trans-Cyclo­hexane-1,4-diammonium tetra­thio­tungstate(VI)

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.

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

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Computing details

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)

Crystal data

(C6H16N2)[WS4]	Z = 2
Mr = 428.30	F(000) = 408
Triclinic, P1	Dx = 2.201 Mg m^−3
a = 7.0354 (9) Å	Mo Kα radiation, λ = 0.71073 Å
b = 9.6783 (14) Å	Cell parameters from 72 reflections
c = 10.5523 (19) Å	θ = 10–15°
α = 108.672 (14)°	µ = 9.55 mm^−1
β = 92.673 (14)°	T = 293 K
γ = 106.228 (12)°	Block, yellow
V = 646.22 (17) Å^3	0.11 × 0.09 × 0.07 mm

Data collection

Stoe AED-II four-circle diffractometer	3105 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.031
Graphite monochromator	θmax = 30.0°, θmin = 2.1°
ω/θ scans	h = 0→9
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1998)	k = −13→13
Tmin = 0.365, Tmax = 0.502	l = −14→14
4059 measured reflections	4 standard reflections every 120 min
3776 independent reflections	intensity decay: none

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.023	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.052	H-atom parameters constrained
S = 1.00	w = 1/[σ^2(Fo^2) + (0.021P)^2] where P = (Fo^2 + 2Fc^2)/3
3776 reflections	(Δ/σ)max = 0.002
118 parameters	Δρmax = 0.70 e Å^−3
0 restraints	Δρmin = −0.74 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
W1	0.24741 (2)	1.040881 (17)	0.777124 (16)	0.02414 (5)
S1	0.04268 (15)	1.14331 (11)	0.70563 (11)	0.0314 (2)
S2	0.52822 (15)	1.10921 (13)	0.69854 (11)	0.0366 (2)
S3	0.11357 (17)	0.78972 (11)	0.69843 (11)	0.0364 (2)
S4	0.30427 (19)	1.12785 (13)	0.99794 (11)	0.0398 (2)
N1	0.8361 (5)	1.2407 (4)	0.9931 (4)	0.0325 (7)
H1N1	0.8859	1.1999	1.0461	0.049*
H2N1	0.8983	1.2321	0.9208	0.049*
H3N1	0.7057	1.1915	0.9669	0.049*
C1	0.8671 (6)	1.4086 (4)	1.0707 (4)	0.0306 (8)
H1	0.7941	1.4152	1.1482	0.037*
C2	0.7838 (6)	1.4825 (5)	0.9837 (4)	0.0340 (9)
H2A	0.7741	1.5802	1.0414	0.041*
H2B	0.6497	1.4174	0.9401	0.041*
C3	0.9112 (7)	1.5091 (5)	0.8752 (4)	0.0334 (8)
H3A	0.8970	1.4107	0.8065	0.040*
H3B	0.8603	1.5691	0.8323	0.040*
N2	0.6909 (6)	0.8183 (4)	0.5511 (4)	0.0366 (8)
H1N2	0.7017	0.8463	0.4786	0.055*
H2N2	0.8102	0.8193	0.5842	0.055*
H3N2	0.6468	0.8835	0.6137	0.055*
C11	0.5464 (6)	0.6600 (4)	0.5123 (4)	0.0297 (8)
H11	0.4152	0.6616	0.4785	0.036*
C12	0.6139 (7)	0.5497 (5)	0.3998 (4)	0.0362 (9)
H12A	0.7487	0.5533	0.4287	0.043*
H12B	0.6158	0.5802	0.3207	0.043*
C13	0.4728 (7)	0.3864 (4)	0.3633 (4)	0.0336 (8)
H13A	0.3418	0.3801	0.3240	0.040*
H13B	0.5236	0.3161	0.2965	0.040*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
W1	0.02307 (7)	0.02128 (7)	0.02633 (7)	0.00591 (5)	0.00204 (5)	0.00705 (5)
S1	0.0285 (5)	0.0288 (4)	0.0392 (5)	0.0115 (4)	0.0039 (4)	0.0128 (4)
S2	0.0260 (5)	0.0428 (6)	0.0404 (5)	0.0107 (4)	0.0059 (4)	0.0134 (4)
S3	0.0404 (6)	0.0220 (4)	0.0422 (6)	0.0063 (4)	−0.0024 (4)	0.0092 (4)
S4	0.0492 (6)	0.0382 (5)	0.0270 (5)	0.0113 (5)	0.0022 (4)	0.0072 (4)
N1	0.0344 (18)	0.0256 (15)	0.0369 (18)	0.0057 (14)	0.0017 (14)	0.0136 (13)
C1	0.035 (2)	0.0252 (18)	0.0303 (19)	0.0091 (16)	0.0062 (16)	0.0079 (15)
C2	0.0267 (19)	0.0263 (18)	0.047 (2)	0.0088 (15)	−0.0010 (17)	0.0108 (17)
C3	0.042 (2)	0.0273 (18)	0.0304 (19)	0.0114 (17)	−0.0045 (17)	0.0106 (15)
N2	0.040 (2)	0.0256 (16)	0.0390 (19)	0.0059 (15)	−0.0034 (16)	0.0095 (14)
C11	0.0287 (19)	0.0247 (17)	0.0313 (19)	0.0049 (15)	−0.0013 (15)	0.0076 (14)
C12	0.041 (2)	0.031 (2)	0.032 (2)	0.0032 (18)	0.0115 (18)	0.0109 (16)
C13	0.042 (2)	0.0262 (18)	0.0272 (18)	0.0055 (17)	0.0065 (16)	0.0056 (14)

