Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768105005380/ws5018sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768105005380/ws5018sup2.fcf |
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).
MnO4Re | F(000) = 264 |
Mr = 305.14 | Dx = 7.384 Mg m−3 |
Monoclinic, P2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 4.8022 (5) Å | Cell parameters from 664 reflections |
b = 5.6318 (6) Å | θ = 3.6–32.4° |
c = 5.0803 (6) Å | µ = 48.46 mm−1 |
β = 92.762 (9)° | T = 304 K |
V = 137.24 (3) Å3 | Prism, black |
Z = 2 | 0.05 × 0.04 × 0.03 mm |
Oxford Diffraction Xcalibur (TM) Single Crystal X-ray Diffractometer with Sapphire CCD detector | 272 independent reflections |
Radiation source: fine-focus sealed tube | 263 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 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 = −5→5 |
Tmin = 0.257, Tmax = 0.401 | k = −6→7 |
823 measured reflections | l = −6→6 |
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)] = 0.028 | w = 1/[σ2(Fo2) + (0.0383P)2 + 2.3979P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.066 | (Δ/σ)max = 0.001 |
S = 1.17 | Δρmax = 2.28 e Å−3 |
272 reflections | Δρmin = −2.38 e Å−3 |
30 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.003 (2) |
MnO4Re | V = 137.24 (3) Å3 |
Mr = 305.14 | Z = 2 |
Monoclinic, P2/c | Mo Kα radiation |
a = 4.8022 (5) Å | µ = 48.46 mm−1 |
b = 5.6318 (6) Å | T = 304 K |
c = 5.0803 (6) Å | 0.05 × 0.04 × 0.03 mm |
β = 92.762 (9)° |
Oxford Diffraction Xcalibur (TM) Single Crystal X-ray Diffractometer with Sapphire CCD detector | 272 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 = 0.401 | Rint = 0.038 |
823 measured reflections |
R[F2 > 2σ(F2)] = 0.028 | 30 parameters |
wR(F2) = 0.066 | 0 restraints |
S = 1.17 | Δρmax = 2.28 e Å−3 |
272 reflections | Δρmin = −2.38 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Re1 | 0.0000 | 0.16966 (10) | 0.2500 | 0.0067 (4) | |
Mn1 | 0.5000 | 0.6811 (4) | 0.2500 | 0.0082 (5) | |
O1 | 0.2078 (16) | 0.1056 (14) | 0.9375 (15) | 0.0076 (15) | |
O2 | 0.2595 (18) | 0.3712 (13) | 0.3881 (16) | 0.0092 (16) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Re1 | 0.0069 (5) | 0.0060 (4) | 0.0074 (4) | 0.000 | 0.0013 (2) | 0.000 |
Mn1 | 0.0077 (13) | 0.0081 (12) | 0.0091 (12) | 0.000 | 0.0038 (10) | 0.000 |
O1 | 0.007 (4) | 0.009 (3) | 0.006 (3) | −0.005 (3) | 0.001 (3) | 0.001 (3) |
O2 | 0.016 (4) | 0.005 (3) | 0.007 (3) | −0.004 (3) | 0.005 (3) | 0.000 (3) |
Re1—O2 | 1.803 (8) | Mn1—O1viii | 2.109 (7) |
Re1—O2i | 1.803 (8) | Mn1—O2vii | 2.144 (9) |
Re1—O1ii | 1.949 (7) | Mn1—O2viii | 2.144 (9) |
Re1—O1iii | 1.949 (7) | Mn1—O2 | 2.225 (8) |
Re1—O1iv | 2.053 (8) | Mn1—O2ix | 2.225 (8) |
Re1—O1v | 2.053 (8) | O1—Re1x | 1.949 (7) |
Re1—Re1vi | 3.1787 (7) | O1—Re1iv | 2.053 (8) |
Re1—Re1iv | 3.1787 (7) | O1—Mn1viii | 2.109 (7) |
Mn1—O1vii | 2.109 (7) | O2—Mn1viii | 2.144 (9) |
O2—Re1—O2i | 102.0 (5) | O1iv—Re1—Re1iv | 84.2 (2) |
O2—Re1—O1ii | 99.9 (3) | O1v—Re1—Re1iv | 36.3 (2) |
O2i—Re1—O1ii | 93.6 (3) | Re1vi—Re1—Re1iv | 106.09 (3) |
