Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807033284/cf2109sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807033284/cf2109Isup2.hkl |
CCDC reference: 209415
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.006 Å
- R factor = 0.043
- wR factor = 0.128
- Data-to-parameter ratio = 18.6
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.99
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C34 H52 Cl2 K2 N4 Ni1 O12 S Atom count from _chemical_formula_moiety:C58 H100 Cl2 K2 N4 Ni1 O24 PLAT794_ALERT_5_G Check Predicted Bond Valency for Ni1 (2) 2.13 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 3
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 2 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 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
To a solution of 18-crown-6 (2.0 mmol) in 1,2-dichloroethane (10.0 ml) was added 5 ml of 1,2-dichloroethane containing NiCl2 (0.5 mmol) and K2(i-mnt) (1 mmol). The reaction mixture was stirred for 2 h at room temperature and then filtered. The precipitate was dissolved in 4:1 diethyl ether/1,2-dichloroethane. Colorless single crystals were obtained by slowly evaporating the solution. Elemental analysis found: H 5.02, C 39.08, N 5.36%; calculated for C34H52Cl2K2N4O12S4Ni: H 5.23, C 38.93, N 5.12%.
All H atoms were positioned geometrically and treated as riding on their parent atoms, with 0.97Å and the Uiso(H) values were set at 1.2Ueq(C) for C-bound H atoms..
In recent years, metal coordination complexes with one-dimensional polymeric structures have attracted interest owing to their important applications as materials with unusual properties (Chen &Suslick, 1993). The complexes formed by crown ethers, alkali metal cations, and transition metal bis(dithiolate) anions, in which the bis(dithiolate) ligands include i-mnt (Long et al., 1998) have attracted widespread interest due to their unusual crystal structures and nusual electrical, magnetic and optical properties (Nakamura et al., 1998). The title complex consists of two [K(18 C6)]+ complex cations, one centrosymmetric [Ni(i-mnt)2]2- complex anion, and a solvent molecule. The Ni atom is located on an inversion center and does not bond directly to the O atoms of the crown ether. It is coordinated by four S atoms from two i-mnt ligands. The NiS4 group is square planar. In the complex cation [K(18 C6)]+, the potassium ion lies within the crown ether cavity, 0.2038Å out of the plane formed by the six ether oxygen atoms. The K+ ion is also coordinated by two N atoms from i-mnt ligands of different [Ni(i-mnt)2]2- complex anions. Thus the [K(18 C6)]+ cations and [Ni(i-mnt)2]2- complex anions form a two-dimensional network bridged by K—N interactions. The solvent molecule also lies on an inversion center.
