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The novel PtII–dibenzo-18-crown-6 (DB18C6) title complex, μ-[tetrakis­(thio­cyanato-S)­platinum(II)]-N:N′-bis{[2,5,8,­15,18,21-hexa­oxa­tri­cyclo­[20.4.0.19,14]­hexa­cosa-1(22),9(14),10,12,23,25-hexaene-κ6O]­potassium(I)}, [K(C20H24O6)]2[Pt(SCN)4], has been isolated and characterized by X-ray diffraction analysis. The structure analysis shows that the complex displays a quasi-one-dimensional infinite chain of two [K(DB18C6)]+ complex cations and a [Pt(SCN)4]2− anion, bridged by K+...π interactions between adjacent [K(DB18C6)]+ units.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S010827010000929X/oa1101sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010827010000929X/oa1101Isup2.hkl
Contains datablock I

CCDC reference: 152589

Comment top

In 1981, Sunner showed for the first time that K+ binds to benzene in the gas phase (Sunner et al., 1981). The cation–π interaction has become a major goal in physical organic chemistry (Ma et al., 1997). The potential for such an interaction has always been evident from an electrostatic analysis of benzene. Some X-ray single-crystal diffraction analyses of this kind of compound also demonstrated the K+···π interaction, for example, K+–benzene or –phenyl (Eaborn et al., 1995), K+–phospholide anions (Paul et al., 1996), K+–boratabenzene (Hoic et al., 1997) and K+–calixarenes (Beer et al., 1994). We have also synthesized and characterized a series metal complexes with macrocyclic ligands (Wang et al., 1987, 1991). We report here the synthesis and crystal structure of the novel complex of DB18C6 with K2[Pt(SCN)4], namely [2,5,8,15,18,21-hexaoxatricyclo[20.4.0.19,14]hexacosa- 1(22)9(14),10,12,23,25-hexadiene-κ6O]potassium(I) tetrakis(thiocyanato-S)platinum(II), (I), which has cation–π interactions.

The title compound consists of two [K(DB18C6)]+ complex cations and a [Pt(SCN)4]2− complex anion. The Pt atom lies on a crystallographic center of symmetry and is coordinated by four S atoms from four SCN groups to form the regular square-planar complex anion [Pt(SCN)4]2−. The coordination environment of the K+ cation is, however, very unusual. The K+ ion is anchored in the crown-ether cavity forming the K(C12H24O6)+ complex cation (Beer et al., 1994). The principal interactions of the K+ cation involve the six O atoms of the crown [K1—O bond lengths vary from 2.716 (3) to 2.795 (3) Å] and one N atom from the SCN group at the distance of 2.792 (5) Å. The reminder of its coordinating sphere is made up of close K···C contacts with the phenyl ring of the DB18-crown-6 in another molecule, thus forming a K···C-bridged quasi-one-dimensional infinite chain. The K1···C172 and K1···C173 distances of 3.288 (6) and 3.279 (6) Å, respectively, are similar to those in other quasi-one-dimensional infinite-chain structures, such as K[Nd(O-2,6-iPr2—C6H3)4] (3.30 Å; Wang et al., 1987) and KBPh4 (3.29 Å; Clack et al., 1992).

In the crown-ether ring, the average C—C and C—O bond distances are 1.432 and 1.426 Å, and the average O—-C–C and C—O—C angles are 109.3 and 111.2%, respectively. These values are similar to those reported elsewhere (Wang et al., 1987, 1991).

Experimental top

[K(DB18C6)]2[Pt(SCN)4] was prepared by adding an aqueous mixture of K2PtCl4 (0.025 mol l−1, 10 ml) and KSCN (2 mol l−1, 10 ml) to dibenzo-18-crown-6 (0.1 mol l−1, 10 ml) in 1,2-dichloroethane. The reaction mixture was stirred for 2 h at room temperature and then filtered. The single-crystal used for analysis was obtained from a 4:1 diethyl ether/acetone solution.

Refinement top

The H atoms of the phenyl and CH2 groups were included in riding positions, with C—H = 0.93 and 0.97 Å, and U(H) = 1.2Ueq(C).

