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In the title compound, K[Ni(C3S5)2]·C20H24O6·C3H6O, K+ is incorporated in the cavity of the 1,4,7,10,13,16-hexaoxa­-2,3:11,12-dibenzocyclo­octadeca-2,11-diene (DB18c6) mol­ecule and is coordinated by the six DB18c6 O atoms and the propanone O atom. Two {K+(DB18c6)[(CH3)2CO]} units form a dimer which is aligned in a one-dimensional manner along the a axis through a face-to-face interaction between the benzene rings of neighboring DB18c6 mol­ecules. [Ni(dmit)2] anions are also aligned along the a axis through side-by-side S...S interactions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101013713/oa1119sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270101013713/oa1119Isup2.hkl
Contains datablock I

CCDC reference: 175068

Comment top

[Ni(dmit)2]- is a planar π-conjugated anion and has an open-shell electronic structure with S = 1/2 spin. [Ni(dmit)2]- salts with various counter-cations have been reported and some possess interesting magnetic properties, such as spin-ladder properties (Imai et al., 1999). Counter-cations for [Ni(dmit)2]- salts are necessary to neutralize the total charge in the crystal and affect the whole crystal structure. We have introduced supramolecular cation (SC+) structures composed of metal cations and crown ethers as the counter-cation for [Ni(dmit)2]- in order to control the spin arrangements of [Ni(dmit)2]-. In the crystal, SC+ showed a variety of structures, such as the typical disc-shaped structure, in which K+ is completely included at the center of the crown-ether cavity, and the sandwich-type Ca2+(15-crown-5)2, in which Ca2+ is located at the midpoint between two crown ether molecules (Takamatsu et al., 2000; Akutagawa et al., 2001).

2,3:11,12-Dibenzo-1,4,7,10,13,16-hexaoxocyclooctadeca-2,11-diene (DB18c6) is a typical crown ether having two phenyl rings. A novel SC+ assembly through ππ interaction is expected within the [Ni(dmit)2]- crystal using DB18c6 as a building block for the SC+ structure. In the present study, we report the crystal structure of K[Ni(dmit)2](DB18c6)·(CH3)2CO, (I), in which DB18c6 forms a one-dimensional array through ππ interactions of the dibenzo moieties.

Fig. 1 represents an ORTEPIII (Burnett & Johnson, 1996) view of salt (I). The six O atoms of the DB18c6 unit are coplanar, as reported in literature (Bright & Truter, 1970), and K+ is incorporated at the center of the DB18c6 cavity. The six K—O distances are in the range 2.691 (3)–2.794 (3) Å. In addition, the propanone O atom is coordinated to K+ with a K—O distance of 2.611 (4) %A. The DB18c6 molecule has a V-shaped conformation, with a dihedral angle of 100.46° between the two benzene rings. One propanone molecule is enclosed by the V-shaped DB18c6 molecule and is fixed by a short K—O coordination.

The [Ni(dmit)2]- complex anion is planar in the crystal, as is usually reported (Pullen & Olk, 1999). The maximum deviation from the least-squares plane of [Ni(dmit)2]- is 0.105 Å for S7. Within the crystal, [Ni(dmit)2]- anions are arranged along the a axis and the direction of the molecular long axis alternately turns toward [012] and [012], as shown in Fig. 2. The angles between the long axes of adjacent [Ni(dmit)2]- anions are 57.26 and 57.48°. Short S···S contact distances observed in the side-by-side S···S interactions between neighboring molecules are nearly equal to or less than the van der Waals S···S contact distance of 3.60 Å (Bondi, 1964). S···S contacts less than 3.70 Å are summarized in Table 1. The side-by-side S···S contacts arrange the [Ni(dmit)2]- anions in a one-dimensional manner.

As shown in Fig. 3, SC+ is aligned along the a axis, forming a one-dimensional structure. Two {K+(DB18c6)[(CH3)2CO]} units form a dimer related by C2 symmetry, which is a repeating unit. In the dimer, the molecular planes of the propanone molecule are parallel and the directions of the CO bonds are opposite to each other. Intermolecular distances between carbonyl groups are 3.276 (9) (C27···C27) and 3.385 (6) Å (C27···O7), and these distances are close to the van der Waals C···O contact distance of 3.22 Å (Bondi, 1964). Since the propanone molecule has a strong dipole moment (2.88 D), dipole–dipole interactions between the carbonyl groups can contribute to the formation of the dimer structure.

