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The new antimony oxyhalide Sb 3 O 4 Cl has been synthesized hydrothermally. Its crystal structure has been determined using a twinned specimen. Sb 3 O 4 Cl crystallizes monoclinic in  P 2/ c ,  a  = 9.6531 (8) Å,  b  = 5.3059(3) Å,  c  = 5.5981(4) Å and  β  = 94.745(10)°. Sb 3 O 4 Cl consists of infinite Sb 3 O 4  layers parallel to (100) and interlayer Cl atoms. Twinning occurs if (100) mirror planes are inserted instead of the twofold rotation axes at the Cl positions. One-dimensional disorder including orthorhombic  Pmca  micro-domains gives rise to the weak diffuse reflections along  ξkl .

Structure of triantimony tetraoxide chloride, Sb 3 O 4 Cl: twinning and one-dimensional disorder