Inorganic Chemistry
Article
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atmosphere with a flow of 20 mL min and a heating rate of 10 °C
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1
min . The Brunauer−Emmet−Teller (BET) surface areas were
determined by N2 adsorption at −196 °C, whereas the CO
contacting The Cambridge Crystallographic Data Centre, 12
Union Road, Cambridge CB2 1EZ, UK; fax: +44 1223 336033.
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adsorption isotherms were determined at 0 °C using a Micromeritics
ASAP 2010 sorptometer. Prior to the measurements of adsorption/
desorption isotherms, the samples were outgassed for 20 h under a
pressure of 0.25 mmHg. The DLS spectra were recorded on
NanoPlus-3 (Nano Particle Size and Zeta Potential Analyzer from
Micromeritics Corp). The morphologies and elemental distribution of
the obtained materials were characterized by scanning electron
microscopy (SEM, XL 30 ESEMFEG, FEI Company). Diffraction
data were collected by ω-scan techniques at room temperature for
ligand L on a Rigaku Super Nova four-circle diffractometer with an
Atlas CCD detector and mirror-monochromated Cu Kα radiation (λ
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Corresponding Author
Artur R. Stefankiewicz − Faculty of Chemistry, Adam
Mickiewicz University, 61-614 Poznan
,
́
=
1.54178 Å) and for complex [FeL ] (SiF )(BF ) ·12H OC2 at
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2
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4
2
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00 (1) K, on the Rigaku Xcalibur four-circle diffractometer with an
Eos CCD detector and graphite-monochromated Mo Kα radiation
λ = 0.71069 Å). Data were corrected for Lorentz polarization as well
(
Authors
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as for absorption effects. Precise unit-cell parameters were
determined by a least-squares fit of reflections of the highest intensity,
chosen from the whole experiment. Using Olex2, the structures
were solved with the olex2.solve structure solution program using
charge flipping for complex C2 and with SHELXT-2013 for ligand L
Anna Brzechwa-Chodzyn
Mickiewicz University, 61-614 Poznan,
Advanced Technologies, 61-614 Poznan,
Michał Zielin
University, 61-614 Poznan,
Mirosław Gilski − Faculty of Chemistry, Adam Mickiewicz
Poland; Center for
́
ska − Faculty of Chemistry, Adam
́
Poland; Center for
Poland
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Poland
and refined with the ShelXL refinement package using least squares
minimization. Diffraction data for complex [FeL ](BF ) ·9H OC1
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4
2
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University, 61-614 Poznan
Biocrystallographic Research, Institute of Bioorganic Chemistry,
Polish Academy of Sciences, 61-704 Poznan, Poland
,
́
were collected at 100 K and λ = 0.9763 Å using synchrotron X-ray
radiation at the EMBL P13 beamline of the Petra III storage ring,
Hamburg. The complex C1 deposited as dark red, rhombic crystals,
space group Fdd2. Integration, scaling, and merging of the intensity
data were carried out in the XDS package. The unit-cell parameters,
Bravais lattice, and symmetry were determined using the XPREP
package. The structures were solved by using SHELXT. Detailed
analysis of the diffraction data indicated that the crystal appeared to
be merohedrally twinned by inversion with two domains. and twin
fractions were refined to 0.44 and 0.56, respectively. The structures
were refined by using SHELXL with anisotropic displacement
parameters for all non-hydrogen atoms and TWIN instruction. All
hydrogen atoms were included at geometrically predicted coordinates.
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Jack M. Harrowfield − ISIS, Universite de Strasbourg, 67083
Strasbourg, France
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Author Contributions
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The manuscript was written through contributions of all
authors. All authors have given approval to the final version of
the manuscript.
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Spectroscopic Data. L. Yield: 50%. H NMR (300 MHz, DMSO-
3
2
d ): δ [ppm] 8.98 (d, J = 1.8 Hz, 1H, H ), 8.73 (s, 1H, H ), 8.69 (d, J
Funding
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=
4.1 Hz, 1H, H ), 8.41 (m, 2H, H , H ), 8.20 (dd, J = 2.4, 8.3 Hz,
H, H ), 7.95 (td, J = 1.7, 7.7, 15.5 Hz, 1H, H ), 7.45 (m, 1H, H ),
.96 (s 1H, H ). C NMR (75 MHz, DMSO-d ): δ [ppm] 163.26,
56.21, 154.97, 153.55, 149.34, 145.89, 137.33, 133.43, 131.26,
24.10, 120.40, 120.25, 118.72. IR (FT-ATR): ν 3316, 3151, 1651,
589 cm . HRMS (ESI) m/z calcd for C H N : 250.1087. Found:
L + H] = 250.1089. Elemental analysis calcd (%) for C H N : C,
A.R.S. thanks the National Science Centre (grant SONATA
BIS 2018/30/E/ST5/00032) for financial support. The work
was supported by grant no. POWR.03.02.00-00-I026/16
cofinanced by the European Union through the European
Social Fund under the Operational Program Knowledge
Education Development.
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8
7
1
6
1
1
1
1
13
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1
4
12
5
+
[
14 12 5
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7.46; H, 4.45; N, 28.10. Found: C, 66.41; H, 4.86; N, 28.92.
Notes
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[
FeL ](BF ) ·9H OC1. Yield: 80%. H NMR (600 MHz, MeCN-
3
4 2
2
The authors declare no competing financial interest.
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d ): δ [ppm] 8.57 (m 6H, H ,H ), 8.29 (m, 9H, H ,H ), 8.16 (m, 3H,
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H ), 7.49 (m, 9H, H , H , H ), 5.82 (d, J = 15.6 Hz, 6H, H ). IR (FT-
ATR): ν 3373, 3196, 1620, 1595, 1024 cm . HRMS (ESI) m/z calcd
for C H FeN : 401.6191. Found: [3L + Fe] = 401.6198.
Elemental analysis calcd (%) for [FeL ](BF ) ·9H O: C, 44.27; H,
4
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ACKNOWLEDGMENTS
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A.R.S and A.B.-C. would like to thank Prof. Maciej Kubicki and
G. Dutkiewicz for their help with X-ray analysis. We are
grateful to the EMBL/DESY personnel, especially Dr. G.
Pompidor for assistance at the P13 beamline of the Petra III,
Hamburg.
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4
2
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.51; N, 18.44. Found: C, 45.17; H, 4.11; N, 19.40.
ASSOCIATED CONTENT
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*
sı Supporting Information
REFERENCES
Synthesis and NMR analysis of compounds 2, 3, 4, L,
C1; ESI-MS analysis, IR spectra, dynamic light scattering
analysis of L; scanning electron microscopy image of L;
temperature coefficient of the NH signal; crystal data
and structure refinement for L and C1; VT−UV−vis
analysis for C1 extended structure definition for
7
1
(
4674.
2) Batten, S. R.; Champness, N. R.; Chen, X.-M.; Garcia-Martinez,
̈
J.; Kitagawa, S.; Ohrstro
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H
Inorg. Chem. XXXX, XXX, XXX−XXX