Azide-bridged manganese(III) onedimensional chain: Synthesis, structure, and magnetic study

Article abstract of DOI:10.1080/00958972.2012.744971

A new end-to-end azide-bridged one-dimensional coordination polymer, [Mn^III(L)(μ_1,3-N₃)]_n (1) (where L represents the dianionic form of the neutral tetradentate Schiff base H2L obtained by 1 : 2 condensation of

Full text of DOI:10.1080/00958972.2012.744971

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Azide-bridged manganese(III) one-
dimensional chain: synthesis,
structure, and magnetic study
Partha Pratim Chakrabarty a , Sandip Saha a , Dieter Schollmeyer
b , Athanassios K. Boudalis c , Atish Dipankar Jana d & Dominique
Luneau e
a Department of Chemistry, Acharya Prafulla Chandra College,
Kolkata, India
b Institut fur Organische Chemie, Universit at Mainz, Mainz,
Germany
c Institute of Materials Science, NCSR ‘‘Demokritos”, Aghia
Paraskevi Attikis, Greece
d Department of Physics, Behala College, Kolkata, India
e Université Claude Bernard Lyon 1 Groupe de Cristallographie
et Ingénierie Moléculaire Laboratoire des Multimatériaux et
Interfaces (UMR 5615) Bâtiment Berthollet – Domaine Scientifique
de la Doua 69622, Villeurbanne Cedex, France
Accepted author version posted online: 08 Nov 2012.Version of
record first published: 10 Dec 2012.
To cite this article: Partha Pratim Chakrabarty , Sandip Saha , Dieter Schollmeyer , Athanassios
K. Boudalis , Atish Dipankar Jana & Dominique Luneau (2013): Azide-bridged manganese(III) one-
dimensional chain: synthesis, structure, and magnetic study, Journal of Coordination Chemistry,
66:1, 9-17
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Journal of Coordination Chemistry
Vol. 66, No. 1, 10 January 2013, 9–17
Azide-bridged manganese(III) one-dimensional chain:
synthesis, structure, and magnetic study
PARTHA PRATIM CHAKRABARTYy, SANDIP SAHAy*, DIETER SCHOLLMEYERz,
x
{
ATHANASSIOS K. BOUDALIS , ATISH DIPANKAR JANA and DOMINIQUE
LUNEAUk
†Department of Chemistry, Acharya Prafulla Chandra College, Kolkata, India
‡Institut fur Organische Chemie, Universit at Mainz, Mainz, Germany
§Institute of Materials Science, NCSR ‘‘Demokritos”, Aghia Paraskevi Attikis, Greece;
{
Department of Physics, Behala College, Kolkata, India
kUniversité Claude Bernard Lyon 1 Groupe de Cristallographie et Ingénierie Moléculaire
Laboratoire des Multimatériaux et Interfaces (UMR 5615) Bâtiment Berthollet – Domaine
Scientifique de la Doua 69622, Villeurbanne Cedex, France
(Received 16 June 2012; in final form 26 September 2012)
A new end-to-end azide-bridged one-dimensional coordination polymer, [MnIII(L)(μ1,3–N3)]n (1)
(where L represents the dianionic form of the neutral tetradentate Schiff base H2L obtained by 1 : 2
condensation of ethane-1,2-diamine, and 5-chloro-2-hydroxyacetophenone in methanol), has been
synthesized and characterized by elemental analyses, IR spectroscopy, single-crystal X-ray
diffraction, and variable temperature magnetic study. X-ray crystal structure determination of 1
reveals that a chain system with the repeating unit [MnIII(L)(μ1,3–N3)]n bridged by μ1,3 azide. Each
manganese(III) is a distorted octahedral geometry. Variable-temperature magnetic study (between 2
and 300 K) suggests a moderate antiferromagnetic interaction in this complex, similar to other
studies reported.
Keywords: Manganese(III); Chain; Azide-bridged; Crystal structure; Magnetic study
1. Introduction
Molecule-based magnetic materials with exotic properties like single-molecule magnets
[1–5] and single-chain magnets [6–8] have been studied for their potential applications in
magnetic devices. To synthesize the aforementioned molecular magnetic systems, it is nec-
essary to select appropriate bridging ligands that can hold paramagnetic centers closely
together and communicate effective magnetic exchange coupling between them. It is desir-
able to use ligands with short paths such as oxide, cyanide, carboxylate, or azide [9–12].
Azide acts as a bridge in diverse binding modes and many structures with azide have been
reported using paramagnetic transition-metal ions such as Mn2+, Mn3+, Fe2+, Co2+, Ni2+,
Cu2+, etc. and magnetic properties relying on the metal contents have also been evaluated
*Corresponding author. Email: sandipsaha2000@yahoo.com
Journal of Coordination Chemistry
ISSN 0095-8972 print/ISSN 1029-0389 online Ó 2012 Taylor & Francis
http://dx.doi.org/10.1080/00958972.2012.744971

