[Re
6
(μ
3
-Se)
8
]
2+
core-containing cluster complexes with isonicotinic acid: synthesis, structural characterization, and hydrogen-bonded assemblies
William C. Corbin
†
• Gary S. Nichol
‡
• Zhiping Zheng
†
*
†
Department of Chemistry and Biochemistry, The University of Arizona, Tucson, AZ 85721, USA
‡ School of Chemistry, The University of Edinburgh, West Mains Road, Edinburgh, Scotland, EH9 3JJ, UK
* Corresponding author. Email: zhiping@email.arizona.edu
. Fax: (520) 621-8407
Journal of Cluster Science
S1. 31 P NMR and 1 H NMR of 1 in CD
2
Cl
2
*
S2. 31 P NMR and 1 H NMR of 2 in CD
3
OD*
S3. 31 P NMR and 1 H NMR of 3 in CD
2
Cl
2
*
S4. High resolution mass spectra of compounds
S5. Zoomed high resolution mass spectra of compounds
S6. Theoretical high resolution mass spectra of 1
S7. Theoretical high resolution mass spectra of 2 and 3
S8. Mass spectrometer parameters and spectra data
S9. Crystal packing of 1
S10. Crystal packing of 2a
S.11 Crystal packing of 2b
S.12 Crystal packing of 3

S1. 31 P NMR (top) and 1 H NMR (bottom) of (1) in CD
2
Cl
2
*

S2. 31 P NMR (top) and 1 H NMR (bottom) of (2) in CD
3
OD*.

S3. 31 P NMR (top) and 1 H NMR (bottom) of (3) in CD
2
Cl
2
*

Intens.
x10
9
6
4
2
4
2 x10
0
9
5
4
3
2
1 x10
0
9
6
0
0
1233.74655
622.02896
922.00977
1233.74615
1521.97162
622.02897
922.00972
1231.27310
1521.97185
2121.93299
2121.93273
14_0342_I_126_000003.d: +MS
14_0396_I_124_000002.d: +MS
14_0396_I_125_000002.d: +MS
500 1500 2000 2500 3000 1000
S4. High resolution mass spectra of (3) (top), (2) (middle), and (1) (bottom)
3500 4000 m/z

Intens.
x10
9
6
4
1233.74655
14_0342_I_126_000003.d: +MS
2
4
2
1 x10
0
9
3
2 x10
0
9
5
4
6
0
1231.27310
1233.74615
1220 1230 1235 1240 1245 1250 1255 1225
S5. Zoomed high resolution mass spectra of (3) (top), (2) (middle), and (1) (bottom)
14_0396_I_124_000002.d: +MS
14_0396_I_125_000002.d: +MS m/z

S6. Theoretical high resolution mass spectra of (1)

S7. Theoretical high resolution mass spectra of (2) and (3)

Accurate Mass Determination
Instrument: Bruker 9.4 T Apex-Qh Hybrid Fourier Transfer Ion-Cyclotron Resonance (FT-ICR) instrument
Ionization: Electrospray ionization (ESI) at 100 K, spray voltage 4500 V, spray solvent MeOH/MeCN, infusion flow rate 3μL/min.
Sample ID
(3)
Ion
M - H
M +2
2M - H
Charge
1
2
3
Measured m/z
2466.48166
1233.74655
1644.66106
Theoretical m/z
2466.48723
1233.747253
1644.6645
Error (mDa)
5.57
-0.703
-3.44
Relative Error (ppm)
2.258272385
-0.569808766
-2.091611998
(2)
(1)
M - H
M +2
2M - H
M - H
M +2
2M - H
M + SbF6-
1
2
3
2466.48612
1233.74615
1644.66106
2466.48723
1233.747253
1644.66593
1.11
-1.103
-4.87
1
2
3
1
2461.547665
1231.2731
1642.039013
2699.448345
2461.546329
1231.276803
1642.0364
2699.43926
-1.336
-3.703
2.613
9.085
S8. Mass spectrometer parameters and spectral data
0.450032738
-0.89402428
-2.961087666
-0.542747971
-3.007447221
1.591316733
3.36551377

S9. Crystal packing of (1) looking down the a axis. Blue dotted lines indicate hydrogen bonds. Hydrogen atoms omitted for clarity. Anisotropic displacement ellipsoids are drawn at the 50% probability.

S10. Crystal packing of (2a) looking down the a axis. Blue dotted lines indicate hydrogen bonds. Hydrogen atoms omitted for clarity. Anisotropic displacement ellipsoids are drawn at the 50% probability.

S11. Crystal packing of (2b) looking down the a axis. Blue dotted lines indicate hydrogen bonds. Hydrogen atoms omitted for clarity. Anisotropic displacement ellipsoids are drawn at the 50% probability.

S12. Crystal packing of (3) looking down the a axis. Red dotted lines indicate hydrogen bonds. Hydrogen atoms omitted for clarity. Anisotropic displacement ellipsoids are drawn at the 50% probability.