The benzene rings of neighboring DB18c6 molecules have a face-to-face orientation and the mean interplanar distance between them is 3.421 Å, which is nearly equal to the van der Waals contacts of aromatic hydrocarbons, ca 3.4 Å. Selected intermolecular distances less than 3.6 Å between two benzene rings are summarized in Table 1. A one-dimensional supramolecular array of (pyridinium)+(DB18c6)BF4- has been reported in which pyridinium and the V-shaped DB18c6 molecule stack alternately to form a one-dimensional column by utilizing intermolecular face-to-face ππ interactions and hydrogen bonding between the host and guest molecules (Lämsä et al., 1998; Talanova et al., 1999). In the present case, intermolecular ππ interactions between the benzene rings of host molecules form a one-dimensional [K+(DB18c6)(CH3)2CO]2 dimer array.

Related literature top

For related literature, see: Akutagawa et al. (2001); Bondi (1964); Bright & Truter (1970); Burnett & Johnson (1996); Imai et al. (1999); Lämsä et al. (1998); Pullen & Olk (1999); Takamatsu et al. (2000); Talanova et al. (1999).

Experimental top

The title crystal was prepared by slow evaporation of an propanone solution of (nBu4N)[Ni(dmit)2], DB18c6 and KClO4. Shiny black plate-like crystals were obtained.

Refinement top

The molecule of (I) crystallized in the monoclinic system; space group C2/c was assumed from the systematic absences. The propanone methyl groups undergo motion or are slightly disordered. [Please provide some information on how the H atoms were treated in the refinement, including the range of constrained C—H distances]

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: TEXSAN (Molecular Structure Corporation and Rigaku, 1999); molecular graphics: ORTEPIII (Burnett & Johnson, 1996).

