metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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ISSN: 2056-9890

Tetra­kis­[(benzene-18-crown-6)potassium]bis­[tris­(thio­cyanato)copper(I)]

aCollege of Chemistry and Chemical Engineering, Liaocheng University, Shandong 252059, People's Republic of China
*Correspondence e-mail: msong@lcu.edu.cn

(Received 13 January 2008; accepted 14 February 2008; online 20 February 2008)

The title complex, bis­(μ-benzene-18-crown-6)-3κ6O:4κO;4κ6O:3κO-bis­(benzene-18-crown-6)-1κ6O,6κ6O-tetra-μ-thiocyanato-1:2κ2S:N;2:3κ2N:S;4:5κ2S:N;5:6κ2N:S-dithio­cyanato-2κN,5κN-2,5-dicopper(I)-1,3,4,6-tetra­potassium(I), [K4Cu2(NCS)6(C16H24O6)4] or {[K(C16H24O6)]4[Cu(NCS)3]2}, consists of four [K(benzene-18-crown-6)]+ cations and two [Cu(NCS)3]2− anions, forming a dimeric structure with site symmetry [\overline{1}]. In each [Cu(NCS)3]2− anion, the CuI atom is coordinated by three N atoms of thio­cyanate ligands in a trigonal–planar coordination geometry. Each [Cu(NCS)3]2− anion bridges two [K(benzene-18-crown-6)]+ cations, with K—S distances of 3.317 (3) and 3.198 (3) Å, and two [K(benzene-18-crown-6)]+ cations are linked across a crystallographic centre of inversion, with K—O distances of 2.903 (5) Å.

Related literature

For structures incorporating [Cu(NCS)3]2− anions, see: Rusanova et al. (2000[Rusanova, J. A., Domasevitch, K. V., Vassilyeva, O. Yu., Kokozay, V. N. & Rusanov, E. B. (2000). J. Chem. Soc. Dalton Trans. pp. 2175-2182.]); Wang et al. (1987[Wang, M., Zheng, P.-J., Zhang, J.-Z., Chen, Z., Shen, J.-M. & Yang, Y.-H. (1987). Acta Cryst. C43, 1544-1546.]). For polymeric structures incorporating crown ethers, see: Desai et al. (2001[Desai, S. B., Desai, P. B. & Desai, K. R. (2001). Heterocycl. Commun. 1, 83-90.]); Bastos et al. (2000[Bastos, M. B. R., Moreira, J. C. & Farias, P. A. M. (2000). Anal. Chim. Acta, 408, 83-88.]).

[Scheme 1]

Experimental

Crystal data
  • [K4Cu2(NCS)6(C16H24O6)4]

  • Mr = 1881.36

  • Triclinic, [P \overline 1]

  • a = 9.702 (3) Å

  • b = 13.119 (4) Å

  • c = 17.968 (6) Å

  • α = 91.015 (6)°

  • β = 97.167 (6)°

  • γ = 105.558 (6)°

  • V = 2182.9 (12) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 0.89 mm−1

  • T = 273 (2) K

  • 0.49 × 0.21 × 0.16 mm

Data collection
  • Bruker SMART CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.668, Tmax = 0.870

  • 11606 measured reflections

  • 7633 independent reflections

  • 2441 reflections with I > 2σ(I)

  • Rint = 0.076

Refinement
  • R[F2 > 2σ(F2)] = 0.062

  • wR(F2) = 0.160

  • S = 0.85

  • 7633 reflections

  • 505 parameters

  • H-atom parameters constrained

  • Δρmax = 0.41 e Å−3

  • Δρmin = −0.34 e Å−3

Table 1
Selected geometric parameters (Å, °)

Cu1—N1 1.873 (8)
Cu1—N2 1.910 (7)
Cu1—N3 1.915 (7)
K1—O5 2.683 (5)
K1—O2 2.718 (5)
K1—O1 2.727 (5)
K1—O3 2.756 (5)
K1—O6 2.761 (5)
K1—O4 2.875 (5)
K1—O4i 2.903 (5)
K1—S1 3.317 (3)
K2—O12 2.729 (5)
K2—O11 2.730 (5)
K2—O9 2.765 (5)
K2—O8 2.773 (5)
K2—O10 2.797 (5)
K2—O7 2.819 (5)
K2—S2 3.198 (3)
N1—Cu1—N2 121.2 (3)
N1—Cu1—N3 121.5 (3)
N2—Cu1—N3 117.1 (3)
Symmetry code: (i) -x+1, -y, -z+1.

