(1,4,7,10,13,16-Hexaoxa­cyclo­octa­decane)­potassium dithiocyanatoaurate(I)

In the title compound, [K(C₁₂H₂₄O₆)][Au(SCN)₂], the Au^I atom is in a linear configuration with respect to the coordinating S atoms. The encapsulation of the K⁺ ion by the 18-crown-6 ligand produces a large cation and prevents Au...Au interactions within the extended structure. Both Au and K occupy inversion centers.

Key indicators

• Single-crystal X-ray study
• T = 150 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.018
• wR factor = 0.038
• Data-to-parameter ratio = 31.2

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          1
            AU1 -S1  -C1  -N1   -170.00  3.00   1.555   1.555   1.555   1.555

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   2 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   1 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
   1 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2002); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

(1,4,7,10,13,16-hexaoxacyclooctadecane)potassium dithiocyanatogold(I)

Crystal data

[K(C12H24O6)][Au(SCN)2]	Z = 1
Mr = 616.54	F(000) = 300
Triclinic, P1	Dx = 1.911 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.2401 (2) Å	Cell parameters from 4565 reflections
b = 8.0946 (2) Å	θ = 2.1–32.2°
c = 10.2386 (3) Å	µ = 7.29 mm^−1
α = 75.814 (1)°	T = 150 K
β = 70.486 (1)°	Plate, colorless
γ = 73.894 (1)°	0.12 × 0.12 × 0.08 mm
V = 535.63 (3) Å^3

Data collection

Bruker SMART 6000 CCD diffractometer	3771 independent reflections
Radiation source: fine-focus sealed tube	3768 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.021
ω scans	θmax = 32.2°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 2001)	h = −10→10
Tmin = 0.447, Tmax = 0.558	k = −12→11
9875 measured reflections	l = −15→15

Refinement

Refinement on F^2	Primary atom site location: Patterson
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.018	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.039	H-atom parameters constrained
S = 1.09	w = 1/[σ^2(Fo^2) + (0.0096P)^2 + 0.467P] where P = (Fo^2 + 2Fc^2)/3
3771 reflections	(Δ/σ)max = 0.002
121 parameters	Δρmax = 0.82 e Å^−3
0 restraints	Δρmin = −0.53 e Å^−3

Special details

Experimental. The crystal was mounted on the tip of a glass fiber with paratone-N and immediately transferred to the goniostat bathed in a cold stream.

The final unit cell is obtained from the refinement of the XYZ weighted centroids of reflections with I > 20σ(I).

Note that the absorption correction parameters Tmin and Tmax also reflect beam corrections, etc. As a result, the numerical values for Tmin and Tmax may differ from expected values based solely absorption effects and crystal size.

