Crystal structure and thermal expansion of Mn1−xFexGe

Dyadkin, V.; Grigoriev, S.; Ovsyannikov, S.V.; Bykova, E.; Dubrovinsky, L.; Tsvyashchenko, A.; Fomicheva, L.N.; Chernyshov, D.

doi:10.1107/S2052520614006611

Crystal structure and thermal expansion of Mn_1-xFe_xGe

V. Dyadkin, S. Grigoriev, S. V. Ovsyannikov, E. Bykova, L. Dubrovinsky, A. Tsvyashchenko, L. N. Fomicheva and D. Chernyshov

A series of temperature-dependent single-crystal and powder diffraction experiments has been carried out using synchrotron radiation in order to characterize the monogermanides of Mn, Fe and their solid solutions. The MnGe single crystal is found to be enantiopure and we report the absolute structure determination. The thermal expansion, parametrized with the Debye model, is discussed from the temperature-dependent powder diffraction measurements for Mn_1-xFe_xGe (x = 0, 0.1, 0.2, 0.25, 0.3, 0.4, 0.5, 0.6, 0.7, 0.75, 0.8, 0.9). Whereas the unit-cell dimension and the Debye temperature follow a linear trend as a function of composition, the thermal expansion coefficient deviates from linear dependence with increasing Mn content. No structural phase transformations have been observed for any composition in the temperature range 80-500 K for both single-crystal and powder diffraction, indicating that the phase transition previously observed with neutron powder diffraction most probably has a magnetic origin.

Keywords: thermal expansion; powder diffraction; monogermanides.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520614006611/hw5031sup1.cif Contains datablocks 250K, 90K
	Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006611/hw5031250Ksup2.hkl Contains datablock shelx
	Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006611/hw503190Ksup3.hkl Contains datablock shelx

CCDC references: 993598; 993599

Experimental top

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1.

Results and discussion top

Computing details top

For both compounds, program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).

Figures top

(250K) top

Crystal data top

Ge₄Mn₄	D_x = 7.668 Mg m⁻³
M_r = 510.12	Synchrotron radiation, λ = 0.68239 Å
Cubic, P2₁3	Cell parameters from 316 reflections
Hall symbol: P 2ac 2ab 3	θ = 7.1–28.6°
a = 4.7983 (11) Å	µ = 37.66 mm⁻¹
V = 110.47 (4) Å³	T = 250 K
Z = 1	Block, metallic dark grey
F(000) = 228	0.02 × 0.02 × 0.01 mm

Data collection top

Pilatus@SNBL diffractometer	78 independent reflections
Radiation source: ESRF bending magnet	76 reflections with I > 2σ(I)
Silicon monochromator	R_int = 0.031
ϕ scan	θ_max = 24.9°, θ_min = 5.8°
Absorption correction: multi-scan SADABS v.2.06 (Sheldrick, 2003)	h = −5→5
T_min = 0.472, T_max = 0.685	k = −5→5
522 measured reflections	l = −5→5

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.022	w = 1/[σ²(F_o²) + (0.018P)² + 0.6307P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.050	(Δ/σ)_max < 0.001
S = 1.19	Δρ_max = 0.34 e Å⁻³
78 reflections	Δρ_min = −0.68 e Å⁻³
7 parameters	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
0 restraints	Absolute structure parameter: 0.07 (11)

Crystal data top

Ge₄Mn₄	Z = 1
M_r = 510.12	Synchrotron radiation, λ = 0.68239 Å
Cubic, P2₁3	µ = 37.66 mm⁻¹
a = 4.7983 (11) Å	T = 250 K
V = 110.47 (4) Å³	0.02 × 0.02 × 0.01 mm

Data collection top

Pilatus@SNBL diffractometer	78 independent reflections
Absorption correction: multi-scan SADABS v.2.06 (Sheldrick, 2003)	76 reflections with I > 2σ(I)
T_min = 0.472, T_max = 0.685	R_int = 0.031
522 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.022	0 restraints
wR(F²) = 0.050	Δρ_max = 0.34 e Å⁻³
S = 1.19	Δρ_min = −0.68 e Å⁻³
78 reflections	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
7 parameters	Absolute structure parameter: 0.07 (11)

Special details top

Experimental. Comment on transmission values: The program SADABS (v2.06) outputs the ratio of minimum to maximum apparent transmission (0.689334). We have set T(max) to the expected value, i.e. exp(-r_min*mu) and we calculate T(min) from the minimum to maximum apparent transmission given by SADABS.

