6
K. RAMALINGAM AND A. ILAKKIYA
Preparations
obtained was washed with dichloromethane and dried in
air.
Preparation of sodium salt of dithiocarbamate (Nadtc)
Amine (10 mmol) (N-ethylethanamine (de): 1.0 mL; N-
methylmethanamine (dm): 0.5 mL; N-prop-2-enyl-prop-2-
en-1-amine (da): 1.2 mL; N-methylcyclohexanamine (chm):
Preparation of [M(dedtc) ] (where M = Pb or Cd)
Lead nitrate (0.33 g, 1 mmol)/cadmium nitrate (0.30 g, 1 mmol)
were dissolved in water and an aqueous solution of sodium
diethyldithiocarbamate (0.45 g, 2 mmol) in ethanol–water (1:1)
was added with continuous stirring. Solid crystalline precipi-
tates were obtained, which were washed with ethanol and dried
in air, and the yield was about 80%.
1
.3 mL; N-ethylcyclohexanamine (che): 1.4 mL), and car-
bondisulfide (molar excess) in ethanol (5 mL) were mixed under
ice-cold condition (5°C) to form yellow solution of the corre-
sponding dithiocarbamic acid. An aqueous solution of sodium
hydroxide (0.4 g; 10 mmol) was then added with continuous stir-
ring. A pale yellow solution was obtained. Solid sodium salt was
obtained by slow evaporation of ethanol solution.3
References
1
. Kickelbick, G. (Ed.). Hybrid Materials, Synthesis, Characterization and
Applications; Wiley-VCH Verlag: Weinheim, Germany, 2007.
. Rath T.; Trimmel, G. Hybrid Mater. 2013, 1, 15-36.
Preparation of intercalated PbI and CdI
2
3
4
5
Sodium salts of dithiocarbamates (Nadedtc = sodium
diethyldithiocarbamate (0.11 g; 0.5 mmol), Nadmdtc = sodium
dimethyldithiocarbamate (0.07 g; 0.5 mmol), Nadaldtc =
sodium diallyldithiocarbamate (0.09 g; 0.5 mmol), Nachmdtc =
sodium cyclohexylmethyldithiocarbamate (0.10 g; 0.5 mmol),
Nachedtc = sodium cyclohexylethyldithiocarbamate (0.11 g;
. Kickelbick, G. Hybrid Mater. 2014, 1, 39-51.
. Kamat, P. V. J. Am. Chem. Soc. 2014, 136, 3713-3714.
. Burschka, J.; Pellet, N.; Moon, S-J.; Humpry-Baker, R.; Gao, P.;
Nazeeruddin, M. K.; Graetzel, M. Nature 2013, 499, 316-319.
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G.; Graetzel, M.; White, T. J. J. Mater. Chem. A 2013, 1, 5628-5641.
7
8
. Stoumpos, C. C.; Malliakas, C. D.; Kanatzidis, M. G. Inorg. Chem. 2013,
0
0
.5 mmol)) were allowed to react with a solution of PbI2 (0.23;
5
2, 9019-9038.
.5 mmol) in hot water (10 mL) and the formation of a flu-
. Wang, Y.; Gould, T.; Dobson, J. F.; Zhang, H.; Yang, H.; Yao, X.; Zhao,
orescent green precipitate was observed. The precipitate was
quickly filtered, washed with hot water, and dried in air. The
cadmium analogues were prepared by dissolving CdI2 (0.36 g;
H. Phys. Chem. Chem. Phys. 2014, 16, 1424-1429.
9. Gomez-Romero, G., Sanchez, C (Eds.). Functional Hybrid Materials;
Wiley-VCH Verlag: Weinheim, Germany, 2004.
1
1
0. Subba Rao, G. V.; Shafer, M. W. Levy, F (Ed.). Physics and Chemistry of
Materials with Layered Structures; Reidel: The Netherlands, 1979.
1. Gurina, G. I.; Savchenko, K. V. J. Solid State Chem. 2004, 177, 909-915.
1
mmol) in ethanol (10 mL) and reacting with equi-molar
sodium dithiocarbamates in ethanol. The yields obtained, melt-
ing points, and elemental analyses are as follows: [PbI2(dedtc)2]
12. Gurina, G. I.; Savchenko, K. V. J. Photochem. Photobiol. A 1995, 86,
(
1): C10H20 I2N2PbS4, Mol. Wt: 757.2; Anal. Calcd. (%): C,
81-84.
1
3. Mehrotra, V.; Lombardo, S.; Thompson, M. O.; Giannelis, E. P. Phys.
Rev. B 1991, 44, 5786-5790.
4. Glatfelter, A.; Dybowski, C.; Bai, S.; Perry, D. L. Mater. Lett. 2007, 61,
1
5.86; H, 2.66; N, 3.70; Found: C, 15.82; H, 2.63; N, 3.67;
[
PbI2(dmdtc)2]·C2H5OH·H2O (2): C8H20I2N2O2PbS4, Mol.
