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
CCDC reference: 200721
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (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.
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.
Crystal data top
(C2H10N2)[WS4] | Dx = 2.609 Mg m−3 |
Mr = 374.21 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P212121 | Cell parameters from 8000 reflections |
a = 8.6401 (4) Å | θ = 8–25° |
b = 9.3228 (5) Å | µ = 12.93 mm−1 |
c = 11.8281 (7) Å | T = 293 K |
V = 952.75 (9) Å3 | Plate, yellow |
Z = 4 | 0.13 × 0.1 × 0.05 mm |
F(000) = 696 | |
Data collection top
Stoe IPDS diffractometer | 2308 independent reflections |
Radiation source: fine-focus sealed tube | 2207 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.040 |
φ scans | θmax = 28.1°, θmin = 2.8° |
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1998) | h = −11→11 |
Tmin = 0.237, Tmax = 0.527 | k = −12→12 |
8270 measured reflections | l = −15→15 |
Refinement top
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H-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 = 1.04 | Δρmax = 1.44 e Å−3 |
2308 reflections | Δρmin = −2.17 e Å−3 |
83 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0101 (4) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack (1983) |
Secondary atom site location: difference Fourier map | Absolute 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 | x | y | z | Uiso*/Ueq | |
W1 | 0.22871 (2) | 0.95126 (2) | 0.395585 (17) | 0.01863 (8) | |
S1 | 0.00572 (16) | 1.06275 (18) | 0.40603 (13) | 0.0289 (3) | |
S2 | 0.24861 (18) | 0.84547 (16) | 0.23137 (11) | 0.0281 (3) | |
S3 | 0.24657 (18) | 0.79105 (15) | 0.53087 (12) | 0.0281 (3) | |
S4 | 0.41419 (18) | 1.10907 (17) | 0.41289 (14) | 0.0282 (3) | |
N1 | 0.9322 (5) | 0.9442 (7) | 0.6633 (4) | 0.0303 (11) | |
H1N1 | 1.0065 | 0.9271 | 0.7137 | 0.045* | |
H2N1 | 0.9737 | 0.9816 | 0.6011 | 0.045* | |
H3N1 | 0.8845 | 0.8625 | 0.6462 | 0.045* | |
C1 | 0.8188 (7) | 1.0466 (8) | 0.7118 (5) | 0.0317 (12) | |
H1A | 0.8708 | 1.1366 | 0.7278 | 0.038* | |
H1B | 0.7803 | 1.0086 | 0.7827 | 0.038* | |
C2 | 0.6847 (8) | 1.0747 (7) | 0.6344 (6) | 0.0354 (15) | |
H2A | 0.6337 | 1.1625 | 0.6579 | 0.042* | |
H2B | 0.7234 | 1.0892 | 0.5583 | 0.042* | |
N2 | 0.5706 (5) | 0.9580 (7) | 0.6330 (4) | 0.0283 (10) | |
H1N3 | 0.4932 | 0.9810 | 0.5868 | 0.042* | |
H2N3 | 0.5339 | 0.9445 | 0.7025 | 0.042* | |
H3N3 | 0.6156 | 0.8778 | 0.6089 | 0.042* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
W1 | 0.01951 (11) | 0.01741 (10) | 0.01899 (10) | 0.00011 (7) | −0.00033 (7) | 0.00052 (9) |
S1 | 0.0240 (6) | 0.0345 (8) | 0.0283 (7) | 0.0082 (5) | 0.0018 (5) | 0.0037 (8) |
S2 | 0.0350 (8) | 0.0283 (6) | 0.0212 (5) | 0.0010 (6) | −0.0001 (5) | −0.0051 (5) |
S3 | 0.0363 (8) | 0.0237 (6) | 0.0242 (6) | −0.0006 (6) | −0.0038 (6) | 0.0076 (5) |
S4 | 0.0283 (7) | 0.0278 (7) | 0.0285 (8) | −0.0083 (5) | −0.0024 (5) | 0.0009 (6) |
N1 | 0.023 (2) | 0.038 (3) | 0.030 (3) | −0.001 (2) | −0.0017 (17) | 0.002 (3) |
C1 | 0.030 (3) | 0.028 (3) | 0.037 (3) | −0.005 (3) | −0.006 (2) | −0.006 (3) |
C2 | 0.032 (3) | 0.027 (3) | 0.047 (4) | 0.003 (2) | −0.007 (3) | 0.009 (3) |
N2 | 0.022 (2) | 0.034 (3) | 0.029 (3) | 0.002 (2) | −0.0026 (16) | 0.002 (3) |
Geometric parameters (Å, º) top
W1—S4 | 2.1851 (14) | C1—H1A | 0.9700 |
W1—S2 | 2.1852 (13) | C1—H1B | 0.9700 |
W1—S1 | 2.1927 (14) | C2—N2 | 1.468 (8) |
W1—S3 | 2.1943 (13) | C2—H2A | 0.9700 |
N1—C1 | 1.483 (8) | C2—H2B | 0.9700 |
N1—H1N1 | 0.8900 | N2—H1N3 | 0.8900 |
N1—H2N1 | 0.8900 | N2—H2N3 | 0.8900 |
N1—H3N1 | 0.8900 | N2—H3N3 | 0.8900 |
C1—C2 | 1.500 (9) | | |
| | | |
S4—W1—S2 | 109.23 (6) | N1—C1—H1B | 109.0 |
S4—W1—S1 | 108.66 (7) | C2—C1—H1B | 109.0 |
S2—W1—S1 | 109.46 (6) | H1A—C1—H1B | 107.8 |
S4—W1—S3 | 109.78 (6) | N2—C2—C1 | 113.3 (5) |
S2—W1—S3 | 109.60 (6) | N2—C2—H2A | 108.9 |
S1—W1—S3 | 110.08 (6) | C1—C2—H2A | 108.9 |
C1—N1—H1N1 | 109.5 | N2—C2—H2B | 108.9 |
C1—N1—H2N1 | 109.5 | C1—C2—H2B | 108.9 |
H1N1—N1—H2N1 | 109.5 | H2A—C2—H2B | 107.7 |
C1—N1—H3N1 | 109.5 | C2—N2—H1N3 | 109.5 |
H1N1—N1—H3N1 | 109.5 | C2—N2—H2N3 | 109.5 |
H2N1—N1—H3N1 | 109.5 | H1N3—N2—H2N3 | 109.5 |
N1—C1—C2 | 112.8 (5) | C2—N2—H3N3 | 109.5 |
N1—C1—H1A | 109.0 | H1N3—N2—H3N3 | 109.5 |
C2—C1—H1A | 109.0 | H2N3—N2—H3N3 | 109.5 |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1N1···S4i | 0.89 | 2.48 | 3.274 (5) | 149 |
N1—H1N1···S2i | 0.89 | 3.00 | 3.478 (6) | 115 |
N1—H2N1···S1ii | 0.89 | 2.44 | 3.300 (6) | 161 |
N1—H3N1···S2iii | 0.89 | 2.69 | 3.370 (6) | 134 |
N1—H3N1···S3iii | 0.89 | 2.80 | 3.558 (6) | 144 |
N2—H1N3···S4 | 0.89 | 2.47 | 3.254 (5) | 147 |
N2—H1N3···S3 | 0.89 | 2.85 | 3.424 (6) | 124 |
N2—H2N3···S1iv | 0.89 | 2.43 | 3.301 (5) | 166 |
N2—H3N3···S3iii | 0.89 | 2.55 | 3.385 (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. |