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

	x	y	z	U_iso*/U_eq
Ge01	0.15652 (16)	0.15652 (16)	0.15652 (16)	0.0090 (4)
Mn02	0.8627 (2)	0.8627 (2)	0.8627 (2)	0.0089 (5)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ge01	0.0090 (4)	0.0090 (4)	0.0090 (4)	−0.0003 (3)	−0.0003 (3)	−0.0003 (3)
Mn02	0.0089 (5)	0.0089 (5)	0.0089 (5)	−0.0010 (5)	−0.0010 (5)	−0.0010 (5)

Geometric parameters (Å, º) top

Ge01—Mn02ⁱ	2.442 (2)	Mn02—Ge01^xi	2.5119 (12)
Ge01—Mn02ⁱⁱ	2.5119 (12)	Mn02—Ge01^xii	2.6821 (15)
Ge01—Mn02ⁱⁱⁱ	2.5119 (12)	Mn02—Ge01^xiii	2.6821 (15)
Ge01—Mn02^iv	2.5119 (12)	Mn02—Ge01^xiv	2.6821 (15)
Ge01—Mn02^v	2.6821 (15)	Mn02—Mn02^xv	2.9431 (7)
Ge01—Mn02^vi	2.6821 (15)	Mn02—Mn02^xvi	2.9431 (7)
Ge01—Mn02^vii	2.6821 (15)	Mn02—Mn02^xvii	2.9431 (7)
Mn02—Ge01^viii	2.442 (2)	Mn02—Mn02^xviii	2.9431 (7)
Mn02—Ge01^ix	2.5119 (12)	Mn02—Mn02^xix	2.9431 (7)
Mn02—Ge01^x	2.5119 (12)

