Crystal Structure Investigation of Amide Sulfate Tetrahydrates with Divalent Cations

Autor(en)

Ekkehart Tillmanns, Manfred Wildner, Paul Angerer

Abstrakt

Single crystals of three amide sulfate tetrahydrate compds., Ca(NH2SO3)2×4H2O, Mn(NH2SO3)2×4H2O and Ni(NH2SO3)2×4H2O, were synthesized by controlled evapn. of aq. solns. The crystal structures were studied using single-crystal x-ray diffraction methods. Ca(NH2SO3)2×4H2O: space group C2/c, Z = 4, a 11.616(3), b 7.761(2), c 11.638(3) .ANG., beta 98.93(1)°, R1 = 0.026; Mn(NH2SO3)2×4H2O: space group P21/c, Z = 2, a 6.143(2), b 5.324(2), c 15.441(5) .ANG., beta 91.72(1)°, R1 = 0.024; Ni(NH2SO3)2×4H2O: space group P.hivin.1, Z = 1, a 6.331(8), b 6.731(9), c 6.784(8) .ANG., alpha 88.93(9), beta 67.87(5), gamma 67.76(6)°, R1 = 0.030. In Ca(NH2SO3)2×4H2O antiprismatic CaO8 polyhedra share four O atoms with NH2SO3 tetrahedra forming sheets parallel (001). In Mn(NH2SO3)2×4H2O and Ni(NH2SO3)2×4H2O, MnO6 octahedra and NiN2O4 octahedra, resp., are linked by common corners with two NH2SO3 tetrahedra forming isolated groups. These units are interconnected by H 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 .ANG., resp. The av. cation-O distances are 2.456 .ANG. (Ca-O), 2.173 .ANG. (Mn-O), and 2.049 .ANG. (Ni-O), both Ni-N bond lengths are 2.153 .ANG.. Three different types of H bonds are obsd. in the title compds., O-H×××O bonds from 2.680 to 2.968 .ANG., N-H×××O bonds between 2.966 and 3.339 .ANG., and one O-H×××N bond with 2.905 .ANG.. Generally, obsd. interat. bond lengths and angles comply well with crystal chem. expectations.

Organisation(en)

Institut für Mineralogie und Kristallographie

Externe Organisation(en)

Kompetenzzentrum für elektrochemische Oberflächentechnologie GmbH

Journal

Croatica Chemica Acta

Band

72

Seiten

295-310

Anzahl der Seiten

16

ISSN

0011-1643

Publikationsdatum

1999

Peer-reviewed

Ja

ÖFOS 2012

105113 Kristallographie

Link zum Portal

https://ucrisportal.univie.ac.at/de/publications/crystal-structure-investigation-of-amide-sulfate-tetrahydrates-with-divalent-cations(ab1ae285-c00b-461f-9a9e-d842abc1f37e).html