A synchrotron single crystal X-ray structure determination of a small crystal: Mo-Mo double bonds in the 3-D microporous molybdenum phosphate NH sub 4 (Mo sub 2 P sub 2 O sub 10 )ter dot H sub 2 O
- Exxon Research and Engineering Co., Annandale, NJ (United States)
Black crystals of NH{sub 4}(Mo{sub 2}P{sub 2}O{sub 10}){center dot}H{sub 2}O, (1), can be isolated by reacting MoO{sub 3}, Mo, (NH{sub 4}){sub 2}HPO{sub 4}, H{sub 3}PO{sub 4}, and H{sub 2}O in a mole ratio of 3:1.1:2:4:120 for 16 hr at 360C. The structure of phosphate (1) was determined and refined from single crystal data collected on a 35{times}20{times}10{mu}m{sup 3} crystal at beamline X10A at NSLS, Brookhaven National Laboratory. Compound (1) is monoclinic, space group P2{sub 1}/n with a=9.780(10), b=9.681(5), c=9.884(8) {angstrom}, {beta}=102.17(8), V=915(1) {angstrom}{sup 3} and R(R{sub W})=0.029(0.024) and contains MoO{sub 6} octahedra and PO{sub 4} tetrahedra. The structure is built up from Mo{sub 4} oxo units that have two edge-sharing Mo{sup 4+}O{sub 6} octahedra that contain Mo-Mo double bonds (2.453(2) {angstrom}), with the same two oxygens that bridge the Mo{sup 4+} also serving as a corner for two additional Mo{sup 5+}O{sub 6} octahedra. The Mo{sub 4} units are connected by phosphate groups into a 3-D array which generates several types of tunnel which are filled with NH{sub 4}{sup +} cations and H{sub 2}O. The material is isotypic with the mineral leucophosphite, K(Fe{sub 2}(OH)(H{sub 2}O)(PO{sub 4}){sub 2}){center dot}H{sub 2}O. Water absorption isotherms show that (1) is microporous and has about 10-12 vol% internal void space that can be filled by water.
- OSTI ID:
- 7039050
- Journal Information:
- Journal of Solid State Chemistry; (United States), Journal Name: Journal of Solid State Chemistry; (United States) Vol. 92:1; ISSN 0022-4596; ISSN JSSCB
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
400201* -- Chemical & Physicochemical Properties
AMMONIUM COMPOUNDS
BREMSSTRAHLUNG
CHEMICAL BONDS
CHEMICAL PREPARATION
COHERENT SCATTERING
CRYSTAL LATTICES
CRYSTAL STRUCTURE
CRYSTALS
DATA
DIFFRACTION
ELECTROMAGNETIC RADIATION
EXPERIMENTAL DATA
HYDROGEN COMPOUNDS
INFORMATION
LATTICE PARAMETERS
MATERIALS
MICROSTRUCTURE
MOLECULAR STRUCTURE
MOLYBDENUM COMPOUNDS
MOLYBDENUM PHOSPHATES
MONOCLINIC LATTICES
MONOCRYSTALS
NUMERICAL DATA
OXYGEN COMPOUNDS
PHOSPHATES
PHOSPHORUS COMPOUNDS
POROSITY
POROUS MATERIALS
RADIATIONS
REFRACTORY METAL COMPOUNDS
SCATTERING
SORPTIVE PROPERTIES
STOICHIOMETRY
SURFACE PROPERTIES
SYNCHROTRON RADIATION
SYNTHESIS
TRANSITION ELEMENT COMPOUNDS
WATER
X-RAY DIFFRACTION