Data collection: SMART (Bruker, 1997[Bruker (1997). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 1997[Bruker (1997). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

Much interest has been focused on crown ethers and their metal cations, because they can act as modules to form polymeric supramolecular structures (Desai et al., 2001; Bastos et al., 2000).

The title complex consists of four [K(benzene-18-crown-6)]+ cations and two [Cu(NCS)3]2- anions. The CuI atom is coordinated by three N atoms in a trigonal-planar geometry (Table 1). The K+ ions are coordinated by six O atoms, and lie approximately in the plane of the crown ether. The K—O bond lengths vary from 2.683 (5)–2.903 (5) Å for K1 and 2.729 (5)–2.819 (5) Å for K2. In addition, K+ is coordinated by one S atom from [Cu(NCS)3]2-, with K1—S1 = 3.317 (3) Å and K2—S2 = 3.198 (3) Å.

Related literature top

For structures incorporating [Cu(NCS)3]2- anions, see: Rusanova et al. (2000); Wang et al. (1987). For polymeric structures incorporating crown ethers, see: Desai et al. (2001); Bastos et al. (2000).

Experimental top

Cu(NCS) (0.1853 g, 1.5 mmol) and K(NCS) (0.1448 g, 1.5 mmol) in 15 ml absolute alcohol were refluxed for 4 h, then benzene-18-crown-6 (0.4675 g, 1.5 mmol) was added slowly and the mixture was refluxed for a further 4 h. After cooling to room temperature, the mixture was filtered and the solid recrystallized from diethyl ether. Elemental analysis: calculated C 44.69, H 5.14, N 4.47%; found: C 44.76, H 5.17, N 4.51%.

Refinement top

H atoms were positioned geometrically and refined using a riding model with C—H = 0.93–0.97 Å and Uiso(H) = 1.2Ueq(C).

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The title complex (H atoms omitted) showing the numbering scheme for Cu, K, N and S atoms. Displacement ellipsoids are drawn at the 30% probability level. Atoms with the suffix A are generated by the symmetry operator 1 - x, -y, 1 - z.
bis(µ-benzene-18-crown-6)–3κ6O:4κO;4κ6O:3κO-bis(benzene-18-crown-6)- 1κ6O,6κ6O-tetra-µ-thiocyanato- 1:2κ2S:N;2:3κ2N:S;4:5κ2S:N;5:6κ2N:S-dithiocyanato- 2κN,5κN-2,5-dicopper(I)-1,3,4,6-tetrapotassium(I) top
Crystal data top
[K4Cu2(NCS)6(C16H24O6)4]Z = 1
Mr = 1881.36F(000) = 980
Triclinic, P1Dx = 1.431 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.702 (3) ÅCell parameters from 1026 reflections
b = 13.119 (4) Åθ = 2.3–19.0°
c = 17.968 (6) ŵ = 0.89 mm1
α = 91.015 (6)°T = 273 K
β = 97.167 (6)°Block, green
γ = 105.558 (6)°0.49 × 0.21 × 0.16 mm
V = 2182.9 (12) Å3
Data collection top
Bruker SMART CCD
diffractometer
7633 independent reflections
Radiation source: fine-focus sealed tube2441 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.077
ω scansθmax = 25.0°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1111
Tmin = 0.669, Tmax = 0.870k = 1115
11606 measured reflectionsl = 2119
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)] = 0.062Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.160H-atom parameters constrained
S = 0.85 w = 1/[σ2(Fo2) + (0.0464P)2]
where P = (Fo2 + 2Fc2)/3
7633 reflections(Δ/σ)max < 0.001
505 parametersΔρmax = 0.41 e Å3
0 restraintsΔρmin = 0.34 e Å3
Crystal data top
[K4Cu2(NCS)6(C16H24O6)4]γ = 105.558 (6)°
Mr = 1881.36V = 2182.9 (12) Å3
Triclinic, P1Z = 1
a = 9.702 (3) ÅMo Kα radiation
b = 13.119 (4) ŵ = 0.89 mm1
c = 17.968 (6) ÅT = 273 K
α = 91.015 (6)°0.49 × 0.21 × 0.16 mm
β = 97.167 (6)°
Data collection top
Bruker SMART CCD
diffractometer
7633 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
2441 reflections with I > 2σ(I)
Tmin = 0.669, Tmax = 0.870Rint = 0.077
11606 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0620 restraints
wR(F2) = 0.160H-atom parameters constrained
S = 0.85Δρmax = 0.41 e Å3
7633 reflectionsΔρmin = 0.34 e Å3
505 parameters
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
Cu10.10846 (12)0.10295 (8)0.25933 (6)0.0631 (4)
K10.35951 (18)0.15952 (12)0.48793 (9)0.0492 (5)
K20.03041 (19)0.27283 (12)0.09562 (10)0.0566 (5)
N10.0459 (8)0.1929 (6)0.3274 (4)0.072 (2)
N20.0190 (8)0.0283 (5)0.2376 (4)0.066 (2)
N30.2976 (8)0.1432 (5)0.2030 (4)0.065 (2)
O10.4114 (6)0.3250 (4)0.5657 (3)0.0529 (14)
O20.4960 (5)0.2967 (4)0.4361 (3)0.0490 (14)
O30.4511 (5)0.1319 (4)0.3487 (3)0.0501 (14)
O40.3773 (5)0.0397 (4)0.4201 (3)0.0502 (14)
O50.1858 (5)0.0452 (4)0.5271 (3)0.0542 (14)
O60.2402 (5)0.2078 (4)0.6189 (3)0.0523 (14)
O70.2852 (5)0.2777 (4)0.1540 (3)0.0526 (15)
O80.0563 (6)0.4250 (4)0.1980 (3)0.0598 (15)
O90.1587 (6)0.4733 (4)0.1018 (3)0.0632 (16)
O100.1230 (6)0.3411 (4)0.0244 (3)0.0571 (15)
O110.0473 (6)0.1308 (4)0.0203 (3)0.0626 (16)
O120.2782 (6)0.1135 (4)0.0589 (3)0.0632 (16)
S10.0692 (3)0.34102 (19)0.40627 (13)0.0706 (7)
S20.2182 (3)0.21181 (19)0.20496 (16)0.0946 (9)
S30.5419 (3)0.21268 (18)0.09955 (14)0.0814 (8)
C10.5322 (8)0.3583 (6)0.5560 (5)0.043 (2)