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), with displacement ellipsoids at the 50% probablity level and H atoms omitted for clarify.
[Figure 2] Fig. 2. Packing diagram of (I) viewed along the a axis. The directions of [Ni(dmit)2]- are almost [012] and [012].
[Figure 3] Fig. 3. SC+ arrangements viewed along the b axis. The dimer is aligned along the a axis.
Potassium bis(4,5-dimercapto-1,3-dithiole-2-thionato)nickelate 2,3:11,12-dibenzo-1,4,7,10,13,16-hexaoxocyclooctadeca-2,11-diene propanone solvate top
Crystal data top
K[Ni(C3S5)2](C20H24O6)·C3H6OF(000) = 3736.00
Mr = 908.95Dx = 1.575 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.7107 Å
a = 12.8232 (5) ÅCell parameters from 18032 reflections
b = 22.4666 (8) Åθ = 2.4–27.5°
c = 26.612 (1) ŵ = 1.20 mm1
β = 90.201 (2)°T = 296 K
V = 7666.6 (5) Å3Plate, black
Z = 80.35 × 0.35 × 0.10 mm
Data collection top
Rigaku RAXIS-RAPID Imaging Plate
diffractometer
8776 independent reflections
Radiation source: X-ray tube4422 reflections with F2 > 2σ(F2)
Graphite monochromatorRint = 0.050
ω scansθmax = 27.5°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 016
Tmin = 0.699, Tmax = 0.887k = 029
36400 measured reflectionsl = 3434
Refinement top
Refinement on F2H-atom parameters not refined
R[F2 > 2σ(F2)] = 0.035 w = 1/[σ2(Fo2) + {0.05[Max(Fo2,0) + 2Fc2]/3}2]
wR(F2) = 0.088(Δ/σ)max = 0.0004
S = 1.05Δρmax = 0.32 e Å3
4422 reflectionsΔρmin = 0.24 e Å3
433 parameters
Crystal data top
K[Ni(C3S5)2](C20H24O6)·C3H6OV = 7666.6 (5) Å3
Mr = 908.95Z = 8
Monoclinic, C2/cMo Kα radiation
a = 12.8232 (5) ŵ = 1.20 mm1
b = 22.4666 (8) ÅT = 296 K
c = 26.612 (1) Å0.35 × 0.35 × 0.10 mm
β = 90.201 (2)°
Data collection top
Rigaku RAXIS-RAPID Imaging Plate
diffractometer
8776 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
4422 reflections with F2 > 2σ(F2)
Tmin = 0.699, Tmax = 0.887Rint = 0.050
36400 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.035433 parameters
wR(F2) = 0.088H-atom parameters not refined
S = 1.05Δρmax = 0.32 e Å3
4422 reflectionsΔρmin = 0.24 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.20907 (4)0.34532 (2)0.30741 (2)0.0481 (1)
K10.23407 (7)0.07948 (4)0.37070 (4)0.0558 (3)
S10.2017 (1)0.41861 (6)0.47451 (4)0.0739 (4)
S20.0396 (1)0.42245 (8)0.55355 (5)0.0955 (5)
S30.00084 (9)0.36739 (6)0.45358 (5)0.0716 (4)
S40.06295 (8)0.33406 (6)0.34707 (4)0.0620 (4)
S50.28303 (9)0.38915 (6)0.37053 (4)0.0617 (4)
S60.42061 (8)0.31821 (5)0.16269 (4)0.0590 (3)
S70.3850 (1)0.25845 (7)0.06486 (5)0.0866 (5)
S80.21953 (9)0.26528 (5)0.14243 (4)0.0605 (4)
S90.13743 (8)0.29895 (5)0.24532 (4)0.0566 (3)
S100.35396 (8)0.35776 (5)0.26713 (4)0.0533 (3)
O10.3536 (2)0.0214 (1)0.3022 (1)0.0518 (8)
O20.3555 (2)0.1353 (1)0.3032 (1)0.0553 (9)
O30.2535 (2)0.1985 (1)0.3796 (1)0.0606 (9)
O40.1119 (2)0.1392 (1)0.4413 (1)0.0589 (9)
O50.0946 (2)0.0251 (1)0.4331 (1)0.0563 (9)
O60.2301 (2)0.0414 (1)0.3700 (1)0.0554 (9)
O70.0654 (3)0.0767 (2)0.3155 (1)0.098 (1)
C10.3647 (3)0.0478 (2)0.2560 (2)0.048 (1)
C20.3651 (3)0.1098 (2)0.2565 (2)0.051 (1)