Computing details top

Data collection: CAD-4 Manual (Enraf-Nonius, 1988); cell refinement: CAD-4 Manual; data reduction: SDP-Plus (Frenz, 1985); program(s) used to solve structure: DIRDIF96 (Beurskens et al., 1996); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1996); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The structure of (I) showing 30% probability displacement ellipsoids.
[Figure 2] Fig. 2. The packing of (I) showing 30% probability displacement ellipsoids.
[2,5,8,15,18,21-hexaoxatricyclo[20.4.0.19,14]hexacosa- 1(22)9(14),10,12,23,25-hexadiene-κ6O]potassium(I) tetrakis(thiocyanato-S)platinum(II) top
Crystal data top
[K(C20H24O6)]2[Pt(SCN)4]Z = 1
Mr = 1226.40F(000) = 616
Triclinic, P1Dx = 1.627 Mg m3
a = 8.553 (5) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.127 (3) ÅCell parameters from 25 reflections
c = 11.819 (3) Åθ = 11.1–14.4°
α = 106.21 (2)°µ = 3.20 mm1
β = 82.77 (3)°T = 293 K
γ = 99.72 (3)°Prism, orange
V = 1251.6 (8) Å30.30 × 0.25 × 0.25 mm
Data collection top
Enraf-Nonius CAD-4
diffractometer
4124 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.014
Graphite monochromatorθmax = 25.2°, θmin = 1.6°
ω/2θ scansh = 1010
Absorption correction: ψ scan
(North et al., 1968)
k = 015
Tmin = 0.400, Tmax = 0.449l = 1413
4702 measured reflections3 standard reflections every 200 reflections
4487 independent reflections intensity decay: 3.9%
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)] = 0.025Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.075H-atom parameters constrained
S = 0.91 w = 1/[σ2(Fo2) + (0.0595P)2 + 0.5854P]
where P = (Fo2 + 2Fc2)/3
4487 reflections(Δ/σ)max < 0.001
304 parametersΔρmax = 1.17 e Å3
0 restraintsΔρmin = 0.56 e Å3
Crystal data top
[K(C20H24O6)]2[Pt(SCN)4]γ = 99.72 (3)°
Mr = 1226.40V = 1251.6 (8) Å3
Triclinic, P1Z = 1
a = 8.553 (5) ÅMo Kα radiation
b = 13.127 (3) ŵ = 3.20 mm1
c = 11.819 (3) ÅT = 293 K
α = 106.21 (2)°0.30 × 0.25 × 0.25 mm
β = 82.77 (3)°
Data collection top
Enraf-Nonius CAD-4
diffractometer
4124 reflections with I > 2σ(I)
Absorption correction: ψ scan
(North et al., 1968)
Rint = 0.014
Tmin = 0.400, Tmax = 0.4493 standard reflections every 200 reflections
4702 measured reflections intensity decay: 3.9%
4487 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0250 restraints
wR(F2) = 0.075H-atom parameters constrained
S = 0.91Δρmax = 1.17 e Å3
4487 reflectionsΔρmin = 0.56 e Å3
304 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
Pt10.50000.00000.50000.04409 (9)
S10.4189 (2)0.16702 (10)0.56576 (12)0.0807 (4)
S20.59788 (18)0.02369 (11)0.68162 (10)0.0737 (3)
N10.3798 (7)0.2485 (4)0.3746 (5)0.0974 (15)
N20.6689 (9)0.2439 (4)0.7860 (4)0.119 (2)
C10.3947 (6)0.2095 (4)0.4483 (5)0.0688 (12)
C20.6399 (7)0.1550 (5)0.7407 (4)0.0771 (14)
O10.0744 (4)0.3825 (2)0.3810 (3)0.0646 (7)
O20.1247 (4)0.4522 (2)0.2284 (3)0.0700 (8)
O30.3247 (4)0.3183 (3)0.0689 (3)0.0671 (8)
O40.2723 (4)0.0992 (2)0.0632 (3)0.0629 (7)
O50.0648 (4)0.0274 (2)0.2113 (3)0.0596 (7)
O60.0996 (4)0.1683 (3)0.3897 (2)0.0620 (7)
C110.1234 (6)0.4565 (3)0.3377 (4)0.0657 (11)
