Sintesis dan penentuan struktur kompleks di-tert-butilstanum (IV) ditiokarbamat

Translated title of the contribution: Synthesis and structure determination of di-tert-butyltin (IV) dithiocarbamate

Amirah Faizah Abdul Muthalib, Ibrahim Baba, Yang Farina Abdul Aziz, Wahid Samsudin

Research output: Contribution to journalArticle

Abstract

New diorganotin(IV) dithiocarbamate complexes have been synthesized from di-tert-butyltin(IV) dichloride, N-dialkylamine and carbon disulphide. Elemental and gravimetric analysis confirmed the general formula of these complexes as (t-C4H9)2Sn[S2CNR1R2]2 (R1 = CH3, C2H5, C7H7 dan R2 = C2H5, C6H11, iC3H7, CH3, C2H5, C4H9, C7H7). The structures of these complexes have been elucidated on the basis of infrared, ultraviolet, 1H, 13C & 119Sn NMR spectroscopy and X-ray crystallography. The infrared spectra of these complexes showed three main peaks for v(C - N), v(C - S) and v(Sn-S) bands that appeared in the region of 1447-1496, 947-988 and 352-370 cm-1, respectively. The 13C NMR spectrum showed the chemical shift for δ(N13CS2) in the range of 199.1-201.8 ppm. X-ray single crystal structure (C4H9)2Sn[S2CN(CH3)(iC3H7)]2 demonstrated a six-coordination geometry around the tin atom adopting a monoclinic system with a space group of P2/n with a = 11.2934(11) Å, b = 7.0175(7) Å, c = 15.6894(15) Å; β = 95.016(1)°. The (N-benzyl-N-ethyldithiocarbamato)chlorido di-tert-butyltin(IV) and (N, N-dibenzyldithiocarbamato)chlorido-di-(tert-butyl)tin(IV) formed a different geometry with one dithiocarbamate ligand and one chlorine atom attached to the tin centre to form a five-coordinate structure. Crystal of (N-benzyl-N-ethyldithiocarbamato)chlorido di-tert-butyltin(IV) adopts a triclinic system with space group of P1 and cell parameter of a = 8.6140 (2) Å, b = 10.9604 (3) Å, c = 11.4765 (3) Å; α = 91.858 (2) °, β = 96.193 (2) °, γ = 96.011 (2) °, while (N,N-dibenzyldithiocarbamato)chlorido-di-(tert-butyl)tin(IV) adopts a monoclinic system with space group of P2i with cell parameter a = 9.0600 (2) Å, b = 10.9238 (2) Å, c = 12.7845 (3) Å; β = 102.759 (2) °.

Original languageUndefined/Unknown
Pages (from-to)214-223
Number of pages10
JournalMalaysian Journal of Analytical Sciences
Volume17
Issue number2
Publication statusPublished - 2013

Fingerprint

Tin
Carbon Disulfide
Infrared radiation
Atoms
Geometry
Gravimetric analysis
X ray crystallography
Chlorine
Chemical shift
Nuclear magnetic resonance spectroscopy
Crystal structure
Nuclear magnetic resonance
Single crystals
Ligands
X rays
Crystals
Chemical analysis

Keywords

  • Di-tert-butyltin(IV)
  • Dithiocarbamate

ASJC Scopus subject areas

  • Analytical Chemistry

Cite this

Sintesis dan penentuan struktur kompleks di-tert-butilstanum (IV) ditiokarbamat. / Muthalib, Amirah Faizah Abdul; Baba, Ibrahim; Abdul Aziz, Yang Farina; Samsudin, Wahid.

In: Malaysian Journal of Analytical Sciences, Vol. 17, No. 2, 2013, p. 214-223.

Research output: Contribution to journalArticle

Muthalib, Amirah Faizah Abdul ; Baba, Ibrahim ; Abdul Aziz, Yang Farina ; Samsudin, Wahid. / Sintesis dan penentuan struktur kompleks di-tert-butilstanum (IV) ditiokarbamat. In: Malaysian Journal of Analytical Sciences. 2013 ; Vol. 17, No. 2. pp. 214-223.
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abstract = "New diorganotin(IV) dithiocarbamate complexes have been synthesized from di-tert-butyltin(IV) dichloride, N-dialkylamine and carbon disulphide. Elemental and gravimetric analysis confirmed the general formula of these complexes as (t-C4H9)2Sn[S2CNR1R2]2 (R1 = CH3, C2H5, C7H7 dan R2 = C2H5, C6H11, iC3H7, CH3, C2H5, C4H9, C7H7). The structures of these complexes have been elucidated on the basis of infrared, ultraviolet, 1H, 13C & 119Sn NMR spectroscopy and X-ray crystallography. The infrared spectra of these complexes showed three main peaks for v(C - N), v(C - S) and v(Sn-S) bands that appeared in the region of 1447-1496, 947-988 and 352-370 cm-1, respectively. The 13C NMR spectrum showed the chemical shift for δ(N13CS2) in the range of 199.1-201.8 ppm. X-ray single crystal structure (C4H9)2Sn[S2CN(CH3)(iC3H7)]2 demonstrated a six-coordination geometry around the tin atom adopting a monoclinic system with a space group of P2/n with a = 11.2934(11) {\AA}, b = 7.0175(7) {\AA}, c = 15.6894(15) {\AA}; β = 95.016(1)°. The (N-benzyl-N-ethyldithiocarbamato)chlorido di-tert-butyltin(IV) and (N, N-dibenzyldithiocarbamato)chlorido-di-(tert-butyl)tin(IV) formed a different geometry with one dithiocarbamate ligand and one chlorine atom attached to the tin centre to form a five-coordinate structure. Crystal of (N-benzyl-N-ethyldithiocarbamato)chlorido di-tert-butyltin(IV) adopts a triclinic system with space group of P1 and cell parameter of a = 8.6140 (2) {\AA}, b = 10.9604 (3) {\AA}, c = 11.4765 (3) {\AA}; α = 91.858 (2) °, β = 96.193 (2) °, γ = 96.011 (2) °, while (N,N-dibenzyldithiocarbamato)chlorido-di-(tert-butyl)tin(IV) adopts a monoclinic system with space group of P2i with cell parameter a = 9.0600 (2) {\AA}, b = 10.9238 (2) {\AA}, c = 12.7845 (3) {\AA}; β = 102.759 (2) °.",
keywords = "Di-tert-butyltin(IV), Dithiocarbamate",
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year = "2013",
language = "Undefined/Unknown",
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pages = "214--223",
journal = "Malaysian Journal of Analytical Sciences",
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T1 - Sintesis dan penentuan struktur kompleks di-tert-butilstanum (IV) ditiokarbamat