Mn02ⁱ—Ge01—Mn02ⁱⁱ	137.43 (2)	Ge01^x—Mn02—Mn02^xv	155.72 (5)
Mn02ⁱ—Ge01—Mn02ⁱⁱⁱ	137.43 (2)	Ge01^xi—Mn02—Mn02^xv	54.138 (17)
Mn02ⁱⁱ—Ge01—Mn02ⁱⁱⁱ	71.72 (3)	Ge01^xii—Mn02—Mn02^xv	104.62 (7)
Mn02ⁱ—Ge01—Mn02^iv	137.43 (2)	Ge01^xiii—Mn02—Mn02^xv	52.80 (3)
Mn02ⁱⁱ—Ge01—Mn02^iv	71.72 (3)	Ge01^xiv—Mn02—Mn02^xv	51.20 (5)
Mn02ⁱⁱⁱ—Ge01—Mn02^iv	71.72 (3)	Ge01^viii—Mn02—Mn02^xvi	115.10 (5)
Mn02ⁱ—Ge01—Mn02^v	69.93 (3)	Ge01^ix—Mn02—Mn02^xvi	155.72 (5)
Mn02ⁱⁱ—Ge01—Mn02^v	68.94 (2)	Ge01^x—Mn02—Mn02^xvi	54.138 (17)
Mn02ⁱⁱⁱ—Ge01—Mn02^v	114.26 (6)	Ge01^xi—Mn02—Mn02^xvi	91.88 (2)
Mn02^iv—Ge01—Mn02^v	134.96 (5)	Ge01^xii—Mn02—Mn02^xvi	51.20 (5)
Mn02ⁱ—Ge01—Mn02^vi	69.93 (3)	Ge01^xiii—Mn02—Mn02^xvi	104.62 (7)
Mn02ⁱⁱ—Ge01—Mn02^vi	114.26 (6)	Ge01^xiv—Mn02—Mn02^xvi	52.80 (3)
Mn02ⁱⁱⁱ—Ge01—Mn02^vi	134.96 (5)	Mn02^xv—Mn02—Mn02^xvi	103.30 (6)
Mn02^iv—Ge01—Mn02^vi	68.94 (2)	Ge01^viii—Mn02—Mn02^xvii	115.10 (5)
Mn02^v—Ge01—Mn02^vi	108.87 (3)	Ge01^ix—Mn02—Mn02^xvii	54.138 (17)
Mn02ⁱ—Ge01—Mn02^vii	69.93 (3)	Ge01^x—Mn02—Mn02^xvii	91.88 (2)
Mn02ⁱⁱ—Ge01—Mn02^vii	134.96 (5)	Ge01^xi—Mn02—Mn02^xvii	155.72 (5)
Mn02ⁱⁱⁱ—Ge01—Mn02^vii	68.94 (2)	Ge01^xii—Mn02—Mn02^xvii	52.80 (3)
Mn02^iv—Ge01—Mn02^vii	114.26 (6)	Ge01^xiii—Mn02—Mn02^xvii	51.20 (6)
Mn02^v—Ge01—Mn02^vii	108.87 (3)	Ge01^xiv—Mn02—Mn02^xvii	104.62 (7)
Mn02^vi—Ge01—Mn02^vii	108.87 (3)	Mn02^xv—Mn02—Mn02^xvii	103.30 (6)
Ge01^viii—Mn02—Ge01^ix	73.64 (4)	Mn02^xvi—Mn02—Mn02^xvii	103.30 (6)
Ge01^viii—Mn02—Ge01^x	73.64 (4)	Ge01^viii—Mn02—Mn02^xviii	58.87 (5)
Ge01^ix—Mn02—Ge01^x	112.39 (3)	Ge01^ix—Mn02—Mn02^xviii	132.45 (9)
Ge01^viii—Mn02—Ge01^xi	73.64 (4)	Ge01^x—Mn02—Mn02^xviii	54.137 (17)
Ge01^ix—Mn02—Ge01^xi	112.39 (3)	Ge01^xi—Mn02—Mn02^xviii	58.26 (4)
Ge01^x—Mn02—Ge01^xi	112.39 (3)	Ge01^xii—Mn02—Mn02^xviii	107.96 (5)
Ge01^viii—Mn02—Ge01^xii	140.27 (2)	Ge01^xiii—Mn02—Mn02^xviii	155.47 (5)
Ge01^ix—Mn02—Ge01^xii	106.93 (5)	Ge01^xiv—Mn02—Mn02^xviii	88.55 (2)
Ge01^x—Mn02—Ge01^xii	69.65 (2)	Mn02^xv—Mn02—Mn02^xviii	109.210 (9)
Ge01^xi—Mn02—Ge01^xii	134.96 (5)	Mn02^xvi—Mn02—Mn02^xviii	60.0
Ge01^viii—Mn02—Ge01^xiii	140.27 (2)	Mn02^xvii—Mn02—Mn02^xviii	146.000 (15)
Ge01^ix—Mn02—Ge01^xiii	69.65 (2)	Ge01^viii—Mn02—Mn02^xix	58.87 (5)
Ge01^x—Mn02—Ge01^xiii	134.96 (5)	Ge01^ix—Mn02—Mn02^xix	54.137 (17)
Ge01^xi—Mn02—Ge01^xiii	106.93 (5)	Ge01^x—Mn02—Mn02^xix	58.26 (4)
Ge01^xii—Mn02—Ge01^xiii	67.22 (4)	Ge01^xi—Mn02—Mn02^xix	132.45 (9)
Ge01^viii—Mn02—Ge01^xiv	140.27 (2)	Ge01^xii—Mn02—Mn02^xix	88.55 (2)
Ge01^ix—Mn02—Ge01^xiv	134.96 (5)	Ge01^xiii—Mn02—Mn02^xix	107.96 (5)
Ge01^x—Mn02—Ge01^xiv	106.93 (5)	Ge01^xiv—Mn02—Mn02^xix	155.47 (5)
Ge01^xi—Mn02—Ge01^xiv	69.65 (2)	Mn02^xv—Mn02—Mn02^xix	146.000 (15)
Ge01^xii—Mn02—Ge01^xiv	67.22 (4)	Mn02^xvi—Mn02—Mn02^xix	109.210 (9)
Ge01^xiii—Mn02—Ge01^xiv	67.22 (4)	Mn02^xvii—Mn02—Mn02^xix	60.0
Ge01^viii—Mn02—Mn02^xv	115.10 (5)	Mn02^xviii—Mn02—Mn02^xix	95.68 (7)
Ge01^ix—Mn02—Mn02^xv	91.88 (2)