C120.0158 (7)0.4952 (3)0.2548 (4)0.0696 (12)
C130.2397 (8)0.4870 (4)0.1428 (5)0.0910 (18)
H13A0.27430.56340.16980.109*
H13B0.19370.47240.06800.109*
C140.3765 (7)0.4270 (4)0.1284 (6)0.0860 (16)
H14A0.46530.45690.08240.103*
H14B0.41070.43140.20500.103*
C150.4496 (5)0.2542 (4)0.0500 (4)0.0714 (12)
H15A0.48410.25470.12530.086*
H15B0.53990.28300.00430.086*
C160.3903 (6)0.1437 (4)0.0143 (4)0.0671 (11)
H16A0.34380.14380.08500.080*
H16B0.47710.10130.03760.080*
C170.2148 (5)0.0079 (4)0.0271 (4)0.0591 (10)
C180.1033 (5)0.0472 (4)0.1077 (4)0.0603 (10)
C190.0457 (6)0.0087 (4)0.2988 (4)0.0675 (12)
H19A0.01460.07160.31290.081*
H19B0.15160.02780.27130.081*
C200.0457 (5)0.0791 (4)0.4098 (4)0.0641 (11)
H20A0.11500.05480.47150.077*
H20B0.06100.09960.43570.077*
C210.1061 (6)0.2558 (4)0.4935 (4)0.0720 (12)
H21A0.00040.28450.51730.086*
H21B0.16850.23150.55780.086*
C220.1804 (6)0.3401 (4)0.4668 (4)0.0713 (12)
H22A0.28260.30990.43540.086*
H22B0.19730.39670.53820.086*
C1120.2691 (7)0.4943 (4)0.3701 (6)0.0850 (15)
H1120.34150.46980.42560.102*
C1130.3046 (8)0.5701 (4)0.3175 (7)0.102 (2)
H1130.40260.59510.33710.122*
C1150.0544 (9)0.5713 (4)0.2069 (6)0.0921 (18)
H1150.01800.59800.15300.111*
C1140.1978 (10)0.6076 (5)0.2380 (7)0.107 (2)
H1140.22300.65850.20470.128*
C1710.2604 (6)0.0755 (4)0.0787 (4)0.0748 (13)
H1710.33270.04950.13320.090*
C1720.1977 (8)0.1833 (5)0.1036 (6)0.0893 (18)
H1720.22940.22950.17500.107*
C1730.0918 (8)0.2222 (5)0.0262 (6)0.0886 (17)
H1730.05240.29490.04380.106*
C1740.0412 (7)0.1536 (4)0.0802 (5)0.0793 (14)
H1740.03450.18000.13240.095*
K10.13057 (11)0.24350 (7)0.24062 (8)0.0566 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.04486 (12)0.04380 (12)0.04286 (12)0.00907 (8)0.00311 (7)0.01147 (8)
S10.1152 (11)0.0597 (7)0.0708 (7)0.0390 (7)0.0033 (7)0.0093 (6)
S20.0959 (9)0.0741 (7)0.0535 (6)0.0182 (6)0.0157 (6)0.0129 (5)
N10.112 (4)0.089 (3)0.108 (4)0.010 (3)0.041 (3)0.042 (3)
N20.187 (6)0.076 (3)0.068 (3)0.040 (4)0.013 (3)0.011 (2)
C10.065 (3)0.057 (2)0.087 (3)0.009 (2)0.021 (2)0.017 (2)
C20.091 (3)0.084 (4)0.051 (2)0.007 (3)0.006 (2)0.021 (2)
O10.0611 (17)0.0650 (18)0.0667 (18)0.0116 (14)0.0033 (14)0.0180 (14)
O20.081 (2)0.0556 (17)0.072 (2)0.0080 (15)0.0080 (16)0.0219 (15)
O30.0658 (18)0.0654 (18)0.0654 (18)0.0006 (14)0.0048 (14)0.0191 (15)
O40.0644 (17)0.0676 (18)0.0549 (16)0.0160 (14)0.0085 (13)0.0153 (14)
O50.0659 (17)0.0566 (16)0.0584 (16)0.0051 (13)0.0021 (13)0.0220 (13)
O60.0658 (17)0.0743 (19)0.0511 (15)0.0086 (14)0.0029 (13)0.0268 (14)
C110.074 (3)0.043 (2)0.071 (3)0.0082 (19)0.015 (2)0.0039 (19)
C120.092 (3)0.044 (2)0.065 (3)0.004 (2)0.013 (2)0.0028 (19)
C130.120 (5)0.053 (3)0.095 (4)0.003 (3)0.017 (3)0.032 (3)
C140.075 (3)0.072 (3)0.099 (4)0.015 (3)0.016 (3)0.028 (3)
C150.054 (2)0.090 (3)0.068 (3)0.010 (2)0.009 (2)0.022 (2)
C160.061 (2)0.085 (3)0.056 (2)0.022 (2)0.0076 (19)0.020 (2)
C170.059 (2)0.069 (3)0.056 (2)0.023 (2)0.0147 (19)0.014 (2)
C180.063 (2)0.061 (2)0.065 (3)0.0176 (19)0.023 (2)0.017 (2)
C190.066 (3)0.071 (3)0.076 (3)0.003 (2)0.010 (2)0.042 (2)