10
P.P. Chakrabarty et al.
[13–23]. From the magnetic view-point, Co2+ and Mn3+ have similarities, because both
ions show strong magnetic anisotropy to give exotic magnetic characteristics such as spin-
canting, metamagnetism, slow magnetic relaxation, and long range order [24–27]. Schiff-
base complexes of Mn3+ are of particular interest because Mn3+, whose oxidation state is
stabilized in the N2O2 environment of tetradentate Schiff bases, allows for significant
magnetic anisotropy in association with typical Jahn–Teller distortion [28]. The use of the
Schiff base in equatorial coordination makes two axial sites available for azide. Accord-
ingly, self-assembly of the MnIII Schiff base with azide led to dinuclear entities [29–32]
and frequently constrained one-dimensional (1-D) chains [20, 29, 33–37]. Polynuclear Mn
(III) species also play an important role in catalytic and biological fields, especially in the
oxygen evolving compound of photosystem II [38, 39].
Three new Mn(III) 1-D coordination polymers have been reported with tetradentate
Schiff bases [37]. The crystal systems differ according to the Schiff bases used and each
manganese has Jahn–Teller distortion. Magnetic measurements show the presence of appar-
ent spin canting. Two complexes exhibit a field-induced metamagnetic transition from an
antiferromagnetic state to a weak ferromagnetic phase, whereas another complex shows a
field-induced, two-step magnetic phase transition. In another study, Bhowmik et al.
reported an end-to-end azide-bridged Mn(III) 1-D chain in which Mn(III) has a six-coordi-
nate, pseudo-octahedral geometry, and the deprotonated di - Schiff base constituted the
equatorial plane and axial positions is occupied by two azides [36]. Magnetic characteriza-
tion shows that the μ1,3-bridging azide mainly transmits an antiferromagnetic interaction
which is very similar to earlier reported cases [20, 33–35].
Here, we extend the examples of polymeric Mn(III) azido complexes containing Schiff
base as a blocking co-ligand, reporting the synthesis, X-ray crystal structure, and magnetic
study of a 1-D polymer, [MnIII(L)(μ1,3–N3)]n (1); L represents the dianionic form of the
neutral tetradentate Schiff base H2L (see scheme 1) prepared by 1:2 condensation of
ethane-1,2-diamine and 5-chloro-2-hydroxyacetophenone.
2. Experimental
2.1. Materials and physical measurements
All reagents and solvents were commercially available and used as received without
purification. IR spectra were recorded as KBr pellets from 4000 to 400 cmꢀ1 on a Perkin–
Elmer Spectrum RXI FTIR Spectrometer. Elemental analyses were carried out using a
Scheme 1. Schematic representation of the neutral H2L.