Symmetry codes: (i) x−1, y−1, z−1; (ii) −x+1, y−1/2, −z+3/2; (iii) x−1/2, −y+3/2, −z+1; (iv) −x+3/2, −y+1, z−1/2; (v) −x+1/2, −y+1, z−1/2; (vi) x−1/2, −y+1/2, −z+1; (vii) −x+1, y−1/2, −z+1/2; (viii) x+1, y+1, z+1; (ix) −x+1, y+1/2, −z+3/2; (x) x+1/2, −y+3/2, −z+1; (xi) −x+3/2, −y+1, z+1/2; (xii) −x+1/2, −y+1, z+1/2; (xiii) x+1/2, −y+1/2, −z+1; (xiv) −x+1, y+1/2, −z+1/2; (xv) −x+2, y−1/2, −z+3/2; (xvi) −x+3/2, −y+2, z−1/2; (xvii) x−1/2, −y+3/2, −z+2; (xviii) −x+2, y+1/2, −z+3/2; (xix) −x+3/2, −y+2, z+1/2.

(90K) top

Crystal data top

Ge₄Mn₄	D_x = 7.709 Mg m⁻³
M_r = 510.12	Synchrotron radiation, λ = 0.68239 Å
Cubic, P2₁3	Cell parameters from 316 reflections
Hall symbol: P 2ac 2ab 3	θ = 7.1–28.6°
a = 4.7896 (12) Å	µ = 37.86 mm⁻¹
V = 109.87 (5) Å³	T = 90 K
Z = 1	Block, metallic dark grey
F(000) = 228	0.02 × 0.02 × 0.01 mm

Data collection top

Pilatus@SNBL diffractometer	78 independent reflections
Radiation source: ESRF bending magnet	78 reflections with I > 2σ(I)
Silicon monochromator	R_int = 0.039
ϕ scan	θ_max = 24.9°, θ_min = 5.8°
Absorption correction: multi-scan SADABS v.2.06 (Sheldrick, 2003)	h = −5→5
T_min = 0.472, T_max = 0.685	k = −5→5
505 measured reflections	l = −5→5

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.024	w = 1/[σ²(F_o²) + (0.0245P)² + 0.0611P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.054	(Δ/σ)_max < 0.001
S = 1.27	Δρ_max = 0.54 e Å⁻³
78 reflections	Δρ_min = −0.62 e Å⁻³
7 parameters	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
0 restraints	Absolute structure parameter: 0.01 (11)

Crystal data top

Ge₄Mn₄	Z = 1
M_r = 510.12	Synchrotron radiation, λ = 0.68239 Å
Cubic, P2₁3	µ = 37.86 mm⁻¹
a = 4.7896 (12) Å	T = 90 K
V = 109.87 (5) Å³	0.02 × 0.02 × 0.01 mm

