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Croatica Chemica Acta, Vol. 72 No. 2-3, 1999.

Original scientific paper

Crystal Structure Investigations of Amide Sulfate Tetrahydrates with Divalent Cations

Paul Angerer ; Institut für Mineralogie und Kristallographie, Universität Wien, Geozentrum, Althanstr. 14, A-1090 Wien, Austria
Ekkehart Tillmanns ; Institut für Mineralogie und Kristallographie, Universität Wien, Geozentrum, Althanstr. 14, A-1090 Wien, Austria
Manfred Wildner ; Institut für Mineralogie und Kristallographie, Universität Wien, Geozentrum, Althanstr. 14, A-1090 Wien, Austria

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Abstract

Single crystals of three amide sulfate tetrahydrate compounds, Ca(NH2SO3)2 ⋅ 4H2O, Mn(NH2SO3)2 ⋅ 4H2O and Ni(NH2SO3)2 ⋅ 4H2O, were synthesized by controlled evaporation of aqueous Solutions. The crystal structures were investigated using single-crystal X-ray diffraction methods. Ca(NH2SO3)2 ⋅ 4H2O: space group C2/c, Z = 4, a = 11.616(3) Å, b = 7.761(2) Å, c = 11.638(3) Å, β = 98.93(1)°, V = 1036.47 Å3, R1 = 0.026; Mn(NH2SO3)2 ⋅ 4H2O: space group P21/c, Z = 2, a = 6.143(2) Å, b = 5.324(2) Å, c = 15.441(5) Å, β = 91.72(1)°, V= 504.78 Å3, R1 = 0.024; Ni(NH2SO3)2 ⋅ 4H2O: space group P1̅, Z= 1, a = 6.331(8) Å, b = 6.731(9) Å, c = 6.784(8) Å, α = 88.93(9)°, β = 67.87(5)°, γ = 67.76(6)°, V = 245.27 Å3, R1 = 0.030. In Ca(NH2SO3)2 ⋅ 4H2O antiprismatic CaO8 polyhedra share four oxygen atoms with NH2SO3 tetrahedra forming sheets parallel (001). In Mn(NH2SO3)2 ⋅ 4H2O and Ni(NH2SO3)2 ⋅ 4H2O, MnO6 octahedra and NiN2O4 octahedra, respectively, are linked by common corners with two NH2SO3 tetrahedra forming isolated groups.
These units are interconnected by hydrogen bonds only to form three-dimensional framework structures. The amide sulfate group has a distorted tetrahedral configuration with mean S−O and S−N bond lengths of 1.449 and 1.654 Å, respectively. The average cat-ion-oxygen distances are 2.456 Å (Ca−O), 2.173 Å (Mn-O), and 2.049 Å (Ni−O), both Ni−N bond lengths are 2.153 Å. Three different types of hydrogen bonds are observed in the title compounds, namely O−H⋅⋅⋅O bonds ranging from 2.680 to 2.968 A, N−H⋅⋅⋅O bonds between 2.966 and 3.339 Å, and one O−H⋅⋅⋅N bond with 2.905 Å. Generally, observed interatomic bond lengths and angles comply well with crystal Chemical expectations.

Keywords

crystal structure; crystal Chemistry; amide sulfates; Ca(NH<sub>2</sub>SO<sub>3</sub>)<sub>2</sub> ⋅ 4H<sub>2</sub>O; Mn(NH<sub>2</sub>SO<sub>3</sub>)<sub>2</sub> ⋅ 4H<sub>2</sub>O; Ni(NH<sub>2</sub>SO<sub>3</sub>)<sub>2</sub> ⋅ 4H<sub>2</sub>O

Hrčak ID:

132168

URI

https://hrcak.srce.hr/132168

Publication date:

1.9.1999.

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