Download citation
Download citation
link to html
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 P\overline 43m. The structure is composed of CuS4 and NbS4 tetrahedra sharing corners and edges.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805022397/wm6081sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805022397/wm6081Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 294 K
  • Mean [sigma](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
Cu3NbS4Dx = 4.111 Mg m3
Mr = 411.78Mo Kα radiation, λ = 0.71073 Å
Cubic, P43mCell parameters from 25 reflections
Hall symbol: P -4 2 3θ = 9–15°
a = 5.5001 (6) ŵ = 12.20 mm1
V = 166.38 (3) Å3T = 294 K
Z = 1Prism, yellow
F(000) = 1920.12 × 0.10 × 0.08 mm
Data collection top
Enraf-Nonius CAD-4
diffractometer
156 reflections with I > 3σ(I)
Radiation source: X-ray tubeRint = 0.043
Graphite monochromatorθmax = 45°, θmin = 1.0°
θ/2θ scansh = 010
Absorption correction: empirical (using intensity measurements)
(Walker & Stuart, 1983)
k = 010
Tmin = 0.245, Tmax = 0.376l = 010
828 measured reflections3 standard reflections every 60 min
177 independent reflections intensity decay: none
Refinement top
Refinement on FWeighting scheme based on measured s.u.'s
Least-squares matrix: full(Δ/σ)max < 0.001
R[F2 > 2σ(F2)] = 0.032Δρmax = 1.21 e Å3
wR(F2) = 0.038Δρmin = 1.02 e Å3
S = 1.17Extinction correction: isotropic (Zachariasen, 1963)
177 reflectionsExtinction coefficient: 4.8353E-06
8 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu0.50000.00000.00000.0170 (3)
Nb0.00000.00000.00000.0058 (4)
S0.2426 (2)0.2426 (2)0.2426 (2)0.0111 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu0.0087 (3)0.0212 (2)0.0212 (2)0.00000.00000.0000
Nb0.0058 (1)0.0058 (1)0.0058 (1)0.00000.00000.0000
S0.0111 (2)0.0111 (2)0.0111 (2)0.0014 (2)0.0014 (2)0.0014 (2)
Geometric parameters (Å, º) top
Nb—Cu2.7501 (3)Nb—S2.3112 (5)
Cu—S2.3589 (6)
Cu—Nb—Cu180 (1)Nb—Cu—S53.13 (2)
Cu—Nb—Cu90 (1)S—Cu—S106.26 (4)
Cu—Nb—S54.74 (2)S—Cu—S111.10 (2)
Cu—Nb—S54.746 (9)Nb—S—Cu72.13 (2)
S—Nb—S109.47 (4)Cu—S—Cu111.028 (1)
S—Nb—S109.47 (2)Cu—S—Cu111.03 (4)
Nb—Cu—Nb180 (1)
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds