Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520614006611/hw5031sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006611/hw5031250Ksup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520614006611/hw503190Ksup3.hkl |
CCDC references: 993598; 993599
Crystal data, data collection and structure refinement details are summarized in Table 1.
For both compounds, program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).
Ge4Mn4 | Dx = 7.668 Mg m−3 |
Mr = 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 |
Pilatus@SNBL diffractometer | 78 independent reflections |
Radiation source: ESRF bending magnet | 76 reflections with I > 2σ(I) |
Silicon monochromator | Rint = 0.031 |
ϕ scan | θmax = 24.9°, θmin = 5.8° |
Absorption correction: multi-scan SADABS v.2.06 (Sheldrick, 2003) | h = −5→5 |
Tmin = 0.472, Tmax = 0.685 | k = −5→5 |
522 measured reflections | l = −5→5 |
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(Fo2) + (0.018P)2 + 0.6307P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.050 | (Δ/σ)max < 0.001 |
S = 1.19 | Δρmax = 0.34 e Å−3 |
78 reflections | Δρmin = −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) |
Ge4Mn4 | Z = 1 |
Mr = 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 |
Pilatus@SNBL diffractometer | 78 independent reflections |
Absorption correction: multi-scan SADABS v.2.06 (Sheldrick, 2003) | 76 reflections with I > 2σ(I) |
Tmin = 0.472, Tmax = 0.685 | Rint = 0.031 |
522 measured reflections |
R[F2 > 2σ(F2)] = 0.022 | 0 restraints |
wR(F2) = 0.050 | Δρmax = 0.34 e Å−3 |
S = 1.19 | Δρmin = −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) |
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. |
x | y | z | Uiso*/Ueq | ||
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) |
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) |
Ge01—Mn02i | 2.442 (2) | Mn02—Ge01xi | 2.5119 (12) |
Ge01—Mn02ii | 2.5119 (12) | Mn02—Ge01xii | 2.6821 (15) |
Ge01—Mn02iii | 2.5119 (12) | Mn02—Ge01xiii | 2.6821 (15) |
Ge01—Mn02iv | 2.5119 (12) | Mn02—Ge01xiv | 2.6821 (15) |
Ge01—Mn02v | 2.6821 (15) | Mn02—Mn02xv | 2.9431 (7) |
Ge01—Mn02vi | 2.6821 (15) | Mn02—Mn02xvi | 2.9431 (7) |
Ge01—Mn02vii | 2.6821 (15) | Mn02—Mn02xvii | 2.9431 (7) |
Mn02—Ge01viii | 2.442 (2) | Mn02—Mn02xviii | 2.9431 (7) |
Mn02—Ge01ix | 2.5119 (12) | Mn02—Mn02xix | 2.9431 (7) |
Mn02—Ge01x | 2.5119 (12) | ||
Mn02i—Ge01—Mn02ii | 137.43 (2) | Ge01x—Mn02—Mn02xv | 155.72 (5) |
Mn02i—Ge01—Mn02iii | 137.43 (2) | Ge01xi—Mn02—Mn02xv | 54.138 (17) |
Mn02ii—Ge01—Mn02iii | 71.72 (3) | Ge01xii—Mn02—Mn02xv | 104.62 (7) |
Mn02i—Ge01—Mn02iv | 137.43 (2) | Ge01xiii—Mn02—Mn02xv | 52.80 (3) |
Mn02ii—Ge01—Mn02iv | 71.72 (3) | Ge01xiv—Mn02—Mn02xv | 51.20 (5) |