Data collection top

Pilatus@SNBL diffractometer	78 independent reflections
Absorption correction: multi-scan SADABS v.2.06 (Sheldrick, 2003)	78 reflections with I > 2σ(I)
T_min = 0.472, T_max = 0.685	R_int = 0.039
505 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.024	0 restraints
wR(F²) = 0.054	Δρ_max = 0.54 e Å⁻³
S = 1.27	Δρ_min = −0.62 e Å⁻³
78 reflections	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
7 parameters	Absolute structure parameter: 0.01 (11)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ge01	0.15643 (16)	0.15643 (16)	0.15643 (16)	0.0055 (5)
Mn02	0.8624 (2)	0.8624 (2)	0.8624 (2)	0.0059 (5)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ge01	0.0055 (5)	0.0055 (5)	0.0055 (5)	−0.0006 (3)	−0.0006 (3)	−0.0006 (3)
Mn02	0.0059 (5)	0.0059 (5)	0.0059 (5)	−0.0001 (5)	−0.0001 (5)	−0.0001 (5)

Geometric parameters (Å, º) top

Ge01—Mn02ⁱ	2.439 (2)	Mn02—Ge01^xi	2.5085 (12)
Ge01—Mn02ⁱⁱ	2.5085 (12)	Mn02—Ge01^xii	2.6753 (15)
Ge01—Mn02ⁱⁱⁱ	2.5085 (12)	Mn02—Ge01^xiii	2.6753 (15)
Ge01—Mn02^iv	2.5085 (12)	Mn02—Ge01^xiv	2.6753 (15)
Ge01—Mn02^v	2.6753 (15)	Mn02—Mn02^xv	2.9380 (8)
Ge01—Mn02^vi	2.6753 (15)	Mn02—Mn02^xvi	2.9380 (8)
Ge01—Mn02^vii	2.6753 (15)	Mn02—Mn02^xvii	2.9380 (7)
Mn02—Ge01^viii	2.439 (2)	Mn02—Mn02^xviii	2.9380 (8)
Mn02—Ge01^ix	2.5085 (12)	Mn02—Mn02^xix	2.9380 (8)
Mn02—Ge01^x	2.5085 (12)

