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The structure of the title complex, (C2H10N2)[WS4], consists of tetrahedral [WS4]2- anions which are connected to the organic ethyl­enedi­ammonium dications via hydrogen bonding. All atoms are located in general positions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802017841/bt6196sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802017841/bt6196Isup2.hkl
Contains datablock I

CCDC reference: 200721

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.009 Å
  • R factor = 0.023
  • wR factor = 0.054
  • Data-to-parameter ratio = 27.8

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

General Notes

REFLT_03 From the CIF: _diffrn_reflns_theta_max 28.07 From the CIF: _reflns_number_total 2308 Count of symmetry unique reflns 1350 Completeness (_total/calc) 170.96% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 958 Fraction of Friedel pairs measured 0.710 Are heavy atom types Z>Si present yes Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF.

Computing details top

Data collection: IPDS Program Package (Stoe, 1998); cell refinement: IPDS Program Package; data reduction: IPDS Program Package; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); 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.

(I) top
Crystal data top
(C2H10N2)[WS4]Dx = 2.609 Mg m3
Mr = 374.21Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121Cell parameters from 8000 reflections
a = 8.6401 (4) Åθ = 8–25°
b = 9.3228 (5) ŵ = 12.93 mm1
c = 11.8281 (7) ÅT = 293 K
V = 952.75 (9) Å3Plate, yellow
Z = 40.13 × 0.1 × 0.05 mm
F(000) = 696
Data collection top
Stoe IPDS
diffractometer
2308 independent reflections
Radiation source: fine-focus sealed tube2207 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.040
φ scansθmax = 28.1°, θmin = 2.8°
Absorption correction: numerical
(X-SHAPE; Stoe & Cie, 1998)
h = 1111
Tmin = 0.237, Tmax = 0.527k = 1212
8270 measured reflectionsl = 1515
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.023 w = 1/[σ2(Fo2) + (0.036P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.054(Δ/σ)max = 0.001
S = 1.04Δρmax = 1.44 e Å3
2308 reflectionsΔρmin = 2.17 e Å3
83 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0101 (4)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack (1983)
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0.011 (11)
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
W10.22871 (2)0.95126 (2)0.395585 (17)0.01863 (8)
S10.00572 (16)1.06275 (18)0.40603 (13)0.0289 (3)
S20.24861 (18)0.84547 (16)0.23137 (11)0.0281 (3)
S30.24657 (18)0.79105 (15)0.53087 (12)0.0281 (3)
S40.41419 (18)1.10907 (17)0.41289 (14)0.0282 (3)
N10.9322 (5)0.9442 (7)0.6633 (4)0.0303 (11)
H1N11.00650.92710.71370.045*
H2N10.97370.98160.60110.045*
H3N10.88450.86250.64620.045*
C10.8188 (7)1.0466 (8)0.7118 (5)0.0317 (12)
H1A0.87081.13660.72780.038*
H1B0.78031.00860.78270.038*
C20.6847 (8)1.0747 (7)0.6344 (6)0.0354 (15)
H2A0.63371.16250.65790.042*
H2B0.72341.08920.55830.042*
N20.5706 (5)0.9580 (7)0.6330 (4)0.0283 (10)
H1N30.49320.98100.58680.042*
H2N30.53390.94450.70250.042*
H3N30.61560.87780.60890.042*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W10.01951 (11)0.01741 (10)0.01899 (10)0.00011 (7)0.00033 (7)0.00052 (9)
S10.0240 (6)0.0345 (8)0.0283 (7)0.0082 (5)0.0018 (5)0.0037 (8)
S20.0350 (8)0.0283 (6)0.0212 (5)0.0010 (6)0.0001 (5)0.0051 (5)
S30.0363 (8)0.0237 (6)0.0242 (6)0.0006 (6)0.0038 (6)0.0076 (5)
S40.0283 (7)0.0278 (7)0.0285 (8)0.0083 (5)0.0024 (5)0.0009 (6)
N10.023 (2)0.038 (3)0.030 (3)0.001 (2)0.0017 (17)0.002 (3)
C10.030 (3)0.028 (3)0.037 (3)0.005 (3)0.006 (2)0.006 (3)
C20.032 (3)0.027 (3)0.047 (4)0.003 (2)0.007 (3)0.009 (3)
N20.022 (2)0.034 (3)0.029 (3)0.002 (2)0.0026 (16)0.002 (3)
Geometric parameters (Å, º) top
W1—S42.1851 (14)C1—H1A0.9700
W1—S22.1852 (13)C1—H1B0.9700
W1—S12.1927 (14)C2—N21.468 (8)
W1—S32.1943 (13)C2—H2A0.9700
N1—C11.483 (8)C2—H2B0.9700
N1—H1N10.8900N2—H1N30.8900
N1—H2N10.8900N2—H2N30.8900
N1—H3N10.8900N2—H3N30.8900
C1—C21.500 (9)
S4—W1—S2109.23 (6)N1—C1—H1B109.0
S4—W1—S1108.66 (7)C2—C1—H1B109.0
S2—W1—S1109.46 (6)H1A—C1—H1B107.8
S4—W1—S3109.78 (6)N2—C2—C1113.3 (5)
S2—W1—S3109.60 (6)N2—C2—H2A108.9
S1—W1—S3110.08 (6)C1—C2—H2A108.9
C1—N1—H1N1109.5N2—C2—H2B108.9
C1—N1—H2N1109.5C1—C2—H2B108.9
H1N1—N1—H2N1109.5H2A—C2—H2B107.7
C1—N1—H3N1109.5C2—N2—H1N3109.5
H1N1—N1—H3N1109.5C2—N2—H2N3109.5
H2N1—N1—H3N1109.5H1N3—N2—H2N3109.5
N1—C1—C2112.8 (5)C2—N2—H3N3109.5
N1—C1—H1A109.0H1N3—N2—H3N3109.5
C2—C1—H1A109.0H2N3—N2—H3N3109.5
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1N1···S4i0.892.483.274 (5)149
N1—H1N1···S2i0.893.003.478 (6)115
N1—H2N1···S1ii0.892.443.300 (6)161
N1—H3N1···S2iii0.892.693.370 (6)134
N1—H3N1···S3iii0.892.803.558 (6)144
N2—H1N3···S40.892.473.254 (5)147
N2—H1N3···S30.892.853.424 (6)124
N2—H2N3···S1iv0.892.433.301 (5)166
N2—H3N3···S3iii0.892.553.385 (6)157
Symmetry codes: (i) x+3/2, y+2, z+1/2; (ii) x+1, y, z; (iii) x+1/2, y+3/2, z+1; (iv) x+1/2, y+2, z+1/2.
 

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