Potassium N-bromo-4-chloro-2-methylbenzenesulfonamidate monohydrate

In the title compound, K+·C7H6BrClNO2S−·H2O, the K+ cation is heptacoordinated by two water O atoms, four sulfonyl O atoms of four different N-bromo-4-chloro-2-methylbenzenesulfonamidate anions, and one Br atom of one of the anions. The S—N distance of 1.584 (3) Å is consistent with an S=N double bond. In the crystal, the anions are linked into layers by O—H⋯Br and O—H⋯N hydrogen bonds.

In the title compound, K + ÁC 7 H 6 BrClNO 2 S À ÁH 2 O, the K + cation is heptacoordinated by two water O atoms, four sulfonyl O atoms of four different N-bromo-4-chloro-2methylbenzenesulfonamidate anions, and one Br atom of one of the anions. The S-N distance of 1.584 (3) Å is consistent with an S N double bond. In the crystal, the anions are linked into layers by O-HÁ Á ÁBr and O-HÁ Á ÁN hydrogen bonds.
In the title compound, the K + ion is hepta coordinated by two O atoms from two different water molecules, four sulfonyl O atoms of four different N-bromo-2-methyl-4-chlorobenzenesulfonamide anions and one Br atom of N-bromo-2methyl-4-chlorobenzenesulfonamide anion, similarly to that observed in III. But this is in contrast to the hepta coordination of K + ion by three O atoms from three different water molecules, four sulfonyl O atoms of three different Nbromo-2-methyl-4-chlorobenzenesulfonamide anions in II and IV. In the crystal structure the anions are linked by intermolecular O3-H32···Br1 and O3-H31···N1 hydrogen bonding into layers ( Fig. 2 and Table 1).

Experimental
The title compound was prepared by a method similar to the one described by Gowda & Mahadevappa (Gowda & Mahadevappa, 1983). 2 g of 2-methyl-4-chlorobenzenesulfonamide was dissolved with stirring in 40 ml of 5M KOH at room temperature. The resultant solution was cooled in ice and 4 ml of liquid bromine was added drop wise with constant stirring. The resultant potassium salt of N-bromo-2-methyl-4-chlorobenzenesulfon-amidate was filtered under suction, washed quickly with a minimum quantity of ice cold water. The purity of the compound was checked by determining its melting point (208° C) and estimating, iodometrically, the amount of active bromine present in it. It was further characterized from its infrared spectrum.
Prism like yellow single crystals of the title compound used in the X-ray diffraction studies were obtained from its aqueous solution at room temperature. Å, thus leading to the angle of 107°. All H atoms were refined with isotropic displacement parameters set at 1.2 U eq (Caromatic, O) or 1.5 U eq (C-methyl) of the parent atom. The highest peak and the deepest hole are 0.93 and 0.80 Å from Br1, respectively.   Molecular packing of the title compound with hydrogen bonding shown as dashed lines.

Special details
Experimental. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic)treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. Refinement. Refinement of F 2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F 2 , conventional R-factors R are based on F, with F set to zero for negative F 2 . The threshold expression of F 2 > σ(F 2 ) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F 2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger.