Four fluorinated cesium beta-diketonates, Cs(CF₃COCHCOCF₃) (Cs(hfac)), Cs(CF₃COCHCOCH₃) (Cs(tfac)), Cs(OH₂)((Me)₃CCOCHCOCF₃) (Cs(OH₂)(ptac)), and Cs(OH₂)(PhCOCHCOCF₃) (Cs(OH₂)(btfac)), were synthesized by interaction of the corresponding beta-diketone and Cs₂CO₃ in Et₂O. The formation of Сs(CF₃C(OH)₂CH₂C(OH)₂CF₃)(CF₃COO) or Cs(CF₃C(OH)₂CH₂COCH₃)(tfac) was shown to be dependent on the reaction conditions. The compounds were characterized by elemental analysis, single crystal X-ray diffraction, and TG/DTA analysis. All compounds have ionic structures organized into pseudo chains (in the case of Cs(hfac) and Cs(CF₃C(OH)₂CH₂COCH₃)(tfac)) or pseudo layers (in other cases). According to the TG data Cs(hfac), Cs(tfac), Cs(OH₂)(ptac,) and Cs(OH₂)(btfac) decompose in inert atmosphere within the temperature range 30–550 °C.

Double complex salts (DCSs) [Co(NH₃)₆][Fe(CN)₆] (I) and [Co(NH₃)₆]₂[Cu(C₂O₄)₂]₃ (II) and complex [Co(NH₃)₆]₂(C₂O₄)₃·4H₂O (III) are synthesized and investigated by single crystal XRD, crystal optics, and elemental analysis. The crystalline phases of I, II, and III (R-3, P2₁/c, and Pnnm space groups respectively) have the following crystallographic characteristics: a = 10.9804(2) Å, b = 10.9804(2) Å, c = 10.8224(3) Å, V = 1130.03(4) ų, Z = 3, d _x = 1.65 g/cm³ (I); a = 9.6370(2) Å, b = 10.2452(2) Å, c = 13.2108(3) Å, V = 1932.90(9) ų, Z = 2, d _x= 1.97 g/cm³ (II), and a = 11.7658(3) Å, b = 11.7254(3) Å, c = 14.1913(4) Å, V = 1304.34(5) ų, Z = 2, d _x = 1.68 g/cm³ (III). This paper investigates the products of DCS thermolysis in a hydrogen atmosphere: the intermetallic compound CoFe with the bcc parameter a = 2.852 Å for I and a heterogeneous mixture of Co and Cu in the decomposition of II. The coordinated CN⁻ and C₂O ₄ ²⁻ groups then turn into NH₃, hydrocarbons, and CO₂. The dominant hydrocarbon is methane.