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The crystal structure of Tm5Re2O12, pentathulium dirhenium dodecaoxide, was determined by synchrotron diffraction on a reticular merohedral twin, revealing space group C2/m with a = 12.3717 (7), b = 5.6744 (3), c = 7.4805 (4) Å, β = 107.816 (2)° and Z = 2. Distorted ReO6 octahedra form chains with alternating rhenium–rhenium distances of 2.455 (1) and 3.219 (1) Å. Early reports on Ln2ReO5 compounds are critically reviewed in the light of our results for Tm5Re2O12.

Supporting information

cif

Crystallographic Information File (CIF)
Contains datablocks tm5, global

fcf

Structure factor file (CIF format)
Contains datablock tm5

Computing details top

Program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).

Pentathulium dirhenium dodecaoxide top
Crystal data top
O12Re2Tm5F(000) = 1182
Mr = 1409.05Dx = 9.360 Mg m3
Monoclinic, C2/mSynchrotron radiation, λ = 0.42750 Å
a = 12.3717 (7) ÅCell parameters from 460 reflections
b = 5.6744 (3) Åθ = 3.4–38.9°
c = 7.4805 (4) ŵ = 16.59 mm1
β = 107.816 (2)°T = 293 K
V = 499.96 (5) Å3Needle, black
Z = 2
Data collection top
CCD
diffractometer
4961 independent reflections
Radiation source: synchrotron4165 reflections with I > 2σ(I)
Silicon monochromatorRint = 0.053
ω–scansθmax = 38.9°, θmin = 3.4°
Absorption correction: empirical (using intensity measurements)h = 3636
Tmin = 0.19, Tmax = 0.85k = 1116
8671 measured reflectionsl = 2120
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.068Secondary atom site location: difference Fourier map
wR(F2) = 0.152 w = 1/[σ2(Fo2) + (0.0103P)2 + 1.6684P]
where P = (Fo2 + 2Fc2)/3
S = 1.25(Δ/σ)max < 0.001
4961 reflectionsΔρmax = 14.23 e Å3
52 parametersΔρmin = 12.32 e Å3
Special details top

