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 |
Key indicators
- Single-crystal X-ray study
- T = 294 K
- Mean (Cu-S) = 0.001 Å
- R factor = 0.032
- wR factor = 0.038
- Data-to-parameter ratio = 22.1
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT034_ALERT_1_C No Flack Parameter Given. Z .GT. Si, NonCentro . ? PLAT731_ALERT_1_C Bond Calc 2.3111(11), Rep 2.3112(5) ...... 2.20 su-Rat NB -S 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 54.74(3), Rep 54.75(1) ...... 3.33 su-Rat CU -NB -S 1.555 1.555 1.555
Alert level G REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure From the CIF: _diffrn_reflns_theta_max 45.00 From the CIF: _reflns_number_total 177 Count of symmetry unique reflns 177 Completeness (_total/calc) 100.00% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 0 Fraction of Friedel pairs measured 0.000 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion
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) |