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
Au1	−0.5000	0.5000	0.5000	0.02173 (3)
S1	−0.55322 (8)	0.24085 (7)	0.48166 (6)	0.02939 (10)
C1	−0.3924 (3)	0.2133 (2)	0.3222 (2)	0.0240 (3)
N1	−0.2871 (3)	0.1871 (3)	0.2136 (2)	0.0341 (4)
K1	0.0000	0.0000	0.0000	0.02059 (9)
O2	−0.1995 (2)	0.06876 (19)	−0.21032 (15)	0.0257 (3)
C3	−0.0995 (3)	0.1706 (3)	−0.3354 (2)	0.0305 (4)
H3A	−0.1802	0.2069	−0.4029	0.037*
H3B	0.0326	0.1006	−0.3801	0.037*
C4	−0.0722 (3)	0.3279 (3)	−0.2979 (2)	0.0307 (4)
H4A	−0.0283	0.4115	−0.3844	0.037*
H4B	−0.2009	0.3865	−0.2386	0.037*
O5	0.0746 (2)	0.27454 (18)	−0.22369 (15)	0.0243 (3)
C6	0.1123 (3)	0.4172 (3)	−0.1855 (2)	0.0264 (4)
H6A	−0.0115	0.4760	−0.1218	0.032*
H6B	0.1550	0.5032	−0.2705	0.032*
C7	0.2742 (3)	0.3491 (3)	−0.1131 (2)	0.0278 (4)
H7A	0.3942	0.2811	−0.1733	0.033*
H7B	0.3131	0.4473	−0.0945	0.033*
O8	0.1981 (2)	0.24101 (19)	0.01554 (15)	0.0252 (3)
C9	0.3269 (3)	0.1896 (3)	0.1042 (2)	0.0287 (4)
H9A	0.3531	0.2938	0.1232	0.034*
H9B	0.4567	0.1178	0.0578	0.034*
C10	0.2246 (3)	0.0858 (3)	0.2393 (2)	0.0286 (4)
H10A	0.3065	0.0549	0.3057	0.043*
H10B	0.0922	0.1562	0.2831	0.043*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Au1	0.02505 (5)	0.02037 (5)	0.02029 (5)	−0.00495 (3)	−0.00464 (3)	−0.00681 (3)
S1	0.0349 (3)	0.0264 (2)	0.0273 (2)	−0.0126 (2)	−0.00052 (19)	−0.01013 (18)
C1	0.0224 (8)	0.0210 (8)	0.0314 (9)	−0.0054 (6)	−0.0079 (7)	−0.0085 (7)
N1	0.0299 (9)	0.0357 (10)	0.0382 (10)	−0.0088 (7)	−0.0032 (8)	−0.0164 (8)
K1	0.0241 (2)	0.0208 (2)	0.0182 (2)	−0.00662 (19)	−0.00562 (18)	−0.00414 (18)
O2	0.0286 (7)	0.0259 (7)	0.0251 (6)	−0.0082 (5)	−0.0093 (5)	−0.0036 (5)
C3	0.0361 (11)	0.0335 (10)	0.0250 (9)	−0.0110 (9)	−0.0145 (8)	0.0016 (8)
C4	0.0337 (10)	0.0266 (9)	0.0319 (10)	−0.0070 (8)	−0.0156 (8)	0.0046 (8)
O5	0.0286 (7)	0.0201 (6)	0.0250 (6)	−0.0053 (5)	−0.0096 (5)	−0.0026 (5)
C6	0.0317 (10)	0.0208 (8)	0.0247 (8)	−0.0082 (7)	−0.0034 (7)	−0.0038 (7)
C7	0.0301 (10)	0.0278 (9)	0.0262 (9)	−0.0136 (8)	−0.0032 (7)	−0.0039 (7)
O8	0.0258 (7)	0.0283 (7)	0.0245 (6)	−0.0113 (5)	−0.0075 (5)	−0.0032 (5)
C9	0.0298 (10)	0.0282 (9)	0.0344 (10)	−0.0090 (8)	−0.0133 (8)	−0.0075 (8)
C10	0.0330 (10)	0.0296 (9)	0.0294 (9)	−0.0080 (8)	−0.0138 (8)	−0.0075 (8)

Geometric parameters (Å, º)

