Abstract. M r=288.5, P2Jc, a=7.030 (2), b= 12.924 (4), c= 14.442 (3) A, fl= 97.04 (2) ° , V= 1302.2 (6)/k a, Z = 4, D x = 1.472 (1) Mg m -a, 2(Mo Ka) = 0.71069/k, /t = 0.229 mm -1, F(000) = 600, T= 193 K, R = 0.064 for 2445 reflections. Two NH2py moieties are hydrogen bonded to form an (NH2py)2 H÷ cation; these cations are hydrogen bonded via the amino groups to perchlorate anions. As in the a phase at 295 K, the N-H...N bond is asymmetric and nearly linear with an N...N distance of 2.697 (4)/k. The dihedral angle between the planes of the bridged pyridine rings is 89.8 (5) °.
Crystals of dichloroantimony(III) tetrachlorogallate(III) are monoclinic, space group P21/c with: a = 9.837(2) Å, b = 7.812(2) Å, c = 12.504(2) Å, β = 101.0(2)°. The structure was refined by three dimensional least‐squares method to R = 5.2% for 1051 independent reflections. The antimony atom has two nearest chlorine neighbours at 2.295(4) Å and 2.299(4) Å giving the expected angular conformation and two other neighbours at 2.713(4) Å and 2.772(4) Å completing with the lone pair a trigonal bipyramid environment around antimony. The GaCl4− groups, highly distorted from regular tetrahedral geometry, strongly interact with SbCl2+ via GaCl···Sb bridges giving an endless polymeric chain.
Crystals of [H5O2][Ru(CO)3Cl3] · SbCl3 are triclinic, space group P1, with unit cell of dimensions: a = 7.129(2), b = 10.129(3), c = 10.997(3) Å, α = 75.40(2)°, β = 97.17(2)°; γ = 120.94(2)°. The structure was solved from X‐ray diffractometer data by Patterson and Fourier synthesis and refined by full matrix least‐squares method to R = 3.02% for 3268 independent reflections. The [Ru(CO)3Cl3]− anion has an approximately octahedral fac configuration. The antimony atom has three chlorine neighbours at 2.387(2), 2.364(2) and 2.368(2) Å giving the expected angular conformation and three other neighbours at longer distances completing with the lone pair a monocaped octahedral environment around antimony. The acidic hydrogen has been transfered to two water molecules giving an asymmetric [H5O2]+ ion with a very short hydrogen bond of 2.373(9) Å.
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