Nanocrystalline mixtures of Sn(II) and Sn(IV) oxide powders, potential gas sensor materials, are synthesized via a simple precipitation route using SnCl2 as the precursor. Materials are characterized by powder Xray diffraction, thermogravimetric analysis, UV−visible diffuse reflectance spectroscopy (DRS), and Fourier transform infrared spectroscopy. The ratio of Sn(II)/Sn(IV) in powders precipitated at room temperature, as well as the identity of the primary Sn(II) product (SnO or Sn6O4(OH)4), can be varied by adjusting aging time and washing procedures. The identity of the initial Sn(II) product influences the subsequent phase composition and degree of disorder in the tetragonal SnO2 phase obtained following sintering in air. Analysis of the DRS absorption edge and long-wavelength (Urbach) absorption tail is NOT THE PUBLISHED VERSION; this is the author's final, peer-reviewed manuscript. The published version may be accessed by following the link in the citation at the bottom of the page.