Mn02ⁱ—Ge01—Mn02ⁱⁱ	137.45 (2)	Ge01^x—Mn02—Mn02^xv	54.154 (17)
Mn02ⁱ—Ge01—Mn02ⁱⁱⁱ	137.45 (2)	Ge01^xi—Mn02—Mn02^xv	58.20 (4)
Mn02ⁱⁱ—Ge01—Mn02ⁱⁱⁱ	71.69 (3)	Ge01^xii—Mn02—Mn02^xv	108.00 (5)
Mn02ⁱ—Ge01—Mn02^iv	137.45 (2)	Ge01^xiii—Mn02—Mn02^xv	155.54 (5)
Mn02ⁱⁱ—Ge01—Mn02^iv	71.69 (3)	Ge01^xiv—Mn02—Mn02^xv	88.58 (2)
Mn02ⁱⁱⁱ—Ge01—Mn02^iv	71.69 (3)	Ge01^viii—Mn02—Mn02^xvi	58.80 (5)
Mn02ⁱ—Ge01—Mn02^v	69.95 (3)	Ge01^ix—Mn02—Mn02^xvi	58.20 (4)
Mn02ⁱⁱ—Ge01—Mn02^v	68.96 (2)	Ge01^x—Mn02—Mn02^xvi	132.33 (8)
Mn02ⁱⁱⁱ—Ge01—Mn02^v	114.18 (5)	Ge01^xi—Mn02—Mn02^xvi	54.154 (17)
Mn02^iv—Ge01—Mn02^v	135.00 (5)	Ge01^xii—Mn02—Mn02^xvi	155.54 (5)
Mn02ⁱ—Ge01—Mn02^vi	69.95 (3)	Ge01^xiii—Mn02—Mn02^xvi	88.58 (2)
Mn02ⁱⁱ—Ge01—Mn02^vi	114.18 (5)	Ge01^xiv—Mn02—Mn02^xvi	108.00 (5)
Mn02ⁱⁱⁱ—Ge01—Mn02^vi	135.00 (5)	Mn02^xv—Mn02—Mn02^xvi	95.60 (7)
Mn02^iv—Ge01—Mn02^vi	68.96 (2)	Ge01^viii—Mn02—Mn02^xvii	58.80 (5)
Mn02^v—Ge01—Mn02^vi	108.88 (3)	Ge01^ix—Mn02—Mn02^xvii	54.154 (17)
Mn02ⁱ—Ge01—Mn02^vii	69.95 (3)	Ge01^x—Mn02—Mn02^xvii	58.20 (4)
Mn02ⁱⁱ—Ge01—Mn02^vii	135.00 (5)	Ge01^xi—Mn02—Mn02^xvii	132.33 (8)
Mn02ⁱⁱⁱ—Ge01—Mn02^vii	68.96 (2)	Ge01^xii—Mn02—Mn02^xvii	88.58 (2)
Mn02^iv—Ge01—Mn02^vii	114.18 (5)	Ge01^xiii—Mn02—Mn02^xvii	108.00 (5)
Mn02^v—Ge01—Mn02^vii	108.88 (3)	Ge01^xiv—Mn02—Mn02^xvii	155.54 (5)
Mn02^vi—Ge01—Mn02^vii	108.88 (3)	Mn02^xv—Mn02—Mn02^xvii	95.60 (7)
Ge01^viii—Mn02—Ge01^ix	73.59 (4)	Mn02^xvi—Mn02—Mn02^xvii	95.60 (7)
Ge01^viii—Mn02—Ge01^x	73.59 (4)	Ge01^viii—Mn02—Mn02^xviii	115.04 (5)
Ge01^ix—Mn02—Ge01^x	112.35 (3)	Ge01^ix—Mn02—Mn02^xviii	155.80 (5)
Ge01^viii—Mn02—Ge01^xi	73.59 (4)	Ge01^x—Mn02—Mn02^xviii	54.154 (17)
Ge01^ix—Mn02—Ge01^xi	112.35 (3)	Ge01^xi—Mn02—Mn02^xviii	91.85 (2)
Ge01^x—Mn02—Ge01^xi	112.35 (3)	Ge01^xii—Mn02—Mn02^xviii	51.25 (6)
Ge01^viii—Mn02—Ge01^xii	140.24 (2)	Ge01^xiii—Mn02—Mn02^xviii	104.72 (7)
Ge01^ix—Mn02—Ge01^xii	106.98 (5)	Ge01^xiv—Mn02—Mn02^xviii	52.84 (3)
Ge01^x—Mn02—Ge01^xii	69.66 (2)	Mn02^xv—Mn02—Mn02^xviii	60.0
Ge01^xi—Mn02—Ge01^xii	135.00 (5)	Mn02^xvi—Mn02—Mn02^xviii	145.980 (15)
Ge01^viii—Mn02—Ge01^xiii	140.24 (2)	Mn02^xvii—Mn02—Mn02^xviii	109.199 (9)
Ge01^ix—Mn02—Ge01^xiii	69.66 (2)	Ge01^viii—Mn02—Mn02^xix	115.04 (5)
Ge01^x—Mn02—Ge01^xiii	135.00 (5)	Ge01^ix—Mn02—Mn02^xix	54.154 (17)
Ge01^xi—Mn02—Ge01^xiii	106.98 (5)	Ge01^x—Mn02—Mn02^xix	91.85 (2)
Ge01^xii—Mn02—Ge01^xiii	67.27 (4)	Ge01^xi—Mn02—Mn02^xix	155.80 (5)
Ge01^viii—Mn02—Ge01^xiv	140.24 (2)	Ge01^xii—Mn02—Mn02^xix	52.84 (3)
Ge01^ix—Mn02—Ge01^xiv	135.00 (5)	Ge01^xiii—Mn02—Mn02^xix	51.25 (6)
Ge01^x—Mn02—Ge01^xiv	106.98 (5)	Ge01^xiv—Mn02—Mn02^xix	104.72 (7)
Ge01^xi—Mn02—Ge01^xiv	69.66 (2)	Mn02^xv—Mn02—Mn02^xix	145.980 (15)
Ge01^xii—Mn02—Ge01^xiv	67.27 (4)	Mn02^xvi—Mn02—Mn02^xix	109.199 (9)
Ge01^xiii—Mn02—Ge01^xiv	67.27 (4)	Mn02^xvii—Mn02—Mn02^xix	60.0
Ge01^viii—Mn02—Mn02^xv	58.80 (5)	Mn02^xviii—Mn02—Mn02^xix	103.37 (6)
Ge01^ix—Mn02—Mn02^xv	132.33 (8)