C200.061 (2)0.081 (3)0.059 (2)0.000 (2)0.0029 (19)0.039 (2)
C210.076 (3)0.092 (3)0.044 (2)0.004 (3)0.006 (2)0.023 (2)
C220.068 (3)0.082 (3)0.057 (2)0.014 (2)0.012 (2)0.012 (2)
C1120.079 (3)0.065 (3)0.100 (4)0.018 (3)0.008 (3)0.001 (3)
C1130.096 (4)0.055 (3)0.146 (6)0.030 (3)0.035 (4)0.009 (3)
C1150.124 (5)0.046 (3)0.105 (4)0.018 (3)0.018 (4)0.012 (3)
C1140.136 (6)0.060 (3)0.132 (6)0.027 (4)0.036 (5)0.021 (4)
C1710.075 (3)0.092 (4)0.060 (3)0.036 (3)0.016 (2)0.005 (2)
C1720.096 (4)0.089 (4)0.079 (4)0.035 (3)0.034 (3)0.010 (3)
C1730.103 (4)0.066 (3)0.096 (4)0.015 (3)0.050 (4)0.000 (3)
C1740.084 (3)0.068 (3)0.090 (4)0.005 (3)0.035 (3)0.019 (3)
K10.0568 (5)0.0600 (5)0.0571 (5)0.0116 (4)0.0069 (4)0.0251 (4)
Geometric parameters (Å, º) top
Pt1—S1i2.3064 (13)C15—H15A0.9700
Pt1—S12.3064 (13)C15—H15B0.9700
Pt1—S22.3232 (13)C16—H16A0.9700
Pt1—S2i2.3232 (14)C16—H16B0.9700
S1—C11.681 (5)C17—C1711.370 (6)
S2—C21.664 (6)C17—C181.402 (7)
N1—C11.156 (7)C18—C1741.370 (7)
N1—K12.792 (5)C19—C201.485 (7)
N2—C21.139 (7)C19—H19A0.9700
O1—C111.360 (6)C19—H19B0.9700
O1—C221.440 (6)C20—K13.388 (4)
O1—K12.795 (3)C20—H20A0.9700
O2—C121.377 (6)C20—H20B0.9700
O2—C131.433 (6)C21—C221.487 (7)
O2—K12.793 (3)C21—K13.373 (5)
O3—C141.425 (6)C21—H21A0.9700
O3—C151.428 (6)C21—H21B0.9700
O3—K12.749 (3)C22—H22A0.9700
O4—C171.372 (5)C22—H22B0.9700
O4—C161.437 (5)C112—C1131.402 (9)
O4—K12.716 (3)C112—H1120.9300
O5—C181.380 (5)C113—C1141.359 (10)
O5—C191.436 (5)C113—H1130.9300
O5—K12.729 (3)C115—C1141.361 (10)
O6—C201.416 (6)C115—H1150.9300
O6—C211.430 (6)C114—H1140.9300
O6—K12.720 (3)C171—C1721.388 (8)
C11—C1121.388 (7)C171—H1710.9300
C11—C121.399 (7)C172—C1731.347 (9)
C12—C1151.379 (8)C172—K1ii3.288 (6)
C13—C141.484 (9)C172—H1720.9300
C13—H13A0.9700C173—C1741.393 (8)
C13—H13B0.9700C173—K1ii3.279 (6)
C14—K13.370 (5)C173—H1730.9300
C14—H14A0.9700C174—H1740.9300
C14—H14B0.9700K1—C173ii3.279 (6)
C15—C161.473 (7)K1—C172ii3.288 (6)
C15—K13.323 (5)
S1i—Pt1—S1180.0C21—C22—H22A110.1
S1i—Pt1—S290.10 (5)O1—C22—H22B110.1
S1—Pt1—S289.90 (5)C21—C22—H22B110.1
S1i—Pt1—S2i89.90 (5)H22A—C22—H22B108.4
S1—Pt1—S2i90.10 (5)C11—C112—C113118.6 (6)
S2—Pt1—S2i180.0C11—C112—H112120.7
C1—S1—Pt1108.95 (18)C113—C112—H112120.7
C2—S2—Pt1107.31 (19)C114—C113—C112120.9 (6)
C1—N1—K1134.7 (4)C114—C113—H113119.5
N1—C1—S1173.5 (5)C112—C113—H113119.5
N2—C2—S2176.8 (5)C114—C115—C12120.4 (7)
C11—O1—C22118.0 (4)C114—C115—H115119.8
C11—O1—K1120.2 (3)C12—C115—H115119.8
C22—O1—K1115.0 (3)C113—C114—C115120.6 (6)
C12—O2—C13118.1 (4)C113—C114—H114119.7
C12—O2—K1120.0 (3)C115—C114—H114119.7
C13—O2—K1114.7 (3)C17—C171—C172119.3 (6)
C14—O3—C15111.4 (4)C17—C171—H171120.3
C14—O3—K1103.1 (3)C172—C171—H171120.3
C15—O3—K1100.6 (3)C173—C172—C171121.2 (5)
C17—O4—C16118.0 (3)C173—C172—K1ii77.8 (3)
C17—O4—K1124.5 (2)C171—C172—K1ii114.2 (3)
C16—O4—K1115.7 (3)C173—C172—H172119.4
C18—O5—C19118.1 (4)C171—C172—H172119.4
C18—O5—K1123.7 (2)K1ii—C172—H17278.4
C19—O5—K1116.7 (3)C172—C173—C174120.0 (6)
C20—O6—C21112.8 (3)C172—C173—K1ii78.5 (3)
C20—O6—K1105.6 (2)C174—C173—K1ii112.9 (4)
C21—O6—K1104.4 (2)C172—C173—H173120.0