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
Re10.00000.28367 (4)0.00000.00224 (3)
Tm10.50000.00000.50000.00381 (5)
Tm20.31373 (2)0.50000.17505 (5)0.00319 (4)
Tm30.19638 (2)0.00000.35973 (5)0.00313 (4)
O10.0012 (4)0.00000.1787 (8)0.0057 (5)
O20.4989 (5)0.00000.2053 (9)0.0076 (6)
O30.3459 (3)0.2520 (8)0.4265 (7)0.0060 (4)
O40.1655 (3)0.2461 (8)0.0833 (8)0.0063 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Re10.00213 (4)0.00229 (6)0.00191 (6)0.0000.00005 (4)0.000
Tm10.00333 (8)0.00513 (11)0.00249 (10)0.0000.00018 (7)0.000
Tm20.00319 (6)0.00324 (7)0.00300 (8)0.0000.00074 (6)0.000
Tm30.00343 (6)0.00282 (7)0.00256 (8)0.0000.00006 (6)0.000
O10.0056 (9)0.0044 (11)0.0070 (14)0.0000.0022 (9)0.000
O20.0103 (13)0.0069 (14)0.0041 (13)0.0000.0000 (11)0.000
O30.0082 (9)0.0040 (8)0.0055 (10)0.0007 (7)0.0017 (8)0.0003 (8)
O40.0059 (7)0.0049 (9)0.0077 (12)0.0003 (6)0.0015 (8)0.0006 (8)
Geometric parameters (Å, º) top
Re1—O41.961 (4)Tm2—O4iii2.461 (5)
Re1—O4i1.961 (4)Tm2—O4xii2.461 (5)
Re1—O2ii1.969 (5)Tm2—Re1xi3.3857 (3)
Re1—O2iii1.969 (5)Tm2—Re1iii3.3857 (3)
Re1—O1iv2.089 (4)Tm2—Tm3xiii3.5204 (6)
Re1—O12.089 (4)Tm2—Tm3xiv3.646 (3)
Re1—Re1v2.4551 (5)Tm2—Tm33.646 (3)
Re1—Re1iv3.2193 (5)Tm3—O32.269 (4)
Re1—Tm2vi3.3857 (3)Tm3—O3viii2.269 (4)
Re1—Tm2iii3.3857 (3)Tm3—O3xiii2.307 (5)
Re1—Tm3iv3.4255 (3)Tm3—O3xv2.307 (5)
Re1—Tm33.4256 (3)Tm3—O12.380 (5)
Tm1—O22.201 (6)Tm3—O4viii2.426 (5)
Tm1—O2vii2.201 (6)Tm3—O42.426 (5)
Tm1—O32.311 (4)Tm3—Re1iv3.4256 (3)
Tm1—O3viii2.311 (4)Tm3—Tm2xiii3.5204 (6)
Tm1—O3ix2.311 (4)Tm3—Tm3xiii3.5370 (4)
Tm1—O3vii2.311 (4)Tm3—Tm3xvi3.5370 (4)
Tm1—Tm33.5775 (3)O1—Re1iv2.089 (4)
Tm1—Tm3vii3.5775 (3)O1—Tm2vi2.312 (4)
Tm2—O4x2.267 (4)O2—Re1xvii1.969 (5)
Tm2—O42.267 (4)O2—Re1iii1.969 (5)
Tm2—O3x2.285 (5)O3—Tm3xiii2.307 (5)
Tm2—O32.285 (5)O4—Tm2iii2.461 (5)
Tm2—O1xi2.312 (4)
O4—Re1—O4i167.5 (3)O3x—Tm2—Re1iii130.07 (10)
O4—Re1—O2ii94.3 (2)O3—Tm2—Re1iii93.32 (11)
O4i—Re1—O2ii93.5 (2)O1xi—Tm2—Re1iii37.36 (9)
O4—Re1—O2iii93.5 (2)O4iii—Tm2—Re1iii34.85 (9)
O4i—Re1—O2iii94.3 (2)O4xii—Tm2—Re1iii73.67 (10)
