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- W1982175028 abstract "The synthesis and characterization of the tetrameric lithium thiolate (LiSC6H2-2,4,6-Ph3)4·C7H8 (1), the trimeric lithium thiolate (LiSC6H3-2,6-Mes2)3·C6H14(2) (Mes = 2,4,6-Me3C6H2), the thiol HSC6H3-2,6-Trip2 (3) (Trip = 2,4,6-i-Pr3C6H2), and the complete alkali metal series of dimeric thiolates (MSC6H3-2,6-Trip2)2 (M = Li (4, 5), Na (6), K (7), Rb (8), Cs (9)) are described. The compounds were characterized by 1H, 7Li, and 13C NMR and IR spectroscopy and by X-ray crystallography. The compounds 1 and 2 crystallize as four- and three-rung ladder framework structures. The compounds 4−9 crystallize as dimers with M2S2 cores. In addition, the metal ions interact with the ortho aryl groups to varying degrees in all the structures. The extent of these interactions appears to be determined mainly by ionic sizes and geometric factors. The coordination geometry of the thiolato sulfurs also varies from pyramidal in 1, 2, 4, 5, and 6 and one planar and one slightly pyramidal sulfur geometry in 7 to both sulfurs being planar coordinated in 8 and 9. Crystal data at 130 K are as follows: (LiSC6H2-2,4,6-Ph3)4·C7H8 (1), a = 15.961(2) Å, b = 16.243(3) Å, c = 17.114(3) Å, α = 89.375(14)°, β = 85.334(14)°, γ = 63.343(12)°, V = 3950(1) Å3, space group P1̄, Z = 2, R1 = 0.082; (LiSC6H3-2,6-Mes2)3·C6H14(2), a = 14.554(4) Å, b = 14.010(4) Å, c = 32.832(8) Å, β = 95.20(2)°, V = 6667(2) Å3, space group P21/n, Z = 4, R1 = 0.089; HSC6H3-2,6-Trip2 (3), a = 8.180(2) Å, b = 25.437(5) Å, c = 15.752(3) Å, V = 3278(1) Å3, space group Pnma, Z = 4, R1 = 0.045; (LiC6H3-2,6-Trip2)2 (4), a = 12.652(2) Å, b = 14.218(1) Å, c = 18.713(2) Å, α = 83.56(1)°, β = 84.36(1)°, γ = 73.82(1)°, V = 3205(1) Å3, space group P1̄, Z = 2, R1 = 0.055; (LiC6H3-2,6-Trip2)2·C7H8 (5), a = 15.383(3) Å, b = 14.381(2) Å, c = 16.524(2) Å, β = 111.10(1), V = 3410.3(9) Å3, space group P21/n, Z = 2, R1 = 0.086; (NaSC6H3-2,6-Trip2)2·0.5C7H8 (6), a = 13.952(2) Å, b = 20.267(2) Å, c = 24.475(3) Å, β = 98.673(9)°, V = 6842(1) Å3, space group P21/n, Z = 4, R1 = 0.068; (KSC6H3-2,6-Trip2)2·C7H8 (7), a = 13.683(4) Å, b = 15.071(4) Å, c = 17.824(5) Å, α = 82.73(2), β = 86.09(2), γ = 88.46(2), V = 3637(2) Å3, space group P1̄, Z = 2, R1 = 0.072; (RbSC6H3-2,6-Trip2)2·C7H8 (8), a = 19.710(3) Å, b = 20.892(3) Å, c = 18.755(2) Å, β = 106.900(9)°, V = 7389(2) Å3, space group P21/n, Z = 4, R1 = 0.069; (CsSC6H3-2,6-Trip2)2 (9), a = 13.109(3) Å, b = 15.941(3) Å, c = 17.748(4) Å, α = 101.65(2)°, β = 100.76(2)°, γ = 104.25(2)°, V = 3410(1) Å3, space group P1̄, Z = 2, R1 = 0.048." @default.
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- W1982175028 date "1996-01-01" @default.
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- W1982175028 title "Donor-Free Alkali Metal Thiolates: Synthesis and Structure of Dimeric, Trimeric, and Tetrameric Complexes with Sterically Encumbered Terphenyl Substituents" @default.
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- W1982175028 doi "https://doi.org/10.1021/ic960570t" @default.
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