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The title complex, (C6H16N2)[WS4], consists of tetrahedral [WS4]2- dianions and organic dications. There are two crystallographically independent 1,4-di­methyl­piperazinium (1,4-dmpH2) dications in the asymmetric unit, both of which are located around a centre of inversion, while the anions are located in general positions. The anions and cations are connected by hydrogen bonding.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803016040/bt6303sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803016040/bt6303Isup2.hkl
Contains datablock I

CCDC reference: 221661

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.025
  • wR factor = 0.067
  • Data-to-parameter ratio = 24.8

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Computing details top

Data collection: IPDS (Stoe & Cie, 1998); cell refinement: IPDS; data reduction: IPDS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 1998); software used to prepare material for publication: CIFTAB in SHELXL97.

1,4-dimethylpiperazinium tetrathiotungstate(VI) top
Crystal data top
(C6H16N2)[WS4]Dx = 2.253 Mg m3
Mr = 428.30Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PbcaCell parameters from 8000 reflections
a = 13.3792 (11) Åθ = 15–23°
b = 12.6369 (7) ŵ = 9.77 mm1
c = 14.9381 (9) ÅT = 293 K
V = 2525.6 (3) Å3Block, yellow
Z = 80.14 × 0.09 × 0.06 mm
F(000) = 1632
Data collection top
Stoe IPDS
diffractometer
2946 independent reflections
Radiation source: fine-focus sealed tube2398 reflections with I > 2s(I)
Graphite monochromatorRint = 0.041
φ scansθmax = 28.0°, θmin = 2.6°
Absorption correction: numerical
(X-SHAPE and X-RED; Stoe & Cie, 1998)
h = 1717
Tmin = 0.360, Tmax = 0.555k = 1515
23034 measured reflectionsl = 1819
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.025H-atom parameters constrained
wR(F2) = 0.067 w = 1/[σ2(Fo2) + (0.0453P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max = 0.004
2946 reflectionsΔρmax = 1.66 e Å3
119 parametersΔρmin = 1.39 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00187 (9)
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
W10.248391 (6)0.345321 (12)0.628045 (7)0.01946 (8)
S10.10187 (5)0.28939 (7)0.67238 (5)0.03026 (18)
S20.27210 (6)0.29591 (8)0.48747 (5)0.03188 (19)
S30.36779 (6)0.28653 (8)0.71377 (6)0.0422 (2)
S40.24917 (5)0.51921 (10)0.63317 (6)0.0315 (2)
N10.40873 (17)0.5130 (2)0.44850 (16)0.0259 (5)
H10.36550.48010.48640.031*
C10.4875 (2)0.4348 (3)0.4221 (2)0.0301 (7)
H1A0.53320.46760.38010.036*
H1B0.45630.37500.39240.036*
C20.5454 (2)0.3958 (3)0.5027 (2)0.0298 (7)
H2A0.50100.35770.54260.036*
H2B0.59750.34760.48340.036*
C30.3513 (3)0.5492 (4)0.3687 (2)0.0462 (10)
H3A0.32260.48910.33890.069*
H3B0.39530.58570.32830.069*
H3C0.29900.59630.38740.069*
N110.49326 (17)0.5178 (2)0.09605 (16)0.0242 (5)
H110.54950.48290.11350.029*