1
Wt: 765.1; Anal. Calcd. (%): C, 12.56; H, 2.63; N, 3.66; Found:
C, 12.52; H, 2.60; N, 3.62; [PbI2(daldtc)2] (3): C14H20 I2N2PbS4,
Mol. Wt: 805.2; Anal. Calcd. (%): C, 20.88; H, 2.50; N, 3.48;
Found: C, 20.84; H, 2.47; N, 3.43; [PbI2(chmdtc)2] (4): C16H28
I2N2PbS4, Mol. Wt: 837.3; Anal. Calcd. (%): C, 22.95; H, 3.37;
N, 3.34; Found: C, 22.89; H, 3.33; N, 3.30; [PbI2(chedtc)2] (5):
C18H32 I2N2PbS4, Mol. Wt: 865.4; Anal. Calcd. (%): C, 24.98; H,
4
37-439.
15. Novosad, S. S.; Novosad, I. S.; Goncharuk, V. E.; Kostyk, L. V. Funct.
Mater. 2004, 11, 735-741.
1
6. Matuchová, M.; Prochazková, O.; Zdanský, K.; Zavadil, J.; Maixner, J.
Mat. Sci. Forum 2005, 477, 480-481.
1
7. Wang, W.; Qiao, J.; Wang, L.; Duan, L.; Zhang, D.; Yang, W.; Qiu, Y.
Inorg. Chem. 2007, 46, 10252-10260.
18. Chen, W.; Wang, M.; Liu, X.; Guo, G.; Huang, J. J. Crystal Growth Des.
2006, 6, 2289-2300.
3
.73; N, 3.24; Found: C, 24.94; H, 3.69; N, 3.20; [CdI2(dedtc)2]
6): C10H20Cd I2N2S4, Mol. Wt.: 662.4; Anal. Calcd. (%): C,
8.13; H, 3.04; N, 4.23; Found: C, 18.09; H, 3.00; N, 4.20;
CdI2(dmdtc)2] (7): C6H12CdI2N2S4, Mol. Wt.: 606.3; Anal.
1
9. Baibarak, M.; Baltog, I.; Lafrant, S. Solid State Chem. 2009, 182, 827-
(
8
35.
1
[
2
0. Preda, N.; Mihut, L.; Biabarac, M.; Baltog, I.; Husanu, M.; Bucur, C.;
Velula, T. Rom. J. Phys. 2009, 54, 667-675.
Calcd.(%): C, 11.89; H, 1.99; N, 4.62; Found: C, 11.85; H, 1.95;
N, 5.59; [CdI2(daldtc)2] (8): C14H20CdI2N2S4, Mol. Wt.: 710.4;
Anal. Calcd. (%): C, 23.67; H, 2.84; N, 3.94; Found: C, 23.64; H,
21. Savchuk, A. I.; Fediv, V. I.; Kandyba, Ye. O.; Savchuk, T. A.; Stolyarchuk,
V.; Nikitin, P. I. Mater. Sci. Eng. C 2002, 19, 59-62.
2
2
2
2
2. Schluter, I. Ch.; Schluter, M. Phys. Rev. B 1974, 9, 1652-1655.
3. Robertson, J. Solid State Commun. 1978, 26, 791-794.
4. Hogarth, G. Prog. Inorg. Chem. 2005, 53, 71-561.
2
7
2
.80; N, 3.90; [CdI2(chmdtc)2] (9): C16H28CdI2N2S4, Mol. Wt.:
42.5; Anal. Calcd. (%): C, 25.88; H, 3.80; N, 3.77; Found: C,
5.84; H, 3.76; N, 3.74; [CdI2(chedtc)2] (10): C18H32 Cd I2N2S4,
5. Coucouvanis, D. Prog. Inorg. Chem. 1979, 26, 301-469.
26. Van Wart, H. E.; Scheraga, H. A. Proc. Natl. Acad. Sci. USA 1986, 83,
Mol. Wt.: 770.6; Anal. Calcd.(%): C, 28.06; H, 4.19; N, 3.63;
Found: C, 28.02, H, 4.16; N, 3.59.
3064-3067.
2
2
7. Tubbs, M. R. J. Phys. Chem. Solids 1968, 29, 1191-1203.
8. Thirumaran, S.; Ramalingam, K.; Bocelli, G.; Cantoni, A. Polyhedron
2000, 19, 1279-1282.
2
9. Constantino, V. R. L.; Barbosa, C. A. S.; Bizeto, M. A.; Dias, P. M. An.
Acad. Bras. Ci. 2000, 72, 45-49.
0. Coucouvanis, D. Prog. Inorg. Chem. 1970, 11, 233-271.
1. Ramalingam, K.; Alexander, N.; Rizzoli, C. Monatsh Chem. 2013, 144,
Preparation of [MI (dedtc) ] (where M = Pb or Cd)
3
3
[
M(dedtc)2] (1 mmol) (where M = Pb or Cd) was dissolved
in dichloromethane, and a dilute solution of iodine (1 mmol)
in chloroform (50 mL) was added drop-wise with continuous
stirring over a long period of time (60 min). The precipitate
1
329-1334.
3
2. Alexander, N.; Ramalingam. K.; Rizzoli, C. Inorg. Chim. Acta 2011,
365, 480-483.