C20.6081 (10)0.4018 (6)0.6090 (5)0.064 (2)
H20.57980.41090.65660.077*
C30.7264 (10)0.4328 (7)0.5929 (6)0.075 (3)
H30.77710.46320.62940.090*
C40.7697 (10)0.4188 (7)0.5231 (6)0.075 (3)
H40.84890.44030.51170.090*
C50.6951 (9)0.3726 (6)0.4703 (5)0.058 (2)
H50.72520.36170.42320.069*
C60.5774 (9)0.3425 (6)0.4857 (5)0.045 (2)
C70.5258 (9)0.2889 (6)0.3594 (4)0.057 (2)
H7A0.51440.35880.33670.069*
H7B0.62410.24670.35770.069*
C80.4219 (9)0.2380 (6)0.3185 (4)0.058 (2)
H8A0.43170.23780.26540.070*
H8B0.32390.27710.32400.070*
C90.3642 (8)0.0726 (6)0.3085 (4)0.057 (2)
H9A0.26270.10460.31160.069*
H9B0.37830.07110.25600.069*
C100.4111 (8)0.0383 (6)0.3445 (5)0.062 (2)
H10A0.51440.06690.34500.075*
H10B0.36320.08320.31500.075*
C110.2444 (8)0.0633 (6)0.4253 (5)0.058 (2)
H11A0.16660.01180.39450.069*
H11B0.24820.13290.40680.069*
C120.2161 (9)0.0610 (6)0.5048 (5)0.062 (2)
H12A0.29990.10460.53680.074*
H12B0.13460.08900.50990.074*
C130.1522 (8)0.0568 (6)0.6012 (5)0.062 (2)
H13A0.07180.02800.60700.074*
H13B0.23460.01820.63630.074*
C140.1140 (8)0.1704 (6)0.6171 (4)0.061 (2)
H14A0.07740.18000.66510.073*
H14B0.03920.21050.57850.073*
C150.2126 (9)0.3179 (6)0.6263 (4)0.062 (2)
H15A0.14940.35540.58250.075*
H15B0.16470.33780.67020.075*
C160.3524 (9)0.3477 (6)0.6340 (4)0.057 (2)
H16A0.41850.30720.67580.068*
H16B0.33570.42250.64290.068*
C170.3083 (9)0.3740 (6)0.1718 (4)0.041 (2)
C180.4398 (9)0.3943 (6)0.1667 (4)0.053 (2)
H180.52300.34110.14920.063*
C190.4496 (10)0.4936 (8)0.1874 (4)0.062 (2)
H190.53920.50720.18500.074*
C200.3253 (11)0.5724 (6)0.2114 (4)0.063 (3)
H200.33190.63940.22520.075*
C210.1925 (9)0.5539 (6)0.2154 (4)0.055 (2)
H210.10960.60820.23160.066*
C220.1822 (8)0.4550 (6)0.1955 (4)0.041 (2)
C230.0801 (9)0.5023 (7)0.2165 (5)0.073 (3)
H23A0.15020.46860.24050.087*
H23B0.07050.55610.25170.087*
C240.1317 (9)0.5524 (6)0.1490 (5)0.078 (3)
H24A0.05960.58250.12280.093*
H24B0.21970.60890.16290.093*
C250.2142 (9)0.5112 (6)0.0356 (5)0.072 (3)
H25A0.30080.56940.04790.086*
H25B0.14360.53670.00370.086*
C260.2478 (9)0.4232 (7)0.0036 (4)0.069 (3)
H26A0.29120.44830.04790.083*
H26B0.31670.39730.02920.083*
C270.1488 (10)0.2524 (6)0.0615 (5)0.086 (3)
H27A0.21140.22180.02790.104*
H27B0.19610.27470.10530.104*
C280.0099 (11)0.1736 (6)0.0844 (5)0.077 (3)
H28A0.05670.20670.11270.093*
H28B0.02340.11760.11630.093*
C290.1779 (10)0.0482 (6)0.0361 (5)0.071 (3)
H29A0.15810.01390.05760.085*
H29B0.24480.07070.07250.085*
C300.2434 (9)0.0212 (6)0.0333 (5)0.075 (3)
H30A0.32980.03760.02320.089*
H30B0.17590.00140.07100.089*
C310.3593 (9)0.0944 (6)0.1204 (5)0.072 (3)
H31A0.29960.08220.16490.087*
H31B0.44140.03270.10880.087*
C320.4091 (9)0.1910 (5)0.1331 (5)0.073 (3)
H32A0.46440.20520.08750.088*
H32B0.47040.18020.17260.088*
C330.0053 (8)0.2538 (7)0.3610 (4)0.050 (2)
C340.1016 (9)0.1047 (7)0.2239 (4)0.055 (2)
C350.3980 (10)0.1725 (6)0.1608 (5)0.054 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0681 (8)0.0618 (7)0.0576 (7)0.0144 (6)0.0103 (6)0.0051 (6)
K10.0542 (12)0.0595 (12)0.0424 (11)0.0270 (10)0.0131 (9)0.0074 (9)
K20.0580 (13)0.0523 (11)0.0607 (13)0.0137 (10)0.0162 (10)0.0039 (10)
N10.070 (6)0.076 (6)0.067 (6)0.023 (4)0.005 (4)0.010 (4)