Azide-bridged Manganese(III) One-dimensional Chain
11
Heraeus CHN-O-Rapid elemental analyzer. Variable-temperature magnetic susceptibility
measurements were carried out on a microcrystalline sample from 2 to 300 K using a
Quantum Design MPMS SQUID susceptometer operating under a magnetic field of 0.1 T.
Diamagnetic corrections for the complexes were estimated from Pascal’s constants.
2.2. Preparation of [MnIII(L)(μ1,3–N3)]n (1)
Caution! Since azide compounds of metal ions are potentially explosive, only small
amount of the material should be prepared and handled with care.
To a solution of 5-chloro-2-hydroxyacetophenone (0.340 g, 2 mmol) in 20 mL of metha-
nol, ethane-1,2-diamine (0.06 g, 1 mmol) was added and the resulting mixture was heated
under reflux for 4 h. A methanolic solution (10 mL) of Mn(ClO4)2 ꢁ 6H2O (0.724 g,
2 mmol) was added to this solution. The reaction mixture was refluxed for 2 h. An aqueous
solution of NaN3 (0.26 g, 4 mmol) was then added and stirred for 1.5 h. The resulting
solution was then filtered. After 2 weeks, black needle crystals of 1 were formed with a
70% yield. Anal. Calc. for C18H16Cl2MnN5O2: C, 46.8; H, 3.4; N, 15.2. Found: C, 47.0;
H, 3.5; N, 15.6%.
2.3. Crystal structure determination of 1
Crystal data for 1 are given in table 1. Bond distances and angles for 1 are given in table
2. Four thousand and twenty-four – total independent data for 1 were collected on a STOE
IPDS 2T device with a STOE detector equipped with graphite monochromated Mo Kα
radiation (λ = 0.71073 Å). Data collection was carried out using a STOE detector and for
Table 1. Summary of crystal data and refinement details of 1.
Empirical formula
Formula weight
Crystal dimension (mm)
Crystal system
Space group
a (Å)
C
18H16Cl2MnN5O2
460.20
0.30 ꢂ 0.17 ꢂ 0.05
Orthorhombic
P c a 21
13.3469(5)
12.8284(7)
11.4068(5)
90.00
b (Å)
c (Å)
α (°), β (°), γ (°)
V (Å3)
1953.07(16)
4
Z
Temperature (K)
193(2)
1.565
0.974
936
2.83–29.67
4714
Dcalc (g cmꢀ3
)
μ (mmꢀ1
F(0 0 0)
h (°)
)
Total data
Unique data
3588
R
0.0427
Rw
0.1126
1.039
Goodness-of-fit on F2, S
Rint
0.0846
0.296
ꢀ0.484
Δρmax (e Åꢀ3
)
Δρmin (e Åꢀ3
)
w = 1=½ns^2^ðFo^2^Þ þ ð0:0564PÞ^2^ þ 0:2207Pꢃ; where P ¼ ðFo^2^ þ 2Fc^2^Þ=30.

12
P.P. Chakrabarty et al.
Table 2. Selected bond distances (Å) and angles (°) for 1.
Mn1–O2
Mn1–N1
Mn1–N2
Mn1–N3
Mn1–N5
Cl1–C4
Cl2–C14
O1–C1
O2–C17
N1–C7
N1–C8
N2–C9
N2–C11
N3–N4
N4–N5
N5–Mn1
C1–C2
C1–C6
C2–H2
C2–C3
C3–H3
C3–C4
C4–C5
C5–H5
C5–C6
C6–C7
1.862(3)
1.990(3)
2.003(3)
2.336(3)
2.258(3)
1.752(4)
1.741(4)
1.324(5)
1.317(5)
1.296(5)
1.482(4)
1.479(4)
1.289(5)
1.178(5)
1.189(5)
2.258(3)
1.411(6)
1.412(6)
0.950(4)
1.380(5)
0.950(4)
1.374(6)
1.383(6)
0.950(4)
1.404(5)
1.473(6)
O1–Mn1–O2
O1–Mn1–N1
O1–Mn1–N2
O1–Mn1–N3
O1–Mn1–N5
O2–Mn1–N1
O2–Mn1–N2
O2–Mn1–N3
O2–Mn1–N5
N1–Mn1–N2
N1–Mn1–N3
N1–Mn1–N5
N2–Mn1–N3
N2–Mn1–N5
N3–Mn1–N5
Mn1–O1–C1
Mn1–O2–C17
Mn1–N1–C7
Mn1–N1–C8
C7–N1–C8
92.0(1)
91.4(1)
176.2(1)
94.2(1)
93.4(1)
176.6(1)
91.6(1)
91.5(1)
93.1(1)
85.1(1)
88.9(1)
86.0(1)
84.4(1)
87.7(1)
170.9(1)
128.1(2)
127.4(2)
128.1(2)
110.2(2)
120.4(3)
109.8(2)
127.7(2)
121.3(3)
110.2(2)
178.1(4)
122.2(3)
Mn1–N2–C9
Mn1–N2–C11
C9–N2–C11
Mn1–N3–N4
N3–N4–N5
N4–N5–Mn1
data reduction, STOE X-AREA software package was used. The structure was solved by
SIR 97 [40]. Structure refinement was also performed by full-matrix least squares based
on F2 with SHELXL-97 [41]. All non-hydrogen atoms were refined anisotropically. The
C-bound hydrogens were constrained to ideal geometry and included in the refinement in
the riding model approximation. Data for molecular geometry, intermolecular interactions,
and figures were produced using Platon-2009 [42] and ORTEP 3.2 [43].
3. Results and discussion
3.1. Synthesis and IR spectroscopy
H2L was prepared by 1 : 2 condensation of ethane-1,2-diamine with 5-chloro-2-hydroxy-
acetophenone in methanol. The ligand was not isolated separately but the yellow methano-
lic solution obtained by the condensation was used in the present work. This ligand was
previously reported in the preparation of base adducts of cobalt(II) and nickel(II) chelates
with some Schiff bases using 2,2′-bipyridine and 1,10-phenanthroline [44]. The dianionic
form of the ligand is a N2O2 donor in the reported complexes. The yellow methanolic
solution – reacted with manganese(II) perchlorate hexahydrate and sodium azide in metha-
nol-water mixture with refluxing to prepare the 1-D chain 1. Mn(III) – is six coordinate by
N2O2 donor, L2ꢀ and two bridging azides. Related Schiff bases, viz. 5-OCH3 salen or 5-F
salen, form azide bridged polynuclear compounds under cold condition [34]. Another inter-
esting feature of this ligand is that all other ligands reported were with the salicylaldehyde
analogue, our ligand with o-hydroxy acetophenone analogue.

