Supporting information
Portable Document Format (PDF) file https://doi.org/10.1107/S205252061701647X/ps5066sup3.pdf | |
Crystallographic Information File (CIF) https://doi.org/10.1107/S205252061701647X/ps5066sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S205252061701647X/ps5066Isup2.hkl |
CCDC reference: 1585827
Data collection: CrysAlis PRO, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET); cell refinement: CrysAlis PRO, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET); data reduction: CrysAlis PRO, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2016/6 (Sheldrick, 2016).
Cu3O8TeH4 | Dx = 4.961 Mg m−3 |
Mr = 446.22 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Cmcm | Cell parameters from 857 reflections |
a = 2.93172 (16) Å | θ = 5.9–31.1° |
b = 11.8414 (6) Å | µ = 15.37 mm−1 |
c = 8.6047 (4) Å | T = 293 K |
V = 298.72 (3) Å3 | Triangular plate, translucent emerald green |
Z = 2 | 0.05 × 0.03 × 0.02 mm |
F(000) = 406 |
Xcalibur, Eos diffractometer | 763 independent reflections |
Radiation source: Enhance (Mo) X-ray Source | 649 reflections with I > 2σ(I) |
Detector resolution: 16.0869 pixels mm-1 | Rint = 0.037 |
1K CCD area detector scans | θmax = 32.7°, θmin = 3.4° |
Absorption correction: multi-scan Multi-scan ABSPACK | h = −4→4 |
Tmin = 0.801, Tmax = 1.000 | k = −17→17 |
764 measured reflections | l = −12→12 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H-atom parameters not defined |
R[F2 > 2σ(F2)] = 0.032 | w = 1/[σ2(Fo2) + (0.0378P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.068 | (Δ/σ)max < 0.001 |
S = 1.04 | Δρmax = 1.45 e Å−3 |
326 reflections | Δρmin = −2.09 e Å−3 |
25 parameters |
Experimental. CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. Refined as a 2-component twin. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cu1 | 0.000000 | 0.35007 (10) | 0.750000 | 0.0076 (3) | |
Te2 | −0.500000 | 0.500000 | 0.500000 | 0.0061 (2) | 0.509 (9) |
Cu2 | −0.500000 | 0.500000 | 0.500000 | 0.0061 (2) | 0.491 (9) |
O1 | −0.500000 | 0.4614 (7) | 0.750000 | 0.038 (2) | |
O2 | −0.500000 | 0.2384 (5) | 0.750000 | 0.0086 (12) | |
O3 | −1.000000 | 0.3928 (4) | 0.4789 (4) | 0.0087 (9) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.0051 (5) | 0.0085 (6) | 0.0092 (5) | 0.000 | 0.000 | 0.000 |
Te2 | 0.0039 (3) | 0.0078 (4) | 0.0066 (3) | 0.000 | 0.000 | 0.0005 (3) |
Cu2 | 0.0039 (3) | 0.0078 (4) | 0.0066 (3) | 0.000 | 0.000 | 0.0005 (3) |