N20.069 (6)0.059 (5)0.064 (5)0.005 (4)0.013 (4)0.002 (4)
N30.063 (6)0.067 (5)0.062 (6)0.014 (4)0.009 (4)0.000 (4)
O10.065 (4)0.060 (3)0.047 (4)0.030 (3)0.026 (3)0.023 (3)
O20.061 (4)0.063 (4)0.035 (3)0.032 (3)0.016 (3)0.005 (3)
O30.053 (4)0.058 (4)0.043 (3)0.023 (3)0.002 (3)0.007 (3)
O40.041 (4)0.060 (4)0.052 (4)0.021 (3)0.000 (3)0.006 (3)
O50.052 (4)0.059 (4)0.056 (4)0.023 (3)0.009 (3)0.005 (3)
O60.060 (4)0.054 (4)0.051 (4)0.024 (3)0.017 (3)0.000 (3)
O70.050 (4)0.034 (3)0.072 (4)0.006 (3)0.018 (3)0.003 (3)
O80.047 (4)0.062 (4)0.064 (4)0.008 (3)0.003 (3)0.018 (3)
O90.075 (4)0.059 (4)0.054 (4)0.007 (3)0.026 (3)0.000 (3)
O100.066 (4)0.045 (3)0.066 (4)0.017 (3)0.024 (3)0.004 (3)
O110.079 (5)0.054 (4)0.060 (4)0.022 (3)0.019 (4)0.006 (3)
O120.071 (4)0.044 (3)0.082 (4)0.020 (3)0.027 (4)0.001 (3)
S10.0656 (17)0.0853 (17)0.0639 (17)0.0266 (14)0.0065 (13)0.0060 (14)
S20.0675 (19)0.0794 (18)0.124 (2)0.0000 (15)0.0018 (17)0.0385 (17)
S30.0670 (17)0.0811 (18)0.0795 (19)0.0015 (14)0.0045 (15)0.0047 (14)
C10.041 (5)0.042 (5)0.048 (6)0.020 (4)0.003 (5)0.007 (4)
C20.071 (7)0.072 (6)0.052 (6)0.031 (5)0.011 (5)0.000 (5)
C30.056 (7)0.079 (7)0.095 (9)0.037 (6)0.018 (6)0.001 (6)
C40.055 (7)0.079 (7)0.097 (9)0.034 (6)0.004 (7)0.007 (7)
C50.053 (6)0.055 (6)0.069 (7)0.020 (5)0.011 (5)0.003 (5)
C60.044 (6)0.039 (5)0.049 (6)0.010 (4)0.001 (5)0.001 (4)
C70.066 (6)0.061 (6)0.046 (6)0.017 (5)0.019 (5)0.012 (4)
C80.068 (7)0.069 (6)0.040 (5)0.017 (5)0.019 (5)0.003 (5)
C90.049 (6)0.090 (7)0.036 (5)0.027 (5)0.003 (4)0.013 (5)
C100.052 (6)0.071 (6)0.069 (7)0.030 (5)0.001 (5)0.020 (5)
C110.042 (6)0.064 (6)0.068 (7)0.022 (5)0.006 (5)0.012 (5)
C120.073 (7)0.055 (6)0.065 (7)0.035 (5)0.003 (5)0.009 (5)
C130.056 (6)0.076 (7)0.069 (7)0.041 (5)0.018 (5)0.004 (5)
C140.052 (6)0.075 (6)0.069 (6)0.033 (5)0.027 (5)0.004 (5)
C150.081 (7)0.067 (6)0.047 (6)0.023 (6)0.032 (5)0.021 (5)
C160.071 (7)0.056 (5)0.056 (6)0.029 (5)0.027 (5)0.030 (4)
C170.045 (6)0.055 (6)0.027 (5)0.015 (5)0.015 (4)0.013 (4)
C180.057 (6)0.050 (6)0.053 (6)0.017 (5)0.008 (5)0.000 (4)
C190.066 (7)0.091 (7)0.048 (6)0.045 (6)0.028 (5)0.010 (5)
C200.092 (8)0.053 (6)0.061 (6)0.043 (6)0.027 (6)0.010 (5)
C210.070 (7)0.055 (6)0.040 (5)0.015 (5)0.014 (5)0.009 (4)
C220.041 (5)0.050 (5)0.038 (5)0.019 (5)0.012 (4)0.002 (4)
C230.057 (7)0.086 (7)0.060 (7)0.001 (5)0.001 (5)0.023 (5)
C240.075 (7)0.058 (6)0.082 (8)0.012 (5)0.013 (6)0.021 (6)
C250.081 (7)0.062 (6)0.063 (7)0.004 (5)0.026 (6)0.005 (5)
C260.080 (8)0.087 (7)0.046 (6)0.020 (6)0.026 (5)0.013 (5)
C270.120 (10)0.059 (6)0.099 (8)0.033 (6)0.069 (8)0.010 (6)
C280.136 (10)0.057 (6)0.049 (6)0.037 (6)0.028 (7)0.003 (5)
C290.079 (7)0.045 (6)0.087 (8)0.014 (5)0.016 (6)0.016 (5)
C300.085 (7)0.058 (6)0.090 (8)0.025 (5)0.032 (6)0.004 (6)
C310.082 (7)0.035 (5)0.097 (8)0.001 (5)0.035 (6)0.006 (5)
C320.062 (6)0.035 (5)0.117 (8)0.004 (5)0.030 (6)0.008 (5)
C330.039 (5)0.066 (6)0.040 (5)0.009 (5)0.000 (4)0.012 (5)
C340.052 (6)0.067 (6)0.043 (6)0.022 (5)0.014 (5)0.002 (5)
C350.062 (7)0.045 (5)0.055 (6)0.014 (5)0.015 (5)0.002 (5)
Geometric parameters (Å, º) top
Cu1—N11.873 (8)C7—H7A0.970
Cu1—N21.910 (7)C7—H7B0.970
Cu1—N31.915 (7)C8—H8A0.970
