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The structure of the title complex, (C6H16N2)[WS4], consists of a tetra­hedral [WS4]2− dianion situated in a general position and two crystallographically independent trans-cyclo­hexane-1,4-diammonium cations located on centres of inversion. The anions are linked to the organic ammonium cations via N—H...S hydrogen bonds, resulting in the formation of alternating layers of cations and anions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806049166/is2106sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806049166/is2106Isup2.hkl
Contains datablock I

CCDC reference: 630028

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.023
  • wR factor = 0.052
  • Data-to-parameter ratio = 32.0

checkCIF/PLATON results

No syntax errors found




Alert level C PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT480_ALERT_4_C Long H...A H-Bond Reported H1N1 .. S4 .. 2.95 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H3A .. S1 .. 2.95 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C6 H16 N2
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 2 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 5 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: DIF4 (Stoe & Cie, 1998); cell refinement: DIF4; data reduction: REDU4 (Stoe & Cie, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: CIFTAB in SHELXTL (Bruker, 1998).

trans-Cyclohexane-1,4-diammonium tetrathiotungstate(VI) top
Crystal data top
(C6H16N2)[WS4]Z = 2
Mr = 428.30F(000) = 408
Triclinic, P1Dx = 2.201 Mg m3
a = 7.0354 (9) ÅMo Kα radiation, λ = 0.71073 Å
b = 9.6783 (14) ÅCell parameters from 72 reflections
c = 10.5523 (19) Åθ = 10–15°
α = 108.672 (14)°µ = 9.55 mm1
β = 92.673 (14)°T = 293 K
γ = 106.228 (12)°Block, yellow
V = 646.22 (17) Å30.11 × 0.09 × 0.07 mm
Data collection top
Stoe AED-II four-circle
diffractometer
3105 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.031
Graphite monochromatorθmax = 30.0°, θmin = 2.1°
ω/θ scansh = 09
Absorption correction: numerical
(X-SHAPE; Stoe & Cie, 1998)
k = 1313
Tmin = 0.365, Tmax = 0.502l = 1414
4059 measured reflections4 standard reflections every 120 min
3776 independent reflections intensity decay: none
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.023Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.052H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.021P)2]
where P = (Fo2 + 2Fc2)/3
3776 reflections(Δ/σ)max = 0.002
118 parametersΔρmax = 0.70 e Å3
0 restraintsΔρmin = 0.74 e Å3
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
W10.24741 (2)1.040881 (17)0.777124 (16)0.02414 (5)
S10.04268 (15)1.14331 (11)0.70563 (11)0.0314 (2)
S20.52822 (15)1.10921 (13)0.69854 (11)0.0366 (2)
S30.11357 (17)0.78972 (11)0.69843 (11)0.0364 (2)
S40.30427 (19)1.12785 (13)0.99794 (11)0.0398 (2)
N10.8361 (5)1.2407 (4)0.9931 (4)0.0325 (7)
H1N10.88591.19991.04610.049*
H2N10.89831.23210.92080.049*
H3N10.70571.19150.96690.049*
C10.8671 (6)1.4086 (4)1.0707 (4)0.0306 (8)
H10.79411.41521.14820.037*
C20.7838 (6)1.4825 (5)0.9837 (4)0.0340 (9)
H2A0.77411.58021.04140.041*
H2B0.64971.41740.94010.041*
C30.9112 (7)1.5091 (5)0.8752 (4)0.0334 (8)
H3A0.89701.41070.80650.040*
H3B0.86031.56910.83230.040*