O2ii—Re1—O2iii102.9 (2)Re1xi—Tm2—Re1iii56.774 (9)
O4—Re1—O1iv85.53 (19)O4x—Tm2—Tm3xiii91.66 (15)
O4i—Re1—O1iv84.84 (19)O4—Tm2—Tm3xiii91.66 (15)
O2ii—Re1—O1iv168.14 (17)O3x—Tm2—Tm3xiii40.18 (12)
O2iii—Re1—O1iv88.96 (17)O3—Tm2—Tm3xiii40.18 (12)
O4—Re1—O184.84 (19)O1xi—Tm2—Tm3xiii109.12 (15)
O4i—Re1—O185.53 (19)O4iii—Tm2—Tm3xiii145.12 (12)
O2ii—Re1—O188.96 (17)O4xii—Tm2—Tm3xiii145.12 (12)
O2iii—Re1—O1168.14 (17)Re1xi—Tm2—Tm3xiii128.067 (9)
O1iv—Re1—O179.2 (2)Re1iii—Tm2—Tm3xiii128.067 (9)
O4—Re1—Re1v96.25 (13)O4x—Tm2—Tm3xiv40.63 (14)
O4i—Re1—Re1v96.25 (13)O4—Tm2—Tm3xiv103.31 (12)
O2ii—Re1—Re1v51.44 (12)O3x—Tm2—Tm3xiv36.66 (11)
O2iii—Re1—Re1v51.44 (12)O3—Tm2—Tm3xiv99.01 (12)
O1iv—Re1—Re1v140.40 (12)O1xi—Tm2—Tm3xiv120.67 (6)
O1—Re1—Re1v140.40 (12)O4iii—Tm2—Tm3xiv152.69 (11)
O4—Re1—Re1iv83.75 (13)O4xii—Tm2—Tm3xiv90.32 (11)
O4i—Re1—Re1iv83.75 (13)Re1xi—Tm2—Tm3xiv99.999 (7)
O2ii—Re1—Re1iv128.56 (12)Re1iii—Tm2—Tm3xiv156.003 (9)
O2iii—Re1—Re1iv128.56 (12)Tm3xiii—Tm2—Tm3xiv59.118 (7)
O1iv—Re1—Re1iv39.60 (12)O4x—Tm2—Tm3103.31 (12)
O1—Re1—Re1iv39.60 (12)O4—Tm2—Tm340.63 (14)
Re1v—Re1—Re1iv180.0O3x—Tm2—Tm399.01 (12)
O4—Re1—Tm2vi126.39 (16)O3—Tm2—Tm336.66 (11)
O4i—Re1—Tm2vi45.83 (16)O1xi—Tm2—Tm3120.67 (6)
O2ii—Re1—Tm2vi80.03 (15)O4iii—Tm2—Tm390.32 (11)
O2iii—Re1—Tm2vi139.98 (17)O4xii—Tm2—Tm3152.69 (11)
O1iv—Re1—Tm2vi90.49 (12)Re1xi—Tm2—Tm3156.003 (9)
O1—Re1—Tm2vi42.18 (12)Re1iii—Tm2—Tm399.999 (7)
Re1v—Re1—Tm2vi118.387 (5)Tm3xiii—Tm2—Tm359.118 (7)
Re1iv—Re1—Tm2vi61.613 (5)Tm3xiv—Tm2—Tm3102.187 (13)
O4—Re1—Tm2iii45.83 (16)O3—Tm3—O3viii78.1 (2)
O4i—Re1—Tm2iii126.39 (16)O3—Tm3—O3xiii78.77 (17)
O2ii—Re1—Tm2iii139.98 (17)O3viii—Tm3—O3xiii125.04 (8)
O2iii—Re1—Tm2iii80.03 (15)O3—Tm3—O3xv125.04 (8)
O1iv—Re1—Tm2iii42.18 (12)O3viii—Tm3—O3xv78.77 (17)
O1—Re1—Tm2iii90.48 (12)O3xiii—Tm3—O3xv75.2 (2)
Re1v—Re1—Tm2iii118.387 (5)O3—Tm3—O1137.90 (12)
Re1iv—Re1—Tm2iii61.613 (5)O3viii—Tm3—O1137.90 (12)
Tm2vi—Re1—Tm2iii123.225 (9)O3xiii—Tm3—O189.37 (15)
O4—Re1—Tm3iv128.26 (15)O3xv—Tm3—O189.37 (15)
O4i—Re1—Tm3iv43.82 (16)O3—Tm3—O4viii117.10 (13)
