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N ,N-Dimethylethylenediammonium pentachloroantimonate(III) crystallizes in the monoclinic system, in space group P2 1 /c (a = 12.460(2), b = 10.252(2), c = 10.330(2) Å, β = 97.75(3)°, V = 1307.5(4) Å 3 , Z = 4, d c  = 1.997, d m  = 1.99(2) g/cm 3 ). The crystal structure of [(CH 3 ) 2 NH(CH 2 ) 2 NH 3 ][SbCl 5 ] consists of isolated [SbCl 5 ] 2-  anions and [(CH 3 ) 2 NH(CH 2 ) 2 NH 3 ] 2+  cations. The [SbCl 5 ] 2-  anion has a distorted square pyramidal geometry, presenting one short axial and four long equatorial Sb-Cl bonds. The square pyramids are characteristically stacked one close to the other, parallel to the c axis. The voids between the anionic sublattice are filled by [(CH 3 ) 2 NH(CH 2 ) 2 NH 3 ]2+ cations. The five non-equivalent Sb-Cl bond distances within the [SbCl 5 ] 2-  square pyramid are significantly different. The equatorial Sb-Cl bonds are in the range 2.427(2)-2.968(2) Å, whereas the axial one is 2.384(1) Å long. The study reveals that N-H...C1 hydrogen bonds are responsible for the deformation of equatorial Sb-Cl bonds from the mean value of 2.654(7) Å. Analysis of intermolecular interactions between the [SbCl 5 ] 2-  pyramids in the structure, reflected in changes of Sb-Cl bond lengths from the values characteristic of non-interacting pyramids, leads to the conclusion that the van der Waals radius of Sb is significantly smaller than that estimated by Pauling.

Dependence of the Distortion of the Square Pyramids in N, N-Dimethylethylenediammonium Pentachloroantimonate(III) on the Geometry of Hydrogen Bonds