O2—Re1—O1iii | 93.6 (3) | O1vii—Mn1—O1viii | 110.5 (4) |
O2i—Re1—O1iii | 99.9 (3) | O1vii—Mn1—O2vii | 97.1 (3) |
O1ii—Re1—O1iii | 158.7 (4) | O1viii—Mn1—O2vii | 91.9 (3) |
O2—Re1—O1iv | 165.4 (3) | O1vii—Mn1—O2viii | 91.9 (3) |
O2i—Re1—O1iv | 89.0 (3) | O1viii—Mn1—O2viii | 97.1 (3) |
O1ii—Re1—O1iv | 88.9 (3) | O2vii—Mn1—O2viii | 164.2 (4) |
O1iii—Re1—O1iv | 74.9 (3) | O1vii—Mn1—O2 | 86.4 (3) |
O2—Re1—O1v | 89.0 (3) | O1viii—Mn1—O2 | 162.9 (3) |
O2i—Re1—O1v | 165.4 (3) | O2vii—Mn1—O2 | 84.1 (3) |
O1ii—Re1—O1v | 74.9 (3) | O2viii—Mn1—O2 | 83.6 (3) |
O1iii—Re1—O1v | 88.9 (3) | O1vii—Mn1—O2ix | 162.9 (3) |
O1iv—Re1—O1v | 81.9 (4) | O1viii—Mn1—O2ix | 86.4 (3) |
O2—Re1—Re1vi | 131.5 (2) | O2vii—Mn1—O2ix | 83.6 (3) |
O2i—Re1—Re1vi | 95.4 (3) | O2viii—Mn1—O2ix | 84.1 (3) |
O1ii—Re1—Re1vi | 124.0 (2) | O2—Mn1—O2ix | 76.7 (4) |
O1iii—Re1—Re1vi | 38.6 (2) | Re1x—O1—Re1iv | 105.1 (3) |
O1iv—Re1—Re1vi | 36.3 (2) | Re1x—O1—Mn1viii | 129.8 (4) |
O1v—Re1—Re1vi | 84.2 (2) | Re1iv—O1—Mn1viii | 122.7 (4) |
O2—Re1—Re1iv | 95.4 (3) | Re1—O2—Mn1viii | 125.5 (4) |
O2i—Re1—Re1iv | 131.5 (2) | Re1—O2—Mn1 | 136.9 (4) |
O1ii—Re1—Re1iv | 38.6 (2) | Mn1viii—O2—Mn1 | 96.4 (3) |
O1iii—Re1—Re1iv | 124.0 (2) | ||
O2i—Re1—O2—Mn1viii | 142.7 (6) | Re1vi—Re1—O2—Mn1 | 56.1 (8) |
O1ii—Re1—O2—Mn1viii | 46.9 (5) | Re1iv—Re1—O2—Mn1 | 173.2 (6) |
O1iii—Re1—O2—Mn1viii | −116.4 (5) | O1vii—Mn1—O2—Re1 | 99.9 (7) |
O1iv—Re1—O2—Mn1viii | −79.3 (13) | O1viii—Mn1—O2—Re1 | −74.6 (14) |
O1v—Re1—O2—Mn1viii | −27.5 (5) | O2vii—Mn1—O2—Re1 | 2.4 (7) |
Re1vi—Re1—O2—Mn1viii | −108.8 (4) | O2viii—Mn1—O2—Re1 | −167.7 (8) |
Re1iv—Re1—O2—Mn1viii | 8.3 (5) | O2ix—Mn1—O2—Re1 | −82.4 (6) |
O2i—Re1—O2—Mn1 | −52.3 (5) | O1vii—Mn1—O2—Mn1viii | −92.3 (3) |
O1ii—Re1—O2—Mn1 | −148.1 (6) | O1viii—Mn1—O2—Mn1viii | 93.2 (10) |
O1iii—Re1—O2—Mn1 | 48.6 (6) | O2vii—Mn1—O2—Mn1viii | 170.2 (3) |
O1iv—Re1—O2—Mn1 | 85.7 (15) | O2viii—Mn1—O2—Mn1viii | 0.0 |
O1v—Re1—O2—Mn1 | 137.5 (6) | O2ix—Mn1—O2—Mn1viii | 85.4 (4) |
Symmetry codes: (i) −x, y, −z+1/2; (ii) −x, y, −z+3/2; (iii) x, y, z−1; (iv) −x, −y, −z+1; (v) x, −y, z−1/2; (vi) −x, −y, −z; (vii) x, −y+1, z−1/2; (viii) −x+1, −y+1, −z+1; (ix) −x+1, y, −z+1/2; (x) x, y, z+1. |
Experimental details
Crystal data | |
Chemical formula | MnO4Re |
Mr | 305.14 |
Crystal system, space group | Monoclinic, P2/c |
Temperature (K) | 304 |
a, b, c (Å) | 4.8022 (5), 5.6318 (6), 5.0803 (6) |
β (°) | 92.762 (9) |
V (Å3) | 137.24 (3) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 48.46 |
Crystal size (mm) | 0.05 × 0.04 × 0.03 |
Data collection | |
Diffractometer | Oxford Diffraction Xcalibur (TM) Single Crystal X-ray Diffractometer with Sapphire CCD detector |
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. |
Tmin, Tmax | 0.257, 0.401 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 823, 272, 263 |
Rint | 0.038 |
(sin θ/λ)max (Å−1) | 0.624 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.028, 0.066, 1.17 |
No. of reflections | 272 |
No. of parameters | 30 |
Δρmax, Δρmin (e Å−3) | 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).