Mn02iii—Ge01—Mn02iv | 71.72 (3) | Ge01viii—Mn02—Mn02xvi | 115.10 (5) |
Mn02i—Ge01—Mn02v | 69.93 (3) | Ge01ix—Mn02—Mn02xvi | 155.72 (5) |
Mn02ii—Ge01—Mn02v | 68.94 (2) | Ge01x—Mn02—Mn02xvi | 54.138 (17) |
Mn02iii—Ge01—Mn02v | 114.26 (6) | Ge01xi—Mn02—Mn02xvi | 91.88 (2) |
Mn02iv—Ge01—Mn02v | 134.96 (5) | Ge01xii—Mn02—Mn02xvi | 51.20 (5) |
Mn02i—Ge01—Mn02vi | 69.93 (3) | Ge01xiii—Mn02—Mn02xvi | 104.62 (7) |
Mn02ii—Ge01—Mn02vi | 114.26 (6) | Ge01xiv—Mn02—Mn02xvi | 52.80 (3) |
Mn02iii—Ge01—Mn02vi | 134.96 (5) | Mn02xv—Mn02—Mn02xvi | 103.30 (6) |
Mn02iv—Ge01—Mn02vi | 68.94 (2) | Ge01viii—Mn02—Mn02xvii | 115.10 (5) |
Mn02v—Ge01—Mn02vi | 108.87 (3) | Ge01ix—Mn02—Mn02xvii | 54.138 (17) |
Mn02i—Ge01—Mn02vii | 69.93 (3) | Ge01x—Mn02—Mn02xvii | 91.88 (2) |
Mn02ii—Ge01—Mn02vii | 134.96 (5) | Ge01xi—Mn02—Mn02xvii | 155.72 (5) |
Mn02iii—Ge01—Mn02vii | 68.94 (2) | Ge01xii—Mn02—Mn02xvii | 52.80 (3) |
Mn02iv—Ge01—Mn02vii | 114.26 (6) | Ge01xiii—Mn02—Mn02xvii | 51.20 (6) |
Mn02v—Ge01—Mn02vii | 108.87 (3) | Ge01xiv—Mn02—Mn02xvii | 104.62 (7) |
Mn02vi—Ge01—Mn02vii | 108.87 (3) | Mn02xv—Mn02—Mn02xvii | 103.30 (6) |
Ge01viii—Mn02—Ge01ix | 73.64 (4) | Mn02xvi—Mn02—Mn02xvii | 103.30 (6) |
Ge01viii—Mn02—Ge01x | 73.64 (4) | Ge01viii—Mn02—Mn02xviii | 58.87 (5) |
Ge01ix—Mn02—Ge01x | 112.39 (3) | Ge01ix—Mn02—Mn02xviii | 132.45 (9) |
Ge01viii—Mn02—Ge01xi | 73.64 (4) | Ge01x—Mn02—Mn02xviii | 54.137 (17) |
Ge01ix—Mn02—Ge01xi | 112.39 (3) | Ge01xi—Mn02—Mn02xviii | 58.26 (4) |
Ge01x—Mn02—Ge01xi | 112.39 (3) | Ge01xii—Mn02—Mn02xviii | 107.96 (5) |
Ge01viii—Mn02—Ge01xii | 140.27 (2) | Ge01xiii—Mn02—Mn02xviii | 155.47 (5) |
Ge01ix—Mn02—Ge01xii | 106.93 (5) | Ge01xiv—Mn02—Mn02xviii | 88.55 (2) |
Ge01x—Mn02—Ge01xii | 69.65 (2) | Mn02xv—Mn02—Mn02xviii | 109.210 (9) |
Ge01xi—Mn02—Ge01xii | 134.96 (5) | Mn02xvi—Mn02—Mn02xviii | 60.0 |
Ge01viii—Mn02—Ge01xiii | 140.27 (2) | Mn02xvii—Mn02—Mn02xviii | 146.000 (15) |
Ge01ix—Mn02—Ge01xiii | 69.65 (2) | Ge01viii—Mn02—Mn02xix | 58.87 (5) |
Ge01x—Mn02—Ge01xiii | 134.96 (5) | Ge01ix—Mn02—Mn02xix | 54.137 (17) |
Ge01xi—Mn02—Ge01xiii | 106.93 (5) | Ge01x—Mn02—Mn02xix | 58.26 (4) |
Ge01xii—Mn02—Ge01xiii | 67.22 (4) | Ge01xi—Mn02—Mn02xix | 132.45 (9) |
Ge01viii—Mn02—Ge01xiv | 140.27 (2) | Ge01xii—Mn02—Mn02xix | 88.55 (2) |
Ge01ix—Mn02—Ge01xiv | 134.96 (5) | Ge01xiii—Mn02—Mn02xix | 107.96 (5) |
Ge01x—Mn02—Ge01xiv | 106.93 (5) | Ge01xiv—Mn02—Mn02xix | 155.47 (5) |
Ge01xi—Mn02—Ge01xiv | 69.65 (2) | Mn02xv—Mn02—Mn02xix | 146.000 (15) |
Ge01xii—Mn02—Ge01xiv | 67.22 (4) | Mn02xvi—Mn02—Mn02xix | 109.210 (9) |
Ge01xiii—Mn02—Ge01xiv | 67.22 (4) | Mn02xvii—Mn02—Mn02xix | 60.0 |
Ge01viii—Mn02—Mn02xv | 115.10 (5) | Mn02xviii—Mn02—Mn02xix | 95.68 (7) |
Ge01ix—Mn02—Mn02xv | 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. |