For related literature, see: Chen & Suslick (1993); Long et al. (1998); Nakamura et al. (1998).
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
[K2Ni(C4N2S2)2(C12H24O6)2]·C2H4Cl2 | F(000) = 1088 |
Mr = 1044.85 | Dx = 1.446 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 2404 reflections |
a = 8.271 (1) Å | θ = 2.4–20.9° |
b = 13.067 (2) Å | µ = 0.92 mm−1 |
c = 22.207 (2) Å | T = 298 K |
β = 90.140 (2)° | Block, colourless |
V = 2400.1 (5) Å3 | 0.40 × 0.32 × 0.31 mm |
Z = 2 |
Siemens SMART CCD diffractometer | 4882 independent reflections |
Radiation source: fine-focus sealed tube | 2717 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.041 |
φ and ω scans | θmax = 26.4°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −10→10 |
Tmin = 0.710, Tmax = 0.763 | k = −11→16 |
13861 measured reflections | l = −27→26 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.044 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.128 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0507P)2] where P = (Fo2 + 2Fc2)/3 |
4882 reflections | (Δ/σ)max < 0.001 |
262 parameters | Δρmax = 0.59 e Å−3 |
3 restraints | Δρmin = −0.77 e Å−3 |
[K2Ni(C4N2S2)2(C12H24O6)2]·C2H4Cl2 | V = 2400.1 (5) Å3 |
Mr = 1044.85 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 8.271 (1) Å | µ = 0.92 mm−1 |
b = 13.067 (2) Å | T = 298 K |
c = 22.207 (2) Å | 0.40 × 0.32 × 0.31 mm |
β = 90.140 (2)° |
Siemens SMART CCD diffractometer | 4882 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 2717 reflections with I > 2σ(I) |
Tmin = 0.710, Tmax = 0.763 | Rint = 0.041 |
13861 measured reflections |
R[F2 > 2σ(F2)] = 0.044 | 3 restraints |
wR(F2) = 0.128 | H-atom parameters constrained |
S = 1.01 | Δρmax = 0.59 e Å−3 |
4882 reflections | Δρmin = −0.77 e Å−3 |
262 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Ni1 | 0.5000 | 0.5000 | 0.5000 | 0.0446 (2) | |
K1 | −0.04263 (11) | 0.51950 (6) | 0.17024 (4) | 0.0524 (2) | |
Cl1 | 0.11657 (19) | 0.41379 (12) | 0.56953 (7) | 0.1072 (5) | |
N1 | 0.1579 (4) | 0.6009 (2) | 0.27356 (14) | 0.0524 (2) | |
N2 | 0.2288 (5) | 0.8652 (3) | 0.39120 (16) | 0.0765 (12) | |
O1 | −0.2843 (4) | 0.4976 (2) | 0.25695 (13) | 0.0724 (9) | |
O2 | −0.3427 (4) | 0.6163 (2) | 0.15473 (14) | 0.0680 (8) | |
