Synthesis and crystal structure of two polymorphs of (NH~4~)~2~Mo~4~O~13~, orthorhombic (o) and triclinic (t)
Rachid Benchrifa, M. Leblanc, R. De Pape
Abstract
Rachid Benchrifa, M. Leblanc, R. De Pape
Abstract
The reinvestigation of the (NH 4 ) 2 O-MoO 3 system evidences two varieties of (NH 4 ) 2 Mo 4 O 13 . single crystals are obtained from hydrothermal treatment for the stoechiometric (NH 4 )2O/MoO 3 . The orthorhombic o-polymorph is isotypic of the previously described Tl 2 Mo 4 O 13 ; the structure solved to R=0.032 for 4006 independent reflections (a=7.647(3), b=15.414(7), c=18.994(8) A, Pcba, Z=8). The t-variety is built up from Mo 4 O 18 polyanions; (a=8.264(4), b=8.344(4), c=10.245(5) A, α=104.61(2), β=106.05(2), γ=109.67(2), SG P-1, Z=2, R=0.022 for 4171 independent reflections)
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The reinvestigation of the (NH 4 ) 2 O-MoO 3 system evidences two varieties of (NH 4 ) 2 Mo 4 O 13 . single crystals are obtained from hydrothermal treatment for the stoechiometric (NH 4 )2O/MoO 3 . The orthorhombic o-polymorph is isotypic of the previously described Tl 2 Mo 4 O 13 ; the structure solved to R=0.032 for 4006 independent reflections (a=7.647(3), b=15.414(7), c=18.994(8) A, Pcba, Z=8). The t-variety is built up from Mo 4 O 18 polyanions; (a=8.264(4), b=8.344(4), c=10.245(5) A, α=104.61(2), β=106.05(2), γ=109.67(2), SG P-1, Z=2, R=0.022 for 4171 independent reflections)
Key concepts: Triclinic crystal system, Orthorhombic crystal system, Crystallography, Crystal structure, Chemistry, Hydrothermal synthesis, Inorganic compound, Hydrothermal circulation