O1 | 0.008 (3) | 0.008 (3) | 0.097 (8) | 0.000 | 0.000 | 0.000 |
O2 | 0.005 (3) | 0.009 (3) | 0.011 (3) | 0.000 | 0.000 | 0.000 |
O3 | 0.0097 (19) | 0.008 (2) | 0.008 (2) | 0.000 | 0.000 | 0.0002 (16) |
Cu1—O1i | 1.971 (5) | Te2—O3iv | 1.948 (3) |
Cu1—O1 | 1.971 (5) | Te2—O3v | 1.948 (3) |
Cu1—O2i | 1.974 (4) | Te2—O3i | 1.948 (3) |
Cu1—O2 | 1.974 (4) | Te2—O3 | 1.948 (3) |
Cu1—O3ii | 2.387 (4) | Te2—O1 | 2.1992 (17) |
Cu1—O3i | 2.387 (4) | Te2—O1iv | 2.1992 (17) |
Cu1—Cu1i | 2.9317 (2) | Te2—Te2iii | 2.9317 (1) |
Cu1—Cu1iii | 2.9317 (2) | Te2—Te2i | 2.9317 (2) |
O1i—Cu1—O1 | 96.1 (3) | O3i—Te2—O3 | 97.64 (19) |
O1i—Cu1—O2i | 84.0 (2) | O3iv—Te2—O1 | 92.53 (17) |
O1—Cu1—O2i | 179.9 (2) | O3v—Te2—O1 | 92.53 (17) |
O1i—Cu1—O2 | 179.9 (2) | O3i—Te2—O1 | 87.47 (17) |
O1—Cu1—O2 | 84.0 (2) | O3—Te2—O1 | 87.47 (17) |
O2i—Cu1—O2 | 95.9 (3) | O3iv—Te2—O1iv | 87.47 (17) |
O1i—Cu1—O3ii | 81.85 (7) | O3v—Te2—O1iv | 87.47 (17) |
O1—Cu1—O3ii | 81.85 (7) | O3i—Te2—O1iv | 92.53 (17) |
O2i—Cu1—O3ii | 98.16 (7) | O3—Te2—O1iv | 92.53 (17) |
O2—Cu1—O3ii | 98.16 (7) | O1—Te2—O1iv | 180.0 |
O1i—Cu1—O3i | 81.85 (7) | O3iv—Te2—Te2iii | 138.82 (10) |
O1—Cu1—O3i | 81.85 (7) | O3v—Te2—Te2iii | 41.18 (10) |
O2i—Cu1—O3i | 98.16 (7) | O3i—Te2—Te2iii | 138.82 (10) |
O2—Cu1—O3i | 98.16 (7) | O3—Te2—Te2iii | 41.18 (10) |
O3ii—Cu1—O3i | 155.5 (2) | O1—Te2—Te2iii | 90.000 (1) |
O1i—Cu1—Cu1i | 41.97 (17) | O1iv—Te2—Te2iii | 90.000 (1) |
O1—Cu1—Cu1i | 138.03 (17) | O3iv—Te2—Te2i | 41.18 (10) |
O2i—Cu1—Cu1i | 42.05 (13) | O3v—Te2—Te2i | 138.82 (10) |
O2—Cu1—Cu1i | 137.95 (13) | O3i—Te2—Te2i | 41.18 (10) |
O3ii—Cu1—Cu1i | 90.0 | O3—Te2—Te2i | 138.82 (10) |
O3i—Cu1—Cu1i | 90.0 | O1—Te2—Te2i | 90.000 (1) |
O1i—Cu1—Cu1iii | 138.03 (17) | O1iv—Te2—Te2i | 90.000 (1) |
O1—Cu1—Cu1iii | 41.97 (17) | Te2iii—Te2—Te2i | 180.0 |
O2i—Cu1—Cu1iii | 137.95 (13) | Cu1iii—O1—Cu1 | 96.1 (3) |
O2—Cu1—Cu1iii | 42.05 (13) | Cu1iii—O1—Te2vi | 97.99 (11) |
O3ii—Cu1—Cu1iii | 90.0 | Cu1—O1—Te2vi | 97.99 (11) |
O3i—Cu1—Cu1iii | 90.000 (1) | Cu1iii—O1—Te2 | 97.99 (11) |
Cu1i—Cu1—Cu1iii | 180.0 | Cu1—O1—Te2 | 97.99 (11) |
O3iv—Te2—O3v | 97.64 (19) | Te2vi—O1—Te2 | 156.0 (4) |
O3iv—Te2—O3i | 82.36 (19) | Cu1—O2—Cu1iii | 95.9 (3) |
O3v—Te2—O3i | 180.0 | Te2—O3—Te2iii | 97.63 (19) |
O3iv—Te2—O3 | 180.0 | Te2—O3—Cu1iii | 92.69 (13) |
O3v—Te2—O3 | 82.36 (19) | Te2iii—O3—Cu1iii | 92.69 (13) |
Symmetry codes: (i) x+1, y, z; (ii) x+1, y, −z+3/2; (iii) x−1, y, z; (iv) −x−1, −y+1, −z+1; (v) −x−2, −y+1, −z+1; (vi) −x−1, −y+1, z+1/2. |