O1—C11—C112124.6 (5)C174—C173—H173120.0
O1—C11—C12115.7 (4)K1ii—C173—H17379.1
C112—C11—C12119.7 (5)C18—C174—C173120.0 (6)
O2—C12—C115125.1 (5)C18—C174—H174120.0
O2—C12—C11115.0 (4)C173—C174—H174120.0
C115—C12—C11119.9 (5)O4—K1—O6118.27 (10)
O2—C13—C14107.4 (4)O4—K1—O556.68 (9)
O2—C13—H13A110.2O6—K1—O561.67 (10)
C14—C13—H13A110.2O4—K1—O362.10 (10)
O2—C13—H13B110.2O6—K1—O3170.96 (10)
C14—C13—H13B110.2O5—K1—O3118.43 (10)
H13A—C13—H13B108.5O4—K1—N187.26 (15)
O3—C14—C13107.4 (5)O6—K1—N194.61 (14)
O3—C14—K152.6 (2)O5—K1—N188.88 (13)
C13—C14—K188.0 (3)O3—K1—N194.43 (15)
O3—C14—H14A110.2O4—K1—O2121.89 (10)
C13—C14—H14A110.2O6—K1—O2115.92 (10)
K1—C14—H14A159.2O5—K1—O2163.19 (10)
O3—C14—H14B110.2O3—K1—O261.05 (10)
C13—C14—H14B110.2N1—K1—O2107.91 (13)
K1—C14—H14B72.5O4—K1—O1165.05 (10)
H14A—C14—H14B108.5O6—K1—O161.33 (10)
O3—C15—C16108.9 (4)O5—K1—O1121.47 (10)
O3—C15—K154.4 (2)O3—K1—O1115.70 (10)
C16—C15—K187.7 (3)N1—K1—O1107.67 (15)
O3—C15—H15A109.9O2—K1—O154.79 (9)
C16—C15—H15A109.9O4—K1—C173ii79.66 (14)
K1—C15—H15A71.6O6—K1—C173ii97.79 (16)
O3—C15—H15B109.9O5—K1—C173ii89.81 (12)
C16—C15—H15B109.9O3—K1—C173ii73.25 (16)
K1—C15—H15B160.5N1—K1—C173ii165.13 (19)
H15A—C15—H15B108.3O2—K1—C173ii73.82 (13)
O4—C16—C15107.9 (4)O1—K1—C173ii85.57 (14)
O4—C16—H16A110.1O4—K1—C172ii90.46 (13)
C15—C16—H16A110.1O6—K1—C172ii74.13 (16)
O4—C16—H16B110.1O5—K1—C172ii78.17 (14)
C15—C16—H16B110.1O3—K1—C172ii96.91 (16)
H16A—C16—H16B108.4N1—K1—C172ii165.76 (17)
C171—C17—O4124.6 (5)O2—K1—C172ii85.18 (14)
C171—C17—C18120.0 (5)O1—K1—C172ii74.94 (13)
O4—C17—C18115.3 (4)C173ii—K1—C172ii23.67 (16)
C174—C18—O5124.9 (5)O4—K1—C1544.48 (11)
C174—C18—C17119.5 (5)O6—K1—C15160.26 (12)
O5—C18—C17115.6 (4)O5—K1—C1599.93 (12)
O5—C19—C20108.6 (4)O3—K1—C1524.98 (12)
O5—C19—H19A110.0N1—K1—C1576.95 (16)
C20—C19—H19A110.0O2—K1—C1583.78 (12)
O5—C19—H19B110.0O1—K1—C15138.11 (12)
C20—C19—H19B110.0C173ii—K1—C1588.70 (17)
H19A—C19—H19B108.4C172ii—K1—C15110.83 (16)
O6—C20—C19109.4 (3)O4—K1—C1484.36 (12)
O6—C20—K150.62 (18)O6—K1—C14157.37 (12)
C19—C20—K186.3 (2)O5—K1—C14140.91 (12)
O6—C20—H20A109.8O3—K1—C1424.32 (12)
C19—C20—H20A109.8N1—K1—C1485.90 (17)
K1—C20—H20A159.1O2—K1—C1443.60 (13)
O6—C20—H20B109.8O1—K1—C1496.92 (13)
C19—C20—H20B109.8C173ii—K1—C1485.80 (18)
K1—C20—H20B77.0C172ii—K1—C14107.87 (18)
H20A—C20—H20B108.2C15—K1—C1441.23 (13)
O6—C21—C22108.6 (4)O4—K1—C21140.27 (12)
O6—C21—K151.36 (19)O6—K1—C2124.25 (11)
C22—C21—K188.3 (2)O5—K1—C2184.07 (11)
O6—C21—H21A110.0O3—K1—C21157.50 (12)
C22—C21—H21A110.0N1—K1—C2185.96 (16)
K1—C21—H21A74.1O2—K1—C2197.39 (12)
O6—C21—H21B110.0O1—K1—C2143.89 (12)
C22—C21—H21B110.0C173ii—K1—C21108.63 (17)
K1—C21—H21B158.5C172ii—K1—C2186.84 (16)
H21A—C21—H21B108.3C15—K1—C21162.31 (13)
O1—C22—C21107.9 (4)C14—K1—C21133.95 (14)
O1—C22—H22A110.1
S1i—Pt1—S1—C117 (100)C19—O5—K1—C14171.8 (3)
S2—Pt1—S1—C1159.79 (19)C18—O5—K1—C21169.5 (3)
S2i—Pt1—S1—C120.21 (19)C19—O5—K1—C213.7 (3)
S1i—Pt1—S2—C2154.7 (2)C14—O3—K1—O4154.3 (3)
S1—Pt1—S2—C225.3 (2)C15—O3—K1—O439.2 (3)
S2i—Pt1—S2—C2130 (100)C14—O3—K1—O6110.9 (7)
