A neutron diffraction study of potassium sulphamate, KSO3NH2

Cox, G. W.; Sabine, T. M.; Padmanabhan, V. M.; Ban, Nobuo; Chung, Moon Kyu; Surjadi, A. J.

doi:10.1107/s0365110x67003238

Cited by 40 publications

(14 citation statements)

References 2 publications

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“…Sulfanilic acid is a zwitterion compound, in which the C-N bond must be single, while in Na sulfanilate the p~ electrons of the nitrogen atom can conjugate with the n-system of the benzene ring resulting in a partial double C-N bond. A similar feature has been observed in K sulfamate (Cox, Sabine, Padmanabhan, Tu Ban, Chung & Surjadi, 1967) which has a N-S bond length of 1.666 (6) A compared with 1.76 (2) A in sulfamic acid (Sass, 1960). Here the double-bond character is due to a n-bond between the nitrogen p~ electrons and the sulfur d-orbitals.…”

Section: Discussion Of the Resultssupporting

confidence: 56%

The crystal structure of sodium sulfanilate dihydrate

Bats¹,

Coppens²

1975

Acta Crystallogr Sect B

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The crystal structure of sodium sulfanilate dihydrate (H2NC6H4SOaNa.2H20) has been determined. The compound crystallizes in the orthorhombic space group Pbca with a= 23"895 (5), b = 10.101 (2) and c = 7.944 (2) A. The sodium atom has a distorted octahedral coordination of oxygen atoms; the amino group of the sulfanilate ion is considerably distorted from a planar conformation, partly owing to hydrogen bonding in the crystal.

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Section: Discussion Of the Resultssupporting

confidence: 56%

The crystal structure of sodium sulfanilate dihydrate

Bats¹,

Coppens²

1975

Acta Crystallogr Sect B

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“…The S-N and S-O bond lengths in Pb 3 (OH) 2 (NH 2 SO 3 ) 4 fall in the ranges of 1.614(13)-1.662(12) and 1.434(10)-1.482(9) Å, respectively (Wickleder, 2005). The difference in the bond length between the S-N and S-O bonds has been reported to be related to the difference in the properties of single and double bonds (Cox et al, 1967;Wadhawan & Padmanabhan, 1972). Thus, it is considered from the results obtained in this study that the S-N bond in PbHNSO 3 is substantially a double bond as similar to the S-O bond, and H atoms are not attached to the N atom.…”

Section: X-ray Crystal Structure Descriptionmentioning

confidence: 74%

“…This indicates that there is no significant difference in a quality property between these bonds. On the other hand, there is an obvious difference in the correlation between the S-N and S-O bonds in the ANH 2 SO 3 -type and Pb 3 (OH) 2 (NH 2 SO 3 ) 4 crystals (Belaj et al, 1987;Cox et al, 1967;Fukami et al, 2011;Manickkavachagam & Rajaram, 1984;Wadhawan & Padmanabhan, 1972;Wickleder, 2005). The length of the S-N bond in [NH 2 SO 3 ] -anions of these crystals is significantly longer than that of the S-O bond.…”

Section: X-ray Crystal Structure Descriptionmentioning

confidence: 99%

“…The length of the S-N bond in [NH 2 SO 3 ] -anions of these crystals is significantly longer than that of the S-O bond. For example, the lengths of the S-N and two S-O bonds in KNH 2 SO 3 are 1.666(6), 1.459 (7) and 1.454(4) Å, respectively (Cox et al, 1967). The S-N and S-O bond lengths in Pb 3 (OH) 2 (NH 2 SO 3 ) 4 fall in the ranges of 1.614(13)-1.662(12) and 1.434(10)-1.482(9) Å, respectively (Wickleder, 2005).…”

Section: X-ray Crystal Structure Descriptionmentioning

confidence: 99%

“…It is well known that crystals of an ANH 2 SO 3 -type consist of a monovalent cation ( (Belaj et al, 1987;Cox et al, 1967;H. Haussühl & S. Haussühl, 1995;Manickkavachagam & Rajaram, 1984;Wadhawan & Padmanabhan, 1972).…”

Section: Introductionmentioning

confidence: 99%

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Crystal Growth and Structure of a New PbHNSO3 Crystal

Fukami¹,

Seino²,

Nakasone³

et al. 2013

IJC

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A new type of PbHNSO 3 crystal has been grown by a gel method using agar-agar gel. TG-DTA and X-ray diffraction measurements have been performed on single crystal samples of PbHNSO 3 . It is found that the thermal decomposition of the compound starts at about 960 K. The space group (orthorhombic Pnma) and structural parameters are determined at room temperature with unit cell dimensions: a=8.4690(6), b=5.3934(4) and c=6.9530(4) Å. The crystal structure is found to consist of NSO 3 pseudo-tetrahedra, PbO 9 N 3 polyhedra, and NSO 3 -Pb-NSO 3 frameworks. The dark brown color of the crystal is suggested to be caused by the absorption of blue wavelengths of light which is due to the excitation of excess electrons in potential wells produced by the NSO 3 -Pb-NSO 3 framework.

