The oxygen-deficient orthorhombic oxide YBa2Cu3O7-δ has been the center of intense recent interest because of its high Tc superconducting proper-ties[l-3]. Recently, the structurally related La3Ba3Cu3O15-δ, has received increasing attention[4–9]. The pure Y analog[10,11] cannot be synthesized by usual solid state reaction routes probably because of its metastability near 880°C. Here we report on the successful synthesis of pure tetragonal Y3,Ba3CU6O15-δ (referred to as Y 3–3–6), via the firing of an atomically mixed citrate precursor at a relatively low temperature. X-ray diffraction data characterize Y 3–3–6 to be isostructural with the corresponding La compound. The unit cell composition can then be written as: Y(Ba2−x Yx) CU3O7+δ with the parent compound at x = 0.50. Specimens of Y 3–3–6 at × = 0.50 and 0.375 annealed at 650°C under 1 atmosphere of O2 are non-superconducting. Higher pressure O2 annealing and fluorine-doping leads to a 1–5% superconducting volume fraction with onset at 85K. Annealing near 880°C creates a 10% superconducting fraction which shows near-zero resistivity at 62K and a reproducible, small resistive transition near 260K.