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The ternary oxide MnReO4, manganese rhenium oxide, has been synthesized under a high pressure of 5.5 GPa at 1473 K and its crystal structure has been determined by single-crystal X-ray diffraction. MnReO4 crystallizes in a wolframite-type structure with average bond lengths of <Re-O> = 1.935 and <Mn-O> = 2.160 Å that are in good agreement with the ionic radii of Re6+ and Mn2+. The magnetic properties of MnReO4 have been studied by SQUID measurements, revealing magnetic ordering below 275 (10) K and a weak ferromagnetic component of the ordered magnetic structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768105005380/ws5018sup1.cif
Contains datablocks g:_sc_kirill_mnreo4_k1_shelx_ac_k1ms, global

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768105005380/ws5018sup2.fcf
Contains datablock {g:\sc\kirill\mnreo4\k1\shelx\ac\k1ms}

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction Limited, 2001); cell refinement: CrysAlis RED (Oxford Diffraction Limited, 2001); data reduction: CrysAlis RED (Oxford Diffraction Limited, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: Diamond (Brandenburg, 2001); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
(g:_sc_kirill_mnreo4_k1_shelx_ac_k1ms) top
Crystal data top
MnO4ReF(000) = 264
Mr = 305.14Dx = 7.384 Mg m3
Monoclinic, P2/cMo Kα radiation, λ = 0.71073 Å
a = 4.8022 (5) ÅCell parameters from 664 reflections
b = 5.6318 (6) Åθ = 3.6–32.4°
c = 5.0803 (6) ŵ = 48.46 mm1
β = 92.762 (9)°T = 304 K
V = 137.24 (3) Å3Prism, black
Z = 20.05 × 0.04 × 0.03 mm
Data collection top
Oxford Diffraction Xcalibur (TM) Single Crystal X-ray Diffractometer with Sapphire CCD detector272 independent reflections
Radiation source: fine-focus sealed tube263 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.038
Rotation method data acquisition using ω and phi scans(s)θmax = 26.3°, θmin = 3.6°
Absorption correction: numerical
CrysAlis RED, Oxford Diffraction Ltd., version 170.17, 2003 Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid.
h = 55
Tmin = 0.257, Tmax = 0.401k = 67
823 measured reflectionsl = 66
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.028 w = 1/[σ2(Fo2) + (0.0383P)2 + 2.3979P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.066(Δ/σ)max = 0.001
S = 1.17Δρmax = 2.28 e Å3
272 reflectionsΔρmin = 2.38 e Å3
30 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.003 (2)
Crystal data top
MnO4ReV = 137.24 (3) Å3
Mr = 305.14Z = 2
Monoclinic, P2/cMo Kα radiation
a = 4.8022 (5) ŵ = 48.46 mm1
b = 5.6318 (6) ÅT = 304 K
c = 5.0803 (6) Å0.05 × 0.04 × 0.03 mm
β = 92.762 (9)°
Data collection top
Oxford Diffraction Xcalibur (TM) Single Crystal X-ray Diffractometer with Sapphire CCD detector272 independent reflections
Absorption correction: numerical
CrysAlis RED, Oxford Diffraction Ltd., version 170.17, 2003 Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid.
263 reflections with I > 2σ(I)
Tmin = 0.257, Tmax = 0.401Rint = 0.038
823 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.02830 parameters
wR(F2) = 0.0660 restraints
S = 1.17Δρmax = 2.28 e Å3
272 reflectionsΔρmin = 2.38 e Å3
Special details top