Symmetry codes: (i) x−1, y−1, z−1; (ii) −x+1, y−1/2, −z+3/2; (iii) x−1/2, −y+3/2, −z+1; (iv) −x+3/2, −y+1, z−1/2; (v) −x+1/2, −y+1, z−1/2; (vi) x−1/2, −y+1/2, −z+1; (vii) −x+1, y−1/2, −z+1/2; (viii) x+1, y+1, z+1; (ix) −x+1, y+1/2, −z+3/2; (x) x+1/2, −y+3/2, −z+1; (xi) −x+3/2, −y+1, z+1/2; (xii) −x+1/2, −y+1, z+1/2; (xiii) x+1/2, −y+1/2, −z+1; (xiv) −x+1, y+1/2, −z+1/2; (xv) −x+2, y+1/2, −z+3/2; (xvi) x+1/2, −y+3/2, −z+2; (xvii) −x+3/2, −y+2, z+1/2; (xviii) −x+3/2, −y+2, z−1/2; (xix) x−1/2, −y+3/2, −z+2.

Experimental details

	(250K)	(90K)
Crystal data
Chemical formula	Ge₄Mn₄	Ge₄Mn₄
M_r	510.12	510.12
Crystal system, space group	Cubic, P2₁3	Cubic, P2₁3
Temperature (K)	250	90
a (Å)	4.7983 (11)	4.7896 (12)
V (Å³)	110.47 (4)	109.87 (5)
Z	1	1
Radiation type	Synchrotron, λ = 0.68239 Å	Synchrotron, λ = 0.68239 Å
µ (mm⁻¹)	37.66	37.86
Crystal size (mm)	0.02 × 0.02 × 0.01	0.02 × 0.02 × 0.01

Data collection
Diffractometer	Pilatus@SNBL diffractometer	Pilatus@SNBL diffractometer
Absorption correction	Multi-scan SADABS v.2.06 (Sheldrick, 2003)	Multi-scan SADABS v.2.06 (Sheldrick, 2003)
T_min, T_max	0.472, 0.685	0.472, 0.685
No. of measured, independent and observed [I > 2σ(I)] reflections	522, 78, 76	505, 78, 78
R_int	0.031	0.039
(sin θ/λ)_max (Å⁻¹)	0.617	0.618

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.022, 0.050, 1.19	0.024, 0.054, 1.27
No. of reflections	78	78
No. of parameters	7	7
Δρ_max, Δρ_min (e Å⁻³)	0.34, −0.68	0.54, −0.62
Absolute structure	Flack H D (1983), Acta Cryst. A39, 876-881	Flack H D (1983), Acta Cryst. A39, 876-881
Absolute structure parameter	0.07 (11)	0.01 (11)

Computer programs: SHELXL97 (Sheldrick, 1997).

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Crystal structure and thermal expansion of Mn1-xFexGe

Supporting information

Crystal structure and thermal expansion of Mn_1-xFe_xGe