C30.3585 (3)0.1984 (2)0.3069 (2)0.063 (1)
C40.3543 (3)0.2146 (2)0.3615 (2)0.065 (2)
C50.2343 (4)0.2170 (2)0.4289 (2)0.067 (2)
C60.1240 (4)0.2028 (2)0.4418 (2)0.068 (2)
C70.0119 (3)0.1167 (2)0.4446 (1)0.053 (1)
C80.0033 (3)0.0554 (2)0.4393 (1)0.050 (1)
C90.0909 (4)0.0382 (2)0.4272 (2)0.059 (1)
C100.1990 (4)0.0595 (2)0.4188 (2)0.059 (1)
C110.3329 (3)0.0594 (2)0.3568 (2)0.058 (1)
C120.3518 (3)0.0418 (2)0.3037 (2)0.057 (1)
C130.3741 (3)0.0183 (2)0.2109 (2)0.061 (1)
C140.3847 (4)0.0498 (3)0.1667 (2)0.072 (2)
C150.3841 (4)0.1098 (3)0.1668 (2)0.074 (2)
C160.3746 (3)0.1406 (2)0.2118 (2)0.063 (1)
C170.0762 (4)0.1503 (2)0.4517 (2)0.069 (2)
C180.1743 (4)0.1230 (3)0.4524 (2)0.078 (2)
C190.1817 (4)0.0636 (3)0.4464 (2)0.075 (2)
C200.0939 (4)0.0294 (2)0.4401 (2)0.065 (2)
C210.0785 (4)0.4046 (2)0.4967 (2)0.067 (2)
C220.1855 (3)0.3891 (2)0.4146 (1)0.052 (1)
C230.0913 (3)0.3652 (2)0.4045 (1)0.053 (1)
C240.3441 (3)0.2797 (2)0.1202 (2)0.059 (1)
C250.2349 (3)0.2983 (2)0.2011 (1)0.049 (1)
C260.3292 (3)0.3236 (2)0.2109 (1)0.050 (1)
C270.0252 (5)0.0778 (3)0.3103 (2)0.090 (2)
C280.0843 (7)0.1310 (5)0.3090 (3)0.195 (5)
C290.0858 (7)0.0223 (5)0.3029 (3)0.174 (4)
H10.42080.21310.29130.0763*
H20.29990.21540.28970.0763*
H30.36790.25630.36640.0792*
H40.40900.19340.37980.0792*
H50.27950.19620.45230.0825*
H60.24690.25850.43280.0825*
H70.07780.22040.41730.0840*
H80.10510.21830.47410.0840*
H90.06050.05620.45660.0705*
H100.04780.04840.39890.0705*
H110.20350.10150.42260.0695*
H120.24460.04180.44420.0695*
H130.38460.03980.37850.0708*
H140.34250.10130.36150.0708*
H150.29690.05690.28280.0672*
H160.41660.05760.29140.0672*
H170.37270.02490.21080.0731*
H180.39470.02750.13530.0867*
H190.39060.13080.13490.0911*
H200.37380.18340.21190.0743*
H210.06950.19290.45670.0851*
H220.23580.14670.45760.0962*
H230.25060.04450.44780.0906*
H240.10000.01400.43540.0803*
H250.08140.15100.33890.2087*
H260.06510.15430.28120.2087*
H270.15990.12010.30290.2087*
H280.16000.02990.29760.1957*
H290.06310.00140.27250.1957*
H300.07940.00460.33000.1957*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0473 (3)0.0516 (3)0.0453 (3)0.0004 (2)0.0038 (2)0.0035 (2)
K10.0613 (6)0.0400 (5)0.0663 (6)0.0021 (4)0.0101 (4)0.0049 (4)
S10.0856 (9)0.0887 (9)0.0472 (7)0.0066 (6)0.0006 (6)0.0196 (7)
S20.107 (1)0.130 (1)0.0492 (8)0.0118 (8)0.0117 (7)0.0018 (10)
S30.0604 (7)0.103 (1)0.0518 (7)0.0018 (7)0.0026 (5)0.0047 (7)
S40.0477 (6)0.0869 (9)0.0515 (7)0.0095 (6)0.0027 (5)0.0014 (6)
S50.0608 (7)0.0728 (8)0.0516 (7)0.0065 (6)0.0000 (5)0.0143 (6)
S60.0554 (6)0.0687 (7)0.0529 (6)0.0027 (6)0.0046 (5)0.0007 (6)
S70.103 (1)0.106 (1)0.0517 (8)0.0068 (7)0.0142 (7)0.0015 (9)
S80.0653 (7)0.0677 (8)0.0484 (7)0.0054 (6)0.0044 (5)0.0039 (6)
S90.0462 (6)0.0718 (8)0.0517 (6)0.0050 (5)0.0027 (5)0.0034 (5)
S100.0475 (6)0.0616 (7)0.0508 (6)0.0024 (5)0.0041 (5)0.0034 (5)
O10.062 (2)0.039 (2)0.055 (2)0.000 (1)0.001 (1)0.001 (1)
O20.063 (2)0.036 (2)0.066 (2)0.007 (1)0.001 (1)0.005 (1)
O30.067 (2)0.047 (2)0.068 (2)0.008 (1)0.002 (2)0.012 (1)
O40.071 (2)0.040 (2)0.066 (2)0.003 (1)0.007 (2)0.001 (1)