AU - Muthalib, Amirah Faizah Abdul

AU - Baba, Ibrahim

AU - Abdul Aziz, Yang Farina

AU - Samsudin, Wahid

PY - 2013

Y1 - 2013

N2 - New diorganotin(IV) dithiocarbamate complexes have been synthesized from di-tert-butyltin(IV) dichloride, N-dialkylamine and carbon disulphide. Elemental and gravimetric analysis confirmed the general formula of these complexes as (t-C4H9)2Sn[S2CNR1R2]2 (R1 = CH3, C2H5, C7H7 dan R2 = C2H5, C6H11, iC3H7, CH3, C2H5, C4H9, C7H7). The structures of these complexes have been elucidated on the basis of infrared, ultraviolet, 1H, 13C & 119Sn NMR spectroscopy and X-ray crystallography. The infrared spectra of these complexes showed three main peaks for v(C - N), v(C - S) and v(Sn-S) bands that appeared in the region of 1447-1496, 947-988 and 352-370 cm-1, respectively. The 13C NMR spectrum showed the chemical shift for δ(N13CS2) in the range of 199.1-201.8 ppm. X-ray single crystal structure (C4H9)2Sn[S2CN(CH3)(iC3H7)]2 demonstrated a six-coordination geometry around the tin atom adopting a monoclinic system with a space group of P2/n with a = 11.2934(11) Å, b = 7.0175(7) Å, c = 15.6894(15) Å; β = 95.016(1)°. The (N-benzyl-N-ethyldithiocarbamato)chlorido di-tert-butyltin(IV) and (N, N-dibenzyldithiocarbamato)chlorido-di-(tert-butyl)tin(IV) formed a different geometry with one dithiocarbamate ligand and one chlorine atom attached to the tin centre to form a five-coordinate structure. Crystal of (N-benzyl-N-ethyldithiocarbamato)chlorido di-tert-butyltin(IV) adopts a triclinic system with space group of P1 and cell parameter of a = 8.6140 (2) Å, b = 10.9604 (3) Å, c = 11.4765 (3) Å; α = 91.858 (2) °, β = 96.193 (2) °, γ = 96.011 (2) °, while (N,N-dibenzyldithiocarbamato)chlorido-di-(tert-butyl)tin(IV) adopts a monoclinic system with space group of P2i with cell parameter a = 9.0600 (2) Å, b = 10.9238 (2) Å, c = 12.7845 (3) Å; β = 102.759 (2) °.

AB - New diorganotin(IV) dithiocarbamate complexes have been synthesized from di-tert-butyltin(IV) dichloride, N-dialkylamine and carbon disulphide. Elemental and gravimetric analysis confirmed the general formula of these complexes as (t-C4H9)2Sn[S2CNR1R2]2 (R1 = CH3, C2H5, C7H7 dan R2 = C2H5, C6H11, iC3H7, CH3, C2H5, C4H9, C7H7). The structures of these complexes have been elucidated on the basis of infrared, ultraviolet, 1H, 13C & 119Sn NMR spectroscopy and X-ray crystallography. The infrared spectra of these complexes showed three main peaks for v(C - N), v(C - S) and v(Sn-S) bands that appeared in the region of 1447-1496, 947-988 and 352-370 cm-1, respectively. The 13C NMR spectrum showed the chemical shift for δ(N13CS2) in the range of 199.1-201.8 ppm. X-ray single crystal structure (C4H9)2Sn[S2CN(CH3)(iC3H7)]2 demonstrated a six-coordination geometry around the tin atom adopting a monoclinic system with a space group of P2/n with a = 11.2934(11) Å, b = 7.0175(7) Å, c = 15.6894(15) Å; β = 95.016(1)°. The (N-benzyl-N-ethyldithiocarbamato)chlorido di-tert-butyltin(IV) and (N, N-dibenzyldithiocarbamato)chlorido-di-(tert-butyl)tin(IV) formed a different geometry with one dithiocarbamate ligand and one chlorine atom attached to the tin centre to form a five-coordinate structure. Crystal of (N-benzyl-N-ethyldithiocarbamato)chlorido di-tert-butyltin(IV) adopts a triclinic system with space group of P1 and cell parameter of a = 8.6140 (2) Å, b = 10.9604 (3) Å, c = 11.4765 (3) Å; α = 91.858 (2) °, β = 96.193 (2) °, γ = 96.011 (2) °, while (N,N-dibenzyldithiocarbamato)chlorido-di-(tert-butyl)tin(IV) adopts a monoclinic system with space group of P2i with cell parameter a = 9.0600 (2) Å, b = 10.9238 (2) Å, c = 12.7845 (3) Å; β = 102.759 (2) °.

KW - Di-tert-butyltin(IV)

KW - Dithiocarbamate

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