Ge4Mn4 | Dx = 7.709 Mg m−3 |
Mr = 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 |
Pilatus@SNBL diffractometer | 78 independent reflections |
Radiation source: ESRF bending magnet | 78 reflections with I > 2σ(I) |
Silicon monochromator | Rint = 0.039 |
ϕ scan | θmax = 24.9°, θmin = 5.8° |
Absorption correction: multi-scan SADABS v.2.06 (Sheldrick, 2003) | h = −5→5 |
Tmin = 0.472, Tmax = 0.685 | k = −5→5 |
505 measured reflections | l = −5→5 |
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(Fo2) + (0.0245P)2 + 0.0611P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.054 | (Δ/σ)max < 0.001 |
S = 1.27 | Δρmax = 0.54 e Å−3 |
78 reflections | Δρmin = −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) |
Ge4Mn4 | Z = 1 |
Mr = 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 |
Pilatus@SNBL diffractometer | 78 independent reflections |
Absorption correction: multi-scan SADABS v.2.06 (Sheldrick, 2003) | 78 reflections with I > 2σ(I) |
Tmin = 0.472, Tmax = 0.685 | Rint = 0.039 |
505 measured reflections |
R[F2 > 2σ(F2)] = 0.024 | 0 restraints |
wR(F2) = 0.054 | Δρmax = 0.54 e Å−3 |
S = 1.27 | Δρmin = −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) |
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. |
x | y | z | Uiso*/Ueq | ||
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) |
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) |
Ge01—Mn02i | 2.439 (2) | Mn02—Ge01xi | 2.5085 (12) |
Ge01—Mn02ii | 2.5085 (12) | Mn02—Ge01xii | 2.6753 (15) |
Ge01—Mn02iii | 2.5085 (12) | Mn02—Ge01xiii | 2.6753 (15) |
Ge01—Mn02iv | 2.5085 (12) | Mn02—Ge01xiv | 2.6753 (15) |
Ge01—Mn02v | 2.6753 (15) | Mn02—Mn02xv | 2.9380 (8) |
Ge01—Mn02vi | 2.6753 (15) | Mn02—Mn02xvi | 2.9380 (8) |
Ge01—Mn02vii | 2.6753 (15) | Mn02—Mn02xvii | 2.9380 (7) |
Mn02—Ge01viii | 2.439 (2) | Mn02—Mn02xviii | 2.9380 (8) |
Mn02—Ge01ix | 2.5085 (12) | Mn02—Mn02xix | 2.9380 (8) |
Mn02—Ge01x | 2.5085 (12) | ||
Mn02i—Ge01—Mn02ii | 137.45 (2) | Ge01x—Mn02—Mn02xv | 54.154 (17) |
Mn02i—Ge01—Mn02iii | 137.45 (2) | Ge01xi—Mn02—Mn02xv | 58.20 (4) |
Mn02ii—Ge01—Mn02iii | 71.69 (3) | Ge01xii—Mn02—Mn02xv | 108.00 (5) |
Mn02i—Ge01—Mn02iv | 137.45 (2) | Ge01xiii—Mn02—Mn02xv | 155.54 (5) |
Mn02ii—Ge01—Mn02iv | 71.69 (3) | Ge01xiv—Mn02—Mn02xv | 88.58 (2) |
Mn02iii—Ge01—Mn02iv | 71.69 (3) | Ge01viii—Mn02—Mn02xvi | 58.80 (5) |
Mn02i—Ge01—Mn02v | 69.95 (3) | Ge01ix—Mn02—Mn02xvi | 58.20 (4) |
Mn02ii—Ge01—Mn02v | 68.96 (2) | Ge01x—Mn02—Mn02xvi | 132.33 (8) |
Mn02iii—Ge01—Mn02v | 114.18 (5) | Ge01xi—Mn02—Mn02xvi | 54.154 (17) |
Mn02iv—Ge01—Mn02v | 135.00 (5) | Ge01xii—Mn02—Mn02xvi | 155.54 (5) |
Mn02i—Ge01—Mn02vi | 69.95 (3) | Ge01xiii—Mn02—Mn02xvi | 88.58 (2) |