C110.5237 (2)0.6048 (3)0.0332 (2)0.0271 (7)
H11A0.46520.64500.01560.032*
H11B0.56950.65240.06340.032*
C120.5736 (2)0.5597 (3)0.0492 (2)0.0274 (6)
H12A0.63520.52470.03200.033*
H12B0.59040.61680.08990.033*
C130.4438 (3)0.5618 (3)0.1780 (2)0.0386 (8)
H13A0.42530.50480.21720.058*
H13B0.48930.60820.20840.058*
H13C0.38510.60050.16090.058*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W10.01603 (10)0.02096 (13)0.02140 (11)0.00036 (3)0.00050 (3)0.00104 (4)
S10.0255 (3)0.0339 (5)0.0315 (4)0.0083 (3)0.0074 (3)0.0023 (3)
S20.0328 (3)0.0385 (5)0.0243 (4)0.0032 (3)0.0054 (3)0.0064 (3)
S30.0378 (4)0.0442 (6)0.0446 (5)0.0144 (4)0.0204 (4)0.0072 (4)
S40.0327 (5)0.0186 (6)0.0431 (5)0.0018 (3)0.0004 (3)0.0012 (3)
N10.0238 (11)0.0298 (16)0.0241 (12)0.0004 (10)0.0030 (9)0.0050 (10)
C10.0262 (14)0.037 (2)0.0277 (16)0.0034 (13)0.0030 (12)0.0074 (13)
C20.0298 (15)0.023 (2)0.0365 (18)0.0048 (11)0.0044 (13)0.0008 (12)
C30.042 (2)0.061 (3)0.035 (2)0.0072 (17)0.0080 (14)0.0092 (16)
N110.0244 (11)0.0261 (15)0.0221 (12)0.0003 (10)0.0027 (9)0.0019 (10)
C110.0323 (16)0.0216 (19)0.0273 (16)0.0058 (11)0.0018 (12)0.0013 (11)
C120.0270 (14)0.0278 (19)0.0274 (16)0.0078 (12)0.0001 (11)0.0009 (13)
C130.0475 (19)0.045 (2)0.0234 (16)0.0015 (16)0.0049 (14)0.0062 (15)
Geometric parameters (Å, º) top
W1—S32.1781 (8)C3—H3B0.96
W1—S12.1866 (7)C3—H3C0.96
W1—S42.1988 (12)N11—C131.499 (4)
W1—S22.2136 (8)N11—C12ii1.500 (4)
N1—C31.491 (4)N11—C111.502 (4)
N1—C2i1.495 (4)N11—H110.91
N1—C11.497 (4)C11—C121.512 (5)
N1—H10.91C11—H11A0.97
C1—C21.514 (5)C11—H11B0.97
C1—H1A0.97C12—N11ii1.500 (4)
C1—H1B0.97C12—H12A0.97
C2—N1i1.495 (4)C12—H12B0.97
C2—H2A0.97C13—H13A0.96
C2—H2B0.97C13—H13B0.96
C3—H3A0.96C13—H13C0.96
S3—W1—S1111.67 (4)N1—C3—H3C109.5
S3—W1—S4108.48 (3)H3A—C3—H3C109.5
S1—W1—S4108.46 (3)H3B—C3—H3C109.5
S3—W1—S2110.88 (4)C13—N11—C12ii111.1 (2)
S1—W1—S2108.94 (3)C13—N11—C11111.1 (3)
S4—W1—S2108.32 (3)C12ii—N11—C11110.4 (2)
C3—N1—C2i111.4 (3)C13—N11—H11108.1
C3—N1—C1110.8 (3)C12ii—N11—H11108.1
C2i—N1—C1110.4 (2)C11—N11—H11108.1
C3—N1—H1108.1N11—C11—C12110.7 (3)
C2i—N1—H1108.1N11—C11—H11A109.5
C1—N1—H1108.1C12—C11—H11A109.5
N1—C1—C2111.5 (2)N11—C11—H11B109.5
N1—C1—H1A109.3C12—C11—H11B109.5
C2—C1—H1A109.3H11A—C11—H11B108.1
N1—C1—H1B109.3N11ii—C12—C11111.3 (2)
C2—C1—H1B109.3N11ii—C12—H12A109.4
H1A—C1—H1B108.0C11—C12—H12A109.4
N1i—C2—C1110.3 (3)N11ii—C12—H12B109.4
N1i—C2—H2A109.6C11—C12—H12B109.4
C1—C2—H2A109.6H12A—C12—H12B108.0
N1i—C2—H2B109.6N11—C13—H13A109.5
C1—C2—H2B109.6N11—C13—H13B109.5
H2A—C2—H2B108.1H13A—C13—H13B109.5
N1—C3—H3A109.5N11—C13—H13C109.5
N1—C3—H3B109.5H13A—C13—H13C109.5
H3A—C3—H3B109.5H13B—C13—H13C109.5
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···S20.912.643.347 (3)135
N1—H1···S40.912.733.489 (2)141
N11—H11···S1iii0.912.693.427 (3)139
N11—H11···S4iii0.912.733.468 (2)139
Symmetry code: (iii) x+1/2, y, z+1/2.
 

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