Table 3 Experimental crystal data and structure refinement parameters
the Ministry of Science and Technology (2011CB808505) and
the Open Project Program of Key Laboratory of Theoretical
Chemistry and Molecular Simulation of Ministry of Education
(Hunan University of Science and Technology).
for NH
4
[OV(O
)
2 2
(pprd)]·2H
2
O (8) and NH
4
[OV(O
)
2 2
2
(2-NH -pprd)]·
2
3H O (9)
Compound reference
8
9
Chemical formula
Formula mass
C
9
H
11
N
4
O
7
V
9 18 5 8
C H N O V
375.22
338.16
References
Crystal system
Orthorhombic
12.9276(14)
6.9044(6)
15.8482(13)
90.00
90.00
90.00
1414.6(2)
173(2)
Pnma
4
3638
Monoclinic
7.2721(16)
16.236(4)
12.963(3)
90.00
98.622(4)
90.00
1513.2(6)
173(2)
P21/c
a/Å
b/Å
c/Å
α/°
β/°
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γ/°
3
Unit cell volume/Å
Temperature/K
Space group
No. of formula units per unit cell, Z
No. of reflections measured
No. of independent reflections
4
12 607
3537
1363
R
int
0.0335
0.0408
0.0999
0.0570
0.1037
801329
0.0444
0.0916
0.2173
0.0972
0.2211
801327
Final R
Final wR(F ) values (I > 2σ(I))
Final R values (all data)
1
values (I > 2σ(I))
2
1
2
Final wR(F ) values (all data)
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CCDC number
Spectroscopic measurements
7
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Room temperature solid-state NMR experiments were performed
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5
607.
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51
13
51
7
8.8 MHz for V NMR and 75.5 MHz for C NMR. The
V
7
1
3
chemical shifts were referenced to VOCl , while the C chemi-
3
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cal shifts were referenced to the carbonyl carbon of glycine,
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silane. IR spectra were recorded on a Perkin–Elmer spectrometer
(Spectrum One).
9
The solution NMR spectra were recorded on a 500 MHz
Bruker AV II NMR spectrometer, operating at 500.13 MHz for
1
13
51
H NMR, 125.77 MHz for C NMR and 131.47 MHz for
V
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1
13
was used as an internal reference for H and C chemical shifts.
5
1
V chemical shifts were measured relative to the external stan-
dard VOCl3 with the upfield shifts considered as negative
values. The signal-to-noise ratios were improved by a line-broad-
ening factor of 2 Hz and 10 Hz in the Fourier transformation of
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1
3
51
all C and V spectra. In the NMR experiments, an ionic
−1
medium, 0.15 mol L NaCl D O, was chosen in order to rep-
2
2011, 365, 119–126; (f) B. R. Zeng, R. Q. Fu, S. H. Cai and Z. Chen,
resent physiological conditions. The temperature was generally
Inorg. Chem. Commun., 2009, 12, 1259–1262.
2
2
0 °C, while, in the variable temperature NMR, it varied from
0 °C to 40 °C at steps of 5 °C.
12 (a) A. Gorzsas, I. Anderson and L. Pettersson, J. Inorg. Biochem., 2009,
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7
to Tracey’s method. The main conditions of the experiments
149–151; (e) H. Schmidt, I. Andersson, D. Rehder and L. Pettersson,
−1
were: temperature 25 °C, 15.0 mmol L total vanadate, 0.6 mol
Chem.–Eur. J., 2001, 7, 251–257; (f) A. Gorzsas, I. Andersson and
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−
1
L
KCl, 20 mM HEPES buffer (pH 6.8) and variable amounts
−1
of the pprd-like ligands (0–6.0 mmol L ).
Detailed spectroscopic measurement results may be found in
the ESI.†
1
3 (a) D. A. Beauchamp and S. J. Loeb, Chem. Commun., 2002, 2484–
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Acknowledgements
This work was supported by the National Natural Science Foun-
dation of China (20803020, 20971041, 21172066, 51103122),
1
4 (a) A. Shaver, D. A. Hall, J. B. Ng, A. M. Lebuis, R. C. Hynes and
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This journal is © The Royal Society of Chemistry 2012
Dalton Trans., 2012, 41, 3684–3694 | 3693