Mn02ii—Ge01—Mn02vi | 114.18 (5) | Ge01xiv—Mn02—Mn02xvi | 108.00 (5) |
Mn02iii—Ge01—Mn02vi | 135.00 (5) | Mn02xv—Mn02—Mn02xvi | 95.60 (7) |
Mn02iv—Ge01—Mn02vi | 68.96 (2) | Ge01viii—Mn02—Mn02xvii | 58.80 (5) |
Mn02v—Ge01—Mn02vi | 108.88 (3) | Ge01ix—Mn02—Mn02xvii | 54.154 (17) |
Mn02i—Ge01—Mn02vii | 69.95 (3) | Ge01x—Mn02—Mn02xvii | 58.20 (4) |
Mn02ii—Ge01—Mn02vii | 135.00 (5) | Ge01xi—Mn02—Mn02xvii | 132.33 (8) |
Mn02iii—Ge01—Mn02vii | 68.96 (2) | Ge01xii—Mn02—Mn02xvii | 88.58 (2) |
Mn02iv—Ge01—Mn02vii | 114.18 (5) | Ge01xiii—Mn02—Mn02xvii | 108.00 (5) |
Mn02v—Ge01—Mn02vii | 108.88 (3) | Ge01xiv—Mn02—Mn02xvii | 155.54 (5) |
Mn02vi—Ge01—Mn02vii | 108.88 (3) | Mn02xv—Mn02—Mn02xvii | 95.60 (7) |
Ge01viii—Mn02—Ge01ix | 73.59 (4) | Mn02xvi—Mn02—Mn02xvii | 95.60 (7) |
Ge01viii—Mn02—Ge01x | 73.59 (4) | Ge01viii—Mn02—Mn02xviii | 115.04 (5) |
Ge01ix—Mn02—Ge01x | 112.35 (3) | Ge01ix—Mn02—Mn02xviii | 155.80 (5) |
Ge01viii—Mn02—Ge01xi | 73.59 (4) | Ge01x—Mn02—Mn02xviii | 54.154 (17) |
Ge01ix—Mn02—Ge01xi | 112.35 (3) | Ge01xi—Mn02—Mn02xviii | 91.85 (2) |
Ge01x—Mn02—Ge01xi | 112.35 (3) | Ge01xii—Mn02—Mn02xviii | 51.25 (6) |
Ge01viii—Mn02—Ge01xii | 140.24 (2) | Ge01xiii—Mn02—Mn02xviii | 104.72 (7) |
Ge01ix—Mn02—Ge01xii | 106.98 (5) | Ge01xiv—Mn02—Mn02xviii | 52.84 (3) |
Ge01x—Mn02—Ge01xii | 69.66 (2) | Mn02xv—Mn02—Mn02xviii | 60.0 |
Ge01xi—Mn02—Ge01xii | 135.00 (5) | Mn02xvi—Mn02—Mn02xviii | 145.980 (15) |
Ge01viii—Mn02—Ge01xiii | 140.24 (2) | Mn02xvii—Mn02—Mn02xviii | 109.199 (9) |
Ge01ix—Mn02—Ge01xiii | 69.66 (2) | Ge01viii—Mn02—Mn02xix | 115.04 (5) |
Ge01x—Mn02—Ge01xiii | 135.00 (5) | Ge01ix—Mn02—Mn02xix | 54.154 (17) |
Ge01xi—Mn02—Ge01xiii | 106.98 (5) | Ge01x—Mn02—Mn02xix | 91.85 (2) |
Ge01xii—Mn02—Ge01xiii | 67.27 (4) | Ge01xi—Mn02—Mn02xix | 155.80 (5) |
Ge01viii—Mn02—Ge01xiv | 140.24 (2) | Ge01xii—Mn02—Mn02xix | 52.84 (3) |
Ge01ix—Mn02—Ge01xiv | 135.00 (5) | Ge01xiii—Mn02—Mn02xix | 51.25 (6) |
Ge01x—Mn02—Ge01xiv | 106.98 (5) | Ge01xiv—Mn02—Mn02xix | 104.72 (7) |
Ge01xi—Mn02—Ge01xiv | 69.66 (2) | Mn02xv—Mn02—Mn02xix | 145.980 (15) |
Ge01xii—Mn02—Ge01xiv | 67.27 (4) | Mn02xvi—Mn02—Mn02xix | 109.199 (9) |
Ge01xiii—Mn02—Ge01xiv | 67.27 (4) | Mn02xvii—Mn02—Mn02xix | 60.0 |
Ge01viii—Mn02—Mn02xv | 58.80 (5) | Mn02xviii—Mn02—Mn02xix | 103.37 (6) |
Ge01ix—Mn02—Mn02xv | 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 |
Mr | 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) |
Tmin, Tmax | 0.472, 0.685 | 0.472, 0.685 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 522, 78, 76 | 505, 78, 78 |
Rint | 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 |
Δρmax, Δρmin (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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