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Supporting Information
for
Synthesis and characterization of ML and ML2 metal complexes with amino acid substituted bis(2-picolyl)amine ligands.
Đani Škalamera,a Ernest Sanders,a Robert Vianello,a Aleksandra Maršavelski,a Andrej
Pevec,b Iztok Turelb and Srećko I. Kirin*,a a Ruđer Bošković Institute, Bijenička cesta 54, 10 000 Zagreb, Croatia. E-mail: Srecko.Kirin@irb.hr b Faculty of Chemistry and Chemical Technology, University of Ljubljana, Vecna pot 113, 1000 Ljubljana, Slovenia.
Electronic Supplementary Material (ESI) for Dalton Transactions.This journal is © The Royal Society of Chemistry 2015
S2
Table of contents: 1. NMR spectra of ligands L1‐L5 ...................................................................................... S3‐S15
2. MS spectra of ligands L1‐L5 ....................................................................................... S16‐S20
3. NMR spectra of ML complexes ................................................................................. S21‐S35
4. NMR spectra of complex 12Zn ................................................................................... S36‐S41
5. IR spectra of metal complexes ......................................................................................... S42
6. X‐ray single crystal structure of coordination polymer 2p ............................................... S51
7. Crystallographic numbering scheme ................................................................................ S52
S3
1. N
MR spectra of ligands L1‐L5.
1H NMR (300 M
Hz, CD3CN) of ligand L1. B
pa‐CH2‐CH2‐CO
2Me.
PPM
8.0
7.0
6.0
5.0
4.0
3.0
2.0
1.0
0.0
pp
,;
S4
1H NMR (600 M
Hz, DMSO
‐d6) of ligand L1. B
pa‐CH2‐CH2‐CO
2Me.
9.00308.48288.48168.48038.47878.47498.47368.47218.47087.78077.77777.76797.76507.75527.75237.47247.45937.25847.25687.25027.24857.24607.24427.23797.2362
3.7450
3.5409
3.3130
2.77302.76122.74952.55522.54362.53182.50892.50592.50292.49992.4969
0.0000
S6
1H NMR (600 M
Hz, CDCl 3) of ligand L2. B
pa‐CH2‐CO
2Me.
PPM
8.0
7.0
6.0
5.0
4.0
3.0
2.0
1.0
0.0
pj
S15
13C NMR (75 M
Hz, DMSO
‐d6) of ligand L5. B
qa‐CH(CH3)Nph.
PPM
160
150
140
130
120
110
100
9080
7060
5040
3020
S16
2. M
S spectra of ligands L1 ‐ L5.
MS of ligand L1. B
pa‐CH2‐CH2‐CO
2Me.
2
x10
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.91
+ S
can:
1 (0
.174
-0.4
90 m
in, 2
2 sc
ans)
es_
2_20
1409
29_t
ic.d
286.
3000
0
308.
3000
0
Cou
nts
(%) v
s. M
ass-
to-C
harg
e (m
/z)
2040
6080
100
120
140
160
180
200
220
240
260
280
300
320
340
360
380
400
420
440
460
480
S19
MS of ligand L4. B
pa‐CH(CH3)Ph.
2x1
0
00.
050.1
0.150.
20.
250.3
0.350.
40.
450.5
0.550.
60.
650.7
0.750.
80.
850.9
0.951
+ S
can
(0.1
93-0
.446
min
, 35
scan
s) E
S_6
_201
4042
5_T
IC.d 20
0.30
000
304.
4000
0
105.
3000
0
326.
3000
0
Cou
nts
(%) v
s. M
ass-
to-C
harg
e (m
/z)
2040
6080
100
120
140
160
180
200
220
240
260
280
300
320
340
360
380
400
420
440
460
480
S20
MS of ligand L5. Bqa‐CH(CH3)Nph.
2
x10
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.91
+ S
can:
1 (0
.144
-0.4
45 m
in, 2
1 sc
ans)
ES
_40_
2015
0217
_TIC
.d
454.
3000
0
300.
2000
015
5.20
000
Cou
nts
(%) v
s. M
ass-
to-C
harg
e (m
/z)
2040
6080
100
120
140
160
180
200
220
240
260
280
300
320
340
360
380
400
420
440
460
480
500
520
540
560
580
S26
13C NMR (75 M
Hz, CD3CN) of complex 1b. [Zn
(L1)Br 2].
PPM
180
160
140
120
100
8060
4020
p[
()
]
172.3862
154.6216
149.2576
141.2455
125.4489124.9198118.2601118.0887118.0482
57.7994
52.295049.0471
29.6709
2.11651.84151.56591.2902
S34
1H NMR (300 M
Hz, DMSO
‐d6) of complex 5n. [Zn
(L5)(NO
3) 2].
1.6110
4.0254
4.8936
8.21588.11397.93297.90357.84547.82117.76737.74057.71587.67887.65317.53387.50917.48447.45257.42787.40627.37957.35377.2930
S36
4. N
MR spectra of complex 12Zn
. 1H NMR spectra of complex 12Zn.
1H NMR (300 M
Hz, CD3CN) of complex 12Zn. [Zn
(L1) 2](BF 4) 2.
S41
13C NMR (75 M
Hz, DMSO
‐d6) of complex 12Zn. [Zn
(L1) 2](BF 4) 2.
PPM
160
150
140
130
120
110
100
9080
7060
5040
3020
p[
()]
()
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