O3 | −0.0790 (4) | 0.6762 (2) | 0.08341 (13) | 0.0680 (8) | |
O4 | 0.1728 (4) | 0.5284 (2) | 0.07367 (12) | 0.0675 (8) | |
O5 | 0.2242 (3) | 0.3857 (2) | 0.16313 (12) | 0.0603 (8) | |
O6 | −0.0334 (4) | 0.3540 (2) | 0.24499 (12) | 0.0645 (8) | |
S1 | 0.38775 (13) | 0.48585 (7) | 0.40962 (4) | 0.0531 (3) | |
S2 | 0.43037 (13) | 0.66007 (7) | 0.48093 (4) | 0.0513 (3) | |
C1 | −0.4432 (6) | 0.5184 (4) | 0.2352 (2) | 0.0839 (15) | |
H1A | −0.5184 | 0.5191 | 0.2687 | 0.101* | |
H1B | −0.4763 | 0.4648 | 0.2076 | 0.101* | |
C2 | −0.4478 (6) | 0.6182 (4) | 0.2041 (2) | 0.0783 (14) | |
H2A | −0.5570 | 0.6324 | 0.1905 | 0.094* | |
H2B | −0.4155 | 0.6720 | 0.2318 | 0.094* | |
C3 | −0.3468 (6) | 0.7057 (4) | 0.1196 (2) | 0.0769 (14) | |
H3A | −0.3095 | 0.7636 | 0.1432 | 0.092* | |
H3B | −0.4568 | 0.7194 | 0.1066 | 0.092* | |
C4 | −0.2412 (6) | 0.6917 (4) | 0.0663 (2) | 0.0791 (14) | |
H4A | −0.2785 | 0.6332 | 0.0432 | 0.095* | |
H4B | −0.2484 | 0.7517 | 0.0408 | 0.095* | |
C5 | 0.0254 (6) | 0.6647 (4) | 0.0331 (2) | 0.0811 (15) | |
H5A | 0.0360 | 0.7298 | 0.0125 | 0.097* | |
H5B | −0.0212 | 0.6159 | 0.0050 | 0.097* | |
C6 | 0.1863 (6) | 0.6287 (4) | 0.0522 (2) | 0.0791 (14) | |
H6A | 0.2604 | 0.6308 | 0.0185 | 0.095* | |
H6B | 0.2282 | 0.6729 | 0.0837 | 0.095* | |
C7 | 0.3235 (5) | 0.4777 (4) | 0.08011 (19) | 0.0680 (13) | |
H7A | 0.3939 | 0.5161 | 0.1068 | 0.082* | |
H7B | 0.3761 | 0.4714 | 0.0413 | 0.082* | |
C8 | 0.2907 (6) | 0.3754 (4) | 0.10550 (19) | 0.0698 (13) | |
H8A | 0.2160 | 0.3388 | 0.0796 | 0.084* | |
H8B | 0.3904 | 0.3365 | 0.1078 | 0.084* | |
C9 | 0.1869 (6) | 0.2907 (3) | 0.1902 (2) | 0.0770 (14) | |
H9A | 0.2836 | 0.2490 | 0.1931 | 0.092* | |
H9B | 0.1082 | 0.2543 | 0.1658 | 0.092* | |
C10 | 0.1208 (6) | 0.3092 (4) | 0.2507 (2) | 0.0745 (14) | |
H10A | 0.1128 | 0.2451 | 0.2725 | 0.089* | |
H10B | 0.1920 | 0.3545 | 0.2730 | 0.089* | |
C11 | −0.1054 (6) | 0.3763 (4) | 0.3006 (2) | 0.0877 (16) | |
H11A | −0.0490 | 0.4326 | 0.3199 | 0.105* | |
H11B | −0.0995 | 0.3171 | 0.3268 | 0.105* | |
C12 | −0.2778 (6) | 0.4047 (4) | 0.2898 (2) | 0.0923 (17) | |
H12A | −0.3315 | 0.3508 | 0.2673 | 0.111* | |
H12B | −0.3331 | 0.4127 | 0.3280 | 0.111* | |
C13 | 0.3545 (4) | 0.6152 (3) | 0.41369 (15) | 0.0440 (9) | |
C14 | 0.2763 (4) | 0.6752 (2) | 0.37046 (14) | 0.0455 (9) | |
C15 | 0.2118 (5) | 0.6326 (3) | 0.31712 (16) | 0.0532 (10) | |
C16 | 0.2502 (5) | 0.7801 (3) | 0.38195 (16) | 0.0514 (10) | |
C17 | 0.0361 (7) | 0.5200 (4) | 0.5271 (2) | 0.1024 (19) | |
