triorganotin(iv) cation-promoted dimethyl carbonate ... · supplementary data fig. s2: molecular...
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Supplementary data
Triorganotin(IV) cation-promoted dimethyl carbonate synthesis from CO2 and methanol: Solution and solid-state characterization of an unexpected diorganotin(IV)-oxo cluster
Petr Šveca*, Hélène Catteyb, Zdeňka Růžičkováa, Josef Holubc, Aleš Růžičkaa and Laurent Plasseraudb*
a Department of General and Inorganic Chemistry, Faculty of Chemical Technology, University of Pardubice, Studentská 95, CZ-532 10, Pardubice, Czech Republic.
b Institut de Chimie Moléculaire de l’Université de Bourgogne (ICMUB), UMR CNRS 5260, UFR Sciences et Techniques, 9 allée A. Savary, BP 47870, F-21078 DIJON Cedex, France.
c Institute of Inorganic Chemistry, Academy of Sciences of the Czech Republic, Husinec-Řež 1001, CZ-250 68, Řež, Czech Republic.
*Corresponding author, e-mail: [email protected], [email protected]
Content of the supplementary data:
Fig. S1 - General NMR numbering of LCN, n-Bu, Ph and [CB11H12]– moieties S2
Fig. S2 - Molecular structure of 6 S3
Table S1 - Selected crystallographic data of 4a, 6 and 7 S4
NMR spectra of 1, 2, 4, 5, 6 and 7 S5-S21
S1
Electronic Supplementary Material (ESI) for New Journal of Chemistry.This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2018
Supplementary data
Fig. S1: General NMR numbering of LCN, n-Bu, Ph and [CB11H12]– moieties
S2
Supplementary data
Fig. S2: Molecular structure of 6 (ORTEP presentation, 50% probability level). Hydrogen
atoms are omitted for clarity. Relevant interatomic distances [Å] and angles [°] are very close
to that reported for structurally related methylimidazolium and n-butylpyridinium 1-carba-
closo-dodecaborates* and are thus not included.
* A. S. Larsen, J. D. Holbrey, F. S. Tham, C. A. Reed, J. Am. Chem. Soc., 2000, 122, 7264; J.
Dymon, R. Wibby, J. Kleingardner, J. M. Tanski, I. A. Guzei, J. D. Holbrey, A. S. Larsen,
Dalton Trans., 2008, 2999.
S3
Supplementary data
Table S1: Selected crystallographic data of 4a, 6 and 7
Compound 4a 6 7
Empirical formula C38H38BF15NOSn C11H28B11N C90H220B22O16Sn10
Crystal system triclinic monoclinic triclinic
Space group P-1 C 1 2 1 P-1
a (Å) 12.0570(6) 22.693(4) 13.205(2)
b (Å) 12.2820(6) 7.2234(11) 20.512(3)
c (Å) 13.6270(12) 14.941(3) 24.8670(12)
(°) 103.857(6) 90 88.883(7)
(°) 105.667(6) 131.136(8) 88.070(6)
(°) 94.144(5) 90 87.940(11)
Z 2 4 2
V (Å3) 1866.1(2) 1844.5(6) 6726.2(14)
Dc (g.cm-3) 1.671 1.056 1.473
Crystal size (mm) 0.29 x 0.25 x 0.21 0.35 x 0.27 x 0.17 0.5 x 0.31 x 0.27
Crystal shape block prism block
(mm-1) 0.793 0.051 1.871
F(000) 942 624 2996
h; k; l range -15, 15; -15, 15; -17, 17 -29, 29; -9, 9; -19, 19 -16, 16; -24, 24; -30, 30
range (°) 25.242 - 27.500 3.062- 27.523 1.544 - 25.600
Reflections measured 38020 21921 65542
- independent (Rint) a) 7609 (0.0401) 4253 (0.0399) 24041 (0.1005)
- observed [I>2(I)] 8558 4014 16772
Parameters refined 518 215 1255
Max/min (eÅ-3) 1.326 / -0.867 0.176 / -0.192 4.058 / -3.380
GOF b) 1.116 1.024 1.163
R c) / wR c) 0.0311 / 0.0737 0.0390 / 0.0937 0.0823 / 0.2125
aRint = Σ│Fo2 - Fo,mean
2│/ΣFo2, bGOF = [Σ(w(Fo
2 - Fc2)2)/(Ndiffrs - Nparams)]½ , cWeighting scheme: w =
[σ2(Fo2) + (w1P)2 + w2P]-1, where P = [max(Fo
2) + 2Fc2], R(F) = Σ││Fo│ - │Fc││/Σ│Fo│, wR(F2) =
[Σ(w(Fo2 - Fc
2)2)/(Σw(Fo2)2)]½
S4
Supplementary data
1H NMR spectrum of starting LCN(n-Bu)2SnCl (1)
S5
Supplementary data
13C{1H} NMR spectrum of starting LCN(n-Bu)2SnCl (1)
S6
Supplementary data
119Sn{1H} NMR spectrum of starting LCN(n-Bu)2SnCl (1)
S7
Supplementary data
1H NMR spectrum of starting LCNPh2SnCl (2)
S8
Supplementary data
13C{1H} NMR spectrum of starting LCNPh2SnCl (2)
S9
Supplementary data
119Sn{1H} NMR spectrum of starting LCNPh2SnCl (2)
S10
Supplementary data
1H NMR spectrum of [LCN(n-Bu)2Sn]+[CB11H12]– (4)
S11
Supplementary data
11B{1H} NMR spectrum of [LCN(n-Bu)2Sn]+[CB11H12]– (4)
119Sn{1H} NMR spectrum of [LCN(n-Bu)2Sn]+[CB11H12]– (4)
S12
Supplementary data
13C{1H} NMR spectrum of [LCN(n-Bu)2Sn]+[CB11H12]– (4)
S13
Supplementary data
1H NMR spectrum of [LCNPh2Sn]+[CB11H12]– (5)
S14
Supplementary data
11B{1H} NMR spectrum of [LCNPh2Sn]+[CB11H12]– (5)
119Sn{1H} NMR spectrum of [LCNPh2Sn]+[CB11H12]– (5)
S15
Supplementary data
13C{1H} NMR spectrum of [LCNPh2Sn]+[CB11H12]– (5)
S16
Supplementary data
1H NMR spectrum of [BnNMe3]+[CB11H12]− (6)
S17
Supplementary data
13C{1H} NMR spectrum of [BnNMe3]+[CB11H12]− (6)
S18
Supplementary data
119Sn{1H} NMR spectrum of [(n-Bu)20Sn10O2(OMe)6(CO3)2]2+.[CB11H12]2− (7)
S19
Supplementary data
13C{1H} NMR spectrum of [(n-Bu)20Sn10O2(OMe)6(CO3)2]2+.[CB11H12]2− (7)
S20
Supplementary data
11B{1H} NMR spectrum of [(n-Bu)20Sn10O2(OMe)6(CO3)2]2+.[CB11H12]2− (7)
S21