K1—O52.683 (5)C8—H8B0.970
K1—O22.718 (5)C9—C101.510 (9)
K1—O12.727 (5)C9—H9A0.970
K1—O32.756 (5)C9—H9B0.970
K1—O62.761 (5)C10—H10A0.970
K1—O42.875 (5)C10—H10B0.970
K1—O4i2.903 (5)C11—C121.489 (9)
K1—S13.317 (3)C11—H11A0.970
K2—O122.729 (5)C11—H11B0.970
K2—O112.730 (5)C12—H12A0.970
K2—O92.765 (5)C12—H12B0.970
K2—O82.773 (5)C13—C141.479 (9)
K2—O102.797 (5)C13—H13A0.970
K2—O72.819 (5)C13—H13B0.970
K2—S23.198 (3)C14—H14A0.970
N1—C331.185 (9)C14—H14B0.970
N2—C341.155 (8)C15—C161.501 (9)
N3—C351.129 (9)C15—H15A0.970
O1—C11.384 (8)C15—H15B0.970
O1—C161.421 (7)C16—H16A0.970
O2—C61.370 (8)C16—H16B0.970
O2—C71.443 (7)C17—C181.364 (9)
O3—C81.426 (7)C17—C221.402 (9)
O3—C91.435 (8)C18—C191.379 (9)
O4—C111.419 (8)C18—H180.930
O4—C101.437 (8)C19—C201.376 (10)
O4—K1i2.903 (5)C19—H190.930
O5—C131.411 (8)C20—C211.367 (10)
O5—C121.420 (8)C20—H200.930
O6—C151.408 (7)C21—C221.373 (9)
O6—C141.433 (8)C21—H210.930
O7—C171.379 (8)C23—C241.468 (10)
O7—C321.421 (8)C23—H23A0.970
O8—C221.376 (8)C23—H23B0.970
O8—C231.431 (8)C24—H24A0.970
O9—C251.411 (8)C24—H24B0.970
O9—C241.427 (8)C25—C261.470 (9)
O10—C261.392 (8)C25—H25A0.970
O10—C271.425 (8)C25—H25B0.970
O11—C281.400 (8)C26—H26A0.970
O11—C291.422 (8)C26—H26B0.970
O12—C311.423 (8)C27—C281.468 (11)
O12—C301.425 (7)C27—H27A0.970
S1—C331.626 (9)C27—H27B0.970
S2—C341.622 (9)C28—H28A0.970
S3—C351.625 (9)C28—H28B0.970
C1—C21.359 (10)C29—C301.476 (10)
C1—C61.388 (9)C29—H29A0.970
C2—C31.377 (10)C29—H29B0.970
C2—H20.930C30—H30A0.970
C3—C41.372 (11)C30—H30B0.970
C3—H30.930C31—C321.495 (9)
C4—C51.369 (10)C31—H31A0.970
C4—H40.930C31—H31B0.970
C5—C61.361 (9)C32—H32A0.970
C5—H50.930C32—H32B0.970
C7—C81.483 (9)
N1—Cu1—N2121.2 (3)C10—C9—H9A110.3
N1—Cu1—N3121.5 (3)O3—C9—H9B110.3
N2—Cu1—N3117.1 (3)C10—C9—H9B110.3
O5—K1—O2170.74 (16)H9A—C9—H9B108.6
O5—K1—O1123.77 (17)O4—C10—C9111.5 (6)
O2—K1—O156.17 (15)O4—C10—H10A109.3
O5—K1—O3117.82 (17)C9—C10—H10A109.3
O2—K1—O361.31 (15)O4—C10—H10B109.3
O1—K1—O3117.47 (16)C9—C10—H10B109.3
O5—K1—O662.87 (16)H10A—C10—H10B108.0
O2—K1—O6116.73 (16)O4—C11—C12109.8 (6)
O1—K1—O660.98 (15)O4—C11—H11A109.7
O3—K1—O6172.87 (16)C12—C11—H11A109.7
O5—K1—O462.10 (16)O4—C11—H11B109.7
O2—K1—O4120.45 (16)C12—C11—H11B109.7
O1—K1—O4165.95 (16)H11A—C11—H11B108.2
O3—K1—O461.15 (15)O5—C12—C11109.1 (6)
O6—K1—O4122.24 (16)O5—C12—H12A109.9
O5—K1—O4i97.66 (15)C11—C12—H12A109.9
O2—K1—O4i91.54 (15)O5—C12—H12B109.9
O1—K1—O4i83.25 (14)C11—C12—H12B109.9
O3—K1—O4i98.96 (15)H12A—C12—H12B108.3
O6—K1—O4i87.85 (15)O5—C13—C14109.4 (6)
O4—K1—O4i83.24 (15)O5—C13—H13A109.8
O5—K1—S188.66 (12)C14—C13—H13A109.8
O2—K1—S182.11 (12)O5—C13—H13B109.8
O1—K1—S183.85 (12)C14—C13—H13B109.8
O3—K1—S187.91 (12)H13A—C13—H13B108.2
O6—K1—S185.01 (12)O6—C14—C13109.0 (6)
O4—K1—S1109.70 (12)O6—C14—H14A109.9
O4i—K1—S1167.06 (11)C13—C14—H14A109.9
O12—K2—O1160.81 (17)O6—C14—H14B109.9
O12—K2—O9158.87 (17)C13—C14—H14B109.9
O11—K2—O9120.39 (18)H14A—C14—H14B108.3
O12—K2—O8113.47 (17)O6—C15—C16109.4 (6)
O11—K2—O8169.50 (18)O6—C15—H15A109.8
O9—K2—O861.31 (15)C16—C15—H15A109.8
O12—K2—O10114.86 (17)O6—C15—H15B109.8
O11—K2—O1061.28 (16)C16—C15—H15B109.8
O9—K2—O1059.47 (15)H15A—C15—H15B108.2
O8—K2—O10118.10 (16)O1—C16—C15107.2 (6)