H17A | −0.0443 | 0.5560 | 0.5507 | 0.123* | |
H17B | 0.1220 | 0.5676 | 0.5171 | 0.123* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0458 (4) | 0.0411 (4) | 0.0470 (4) | 0.0044 (3) | −0.0006 (3) | −0.0004 (3) |
K1 | 0.0550 (6) | 0.0498 (5) | 0.0525 (5) | 0.0015 (4) | −0.0030 (4) | 0.0027 (4) |
Cl1 | 0.0982 (12) | 0.1102 (12) | 0.1131 (11) | 0.0054 (9) | 0.0116 (9) | 0.0209 (9) |
N1 | 0.0550 (6) | 0.0498 (5) | 0.0525 (5) | 0.0015 (4) | −0.0030 (4) | 0.0027 (4) |
N2 | 0.109 (3) | 0.051 (2) | 0.070 (2) | 0.015 (2) | −0.027 (2) | 0.001 (2) |
O1 | 0.060 (2) | 0.098 (3) | 0.0594 (18) | −0.0012 (18) | 0.0029 (15) | 0.0034 (17) |
O2 | 0.067 (2) | 0.063 (2) | 0.074 (2) | 0.0108 (16) | −0.0034 (17) | −0.0042 (17) |
O3 | 0.076 (2) | 0.066 (2) | 0.0623 (19) | −0.0012 (16) | −0.0194 (17) | 0.0096 (15) |
O4 | 0.063 (2) | 0.073 (2) | 0.0662 (19) | −0.0087 (16) | 0.0000 (15) | 0.0185 (16) |
O5 | 0.064 (2) | 0.0621 (19) | 0.0545 (17) | 0.0056 (15) | −0.0014 (15) | −0.0014 (15) |
O6 | 0.068 (2) | 0.071 (2) | 0.0554 (18) | 0.0044 (16) | −0.0046 (16) | 0.0133 (15) |
S1 | 0.0644 (7) | 0.0423 (6) | 0.0527 (6) | 0.0048 (5) | −0.0033 (5) | −0.0047 (5) |
S2 | 0.0583 (7) | 0.0412 (6) | 0.0543 (6) | 0.0033 (5) | −0.0100 (5) | −0.0044 (5) |
C1 | 0.055 (3) | 0.124 (5) | 0.072 (3) | 0.002 (3) | 0.006 (3) | −0.003 (3) |
C2 | 0.058 (3) | 0.100 (4) | 0.077 (3) | 0.013 (3) | −0.011 (3) | −0.022 (3) |
C3 | 0.079 (4) | 0.066 (3) | 0.086 (3) | 0.015 (3) | −0.033 (3) | −0.006 (3) |
C4 | 0.089 (4) | 0.070 (3) | 0.079 (3) | 0.000 (3) | −0.028 (3) | 0.013 (3) |
C5 | 0.111 (5) | 0.066 (3) | 0.067 (3) | −0.004 (3) | −0.011 (3) | 0.023 (3) |
C6 | 0.083 (4) | 0.083 (4) | 0.071 (3) | −0.020 (3) | −0.003 (3) | 0.020 (3) |
C7 | 0.051 (3) | 0.094 (4) | 0.059 (3) | −0.006 (3) | 0.000 (2) | −0.006 (3) |
C8 | 0.062 (3) | 0.080 (4) | 0.067 (3) | 0.008 (3) | −0.003 (2) | −0.010 (3) |
C9 | 0.077 (4) | 0.061 (3) | 0.093 (4) | 0.021 (3) | −0.012 (3) | 0.012 (3) |
C10 | 0.080 (4) | 0.073 (3) | 0.071 (3) | 0.008 (3) | −0.017 (3) | 0.026 (3) |
C11 | 0.099 (4) | 0.111 (4) | 0.054 (3) | 0.004 (3) | 0.003 (3) | 0.026 (3) |
C12 | 0.080 (4) | 0.125 (5) | 0.072 (3) | −0.004 (4) | 0.023 (3) | 0.025 (3) |
C13 | 0.040 (2) | 0.042 (2) | 0.050 (2) | −0.0022 (17) | 0.0091 (18) | −0.0034 (18) |
C14 | 0.045 (2) | 0.044 (2) | 0.048 (2) | 0.0009 (18) | −0.0013 (19) | −0.0036 (18) |
C15 | 0.052 (3) | 0.054 (3) | 0.053 (2) | 0.005 (2) | −0.006 (2) | −0.005 (2) |
C16 | 0.056 (3) | 0.054 (3) | 0.044 (2) | 0.002 (2) | −0.009 (2) | 0.007 (2) |