Au1—S1	2.2965 (5)	C4—O5	1.421 (2)
Au1—S1^i	2.2965 (5)	C4—H4A	0.9900
S1—C1	1.684 (2)	C4—H4B	0.9900
C1—N1	1.150 (3)	O5—C6	1.424 (2)
N1—K1	2.8699 (19)	C6—C7	1.500 (3)
K1—O8^ii	2.7829 (14)	C6—H6A	0.9900
K1—O8	2.7829 (14)	C6—H6B	0.9900
K1—O5	2.7966 (14)	C7—O8	1.422 (2)
K1—O5^ii	2.7966 (14)	C7—H7A	0.9900
K1—O2	2.8419 (14)	C7—H7B	0.9900
K1—O2^ii	2.8419 (14)	O8—C9	1.425 (2)
K1—N1^ii	2.8699 (19)	C9—C10	1.503 (3)
O2—C10^ii	1.425 (2)	C9—H9A	0.9900
O2—C3	1.427 (2)	C9—H9B	0.9900
C3—C4	1.496 (3)	C10—O2^ii	1.425 (2)
C3—H3A	0.9900	C10—H10A	0.9900
C3—H3B	0.9900	C10—H10B	0.9900
S1—Au1—S1^i	180.0	C4—C3—H3B	109.9
C1—S1—Au1	99.79 (7)	H3A—C3—H3B	108.3
N1—C1—S1	176.23 (19)	O5—C4—C3	108.86 (17)
C1—N1—K1	159.58 (18)	O5—C4—H4A	109.9
O8^ii—K1—O8	180.00 (3)	C3—C4—H4A	109.9
O8^ii—K1—O5	119.61 (4)	O5—C4—H4B	109.9
O8—K1—O5	60.39 (4)	C3—C4—H4B	109.9
O8^ii—K1—O5^ii	60.39 (4)	H4A—C4—H4B	108.3
O8—K1—O5^ii	119.61 (4)	C4—O5—C6	112.61 (15)
O5—K1—O5^ii	180.0	C4—O5—K1	113.04 (11)
O8^ii—K1—O2	59.58 (4)	C6—O5—K1	113.47 (11)
O8—K1—O2	120.42 (4)	O5—C6—C7	108.69 (16)
O5—K1—O2	61.33 (4)	O5—C6—H6A	110.0
O5^ii—K1—O2	118.67 (4)	C7—C6—H6A	110.0
O8^ii—K1—O2^ii	120.42 (4)	O5—C6—H6B	110.0
O8—K1—O2^ii	59.58 (4)	C7—C6—H6B	110.0
O5—K1—O2^ii	118.67 (4)	H6A—C6—H6B	108.3
O5^ii—K1—O2^ii	61.33 (4)	O8—C7—C6	107.85 (16)
O2—K1—O2^ii	180.00 (7)	O8—C7—H7A	110.1
O8^ii—K1—N1^ii	76.68 (5)	C6—C7—H7A	110.1
O8—K1—N1^ii	103.32 (5)	O8—C7—H7B	110.1
O5—K1—N1^ii	79.27 (5)	C6—C7—H7B	110.1
O5^ii—K1—N1^ii	100.73 (5)	H7A—C7—H7B	108.4
O2—K1—N1^ii	76.87 (5)	C7—O8—C9	113.15 (16)
O2^ii—K1—N1^ii	103.13 (5)	C7—O8—K1	116.04 (11)
O8^ii—K1—N1	103.32 (5)	C9—O8—K1	118.80 (11)
O8—K1—N1	76.68 (5)	O8—C9—C10	107.97 (16)
O5—K1—N1	100.73 (5)	O8—C9—H9A	110.1
O5^ii—K1—N1	79.27 (5)	C10—C9—H9A	110.1
O2—K1—N1	103.13 (5)	O8—C9—H9B	110.1
O2^ii—K1—N1	76.87 (5)	C10—C9—H9B	110.1
N1^ii—K1—N1	180.00 (8)	H9A—C9—H9B	108.4
C10^ii—O2—C3	111.22 (16)	O2^ii—C10—C9	109.09 (17)
C10^ii—O2—K1	112.83 (11)	O2^ii—C10—H10A	109.9
C3—O2—K1	110.82 (11)	C9—C10—H10A	109.9
O2—C3—C4	108.78 (18)	O2^ii—C10—H10B	109.9
O2—C3—H3A	109.9	C9—C10—H10B	109.9
C4—C3—H3A	109.9	H10A—C10—H10B	108.3
O2—C3—H3B	109.9
Au1—S1—C1—N1	−170 (3)	O5—C6—C7—O8	−65.7 (2)
C10^ii—O2—C3—C4	−178.36 (17)	C6—C7—O8—C9	−171.00 (16)
O2—C3—C4—O5	70.8 (2)	C7—O8—C9—C10	176.61 (17)
C3—C4—O5—C6	179.15 (17)	O8—C9—C10—O2^ii	63.3 (2)
C4—O5—C6—C7	−177.77 (16)

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