inorganic compounds
Tricopper tetrathioniobate(V), Cu3NbS4, has been synthesized by chemical transport reaction using iodine as the transport agent. The compound crystallizes in the sulvanite (Cu3VS4) structure type in space group P3m. The structure is composed of CuS4 and NbS4 tetrahedra sharing corners and edges.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805022397/wm6081sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805022397/wm6081Isup2.hkl |
Computing details top
Data collection: CAD-4 Operations Manual (Enraf-Nonius, 1977); cell refinement: CAD-4 Operations Manual; data reduction: BEGIN in SDP-Plus (Frenz, 1985); program(s) used to solve structure: SDP-Plus; program(s) used to refine structure: LSFM in SDP-Plus; molecular graphics: ATOMS (Dowty, 1994); software used to prepare material for publication: MICROVAX 3100 in SDP-Plus.
Tricopper tetrathioniobate(V) top
Crystal data top
Cu3NbS4 | Dx = 4.111 Mg m−3 |
Mr = 411.78 | Mo Kα radiation, λ = 0.71073 Å |
Cubic, P43m | Cell parameters from 25 reflections |
Hall symbol: P -4 2 3 | θ = 9–15° |
a = 5.5001 (6) Å | µ = 12.20 mm−1 |
V = 166.38 (3) Å3 | T = 294 K |
Z = 1 | Prism, yellow |
F(000) = 192 | 0.12 × 0.10 × 0.08 mm |
Data collection top
Enraf-Nonius CAD-4 diffractometer | 156 reflections with I > 3σ(I) |
Radiation source: X-ray tube | Rint = 0.043 |
Graphite monochromator | θmax = 45°, θmin = 1.0° |
θ/2θ scans | h = 0→10 |
Absorption correction: empirical (using intensity measurements) (Walker & Stuart, 1983) | k = 0→10 |
Tmin = 0.245, Tmax = 0.376 | l = 0→10 |
828 measured reflections | 3 standard reflections every 60 min |
177 independent reflections | intensity decay: none |
Refinement top
Refinement on F | Weighting scheme based on measured s.u.'s |
Least-squares matrix: full | (Δ/σ)max < 0.001 |
R[F2 > 2σ(F2)] = 0.032 | Δρmax = 1.21 e Å−3 |
wR(F2) = 0.038 | Δρmin = −1.02 e Å−3 |
S = 1.17 | Extinction correction: isotropic (Zachariasen, 1963) |
177 reflections | Extinction coefficient: 4.8353E-06 |
8 parameters |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Cu | 0.5000 | 0.0000 | 0.0000 | 0.0170 (3) | |
Nb | 0.0000 | 0.0000 | 0.0000 | 0.0058 (4) | |
S | 0.2426 (2) | 0.2426 (2) | 0.2426 (2) | 0.0111 (5) |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu | 0.0087 (3) | 0.0212 (2) | 0.0212 (2) | 0.0000 | 0.0000 | 0.0000 |
Nb | 0.0058 (1) | 0.0058 (1) | 0.0058 (1) | 0.0000 | 0.0000 | 0.0000 |
S | 0.0111 (2) | 0.0111 (2) | 0.0111 (2) | −0.0014 (2) | −0.0014 (2) | −0.0014 (2) |
Geometric parameters (Å, º) top
Nb—Cu | 2.7501 (3) | Nb—S | 2.3112 (5) |
Cu—S | 2.3589 (6) | ||
Cu—Nb—Cu | 180 (1) | Nb—Cu—S | 53.13 (2) |
Cu—Nb—Cu | 90 (1) | S—Cu—S | 106.26 (4) |
Cu—Nb—S | 54.74 (2) | S—Cu—S | 111.10 (2) |
Cu—Nb—S | 54.746 (9) | Nb—S—Cu | 72.13 (2) |
S—Nb—S | 109.47 (4) | Cu—S—Cu | 111.028 (1) |
S—Nb—S | 109.47 (2) | Cu—S—Cu | 111.03 (4) |
Nb—Cu—Nb | 180 (1) |