Geometric parameters (Å, º)

W1—S4	2.1834 (12)	C3—H3A	0.9700
W1—S2	2.1913 (11)	C3—H3B	0.9700
W1—S1	2.1913 (10)	N2—C11	1.496 (5)
W1—S3	2.2001 (11)	N2—H1N2	0.8900
N1—C1	1.514 (5)	N2—H2N2	0.8900
N1—H1N1	0.8900	N2—H3N2	0.8900
N1—H2N1	0.8900	C11—C12	1.516 (5)
N1—H3N1	0.8900	C11—C13^ii	1.518 (6)
C1—C2	1.517 (6)	C11—H11	0.9800
C1—C3^i	1.525 (6)	C12—C13	1.526 (6)
C1—H1	0.9800	C12—H12A	0.9700
C2—C3	1.528 (6)	C12—H12B	0.9700
C2—H2A	0.9700	C13—H13A	0.9700
C2—H2B	0.9700	C13—H13B	0.9700
S4—W1—S2	109.45 (5)	C1^i—C3—H3B	108.8
S4—W1—S1	110.01 (4)	C2—C3—H3B	108.8
S2—W1—S1	107.06 (4)	H3A—C3—H3B	107.7
S4—W1—S3	110.84 (5)	C11—N2—H1N2	109.5
S2—W1—S3	110.55 (5)	C11—N2—H2N2	109.5
S1—W1—S3	108.84 (4)	H1N2—N2—H2N2	109.5
C1—N1—H1N1	109.5	C11—N2—H3N2	109.5
C1—N1—H2N1	109.5	H1N2—N2—H3N2	109.5
H1N1—N1—H2N1	109.5	H2N2—N2—H3N2	109.5
C1—N1—H3N1	109.5	N2—C11—C12	109.9 (3)
H1N1—N1—H3N1	109.5	N2—C11—C13^ii	109.2 (3)
H2N1—N1—H3N1	109.5	C12—C11—C13^ii	112.5 (3)
N1—C1—C2	111.1 (3)	N2—C11—H11	108.4
N1—C1—C3^i	109.6 (3)	C12—C11—H11	108.4
C2—C1—C3^i	111.9 (3)	C13^ii—C11—H11	108.4
N1—C1—H1	108.0	C11—C12—C13	110.4 (3)
C2—C1—H1	108.0	C11—C12—H12A	109.6
C3^i—C1—H1	108.0	C13—C12—H12A	109.6
C1—C2—C3	113.3 (3)	C11—C12—H12B	109.6
C1—C2—H2A	108.9	C13—C12—H12B	109.6
C3—C2—H2A	108.9	H12A—C12—H12B	108.1
C1—C2—H2B	108.9	C11^ii—C13—C12	110.8 (3)
C3—C2—H2B	108.9	C11^ii—C13—H13A	109.5
H2A—C2—H2B	107.7	C12—C13—H13A	109.5
C1^i—C3—C2	113.9 (3)	C11^ii—C13—H13B	109.5
C1^i—C3—H3A	108.8	C12—C13—H13B	109.5
C2—C3—H3A	108.8	H13A—C13—H13B	108.1

Symmetry codes: (i) −x+2, −y+3, −z+2; (ii) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1N1···S3^iii	0.89	2.67	3.372 (4)	137
N1—H1N1···S4^iii	0.89	2.95	3.459 (3)	118
N1—H2N1···S1^iv	0.89	2.53	3.399 (4)	167
N1—H3N1···S4	0.89	2.78	3.600 (4)	155
N1—H3N1···S2	0.89	2.81	3.357 (4)	121
N2—H1N2···S2^v	0.89	2.63	3.349 (4)	139
N2—H1N2···S1^v	0.89	2.72	3.424 (4)	137
N2—H2N2···S3^iv	0.89	2.53	3.412 (4)	170
N2—H3N2···S2	0.89	2.47	3.289 (4)	153
C3—H3A···S1^iv	0.97	2.95	3.810 (4)	148

Symmetry codes: (iii) −x+1, −y+2, −z+2; (iv) x+1, y, z; (v) −x+1, −y+2, −z+1.