O50.065 (2)0.042 (2)0.062 (2)0.002 (1)0.008 (1)0.005 (1)
O60.071 (2)0.045 (2)0.051 (2)0.007 (1)0.004 (1)0.005 (1)
O70.064 (2)0.137 (3)0.091 (3)0.006 (2)0.018 (2)0.008 (2)
C10.038 (2)0.050 (3)0.057 (3)0.006 (2)0.001 (2)0.000 (2)
C20.037 (2)0.058 (3)0.057 (3)0.005 (2)0.003 (2)0.000 (2)
C30.060 (3)0.046 (3)0.082 (3)0.009 (2)0.007 (2)0.004 (2)
C40.063 (3)0.042 (2)0.091 (4)0.001 (2)0.000 (3)0.012 (2)
C50.089 (4)0.040 (3)0.072 (3)0.010 (2)0.004 (3)0.011 (2)
C60.094 (4)0.039 (2)0.072 (3)0.006 (2)0.014 (3)0.004 (2)
C70.062 (3)0.058 (3)0.038 (2)0.004 (2)0.005 (2)0.001 (2)
C80.062 (3)0.054 (3)0.035 (2)0.001 (2)0.005 (2)0.004 (2)
C90.084 (3)0.043 (3)0.049 (3)0.002 (2)0.009 (2)0.011 (2)
C100.091 (3)0.039 (2)0.048 (3)0.008 (2)0.004 (2)0.001 (2)
C110.071 (3)0.036 (2)0.067 (3)0.004 (2)0.003 (2)0.010 (2)
C120.066 (3)0.036 (2)0.068 (3)0.004 (2)0.006 (2)0.003 (2)
C130.058 (3)0.065 (3)0.061 (3)0.004 (2)0.004 (2)0.001 (2)
C140.066 (3)0.088 (4)0.061 (3)0.001 (3)0.008 (2)0.000 (3)
C150.063 (3)0.107 (4)0.052 (3)0.015 (3)0.007 (2)0.002 (3)
C160.050 (3)0.063 (3)0.076 (3)0.023 (3)0.002 (2)0.001 (2)
C170.089 (4)0.067 (3)0.052 (3)0.004 (2)0.011 (2)0.011 (3)
C180.061 (3)0.111 (5)0.063 (3)0.014 (3)0.011 (2)0.013 (3)
C190.072 (3)0.090 (4)0.065 (3)0.009 (3)0.003 (3)0.009 (3)
C200.074 (3)0.069 (3)0.051 (3)0.004 (2)0.007 (2)0.007 (3)
C210.081 (3)0.077 (3)0.043 (3)0.004 (2)0.001 (2)0.008 (3)
C220.061 (3)0.055 (3)0.042 (2)0.005 (2)0.004 (2)0.001 (2)
C230.055 (3)0.060 (3)0.043 (2)0.000 (2)0.000 (2)0.009 (2)
C240.071 (3)0.055 (3)0.049 (3)0.010 (2)0.001 (2)0.006 (2)
C250.054 (2)0.050 (2)0.042 (2)0.000 (2)0.005 (2)0.004 (2)
C260.053 (2)0.046 (2)0.050 (2)0.003 (2)0.002 (2)0.009 (2)
C270.093 (4)0.136 (6)0.041 (3)0.005 (3)0.005 (3)0.016 (4)
C280.196 (9)0.28 (1)0.105 (6)0.015 (7)0.005 (6)0.150 (9)
C290.182 (8)0.23 (1)0.110 (6)0.039 (6)0.015 (5)0.125 (8)
Geometric parameters (Å, º) top
Ni1—S42.168 (1)O5—C81.366 (5)
Ni1—S52.163 (1)O5—C91.431 (5)
Ni1—S92.156 (1)O6—C101.418 (5)
Ni1—S102.166 (1)O6—C111.424 (5)
S1—C211.716 (5)O7—C271.170 (6)
S1—C221.740 (4)C1—C21.395 (6)
S2—C211.645 (4)C1—C131.375 (6)
S3—C211.732 (5)C2—C161.380 (6)
S3—C231.750 (4)C3—C41.498 (6)
S4—C231.719 (4)C5—C61.492 (6)
S5—C221.717 (4)C7—C81.388 (6)
S6—C241.726 (5)C7—C171.372 (6)
S6—C261.746 (4)C8—C201.377 (6)
S7—C241.637 (4)C9—C101.484 (6)
S8—C241.735 (4)C11—C121.486 (6)
S8—C251.741 (4)C13—C141.378 (6)
S9—C251.719 (4)C14—C151.349 (7)
S10—C261.710 (4)C15—C161.389 (7)
O1—C11.372 (4)C17—C181.399 (7)
O1—C121.420 (4)C18—C191.348 (7)
O2—C21.375 (5)C19—C201.373 (7)
O2—C31.421 (5)C22—C231.347 (6)
O3—C41.427 (5)C25—C261.360 (5)
O3—C51.398 (5)C27—C281.416 (10)
O4—C61.436 (5)C27—C291.481 (9)
O4—C71.381 (5)
K1···O12.719 (3)S4···S9i3.637 (2)
K1···O22.691 (3)S6···S10ii3.549 (2)
K1···O32.696 (3)S9···S9i3.534 (2)
K1···O42.794 (3)C1···C1ii3.486 (7)
K1···O52.734 (3)C1···C13ii3.524 (6)
K1···O62.717 (3)C2···C2ii3.479 (7)
K1···O72.611 (4)C2···C16ii3.509 (6)
S4—Ni1—S593.01 (4)C7—C8—C20119.4 (4)
S4—Ni1—S987.14 (4)O5—C9—C10107.9 (3)