K1—N1—C1—S1114 (4)C15—O3—K1—O6133.9 (6)
Pt1—S1—C1—N1158 (4)C14—O3—K1—O5160.9 (3)
Pt1—S2—C2—N2164 (12)C15—O3—K1—O545.8 (3)
C22—O1—C11—C1120.1 (6)C14—O3—K1—N169.8 (3)
K1—O1—C11—C112149.5 (4)C15—O3—K1—N145.4 (3)
C22—O1—C11—C12179.9 (4)C14—O3—K1—O238.3 (3)
K1—O1—C11—C1230.5 (5)C15—O3—K1—O2153.4 (3)
C13—O2—C12—C1151.3 (7)C14—O3—K1—O142.3 (3)
K1—O2—C12—C115150.4 (4)C15—O3—K1—O1157.4 (3)
C13—O2—C12—C11179.1 (4)C14—O3—K1—C173ii118.7 (3)
K1—O2—C12—C1130.1 (5)C15—O3—K1—C173ii126.2 (3)
O1—C11—C12—O20.3 (6)C14—O3—K1—C172ii118.8 (3)
C112—C11—C12—O2179.7 (4)C15—O3—K1—C172ii126.0 (3)
O1—C11—C12—C115179.3 (4)C14—O3—K1—C15115.1 (4)
C112—C11—C12—C1150.7 (7)C15—O3—K1—C14115.1 (4)
C12—O2—C13—C14178.5 (4)C14—O3—K1—C2120.4 (5)
K1—O2—C13—C1427.8 (6)C15—O3—K1—C21135.5 (4)
C15—O3—C14—C13179.5 (4)C1—N1—K1—O4100.4 (7)
K1—O3—C14—C1373.4 (4)C1—N1—K1—O617.7 (7)
C15—O3—C14—K1107.1 (4)C1—N1—K1—O543.7 (7)
O2—C13—C14—O370.2 (6)C1—N1—K1—O3162.1 (6)
O2—C13—C14—K120.6 (4)C1—N1—K1—O2136.9 (6)
C14—O3—C15—C16178.6 (4)C1—N1—K1—O179.1 (7)
K1—O3—C15—C1672.7 (4)C1—N1—K1—C173ii128.7 (7)
C14—O3—C15—K1108.7 (4)C1—N1—K1—C172ii19.4 (12)
C17—O4—C16—C15172.0 (4)C1—N1—K1—C15144.2 (7)
K1—O4—C16—C1522.9 (5)C1—N1—K1—C14175.1 (7)
O3—C15—C16—O467.6 (5)C1—N1—K1—C2140.4 (7)
K1—C15—C16—O416.7 (3)C12—O2—K1—O4131.8 (3)
C16—O4—C17—C1710.9 (6)C13—O2—K1—O418.3 (4)
K1—O4—C17—C171162.8 (3)C12—O2—K1—O625.5 (3)
C16—O4—C17—C18178.4 (4)C13—O2—K1—O6175.6 (4)
K1—O4—C17—C1817.9 (5)C12—O2—K1—O552.0 (5)
C19—O5—C18—C1741.5 (6)C13—O2—K1—O598.0 (5)
K1—O5—C18—C174164.1 (3)C12—O2—K1—O3144.9 (3)
C19—O5—C18—C17178.4 (4)C13—O2—K1—O35.2 (4)
K1—O5—C18—C1716.0 (5)C12—O2—K1—N1130.1 (3)
C171—C17—C18—C1740.4 (6)C13—O2—K1—N179.9 (4)
O4—C17—C18—C174178.9 (4)C12—O2—K1—O130.7 (3)
C171—C17—C18—O5179.7 (4)C13—O2—K1—O1179.2 (4)
O4—C17—C18—O51.0 (5)C12—O2—K1—C173ii65.4 (3)
C18—O5—C19—C20169.5 (3)C13—O2—K1—C173ii84.7 (4)
K1—O5—C19—C2023.9 (4)C12—O2—K1—C172ii44.2 (3)
C21—O6—C20—C19178.8 (4)C13—O2—K1—C172ii105.8 (4)
K1—O6—C20—C1967.8 (4)C12—O2—K1—C15155.8 (3)
C21—O6—C20—K1113.4 (4)C13—O2—K1—C155.8 (4)
O5—C19—C20—O662.8 (5)C12—O2—K1—C14166.6 (4)
O5—C19—C20—K117.0 (3)C13—O2—K1—C1416.5 (4)
C20—O6—C21—C22173.9 (3)C12—O2—K1—C2141.9 (3)
K1—O6—C21—C2271.9 (4)C13—O2—K1—C21168.0 (4)
C20—O6—C21—K1114.2 (3)C11—O1—K1—O451.1 (5)
C11—O1—C22—C21175.9 (4)C22—O1—K1—O499.4 (5)
K1—O1—C22—C2124.7 (5)C11—O1—K1—O6143.6 (3)
O6—C21—C22—O166.3 (5)C22—O1—K1—O66.8 (3)
K1—C21—C22—O118.3 (3)C11—O1—K1—O5129.3 (3)
O1—C11—C112—C113179.4 (5)C22—O1—K1—O521.2 (3)
C12—C11—C112—C1130.5 (7)C11—O1—K1—O326.7 (3)
C11—C112—C113—C1141.3 (9)C22—O1—K1—O3177.2 (3)
O2—C12—C115—C114179.2 (5)C11—O1—K1—N1130.8 (3)
C11—C12—C115—C1141.3 (8)C22—O1—K1—N178.7 (3)
C112—C113—C114—C1150.7 (10)C11—O1—K1—O231.0 (3)
C12—C115—C114—C1130.5 (10)C22—O1—K1—O2178.5 (3)
O4—C17—C171—C172177.8 (4)C11—O1—K1—C173ii42.3 (3)
C18—C17—C171—C1721.4 (6)C22—O1—K1—C173ii108.2 (3)
C17—C171—C172—C1730.6 (8)C11—O1—K1—C172ii63.8 (3)
C17—C171—C172—K1ii90.7 (5)C22—O1—K1—C172ii86.7 (3)
C171—C172—C173—C1741.1 (8)C11—O1—K1—C1540.8 (4)
K1ii—C172—C173—C174109.9 (5)C22—O1—K1—C15168.7 (3)