O12—K2—O759.33 (15)O1—C16—H16A110.3
O11—K2—O7118.88 (17)C15—C16—H16A110.3
O9—K2—O7111.00 (15)O1—C16—H16B110.3
O8—K2—O754.23 (15)C15—C16—H16B110.3
O10—K2—O7141.73 (16)H16A—C16—H16B108.5
O12—K2—S2115.35 (13)C18—C17—O7125.4 (7)
O11—K2—S297.40 (13)C18—C17—C22120.1 (7)
O9—K2—S285.75 (13)O7—C17—C22114.5 (7)
O8—K2—S293.05 (14)C17—C18—C19120.2 (8)
O10—K2—S299.01 (13)C17—C18—H18119.9
O7—K2—S2117.94 (13)C19—C18—H18119.9
C33—N1—Cu1168.9 (7)C20—C19—C18119.3 (8)
C34—N2—Cu1176.3 (7)C20—C19—H19120.3
C35—N3—Cu1168.5 (8)C18—C19—H19120.3
C1—O1—C16117.6 (6)C21—C20—C19121.3 (8)
C1—O1—K1119.3 (4)C21—C20—H20119.4
C16—O1—K1118.6 (4)C19—C20—H20119.4
C6—O2—C7118.6 (6)C20—C21—C22119.7 (8)
C6—O2—K1119.9 (4)C20—C21—H21120.2
C7—O2—K1117.4 (4)C22—C21—H21120.2
C8—O3—C9113.0 (6)C21—C22—O8125.8 (7)
C8—O3—K1102.9 (4)C21—C22—C17119.5 (7)
C9—O3—K1106.0 (4)O8—C22—C17114.7 (7)
C11—O4—C10113.2 (6)O8—C23—C24111.1 (7)
C11—O4—K1106.6 (4)O8—C23—H23A109.4
C10—O4—K1112.5 (4)C24—C23—H23A109.4
C11—O4—K1i120.6 (4)O8—C23—H23B109.4
C10—O4—K1i106.1 (4)C24—C23—H23B109.4
K1—O4—K1i96.76 (15)H23A—C23—H23B108.0
C13—O5—C12113.7 (6)O9—C24—C23108.1 (7)
C13—O5—K1114.9 (4)O9—C24—H24A110.1
C12—O5—K1116.6 (4)C23—C24—H24A110.1
C15—O6—C14113.6 (6)O9—C24—H24B110.1
C15—O6—K1108.0 (4)C23—C24—H24B110.1
C14—O6—K1109.3 (4)H24A—C24—H24B108.4
C17—O7—C32117.2 (6)O9—C25—C26107.9 (7)
C17—O7—K2119.5 (4)O9—C25—H25A110.1
C32—O7—K2117.2 (4)C26—C25—H25A110.1
C22—O8—C23119.9 (6)O9—C25—H25B110.1
C22—O8—K2120.9 (4)C26—C25—H25B110.1
C23—O8—K2109.5 (4)H25A—C25—H25B108.4
C25—O9—C24114.4 (6)O10—C26—C25110.6 (7)
C25—O9—K2118.5 (4)O10—C26—H26A109.5
C24—O9—K2116.9 (4)C25—C26—H26A109.5
C26—O10—C27113.3 (6)O10—C26—H26B109.5
C26—O10—K2113.1 (4)C25—C26—H26B109.5
C27—O10—K2109.5 (4)H26A—C26—H26B108.1
C28—O11—C29114.1 (7)O10—C27—C28108.6 (7)
C28—O11—K2115.8 (4)O10—C27—H27A110.0
C29—O11—K2116.8 (4)C28—C27—H27A110.0
C31—O12—C30112.4 (6)O10—C27—H27B110.0
C31—O12—K2110.9 (4)C28—C27—H27B110.0
C30—O12—K2109.4 (4)H27A—C27—H27B108.3
C33—S1—K193.0 (3)O11—C28—C27109.4 (8)
C34—S2—K289.6 (3)O11—C28—H28A109.8
C2—C1—O1125.6 (8)C27—C28—H28A109.8
C2—C1—C6119.3 (8)O11—C28—H28B109.8
O1—C1—C6115.1 (7)C27—C28—H28B109.8
C1—C2—C3120.6 (9)H28A—C28—H28B108.3
C1—C2—H2119.7O11—C29—C30110.3 (7)
C3—C2—H2119.7O11—C29—H29A109.6
C4—C3—C2120.1 (9)C30—C29—H29A109.6
C4—C3—H3120.0O11—C29—H29B109.6
C2—C3—H3120.0C30—C29—H29B109.6
C5—C4—C3119.2 (9)H29A—C29—H29B108.1
C5—C4—H4120.4O12—C30—C29106.5 (7)
C3—C4—H4120.4O12—C30—H30A110.4
C6—C5—C4121.0 (9)C29—C30—H30A110.4
C6—C5—H5119.5O12—C30—H30B110.4
C4—C5—H5119.5C29—C30—H30B110.4
C5—C6—O2124.8 (8)H30A—C30—H30B108.6
C5—C6—C1119.8 (8)O12—C31—C32106.8 (6)
O2—C6—C1115.4 (7)O12—C31—H31A110.4
O2—C7—C8107.3 (6)C32—C31—H31A110.4
O2—C7—H7A110.2O12—C31—H31B110.4
C8—C7—H7A110.2C32—C31—H31B110.4
O2—C7—H7B110.2H31A—C31—H31B108.6
C8—C7—H7B110.2O7—C32—C31108.1 (7)
H7A—C7—H7B108.5O7—C32—H32A110.1
O3—C8—C7108.7 (7)C31—C32—H32A110.1
O3—C8—H8A110.0O7—C32—H32B110.1
C7—C8—H8A110.0C31—C32—H32B110.1
O3—C8—H8B110.0H32A—C32—H32B108.4
C7—C8—H8B110.0N1—C33—S1177.6 (8)
H8A—C8—H8B108.3N2—C34—S2179.7 (10)
O3—C9—C10107.0 (6)N3—C35—S3179.0 (9)
O3—C9—H9A110.3
Symmetry code: (i) x+1, y, z+1.

