalton Trans., 2010, 39, 11522–11525 | 11525
©