Azide-bridged Manganese(III) One-dimensional Chain
13
In IR spectra of 1, the distinct band at 1589 cmꢀ1 is due to azomethine (C = N) of the
Schiff base. The asymmetric stretch of the azide (νas) is at 2032 cmꢀ1, attributed to the
presence of an end-to-end azide bridge [45].
3.2. Description of the structure
Single-crystal X-ray analysis reveals that 1 consists of a chain system with the repeating
unit [MnIII(L)(μ1,3–N3)]n bridged by μ-1,3 azide (figure 1). There is only one crystallo-
graphically independent Mn(III) in a distorted octahedral geometry, which iꢀs coordinated
by N2O2 donors from one Schiff base in the equatorial mode and two N3 ions in the
axial positions (figure 2). Each azide functions as a trans-μ1,3 bridge to link monomeric
[MnIII(L)]+ units into a 1-D zigzag chain along the crystallographic c axis. In the equato-
rial plane, the Mn(1)–O(1), Mn(1)–O(2), Mn(1)–N(1), and Mn(1)–N(2) bond lengths are
1.866(2), 1.862(3), 1.990(3), and 2.003(3) Å, respectively, which are close to those in other
Mn(III)-salen compounds [29, 33, 34]. As expected, the bond lengths in the axial position
of Mn(1)–N(3) and Mn(1)–N(5A) [2.336(3) and 2.258(3) å] are elongated due to Jahn–
Teller distortion of the high-spin d4 metal [14, 28]. The bond angles of Mn(1)–N(3)–N(4)
and Mn(1)–N(5A)–N(4A) are 110.2(2) and 122.2(3)°, respectively. Deviations of the coor-
dinating atoms in the basal plane, O(1), O(2), N(1), and N(2), from the least-square mean
planes are 0.348, 0.348, 0.331, and 0.331 Å, respectively, and that of Mn(III) from the
same plane is 0.877 Å. For N3ꢀ, N(3)–N(4) and N(4)–N(5A) have almost the same bond
lengths [1.178(5) and 1.189(5) å] and the N(3)–N(4)–N(5A) bond angle is 178.1(4)°, close
to 180°. The manganese–manganese repeating distance is 5.825 Å along the chain.
3.3. Magnetic properties
The magnetic response of 1 was recorded from 2 to 300 K under a 0.1 T field. The
resulting χMT vs. T plot is depicted in figure 3. At 300 K, the χMT is 2.47 cm3 molꢀ1 K,
Figure 1. View of 1-D zigzag chain of 1.

14
P.P. Chakrabarty et al.
Figure 2. ORTEP diagram (30% ellipsoidal probability) with atom numbering scheme.
appreciably lower than the expected value for a well-isolated S = 2 spin (3.0 cm3 molꢀ1 K),
indicating the presence of antiferromagnetic interactions. Upon cooling, this value gradu-
ally decreases to 0.16 cm3 molꢀ1 K, corroborating this assumption. At lower temperatures,
this decrease is more pronounced, probably due to zero-field splitting (zfs) and/or Zeeman
contributions of paramagnetic impurities. Due to this contribution, and to the zfs contribu-
tions of MnIII in 1, theoretical studies were carried out over the 300–20 K regime.
Interchain interactions were disregarded and the Hamiltonian considered was:
X
^ ^
SiSiþ1
^
H ¼ ꢀ2J
i
The χMT versus T data were fitted according to Fisher’s model assuming classical spins
[46], considering a paramagnetic impurity fraction q. The equation used was:
Ng2b2SðS þ 1Þ 1 þ uðKÞ
Ng2b2
3kT
v ¼ ð1 ꢀ qÞ
þ q
SðS þ 1Þ
ð1Þ
3kBT
1 ꢀ uðKÞ
4JSðSþ1Þ
where u(K) = cothK – 1/K and K ¼
.
Substituting with S = Si = Si+1 = 2, thekBbTest-fit parameters were: J = ꢀ7.8(1) cmꢀ1, g = 1.95
(1), and ρ = 8.6(1)% (R = 7.1 ꢂ10ꢀ6).
Manganese(III) 1-D systems with Schiff bases as coligands and with single μ1,3-azido
bridge reported are summarized in table 3. In these systems, the Jahn–Teller axis of the
Mn(III) ions is located in the azido bridge direction, with one electron in the dz2 orbital;
2
2
the dx ꢀy orbital remains empty pointing to the capping ligand.
Escuer et al. [47] analyzed the effects of the structural parameters for Mn(II) end-to-end
azido-bridged systems, with respect to their magnetic interactions, concluding that the
exchange couplings are always antiferromagnetic, being the result of two types of
contributions: σ (through the dZ2 orbital) and π (through the dXY and dYZ orbital). The
exchange coupling constant depends on three structural parameters: the Mn–N distance
(d), the Mn–N1–N2 angle (α), and the Mn–N1–N3–Mn torsion angle (τ). In this way,

