Compounds (CN_3H_6)_2UO_2(OH)_2(NCS)NO_3 (I) and β-Cs_3UO_2(NCS)_5 (II) are synthesized and studied by IR spectroscopy and single-crystal X-ray diffraction. I and II crystallize in the orthorhombic system. For I, a = 12.2015(13) ?, b = 7.3295(8) ?, c = 16.310(2) ?, space group Pnma, Z = 4, and R = 0.0327; for II, a = 21.7891(6) ?, b = 13.5120(3) ?, c = 6.8522(2) ?, space group Pnma, Z = 4, and R = 0.0268. In structure I, complex groups form infinite chains UO_2(OH)_2(NCS) belonging to the AM_2~2 M~1 crystal chemical group of uranyl complexes (A = UO, M~2 = OH~–, and M1 = NCS~–). The main structural elements of crystals II are mononuclear UO_2(NCS)_5~(3–) groups belonging to the AM group of uranyl complexes (A = UO_2~(2+) and M~1 = NCS~–). In I and II, uranium-containing complexes are connected with outer-sphere cations by electrostatic interactions, and in I a system of hydrogen bonds also contributes to their binding. Specific features of the packing of complex UO_2(NCS)_5~(3–) groups in the structures of two modifications of Cs_3UO_2(NCS)_5 are discussed.
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