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Cherkasova, T. G.; Chenskaya, V; Tryasunov, B. G.

doi:10.1023/a:1013025415333

Russian Journal of Coordination Chemistry

2001

DOI: 10.1023/a:1013025415333

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T. G. Cherkasova

V Chenskaya

B. G. Tryasunov

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Crystal structure of hexadimethylsulfoxidenickel(II) tetraisothiocyanatozincate

Cherkasova

Tsalko

2004

Russ J Coord Chem

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In continuation of our studies of Group IIB thiocyanates with organic ligands [1,2], we obtained for the first time and studied a complex of hexadimethylsulfoxidenickel(II) tetraisothiocyanatozincate [Ni(DMSO) 6 ][ Zn ( NCS ) 4 ] ( I ) using X-ray diffraction analysis. EXPERIMENTAL Synthesis. The starting compounds for the synthesis of I were Ni ( NO 3 ) 2 · 6 H 2 O (analytical grade), K 2 [ Zn ( NCS ) 4 ] · 3ç 2 é (reagent grade), and dimethyl sulfoxide (DMSO) (reagent grade). Potassium tetraisothiocyanatozincate K 2 [ Zn ( NCS ) 4 ] · 3ç 2 é was prepared by reacting aqueous solutions of KSCN and Zn ( NCS ) 2 taken at a molar ratio of 2 : 1. Ethanolic solutions of Ni ( NO 3 ) 2 · 6 H 2 O and K 2 [ Zn ( NCS ) 4 ] · 3ç 2 é were mixed at a molar ratio of 1 : 1, and a precipitate of KNO 3 was separated. DMSO (~6 mol) was added to the filtrate that formed. The resulting mixture was slightly concentrated in a water bath and left in air until crystallization completed.Light green plates of the crystalline complex I were isolated by slow crystallization from an ethanolic solution at 25°ë . X-ray diffraction analysis of compound I was carried out on a Bruker P4 diffractometer (Mo K α radiation, graphite monochromator, θ /2 θ scan mode, 2 θ < 50° ). Crystals of I with the molecular formula C 16 H 36 O 6 S 10 NiN 4 Zn ( M = 825.17) are monoclinic: a = 8.4358(8) Å , b = 21.655(2) Å , c = 10.8351(8) Å , β = 105.162(7)°, V = 1910.4(3) Å 3 , space group P 2 1 / m , Z = 2, ρ (calcd) = 1.434 g/cm 3 , µ = 1.699 mm -1 .Intensities of 3661 independent reflections were measured for a crystal 0.4 × 0.4 × 0.2 mm in size. Corrections for a decrease in intensities of reference reflections (to 27.6%) and for absorption were applied by the empirical method taking into account azimuth scan curves (transmission 0.70-0.94).The structure was solved by the direct method using the SHELXS97 program and refined by the leastsquares method in the anisotropic-isotropic (for H atoms) approximation using the SHELXL97 program to wR 2 = 0.1421, S = 1.002 for all reflections ( R = Abstract -A new complex, hexadimethylsulfoxidenickel(II) tetraisothiocyanatozincate [Ni(DMSO) 6 ][ Zn ( NCS ) 4 ] ( I ), is synthesized. Its crystal structure is determined by X-ray diffraction analysis. Compound I forms light green, monoclinic crystals shaped like plates: a = 8.4358(8) Å , b = 21.655(2) Å , c = 10.8351(8) Å , β = 105.162(7)°, V = 1910.4(3) Å 3 , space group P 2 1 / m , Z = 2, ρ (calcd) = 1.434 g/cm 3 , µ = 1.699 mm -1 . The Zn atom has a tetrahedral environment, while the Ni atom has an octahedral environment.

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confidence: 99%

“…The structure was solved by the direct method using the SHELXS97 program and refined by the leastsquares method in the anisotropic-isotropic (for H atoms) approximation using the SHELXL97 program to wR 2 …”

mentioning

confidence: 99%

Crystal structure of hexadimethylsulfoxidenickel(II) tetraisothiocyanatozincate

Cherkasova

Tsalko

2004

Russ J Coord Chem

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Cited by 1 publication

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Crystal structure of hexadimethylsulfoxidenickel(II) tetraisothiocyanatozincate

Crystal structure of hexadimethylsulfoxidenickel(II) tetraisothiocyanatozincate

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