S4—Ni1—S10179.07 (5)O6—C10—C9108.1 (3)
S5—Ni1—S9178.15 (5)O6—C11—C12108.3 (3)
S5—Ni1—S1087.19 (4)O1—C12—C11107.3 (3)
S9—Ni1—S1092.69 (4)C1—C13—C14120.5 (4)
C21—S1—C2297.9 (2)C13—C14—C15120.7 (5)
C21—S3—C2397.2 (2)C14—C15—C16120.0 (4)
Ni1—S4—C23101.8 (1)C2—C16—C15120.1 (4)
Ni1—S5—C22102.2 (1)C7—C17—C18120.1 (5)
C24—S6—C2697.7 (2)C17—C18—C19119.7 (5)
C24—S8—C2597.1 (2)C18—C19—C20120.7 (5)
Ni1—S9—C25102.6 (1)C8—C20—C19120.5 (4)
Ni1—S10—C26102.6 (1)S1—C21—S2123.6 (3)
C1—O1—C12117.3 (3)S1—C21—S3112.9 (2)
C2—O2—C3118.4 (3)S2—C21—S3123.4 (3)
C4—O3—C5113.8 (3)S1—C22—S5122.7 (2)
C6—O4—C7117.6 (3)S1—C22—C23116.0 (3)
C8—O5—C9118.8 (3)S5—C22—C23121.3 (3)
C10—O6—C11114.1 (3)S3—C23—S4122.4 (3)
O1—C1—C2115.0 (4)S3—C23—C22115.9 (3)
O1—C1—C13125.7 (4)S4—C23—C22121.7 (3)
C2—C1—C13119.2 (4)S6—C24—S7123.5 (3)
O2—C2—C1115.1 (4)S6—C24—S8113.1 (2)
O2—C2—C16125.3 (4)S7—C24—S8123.4 (3)
C1—C2—C16119.6 (4)S8—C25—S9122.5 (2)
O2—C3—C4108.0 (3)S8—C25—C26116.6 (3)
O3—C4—C3107.5 (3)S9—C25—C26120.9 (3)
O3—C5—C6108.9 (4)S6—C26—S10123.5 (2)
O4—C6—C5108.2 (4)S6—C26—C25115.4 (3)
O4—C7—C8115.5 (4)S10—C26—C25121.1 (3)
O4—C7—C17124.9 (4)O7—C27—C28123.5 (8)
C8—C7—C17119.6 (4)O7—C27—C29121.2 (7)
O5—C8—C7116.1 (4)C28—C27—C29115.3 (8)
O5—C8—C20124.5 (4)
Ni1—S4—C23—S3178.7 (2)O2—C2—C16—C15179.8 (4)
Ni1—S4—C23—C220.8 (4)O2—C3—C4—O367.5 (4)
Ni1—S5—C22—S1179.3 (2)O3—C5—C6—O464.6 (5)
Ni1—S5—C22—C230.0 (4)O4—C7—C8—O51.9 (5)
Ni1—S9—C25—S8179.5 (2)O4—C7—C8—C20177.5 (4)
Ni1—S9—C25—C260.1 (4)O4—C7—C17—C18177.4 (4)
Ni1—S10—C26—S6178.7 (2)O5—C8—C7—C17178.9 (4)
Ni1—S10—C26—C251.0 (4)O5—C8—C20—C19179.8 (4)
S1—C21—S3—C232.5 (3)O5—C9—C10—O671.4 (4)
S1—C22—C23—S30.4 (5)C1—O1—C12—C11176.7 (3)
S1—C22—C23—S4179.9 (2)C1—C2—O2—C3178.0 (3)
S2—C21—S1—C22179.8 (3)C1—C2—C16—C150.2 (6)
S2—C21—S3—C23179.6 (3)C1—C13—C14—C151.2 (7)
S3—C21—S1—C222.4 (3)C2—O2—C3—C4176.0 (3)
S3—C23—C22—S5179.0 (2)C2—C1—O1—C12179.5 (3)
S4—Ni1—S5—C220.4 (2)C2—C1—C13—C140.6 (6)
S4—Ni1—S9—C25179.5 (1)C2—C16—C15—C140.4 (7)
S4—C23—S3—C21178.7 (3)C3—O2—C2—C162.0 (6)
S4—C23—C22—S50.6 (5)C3—C4—O3—C5173.4 (3)
S5—Ni1—S4—C230.6 (1)C4—O3—C5—C6174.8 (3)
S5—Ni1—S10—C26177.4 (1)C5—C6—O4—C7170.1 (4)
S5—C22—S1—C21179.5 (3)C6—O4—C7—C8174.3 (4)
S6—C24—S8—C250.8 (3)C6—O4—C7—C174.8 (6)
S6—C26—C25—S80.5 (4)C7—C8—O5—C9179.6 (3)
S6—C26—C25—S9178.9 (2)C7—C8—C20—C190.4 (6)
S7—C24—S6—C26179.0 (3)C7—C17—C18—C190.6 (7)
S7—C24—S8—C25178.8 (3)C8—O5—C9—C10177.4 (3)
S8—C24—S6—C260.6 (3)C8—C7—C17—C181.7 (6)
S8—C25—C26—S10179.7 (2)C8—C20—C19—C180.7 (7)
S9—Ni1—S4—C23177.5 (1)C9—O5—C8—C200.2 (6)
S9—Ni1—S10—C260.7 (1)C9—C10—O6—C11179.6 (3)
S9—C25—S8—C24178.6 (3)C10—O6—C11—C12175.6 (3)
S9—C25—C26—S100.8 (5)C12—O1—C1—C130.2 (5)
S10—Ni1—S5—C22179.5 (2)C13—C1—C2—C160.1 (6)
S10—Ni1—S9—C250.4 (1)C13—C14—C15—C161.1 (7)
S10—C26—S6—C24179.7 (3)C17—C7—C8—C201.6 (6)
O1—C1—C2—O20.7 (5)C17—C18—C19—C200.7 (8)
O1—C1—C2—C16179.3 (3)C21—S1—C22—C231.2 (4)
O1—C1—C13—C14179.9 (4)C21—S3—C23—C221.8 (4)
O1—C12—C11—O667.0 (4)C24—S6—C26—C250.1 (4)
O2—C2—C1—C13179.9 (3)C24—S8—C25—C260.8 (4)
Symmetry codes: (i) x, y, z+1/2; (ii) x+1, y, z+1/2.