C17 | 0.070 (4) | 0.113 (5) | 0.125 (5) | −0.026 (3) | 0.035 (4) | −0.025 (4) |
Ni1—S2i | 2.2101 (10) | C2—H2A | 0.970 |
Ni1—S2 | 2.2101 (10) | C2—H2B | 0.970 |
Ni1—S1 | 2.2170 (10) | C3—C4 | 1.483 (6) |
Ni1—S1i | 2.2170 (10) | C3—H3A | 0.970 |
K1—O6 | 2.727 (3) | C3—H3B | 0.970 |
K1—O1 | 2.793 (3) | C4—H4A | 0.970 |
K1—O4 | 2.794 (3) | C4—H4B | 0.970 |
K1—O2 | 2.806 (3) | C5—C6 | 1.473 (6) |
K1—O5 | 2.820 (3) | C5—H5A | 0.970 |
K1—O3 | 2.828 (3) | C5—H5B | 0.970 |
K1—N2ii | 2.879 (4) | C6—H6A | 0.970 |
K1—N1 | 3.021 (3) | C6—H6B | 0.970 |
Cl1—C17 | 1.803 (7) | C7—C8 | 1.476 (6) |
N1—C15 | 1.142 (4) | C7—H7A | 0.970 |
N2—C16 | 1.145 (5) | C7—H7B | 0.970 |
N2—K1iii | 2.879 (4) | C8—H8A | 0.970 |
O1—C12 | 1.417 (5) | C8—H8B | 0.970 |
O1—C1 | 1.426 (5) | C9—C10 | 1.471 (6) |
O2—C2 | 1.402 (5) | C9—H9A | 0.970 |
O2—C3 | 1.406 (5) | C9—H9B | 0.970 |
O3—C4 | 1.408 (5) | C10—H10A | 0.970 |
O3—C5 | 1.422 (5) | C10—H10B | 0.970 |
O4—C6 | 1.399 (5) | C11—C12 | 1.492 (6) |
O4—C7 | 1.418 (5) | C11—H11A | 0.970 |
O5—C8 | 1.401 (4) | C11—H11B | 0.970 |
O5—C9 | 1.413 (5) | C12—H12A | 0.970 |
O6—C11 | 1.403 (5) | C12—H12B | 0.970 |
O6—C10 | 1.409 (5) | C13—C14 | 1.397 (3) |
S1—C13 | 1.715 (4) | C14—C16 | 1.411 (4) |
S2—C13 | 1.721 (4) | C14—C15 | 1.412 (3) |
C1—C2 | 1.475 (6) | C17—C17iv | 1.440 (10) |
C1—H1A | 0.970 | C17—H17A | 0.970 |
C1—H1B | 0.970 | C17—H17B | 0.970 |
S2i—Ni1—S2 | 180 | O2—C3—H3B | 109.9 |
S2i—Ni1—S1 | 101.71 (4) | C4—C3—H3B | 109.9 |
S2—Ni1—S1 | 78.29 (4) | H3A—C3—H3B | 108.3 |
S2i—Ni1—S1i | 78.29 (4) | O3—C4—C3 | 111.4 (4) |
S2—Ni1—S1i | 101.71 (4) | O3—C4—H4A | 109.3 |
S1—Ni1—S1i | 180 | C3—C4—H4A | 109.3 |
O6—K1—O1 | 61.19 (9) | O3—C4—H4B | 109.3 |
O6—K1—O4 | 118.91 (9) | C3—C4—H4B | 109.3 |
O1—K1—O4 | 172.78 (9) | H4A—C4—H4B | 108.0 |
O6—K1—O2 | 117.09 (10) | O3—C5—C6 | 110.9 (4) |
O1—K1—O2 | 59.78 (9) | O3—C5—H5A | 109.5 |
O4—K1—O2 | 116.91 (9) | C6—C5—H5A | 109.5 |
O6—K1—O5 | 61.43 (9) | O3—C5—H5B | 109.5 |
O1—K1—O5 | 122.43 (9) | C6—C5—H5B | 109.5 |
O4—K1—O5 | 58.82 (8) | H5A—C5—H5B | 108.1 |
O2—K1—O5 | 164.70 (9) | O4—C6—C5 | 108.9 (4) |
O6—K1—O3 | 172.71 (9) | O4—C6—H6A | 109.9 |
O1—K1—O3 | 117.98 (10) | C5—C6—H6A | 109.9 |
O4—K1—O3 | 60.89 (9) | O4—C6—H6B | 109.9 |
O2—K1—O3 | 59.83 (9) | C5—C6—H6B | 109.9 |
O5—K1—O3 | 119.51 (9) | H6A—C6—H6B | 108.3 |
O6—K1—N2ii | 75.36 (10) | O4—C7—C8 | 107.4 (4) |
O1—K1—N2ii | 82.66 (10) | O4—C7—H7A | 110.2 |
O4—K1—N2ii | 90.38 (10) | C8—C7—H7A | 110.2 |
O2—K1—N2ii | 77.62 (11) | O4—C7—H7B | 110.2 |
