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New sulfamates KLi(NH 2 SO 3 ) 2 , RbLi ⋅ (NH 2 SO 3 ) 2  and CsLi(NH 2 SO 3 ) 2  were prepared from non-stoichiometric (ratio Li: Me = 3:1) aqueous solutions of LiNH 2 SO 3  and MeNH 2 SO 3  (Me = K, Rb, Cs) at room temperature. Large single crystals of KLi(NH 2 SO 3 ) 2  were grown from these solutions by controlled lowering of the temperature between 293 K and 288 K. The crystal structures were investigated using single-crystal X-ray diffraction methods. KLi(NH 2 SO 3 ) 2 : space group  P 2 1 ,  Z  = 2,  a  = 5.196(1) Å,  b  = 8.475(1) Å,  c  = 8.868(1) Å,  β  = 105.05(1)°,  T  meas . = 293 K,  R 1 = 0.026; RbLi(NH 2 SO 3 ) 2 : space group  P 1̅,  Z  = 4,  a  = 7.844(1) Å,  b  = 9.804(1) Å,  c  = 10.825(1) Å,  α  = 108.77(1)°,  β  = 93.29(1)°,  γ  = 98.64(1)°,  T  meas.  = 293 K,  R 1 = 0.033; CsLi(NH 2 SO 3 ) 2  : space group  P 1̅,  Z  = 2,  a  = 5.535(1) Å,  b  = 7.877(1) Å,  c  = 9.857(1) Å,  α  = 74.07(1)°,  β  = 76.33(1)°,  γ  = 87.07(1)°,  T  meas.  = 200 K;  R 1 = 0.023. The common feature of the three crystal structures are alternating layers of Me +  and lithium cations together with anionic [NH 2 SO 3 ] –  tetrahedra. Li +  coordination polyhedra and [NH 2 SO 3 ] –  anions, linked via common corners, form one type of these sheets. Additionally, these layers are stabilized by hydrogen bonds. Me +  coordination polyhedra are linked to each other and to the above mentioned layers by common corners and edges. RbLi(NH 2 SO 3 ) 2  and CsLi(NH 2 SO 3 ) 2  possess similar structures. Generally, the observed interatomic distances and angles agree with crystal chemical expectations. Differential scanning calorimetry measurements showed that KLi(NH 2 SO 3 ) 2  undergoes a first-order structural phase transition at 401 K and melts at 423 K. Between 153 K and 423 K no indications of further phase transitions were observed. In addition, the refractive indices and the tensor of thermal expansion were measured. Further, the elastic and thermoelastic constants of KLi(NH 2 SO 3 ) 2  were determined from ultrasonic resonant frequencies of thick plane-parallel plates and their shift upon variation of temperature, respectively. The elastic behaviour of KLi(NH 2 SO 3 ) 2  is similar to the average elastic properties of LiNH 2 SO 3  and KNH 2 SO 3 .

zeitschrift für kristallographie - crystalline materials

Crystal structures of sulfamates MeLi(NH 2 SO 3 ) 2  (Me: K, Rb and Cs) and physical properties of KLi(NH 2 SO 3 ) 2  (refractive indices, thermal expansion, elastic properties)