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It is demonstrated that it is possible to perform single-crystal measurements in diamond anvil cells (DACs) with a monochromatic beam at modern hot neutron sources that offer the benefit of short neutron wavelengths with high fluxes. A piston–cylinder DAC with conical Boehler–Almax diamonds that allows for a wide accessibility of the reciprocal space has been developed. The diffraction data collected in this cell using hot neutrons are of very good quality and can be used for a full and reliable structure refinement.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600576718000997/pd5100sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576718000997/pd5100Isup2.hkl
Contains datablock I

CCDC reference: 1817441

Computing details top

(I) top
Crystal data top
Fe4MnSi3Orientation matrix based on 12 centered reflections
Mr = 362.6Dx = 6.331 Mg m3
Hexagonal, P63/mcmX-ray radiation, λ = 1.17 Å
Hall symbol: -P 6c;-2Cell parameters from 12 reflections
a = 6.80 (1) Åθ = 33–36°
c = 4.75 (4) ŵ = 0.02 mm1
V = 190.2 (16) Å3T = 293 K
Z = 20.2, black
F(000) = 95.3150.45 × 0.48 × 0.9 mm
Data collection top
4-circle
diffractometer
Rint = 0.108
Radiation source: reactorθmax = 48.7°, θmin = 5.7°
ω scansh = 88
831 measured reflectionsk = 88
60 independent reflectionsl = 45
52 reflections with I > 3σ(I)
Refinement top
Refinement on F0 restraints
R[F2 > 2σ(F2)] = 0.0780 constraints
wR(F2) = 0.065Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2)
S = 3.15(Δ/σ)max = 0.0002
60 reflectionsΔρmax = 2.66 e Å3
12 parametersΔρmin = 2.17 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Mn10.7577 (16)0.7577 (16)0.250.017 (5)0.30 (3)
Fe10.7577 (16)0.7577 (16)0.250.017 (5)0.70 (3)
Fe20.6666670.33333300.0101 (19)
Si10.3997 (16)0.3997 (16)0.250.011 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.022 (5)0.022 (5)0.009 (11)0.012 (5)00
Fe10.022 (5)0.022 (5)0.009 (11)0.012 (5)00
Fe20.0105 (18)0.0105 (18)0.009 (4)0.0052 (9)00
Si10.011 (5)0.011 (5)0.011 (13)0.006 (5)00
Bond lengths (Å) top
Mn1—Mn1i2.853 (18)Fe1—Fe1iii2.89 (3)
Mn1—Mn1ii2.853 (18)Fe1—Fe1iv2.89 (3)
Mn1—Mn1iii2.89 (3)Fe1—Fe1v2.89 (3)
Mn1—Mn1iv2.89 (3)Fe1—Fe1vi2.89 (3)
Mn1—Mn1v2.89 (3)Fe1—Fe22.887 (16)
Mn1—Mn1vi2.89 (3)Fe1—Fe2vii2.887 (16)
Mn1—Fe10Fe1—Fe2viii2.887 (16)
Mn1—Fe1i2.853 (18)Fe1—Fe2ix2.887 (16)
Mn1—Fe1ii2.853 (18)Fe1—Si12.435 (15)
Mn1—Fe1iii2.89 (3)Fe1—Si1x2.37 (2)
Mn1—Fe1iv2.89 (3)Fe1—Si1xi2.37 (2)
Mn1—Fe1v2.89 (3)Fe1—Si1xii2.61 (4)
Mn1—Fe1vi2.89 (3)Fe1—Si1vii2.61 (4)
Mn1—Fe22.887 (16)Fe2—Fe2xiii2.38 (4)
Mn1—Fe2vii2.887 (16)Fe2—Fe2ix2.38 (4)
Mn1—Fe2viii2.887 (16)Fe2—Si12.393 (15)
Mn1—Fe2ix2.887 (16)Fe2—Si1xiv2.393 (18)
Mn1—Si12.435 (15)Fe2—Si1xi2.393 (16)
Mn1—Si1x2.37 (2)Fe2—Si1xii2.393 (15)
Mn1—Si1xi2.37 (2)Fe2—Si1xv2.393 (16)
Mn1—Si1xii2.61 (4)Fe2—Si1v2.393 (18)
Mn1—Si1vii2.61 (4)Si1—Si1xii2.74 (4)
Fe1—Fe1i2.853 (18)Si1—Si1vii2.74 (4)
Fe1—Fe1ii2.853 (18)
Symmetry codes: (i) y+2, xy+1, z; (ii) x+y+1, x+2, z; (iii) y, x+y+1, z1/2; (iv) y, x+y+1, z+1/2; (v) xy+1, x, z1/2; (vi) xy+1, x, z+1/2; (vii) x+1, y+1, z+1/2; (viii) x+1, y+1, z; (ix) x, y, z+1/2; (x) y+1, xy+1, z; (xi) x+y+1, x+1, z; (xii) x+1, y+1, z1/2; (xiii) x, y, z1/2; (xiv) y+1, xy, z; (xv) y, x+y, z1/2.
 

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