Experimental. CrysAlis CCD, Oxford Diffraction Ltd., version 171.13 beta

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Re10.00000.16966 (10)0.25000.0067 (4)
Mn10.50000.6811 (4)0.25000.0082 (5)
O10.2078 (16)0.1056 (14)0.9375 (15)0.0076 (15)
O20.2595 (18)0.3712 (13)0.3881 (16)0.0092 (16)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Re10.0069 (5)0.0060 (4)0.0074 (4)0.0000.0013 (2)0.000
Mn10.0077 (13)0.0081 (12)0.0091 (12)0.0000.0038 (10)0.000
O10.007 (4)0.009 (3)0.006 (3)0.005 (3)0.001 (3)0.001 (3)
O20.016 (4)0.005 (3)0.007 (3)0.004 (3)0.005 (3)0.000 (3)
Geometric parameters (Å, º) top
Re1—O21.803 (8)Mn1—O1viii2.109 (7)
Re1—O2i1.803 (8)Mn1—O2vii2.144 (9)
Re1—O1ii1.949 (7)Mn1—O2viii2.144 (9)
Re1—O1iii1.949 (7)Mn1—O22.225 (8)
Re1—O1iv2.053 (8)Mn1—O2ix2.225 (8)
Re1—O1v2.053 (8)O1—Re1x1.949 (7)
Re1—Re1vi3.1787 (7)O1—Re1iv2.053 (8)
Re1—Re1iv3.1787 (7)O1—Mn1viii2.109 (7)
Mn1—O1vii2.109 (7)O2—Mn1viii2.144 (9)
O2—Re1—O2i102.0 (5)O1iv—Re1—Re1iv84.2 (2)
O2—Re1—O1ii99.9 (3)O1v—Re1—Re1iv36.3 (2)
O2i—Re1—O1ii93.6 (3)Re1vi—Re1—Re1iv106.09 (3)
O2—Re1—O1iii93.6 (3)O1vii—Mn1—O1viii110.5 (4)
O2i—Re1—O1iii99.9 (3)O1vii—Mn1—O2vii97.1 (3)
O1ii—Re1—O1iii158.7 (4)O1viii—Mn1—O2vii91.9 (3)
O2—Re1—O1iv165.4 (3)O1vii—Mn1—O2viii91.9 (3)
O2i—Re1—O1iv89.0 (3)O1viii—Mn1—O2viii97.1 (3)
O1ii—Re1—O1iv88.9 (3)O2vii—Mn1—O2viii164.2 (4)
O1iii—Re1—O1iv74.9 (3)O1vii—Mn1—O286.4 (3)
O2—Re1—O1v89.0 (3)O1viii—Mn1—O2162.9 (3)
O2i—Re1—O1v165.4 (3)O2vii—Mn1—O284.1 (3)
O1ii—Re1—O1v74.9 (3)O2viii—Mn1—O283.6 (3)
O1iii—Re1—O1v88.9 (3)O1vii—Mn1—O2ix162.9 (3)
O1iv—Re1—O1v81.9 (4)O1viii—Mn1—O2ix86.4 (3)
O2—Re1—Re1vi131.5 (2)O2vii—Mn1—O2ix83.6 (3)
O2i—Re1—Re1vi95.4 (3)O2viii—Mn1—O2ix84.1 (3)
O1ii—Re1—Re1vi124.0 (2)O2—Mn1—O2ix76.7 (4)
O1iii—Re1—Re1vi38.6 (2)Re1x—O1—Re1iv105.1 (3)
O1iv—Re1—Re1vi36.3 (2)Re1x—O1—Mn1viii129.8 (4)
O1v—Re1—Re1vi84.2 (2)Re1iv—O1—Mn1viii122.7 (4)
O2—Re1—Re1iv95.4 (3)Re1—O2—Mn1viii125.5 (4)
O2i—Re1—Re1iv131.5 (2)Re1—O2—Mn1136.9 (4)
O1ii—Re1—Re1iv38.6 (2)Mn1viii—O2—Mn196.4 (3)
O1iii—Re1—Re1iv124.0 (2)
O2i—Re1—O2—Mn1viii142.7 (6)Re1vi—Re1—O2—Mn156.1 (8)
O1ii—Re1—O2—Mn1viii46.9 (5)Re1iv—Re1—O2—Mn1173.2 (6)
O1iii—Re1—O2—Mn1viii116.4 (5)O1vii—Mn1—O2—Re199.9 (7)
O1iv—Re1—O2—Mn1viii79.3 (13)O1viii—Mn1—O2—Re174.6 (14)
O1v—Re1—O2—Mn1viii27.5 (5)O2vii—Mn1—O2—Re12.4 (7)
Re1vi—Re1—O2—Mn1viii108.8 (4)O2viii—Mn1—O2—Re1167.7 (8)
Re1iv—Re1—O2—Mn1viii8.3 (5)O2ix—Mn1—O2—Re182.4 (6)
O2i—Re1—O2—Mn152.3 (5)O1vii—Mn1—O2—Mn1viii92.3 (3)
O1ii—Re1—O2—Mn1148.1 (6)O1viii—Mn1—O2—Mn1viii93.2 (10)
O1iii—Re1—O2—Mn148.6 (6)O2vii—Mn1—O2—Mn1viii170.2 (3)
O1iv—Re1—O2—Mn185.7 (15)O2viii—Mn1—O2—Mn1viii0.0
O1v—Re1—O2—Mn1137.5 (6)O2ix—Mn1—O2—Mn1viii85.4 (4)
Symmetry codes: (i) x, y, z+1/2; (ii) x, y, z+3/2; (iii) x, y, z1; (iv) x, y, z+1; (v) x, y, z1/2; (vi) x, y, z; (vii) x, y+1, z1/2; (viii) x+1, y+1, z+1; (ix) x+1, y, z+1/2; (x) x, y, z+1.

Experimental details

Crystal data
Chemical formulaMnO4Re
Mr305.14
Crystal system, space groupMonoclinic, P2/c
Temperature (K)304
a, b, c (Å)4.8022 (5), 5.6318 (6), 5.0803 (6)
β (°) 92.762 (9)
V3)137.24 (3)
Z2
Radiation typeMo Kα
µ (mm1)48.46
Crystal size (mm)0.05 × 0.04 × 0.03
Data collection
DiffractometerOxford Diffraction Xcalibur (TM) Single Crystal X-ray Diffractometer with Sapphire CCD detector
Absorption correctionNumerical
CrysAlis RED, Oxford Diffraction Ltd., version 170.17, 2003 Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid.
Tmin, Tmax0.257, 0.401
No. of measured, independent and
observed [I > 2σ(I)] reflections
823, 272, 263
Rint0.038
(sin θ/λ)max1)0.624
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.028, 0.066, 1.17
No. of reflections272
No. of parameters30
Δρmax, Δρmin (e Å3)2.28, 2.38

Computer programs: CrysAlis CCD (Oxford Diffraction Limited, 2001), CrysAlis RED (Oxford Diffraction Limited, 2001), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), Diamond (Brandenburg, 2001).

 

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