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Abstract
The title hydrides and their deuterides were synthesized by a solid state reaction at 790–800 K and 120–155 bar hydrogen (deuterium) pressure, and characterized by X-ray single-crystal (Ca compound) and neutron powder diffraction (Ca and Yb compounds). They crystallize with cubic symmetry, space group P 4 3 m, Ca 4Mg 4Co 3H 19: a = 6.6953(2) A ̊ , deuteride: 6.6809(2) Å; Yb 4Mg 4Co 3H 19: a = 6.6727(2) A ̊ , deuteride: 6.6591(1) Å ( T = 295 K). The structures contain tetrahedrally coordinated D anions with bond distances [D3-Mg] = 1.912(5) Å (Ca) and 1.902(7) Å (Yb), [D3-3Ca)] = 2.355(6) Å and [D3-3Yb] = 2.354(5) Å, and square-pyramidal [CoD 5] 4 complex anions in which the equatorial ligands are ordered with bond distances [Co-4D1] = 1.546(3) (Ca), 1.535(5) Å (Yb) and the apical ligands are disordered with bond distances [Co-D2] = 1.586(9) (Ca), 1.60(1) Å (Yb).
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