N20.6909 (6)0.8183 (4)0.5511 (4)0.0366 (8)
H1N20.70170.84630.47860.055*
H2N20.81020.81930.58420.055*
H3N20.64680.88350.61370.055*
C110.5464 (6)0.6600 (4)0.5123 (4)0.0297 (8)
H110.41520.66160.47850.036*
C120.6139 (7)0.5497 (5)0.3998 (4)0.0362 (9)
H12A0.74870.55330.42870.043*
H12B0.61580.58020.32070.043*
C130.4728 (7)0.3864 (4)0.3633 (4)0.0336 (8)
H13A0.34180.38010.32400.040*
H13B0.52360.31610.29650.040*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W10.02307 (7)0.02128 (7)0.02633 (7)0.00591 (5)0.00204 (5)0.00705 (5)
S10.0285 (5)0.0288 (4)0.0392 (5)0.0115 (4)0.0039 (4)0.0128 (4)
S20.0260 (5)0.0428 (6)0.0404 (5)0.0107 (4)0.0059 (4)0.0134 (4)
S30.0404 (6)0.0220 (4)0.0422 (6)0.0063 (4)0.0024 (4)0.0092 (4)
S40.0492 (6)0.0382 (5)0.0270 (5)0.0113 (5)0.0022 (4)0.0072 (4)
N10.0344 (18)0.0256 (15)0.0369 (18)0.0057 (14)0.0017 (14)0.0136 (13)
C10.035 (2)0.0252 (18)0.0303 (19)0.0091 (16)0.0062 (16)0.0079 (15)
C20.0267 (19)0.0263 (18)0.047 (2)0.0088 (15)0.0010 (17)0.0108 (17)
C30.042 (2)0.0273 (18)0.0304 (19)0.0114 (17)0.0045 (17)0.0106 (15)
N20.040 (2)0.0256 (16)0.0390 (19)0.0059 (15)0.0034 (16)0.0095 (14)
C110.0287 (19)0.0247 (17)0.0313 (19)0.0049 (15)0.0013 (15)0.0076 (14)
C120.041 (2)0.031 (2)0.032 (2)0.0032 (18)0.0115 (18)0.0109 (16)
C130.042 (2)0.0262 (18)0.0272 (18)0.0055 (17)0.0065 (16)0.0056 (14)
Geometric parameters (Å, º) top
W1—S42.1834 (12)C3—H3A0.9700
W1—S22.1913 (11)C3—H3B0.9700
W1—S12.1913 (10)N2—C111.496 (5)
W1—S32.2001 (11)N2—H1N20.8900
N1—C11.514 (5)N2—H2N20.8900
N1—H1N10.8900N2—H3N20.8900
N1—H2N10.8900C11—C121.516 (5)
N1—H3N10.8900C11—C13ii1.518 (6)
C1—C21.517 (6)C11—H110.9800
C1—C3i1.525 (6)C12—C131.526 (6)
C1—H10.9800C12—H12A0.9700
C2—C31.528 (6)C12—H12B0.9700
C2—H2A0.9700C13—H13A0.9700
C2—H2B0.9700C13—H13B0.9700
S4—W1—S2109.45 (5)C1i—C3—H3B108.8
S4—W1—S1110.01 (4)C2—C3—H3B108.8
S2—W1—S1107.06 (4)H3A—C3—H3B107.7
S4—W1—S3110.84 (5)C11—N2—H1N2109.5
S2—W1—S3110.55 (5)C11—N2—H2N2109.5
S1—W1—S3108.84 (4)H1N2—N2—H2N2109.5
C1—N1—H1N1109.5C11—N2—H3N2109.5
C1—N1—H2N1109.5H1N2—N2—H3N2109.5
H1N1—N1—H2N1109.5H2N2—N2—H3N2109.5
C1—N1—H3N1109.5N2—C11—C12109.9 (3)
H1N1—N1—H3N1109.5N2—C11—C13ii109.2 (3)
H2N1—N1—H3N1109.5C12—C11—C13ii112.5 (3)
N1—C1—C2111.1 (3)N2—C11—H11108.4
N1—C1—C3i109.6 (3)C12—C11—H11108.4
C2—C1—C3i111.9 (3)C13ii—C11—H11108.4
N1—C1—H1108.0C11—C12—C13110.4 (3)
C2—C1—H1108.0C11—C12—H12A109.6
C3i—C1—H1108.0C13—C12—H12A109.6
C1—C2—C3113.3 (3)C11—C12—H12B109.6
C1—C2—H2A108.9C13—C12—H12B109.6
C3—C2—H2A108.9H12A—C12—H12B108.1
C1—C2—H2B108.9C11ii—C13—C12110.8 (3)
C3—C2—H2B108.9C11ii—C13—H13A109.5
H2A—C2—H2B107.7C12—C13—H13A109.5
C1i—C3—C2113.9 (3)C11ii—C13—H13B109.5
C1i—C3—H3A108.8C12—C13—H13B109.5
C2—C3—H3A108.8H13A—C13—H13B108.1
Symmetry codes: (i) x+2, y+3, z+2; (ii) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1N1···S3iii0.892.673.372 (4)137
N1—H1N1···S4iii0.892.953.459 (3)118
N1—H2N1···S1iv0.892.533.399 (4)167
N1—H3N1···S40.892.783.600 (4)155
N1—H3N1···S20.892.813.357 (4)121
N2—H1N2···S2v0.892.633.349 (4)139
N2—H1N2···S1v0.892.723.424 (4)137
N2—H2N2···S3iv0.892.533.412 (4)170
N2—H3N2···S20.892.473.289 (4)153
C3—H3A···S1iv0.972.953.810 (4)148
Symmetry codes: (iii) x+1, y+2, z+2; (iv) x+1, y, z; (v) x+1, y+2, z+1.
 

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