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π-Complexes of Copper(I) Ionic Salts: Synthesis and Crystal Structure of (4-Allylthiosemicarbazide)(sulfamato)copper(I) and Bis(4-allylthiosemicarbazide)(sulfato-O)dicopper(I)

Mel'nyk

Filinchuk

Schollmeyer

et al. 2001

Z. anorg. allg. Chem.

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Single crystals of [Cu(ATSC)]NH 2 SO 3 (1) (ATSC ±4-allylthiosemicarbazide) were obtained by electrochemical synthesis using alternating current. Compound (1) crystallizes in P2 1 2 1 2 1 sp. gr., a = 6.8284(2), b = 9.3054(3), c = 16.1576(11) A Ê , Z = 4. ATSC moiety acts as tetradentate ligand, chelating two symmetrically related copper atoms. The Cu atom possesses trigonal pyramidal coordination, formed by two sulphur atoms (one of them at the apical position), nitrogen atom and C=C bond. Sulfamate anion is associated via hydrogen bonds. By slow hydrolysis of 1 crystals of [Cu 2 (ATSC) 2 ]SO 4 (2) were obtained: P 1 sp. gr., a = 9.526(2), b = 12.687(2), c = 14.7340(10) A Ê , a = 95.119(10), b = 89.903(12), c = 109.113(14)°, Z = 4. The asymmetric unit of 2 contains two formula units, which are related by pseudosymmetry via a glide plane a. One half of four ATSC molecules act as in 1, the rest as tridentate ligands, which coordinate the two copper atoms in apical positions with sulfate anions. This Cu±S coordination was to date unknown. The structure of the ATSC ligands contributes to the unexpected competitiveness of C=bond in the coordination sphere of Cu I inspite of strong donor atoms. Die p-Komplexe von Kupfer(I)-ionischen Salzen: Die Darstellung und die Kristallstrukturen von (4-Allylthiosemicarbazid)(sulfamato)kupfer(I) und Bis(4-allylthiosemicarbazid)(sulfato-O)dikupfer(I) Inhaltsu È bersicht. Einkristalle von [Cu(ATSC)]NH 2 SO 3 (1) (ATSC±4-allylthiosemicarbazid) wurden durch die elektrochemische Synthese unter Anwendung von Wechselstrom erhalten. Die Verbindung kristallisiert in der Raumgruppe P2 1 2 1 2 1 : a = 6.8284(2), b = 9.3054(3), c = 16.1576(11) A Ê , Z = 4. Die ATSC-Einheit wirkt als vierza È hniger Ligand, die mit den zwei symmetrisch verbundenen Kupferatomen verbru È ckt ist. Das Kupferatom hat trigonal-pyramidale Umgebung mit zwei Schwefelatomen (eines axial), ein Stickstoffatom und eine C=C-Bindung. Das Sulfamatanion ist u È ber Wasserstoffbru È ckenbindungen assoziiert. Durch langsame Hydrolyse der Verbindung 1 wurden Einkristallen von [Cu 2 (ATSC) 2 ]SO 4 (2) gewonnen: Raumgruppe P 1, a = 9.526(2), b = 12.687(2), c = 14.7340(10) A Ê , a = 95.119(10), b = 89.903 (12), c = 109.113(14)°, Z = 4. Die asymmetrische Einheit der Elementarzelle von 2 entha È lt zwei mit der Pseudosymmetrie u È ber die Gleitspiegelebene a verbundene Formeleinheiten. Die Ha È lfte der vier ATSC-Moleku È le wirkt wie in 1, der andere Teil als dreiza È hniger Ligand, der die zwei Kupferatome in den Axialpositionen mit den Sulfatanionen koordiniert. Die Struktur der ATSC-Liganden tra È gt zu der unerwarteten Konkurrenzfa È higkeit der C=C-Bindung in der Koordinationsspha È re des Cu I trotz starker Donoratome bei. Die stereochemische Besonderheit dieser Cu±S-Koordination war bisher nicht bekannt.

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A neutron diffraction study of potassium sulphamate, KSO3NH2

Cited by 40 publications

References 2 publications

The crystal structure of sodium sulfanilate dihydrate

The crystal structure of sodium sulfanilate dihydrate

Crystal Growth and Structure of a New PbHNSO3 Crystal

π-Complexes of Copper(I) Ionic Salts: Synthesis and Crystal Structure of (4-Allylthiosemicarbazide)(sulfamato)copper(I) and Bis(4-allylthiosemicarbazide)(sulfato-O)dicopper(I)

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