C171—C172—C173—K1ii111.0 (5)C11—O1—K1—C1442.9 (3)
O5—C18—C174—C173178.5 (4)C22—O1—K1—C14166.6 (3)
C17—C18—C174—C1731.4 (7)C11—O1—K1—C21165.1 (4)
C172—C173—C174—C182.1 (8)C22—O1—K1—C2114.7 (3)
K1ii—C173—C174—C1891.8 (5)O3—C15—K1—O4127.2 (3)
C17—O4—K1—O614.5 (3)C16—C15—K1—O411.9 (2)
C16—O4—K1—O6178.6 (3)O3—C15—K1—O6160.4 (3)
C17—O4—K1—O517.8 (3)C16—C15—K1—O645.1 (5)
C16—O4—K1—O5178.1 (3)O3—C15—K1—O5140.2 (3)
C17—O4—K1—O3155.2 (3)C16—C15—K1—O524.9 (3)
C16—O4—K1—O38.8 (3)C16—C15—K1—O3115.3 (4)
C17—O4—K1—N1108.3 (3)O3—C15—K1—N1133.3 (3)
C16—O4—K1—N187.6 (3)C16—C15—K1—N1111.4 (3)
C17—O4—K1—O2142.2 (3)O3—C15—K1—O223.2 (3)
C16—O4—K1—O221.8 (3)C16—C15—K1—O2138.5 (3)
C17—O4—K1—O169.9 (5)O3—C15—K1—O131.2 (3)
C16—O4—K1—O194.2 (5)C16—C15—K1—O1146.5 (3)
C17—O4—K1—C173ii78.8 (3)O3—C15—K1—C173ii50.7 (3)
C16—O4—K1—C173ii85.3 (3)C16—C15—K1—C173ii64.6 (3)
C17—O4—K1—C172ii57.6 (3)O3—C15—K1—C172ii59.2 (3)
C16—O4—K1—C172ii106.4 (3)C16—C15—K1—C172ii56.1 (3)
C17—O4—K1—C15177.6 (4)O3—C15—K1—C1434.5 (3)
C16—O4—K1—C1513.5 (3)C16—C15—K1—C14149.7 (4)
C17—O4—K1—C14165.6 (3)O3—C15—K1—C21118.0 (4)
C16—O4—K1—C141.5 (3)C16—C15—K1—C21126.7 (4)
C17—O4—K1—C2128.0 (4)O3—C14—K1—O422.6 (3)
C16—O4—K1—C21168.0 (3)C13—C14—K1—O4136.4 (4)
C20—O6—K1—O439.6 (3)O3—C14—K1—O6157.6 (3)
C21—O6—K1—O4158.8 (3)C13—C14—K1—O643.8 (6)
C20—O6—K1—O536.5 (2)O3—C14—K1—O527.1 (4)
C21—O6—K1—O5155.7 (3)C13—C14—K1—O5140.9 (3)
C20—O6—K1—O3129.6 (6)C13—C14—K1—O3113.8 (5)
C21—O6—K1—O3111.3 (7)O3—C14—K1—N1110.3 (3)
C20—O6—K1—N149.7 (3)C13—C14—K1—N1136.0 (4)
C21—O6—K1—N169.4 (3)O3—C14—K1—O2128.2 (4)
C20—O6—K1—O2162.2 (2)C13—C14—K1—O214.5 (3)
C21—O6—K1—O243.0 (3)O3—C14—K1—O1142.4 (3)
C20—O6—K1—O1157.4 (3)C13—C14—K1—O128.6 (4)
C21—O6—K1—O138.2 (3)O3—C14—K1—C173ii57.4 (3)
C20—O6—K1—C173ii122.1 (3)C13—C14—K1—C173ii56.4 (4)
C21—O6—K1—C173ii118.8 (3)O3—C14—K1—C172ii66.0 (3)
C20—O6—K1—C172ii121.4 (3)C13—C14—K1—C172ii47.7 (4)
C21—O6—K1—C172ii119.4 (3)O3—C14—K1—C1535.5 (3)
C20—O6—K1—C1513.8 (5)C13—C14—K1—C15149.2 (5)
C21—O6—K1—C15133.0 (4)O3—C14—K1—C21169.3 (3)
C20—O6—K1—C14140.1 (4)C13—C14—K1—C2155.6 (4)
C21—O6—K1—C1420.9 (5)O6—C21—K1—O429.9 (4)
C20—O6—K1—C21119.2 (4)C22—C21—K1—O4145.5 (3)
C18—O5—K1—O417.0 (3)C22—C21—K1—O6115.7 (4)
C19—O5—K1—O4177.2 (3)O6—C21—K1—O521.4 (3)
C18—O5—K1—O6159.7 (3)C22—C21—K1—O5137.1 (3)
C19—O5—K1—O66.1 (3)O6—C21—K1—O3157.5 (3)
C18—O5—K1—O310.1 (3)C22—C21—K1—O341.8 (5)
C19—O5—K1—O3175.8 (3)O6—C21—K1—N1110.7 (3)
C18—O5—K1—N1104.5 (3)C22—C21—K1—N1133.7 (3)
C19—O5—K1—N189.7 (3)O6—C21—K1—O2141.8 (3)
C18—O5—K1—O273.5 (5)C22—C21—K1—O226.1 (3)
C19—O5—K1—O292.3 (4)O6—C21—K1—O1128.5 (3)
C18—O5—K1—O1145.4 (3)C22—C21—K1—O112.8 (3)
C19—O5—K1—O120.4 (3)O6—C21—K1—C173ii66.4 (3)
C18—O5—K1—C173ii60.7 (3)C22—C21—K1—C173ii49.3 (3)
C19—O5—K1—C173ii105.1 (3)O6—C21—K1—C172ii57.0 (3)
C18—O5—K1—C172ii81.5 (3)C22—C21—K1—C172ii58.6 (3)
C19—O5—K1—C172ii84.3 (3)O6—C21—K1—C15125.5 (4)
C18—O5—K1—C1527.9 (3)C22—C21—K1—C15118.8 (5)
C19—O5—K1—C15166.3 (3)O6—C21—K1—C14169.0 (3)
C18—O5—K1—C1422.4 (4)C22—C21—K1—C1453.3 (4)
Symmetry codes: (i) x+1, y, z+1; (ii) x, y, z.