O2ii—Re1—Tm3iv137.15 (17)O3viii—Tm3—O4viii74.35 (17)
O2iii—Re1—Tm3iv81.53 (13)O3xiii—Tm3—O4viii158.69 (15)
O1iv—Re1—Tm3iv43.18 (12)O3xv—Tm3—O4viii103.27 (16)
O1—Re1—Tm3iv90.29 (13)O1—Tm3—O4viii69.33 (14)
Re1v—Re1—Tm3iv118.028 (5)O3—Tm3—O474.35 (17)
Re1iv—Re1—Tm3iv61.972 (5)O3viii—Tm3—O4117.10 (13)
Tm2vi—Re1—Tm3iv71.175 (9)O3xiii—Tm3—O4103.27 (16)
Tm2iii—Re1—Tm3iv82.869 (9)O3xv—Tm3—O4158.69 (15)
O4—Re1—Tm343.82 (16)O1—Tm3—O469.33 (14)
O4i—Re1—Tm3128.26 (15)O4viii—Tm3—O470.3 (2)
O2ii—Re1—Tm381.53 (13)O3—Tm3—Re1iv143.46 (13)
O2iii—Re1—Tm3137.15 (17)O3viii—Tm3—Re1iv102.19 (12)
O1iv—Re1—Tm390.29 (13)O3xiii—Tm3—Re1iv125.06 (10)
O1—Re1—Tm343.18 (12)O3xv—Tm3—Re1iv90.07 (11)
Re1v—Re1—Tm3118.028 (5)O1—Tm3—Re1iv36.93 (9)
Re1iv—Re1—Tm361.972 (5)O4viii—Tm3—Re1iv34.02 (9)
Tm2vi—Re1—Tm382.869 (9)O4—Tm3—Re1iv73.26 (11)
Tm2iii—Re1—Tm371.175 (9)O3—Tm3—Re1102.19 (12)
Tm3iv—Re1—Tm3123.944 (9)O3viii—Tm3—Re1143.46 (13)
O2—Tm1—O2vii179.999 (1)O3xiii—Tm3—Re190.07 (11)
O2—Tm1—O390.57 (18)O3xv—Tm3—Re1125.06 (10)
O2vii—Tm1—O389.43 (18)O1—Tm3—Re136.93 (9)
O2—Tm1—O3viii90.57 (18)O4viii—Tm3—Re173.26 (11)
O2vii—Tm1—O3viii89.43 (18)O4—Tm3—Re134.02 (9)
O3—Tm1—O3viii76.4 (2)Re1iv—Tm3—Re156.055 (9)
O2—Tm1—O3ix89.43 (18)O3—Tm3—Tm2xiii93.18 (13)
O2vii—Tm1—O3ix90.57 (18)O3viii—Tm3—Tm2xiii93.18 (13)
O3—Tm1—O3ix103.6 (2)O3xiii—Tm3—Tm2xiii39.71 (12)
O3viii—Tm1—O3ix180.00 (14)O3xv—Tm3—Tm2xiii39.71 (12)
O2—Tm1—O3vii89.43 (18)O1—Tm3—Tm2xiii103.06 (14)
O2vii—Tm1—O3vii90.57 (18)O4viii—Tm3—Tm2xiii142.98 (11)
O3—Tm1—O3vii180.0 (2)O4—Tm3—Tm2xiii142.98 (11)
O3viii—Tm1—O3vii103.6 (2)Re1iv—Tm3—Tm2xiii123.051 (8)
O3ix—Tm1—O3vii76.4 (2)Re1—Tm3—Tm2xiii123.051 (8)
O2—Tm1—Tm391.27 (15)O3—Tm3—Tm3xiii39.78 (12)
O2vii—Tm1—Tm388.73 (15)O3viii—Tm3—Tm3xiii104.03 (11)
O3—Tm1—Tm338.22 (11)O3xiii—Tm3—Tm3xiii39.00 (10)
O3viii—Tm1—Tm338.22 (11)O3xv—Tm3—Tm3xiii101.62 (12)
O3ix—Tm1—Tm3141.78 (11)O1—Tm3—Tm3xiii117.96 (6)
O3vii—Tm1—Tm3141.78 (11)O4viii—Tm3—Tm3xiii154.15 (11)
O2—Tm1—Tm3vii88.73 (15)O4—Tm3—Tm3xiii88.67 (11)
O2vii—Tm1—Tm3vii91.27 (15)Re1iv—Tm3—Tm3xiii152.892 (11)