Experimental details

Crystal data
Chemical formula[K4Cu2(NCS)6(C16H24O6)4]
Mr1881.36
Crystal system, space groupTriclinic, P1
Temperature (K)273
a, b, c (Å)9.702 (3), 13.119 (4), 17.968 (6)
α, β, γ (°)91.015 (6), 97.167 (6), 105.558 (6)
V3)2182.9 (12)
Z1
Radiation typeMo Kα
µ (mm1)0.89
Crystal size (mm)0.49 × 0.21 × 0.16
Data collection
DiffractometerBruker SMART CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.669, 0.870
No. of measured, independent and
observed [I > 2σ(I)] reflections
11606, 7633, 2441
Rint0.077
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.062, 0.160, 0.85
No. of reflections7633
No. of parameters505
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.41, 0.34

Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1997), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected geometric parameters (Å, º) top
Cu1—N11.873 (8)K1—O4i2.903 (5)
Cu1—N21.910 (7)K1—S13.317 (3)
Cu1—N31.915 (7)K2—O122.729 (5)
K1—O52.683 (5)K2—O112.730 (5)
K1—O22.718 (5)K2—O92.765 (5)
K1—O12.727 (5)K2—O82.773 (5)
K1—O32.756 (5)K2—O102.797 (5)
K1—O62.761 (5)K2—O72.819 (5)
K1—O42.875 (5)K2—S23.198 (3)
N1—Cu1—N2121.2 (3)N2—Cu1—N3117.1 (3)
N1—Cu1—N3121.5 (3)
Symmetry code: (i) x+1, y, z+1.
 

Acknowledgements

The authors acknowledge the support of the National Natural Science Foundation of Liaocheng University (No. X051040).

References

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First citationDesai, S. B., Desai, P. B. & Desai, K. R. (2001). Heterocycl. Commun. 1, 83–90.  Google Scholar
First citationRusanova, J. A., Domasevitch, K. V., Vassilyeva, O. Yu., Kokozay, V. N. & Rusanov, E. B. (2000). J. Chem. Soc. Dalton Trans. pp. 2175–2182.  Web of Science CSD CrossRef Google Scholar
First citationSheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationWang, M., Zheng, P.-J., Zhang, J.-Z., Chen, Z., Shen, J.-M. & Yang, Y.-H. (1987). Acta Cryst. C43, 1544–1546.  CSD CrossRef CAS Web of Science IUCr Journals Google Scholar

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