Experimental details

Crystal data
Chemical formula[K(C20H24O6)]2[Pt(SCN)4]
Mr1226.40
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)8.553 (5), 13.127 (3), 11.819 (3)
α, β, γ (°)106.21 (2), 82.77 (3), 99.72 (3)
V3)1251.6 (8)
Z1
Radiation typeMo Kα
µ (mm1)3.20
Crystal size (mm)0.30 × 0.25 × 0.25
Data collection
DiffractometerEnraf-Nonius CAD-4
diffractometer
Absorption correctionψ scan
(North et al., 1968)
Tmin, Tmax0.400, 0.449
No. of measured, independent and
observed [I > 2σ(I)] reflections
4702, 4487, 4124
Rint0.014
(sin θ/λ)max1)0.598
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.025, 0.075, 0.91
No. of reflections4487
No. of parameters304
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.17, 0.56

Computer programs: CAD-4 Manual (Enraf-Nonius, 1988), CAD-4 Manual, SDP-Plus (Frenz, 1985), DIRDIF96 (Beurskens et al., 1996), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1996), SHELXL97.

Selected geometric parameters (Å, º) top
Pt1—S12.3064 (13)O4—C161.437 (5)
Pt1—S22.3232 (13)O4—K12.716 (3)
N1—K12.792 (5)O5—C181.380 (5)
O1—C111.360 (6)O5—C191.436 (5)
O1—C221.440 (6)O5—K12.729 (3)
O1—K12.795 (3)O6—C201.416 (6)
O2—C121.377 (6)O6—C211.430 (6)
O2—C131.433 (6)O6—K12.720 (3)
O2—K12.793 (3)C172—K1i3.288 (6)
O3—C141.425 (6)C173—K1i3.279 (6)
O3—C151.428 (6)K1—C173i3.279 (6)
O3—K12.749 (3)K1—C172i3.288 (6)
O4—C171.372 (5)
S1ii—Pt1—S1180.0O6—K1—O2115.92 (10)
S1ii—Pt1—S290.10 (5)O5—K1—O2163.19 (10)
O4—K1—O6118.27 (10)O3—K1—O261.05 (10)
O4—K1—O556.68 (9)O4—K1—O1165.05 (10)
O6—K1—O561.67 (10)O6—K1—O161.33 (10)
O4—K1—O362.10 (10)O5—K1—O1121.47 (10)
O6—K1—O3170.96 (10)O3—K1—O1115.70 (10)
O5—K1—O3118.43 (10)O2—K1—O154.79 (9)
O4—K1—O2121.89 (10)C173i—K1—C172i23.67 (16)
S2—Pt1—S1—C1159.79 (19)
Symmetry codes: (i) x, y, z; (ii) x+1, y, z+1.
 

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