Experimental details

Crystal data
Chemical formulaK[Ni(C3S5)2](C20H24O6)·C3H6O
Mr908.95
Crystal system, space groupMonoclinic, C2/c
Temperature (K)296
a, b, c (Å)12.8232 (5), 22.4666 (8), 26.612 (1)
β (°) 90.201 (2)
V3)7666.6 (5)
Z8
Radiation typeMo Kα
µ (mm1)1.20
Crystal size (mm)0.35 × 0.35 × 0.10
Data collection
DiffractometerRigaku RAXIS-RAPID Imaging Plate
diffractometer
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.699, 0.887
No. of measured, independent and
observed [F2 > 2σ(F2)] reflections
36400, 8776, 4422
Rint0.050
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.035, 0.088, 1.05
No. of reflections4422
No. of parameters433
No. of restraints?
H-atom treatmentH-atom parameters not refined
Δρmax, Δρmin (e Å3)0.32, 0.24

Computer programs: PROCESS-AUTO (Rigaku, 1998), PROCESS-AUTO, SIR92 (Altomare et al., 1994), TEXSAN (Molecular Structure Corporation and Rigaku, 1999), ORTEPIII (Burnett & Johnson, 1996).

Selected interatomic distances (Å) top
S4···S9i3.637 (2)C1···C13ii3.524 (6)
S6···S10ii3.549 (2)C2···C2ii3.479 (7)
S9···S9i3.534 (2)C2···C16ii3.509 (6)
C1···C1ii3.486 (7)
Symmetry codes: (i) x, y, z+1/2; (ii) x+1, y, z+1/2.
 

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