Azide-bridged Manganese(III) One-dimensional Chain
15
Figure 3. χMT vs. T data for 1 and best-fit curve according to the model described in the text.
Table 3. Selected structural and magnetic parameters for 1-D manganese compounds with μ1,3-azido bridge
P
(H = ꢀJ ij Si Sj); α = Mn–N–N angles; τ = Mn–N1–N3–Mn torsion angle.
d (Mn–N)/Å
α/°
τ/°
J/cmꢀ1
Ref.
[Mn(5–Fsalen)(N3)]n
[Mn(5-Meosalen)(N3)]n
[Mn(salen)(N3)]n
[Mn(5–Brsalen)(N3)]n
[Mn(salpn)(N3)]n
2.31
2.31
2.31
2.20
2.34
2.33
116.6
118.4
116.5
119.3
127.6
110.2
110.6
104.7
109.8
106.5
126.8
115.5
ꢀ8.8
ꢀ6.0
ꢀ5.2
ꢀ6.5
ꢀ6.2
ꢀ7.8
[34]
[34]
[33]
[29]
[20, 35]
Our study
[Mn(L)(N3)]n (1)
Salen = tetradentate Schiff base obtained from the condensation of salicylaldehyde with ethane-1,2-diamine.
Salpn = tetradentate Schiff base obtained from the condensation of salicylaldehyde with propane-1,3-diamine.
systems with short Mn–N distances, α angles close to 110°, and τ torsion angles similar to
0° (or 180°) should show the most antiferromagnetic interactions.
The exchange coupling of our compound, in agreement with every compound reported
in previous work (see table 3), shows antiferromagnetic behavior. However, comparing the
three factors mentioned above, it is not possible to establish any direct magneto-structural
correlations with the strength of the exchange coupling. It appears that these factors are
very much relevant and the first two are the deciding factors to control the strength of the
exchange coupling for these types of complexes [34, 37]. Therefore, it may be concluded
that 1 shows similar Mn–N distance found for this type of Mn(III) system (see table 3), α
angles close to 110°, and as a result, moderate antiferromagnetic behavior.
4. Conclusion
A new MnIII–Schiff base complex has been synthesized and characterized structurally,
showing that azide bridges successive Mn(III)–Schiff base units into a 1-D coordination
polymeric chain. Low-temperature magnetic measurements of the system reveal that μ1,3
-
bridging azides mediate antiferromagnetic interaction among the MnIII centers. The

16
P.P. Chakrabarty et al.
strength of antiferromagnetic interaction in this system is moderate and compares well with
other structurally identical azido-bridged MnIII chain systems. Preparation of the present
complex enriches the azide-based magneto chemistry, but also indicates that other closely
related magnetic systems can be designed by varying the Schiff base as well as the
transition metal.
Supplementary material
Crystallographic data for 1 have been deposited at the Cambridge Crystallographic Data
Center (CCDC) as Supplementary Publication CCDC No. 883775. Copies of the data can
be obtained free of charge on application to the CCDC, 12 Union Road, Cambridge CB2
1EZ, UK (Fax: +44 1223 336 033; E-mail: deposit@ccdc.cam.ac.uk or http://www.ccdc.
cam.ac.uk/conts/retrieving.html).
Acknowledgments
Financial support from DST [Sanction no. SR/FT/CS-060/2009] and UGC [Sanction no.
F.38-5/2009 (SR)], New Delhi to S. S. are gratefully acknowledged.
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