O3—Tm1—Tm3vii141.78 (11)Re1—Tm3—Tm3xiii97.833 (8)
O3viii—Tm1—Tm3vii141.78 (11)Tm2xiii—Tm3—Tm3xiii62.211 (11)
O3ix—Tm1—Tm3vii38.22 (11)O3—Tm3—Tm3xvi104.03 (11)
O3vii—Tm1—Tm3vii38.22 (11)O3viii—Tm3—Tm3xvi39.78 (12)
Tm3—Tm1—Tm3vii180.0O3xiii—Tm3—Tm3xvi101.62 (12)
O4x—Tm2—O478.9 (2)O3xv—Tm3—Tm3xvi39.00 (10)
O4x—Tm2—O3x77.20 (18)O1—Tm3—Tm3xvi117.96 (6)
O4—Tm2—O3x124.16 (14)O4viii—Tm3—Tm3xvi88.67 (11)
O4x—Tm2—O3124.16 (14)O4—Tm3—Tm3xvi154.15 (11)
O4—Tm2—O377.20 (18)Re1iv—Tm3—Tm3xvi97.834 (8)
O3x—Tm2—O376.1 (2)Re1—Tm3—Tm3xvi152.892 (11)
O4x—Tm2—O1xi136.01 (13)Tm2xiii—Tm3—Tm3xvi62.211 (11)
O4—Tm2—O1xi136.01 (13)Tm3xiii—Tm3—Tm3xvi106.672 (17)
O3x—Tm2—O1xi93.96 (15)Re1iv—O1—Re1100.8 (2)
O3—Tm2—O1xi93.96 (15)Re1iv—O1—Tm2vi100.46 (15)
O4x—Tm2—O4iii113.09 (9)Re1—O1—Tm2vi100.46 (15)
O4—Tm2—O4iii70.80 (19)Re1iv—O1—Tm399.89 (14)
O3x—Tm2—O4iii164.26 (15)Re1—O1—Tm399.89 (14)
O3—Tm2—O4iii105.28 (16)Tm2vi—O1—Tm3147.8 (3)
O1xi—Tm2—O4iii70.33 (15)Re1xvii—O2—Re1iii77.1 (2)
O4x—Tm2—O4xii70.80 (19)Re1xvii—O2—Tm1141.43 (12)
O4—Tm2—O4xii113.09 (9)Re1iii—O2—Tm1141.43 (12)
O3x—Tm2—O4xii105.28 (16)Tm3—O3—Tm2106.39 (18)
O3—Tm2—O4xii164.26 (15)Tm3—O3—Tm3xiii101.23 (17)
O1xi—Tm2—O4xii70.33 (15)Tm2—O3—Tm3xiii100.12 (16)
O4iii—Tm2—O4xii69.1 (2)Tm3—O3—Tm1102.71 (17)
O4x—Tm2—Re1xi99.45 (12)Tm2—O3—Tm1120.0 (2)
O4—Tm2—Re1xi140.21 (15)Tm3xiii—O3—Tm1123.9 (2)
O3x—Tm2—Re1xi93.32 (11)Re1—O4—Tm2134.1 (2)
O3—Tm2—Re1xi130.07 (10)Re1—O4—Tm3102.2 (2)
O1xi—Tm2—Re1xi37.36 (9)Tm2—O4—Tm3101.88 (19)
O4iii—Tm2—Re1xi73.67 (10)Re1—O4—Tm2iii99.3 (2)
O4xii—Tm2—Re1xi34.85 (9)Tm2—O4—Tm2iii109.20 (19)
O4x—Tm2—Re1iii140.21 (15)Tm3—O4—Tm2iii108.40 (17)
O4—Tm2—Re1iii99.45 (12)
Symmetry codes: (i) x, y, z; (ii) x1/2, y+1/2, z; (iii) x+1/2, y+1/2, z; (iv) x, y, z; (v) x, y+1, z; (vi) x1/2, y1/2, z; (vii) x+1, y, z+1; (viii) x, y, z; (ix) x+1, y, z+1; (x) x, y+1, z; (xi) x+1/2, y+1/2, z; (xii) x+1/2, y+1/2, z; (xiii) x+1/2, y+1/2, z+1; (xiv) x, y+1, z; (xv) x+1/2, y1/2, z+1; (xvi) x+1/2, y1/2, z+1; (xvii) x+1/2, y1/2, z.
 
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