O5—K1—N2ii | 87.53 (10) | C8—C7—H7B | 110.2 |
O3—K1—N2ii | 97.37 (10) | H7A—C7—H7B | 108.5 |
O6—K1—N1 | 78.60 (9) | O5—C8—C7 | 109.6 (4) |
O1—K1—N1 | 84.54 (9) | O5—C8—H8A | 109.8 |
O4—K1—N1 | 102.62 (9) | C7—C8—H8A | 109.8 |
O2—K1—N1 | 114.72 (9) | O5—C8—H8B | 109.8 |
O5—K1—N1 | 80.37 (8) | C7—C8—H8B | 109.8 |
O3—K1—N1 | 108.67 (9) | H8A—C8—H8B | 108.2 |
N2ii—K1—N1 | 153.96 (10) | O5—C9—C10 | 109.0 (4) |
C15—N1—K1 | 169.6 (3) | O5—C9—H9A | 109.9 |
C16—N2—K1iii | 132.7 (3) | C10—C9—H9A | 109.9 |
C12—O1—C1 | 111.8 (4) | O5—C9—H9B | 109.9 |
C12—O1—K1 | 114.6 (3) | C10—C9—H9B | 109.9 |
C1—O1—K1 | 114.1 (2) | H9A—C9—H9B | 108.3 |
C2—O2—C3 | 114.0 (4) | O6—C10—C9 | 108.9 (4) |
C2—O2—K1 | 117.5 (3) | O6—C10—H10A | 109.9 |
C3—O2—K1 | 117.6 (3) | C9—C10—H10A | 109.9 |
C4—O3—C5 | 112.5 (3) | O6—C10—H10B | 109.9 |
C4—O3—K1 | 112.8 (3) | C9—C10—H10B | 109.9 |
C5—O3—K1 | 113.3 (2) | H10A—C10—H10B | 108.3 |
C6—O4—C7 | 113.7 (3) | O6—C11—C12 | 108.5 (4) |
C6—O4—K1 | 110.6 (3) | O6—C11—H11A | 110.0 |
C7—O4—K1 | 117.7 (2) | C12—C11—H11A | 110.0 |
C8—O5—C9 | 113.0 (3) | O6—C11—H11B | 110.0 |
C8—O5—K1 | 114.8 (2) | C12—C11—H11B | 110.0 |
C9—O5—K1 | 110.4 (2) | H11A—C11—H11B | 108.4 |
C11—O6—C10 | 113.2 (3) | O1—C12—C11 | 109.3 (4) |
C11—O6—K1 | 111.1 (3) | O1—C12—H12A | 109.8 |
C10—O6—K1 | 114.1 (2) | C11—C12—H12A | 109.8 |
C13—S1—Ni1 | 86.39 (12) | O1—C12—H12B | 109.8 |
C13—S2—Ni1 | 86.45 (12) | C11—C12—H12B | 109.8 |
O1—C1—C2 | 110.4 (4) | H12A—C12—H12B | 108.3 |
O1—C1—H1A | 109.6 | C14—C13—S1 | 126.2 (3) |
C2—C1—H1A | 109.6 | C14—C13—S2 | 124.9 (3) |
O1—C1—H1B | 109.6 | S1—C13—S2 | 108.9 (2) |
C2—C1—H1B | 109.6 | C13—C14—C16 | 119.4 (3) |
H1A—C1—H1B | 108.1 | C13—C14—C15 | 121.9 (3) |
O2—C2—C1 | 109.6 (4) | C16—C14—C15 | 118.5 (3) |
O2—C2—H2A | 109.7 | N1—C15—C14 | 178.0 (4) |
C1—C2—H2A | 109.7 | N2—C16—C14 | 179.9 (5) |
O2—C2—H2B | 109.7 | C17iv—C17—Cl1 | 108.1 (6) |
C1—C2—H2B | 109.7 | C17iv—C17—H17A | 110.1 |
H2A—C2—H2B | 108.2 | Cl1—C17—H17A | 110.1 |
O2—C3—C4 | 109.1 (4) | C17iv—C17—H17B | 110.1 |
O2—C3—H3A | 109.9 | Cl1—C17—H17B | 110.1 |
C4—C3—H3A | 109.9 | H17A—C17—H17B | 108.4 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, y−1/2, −z+1/2; (iii) −x, y+1/2, −z+1/2; (iv) −x, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [K2Ni(C4N2S2)2(C12H24O6)2]·C2H4Cl2 |
Mr | 1044.85 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 298 |
a, b, c (Å) | 8.271 (1), 13.067 (2), 22.207 (2) |
β (°) | 90.140 (2) |
V (Å3) | 2400.1 (5) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.92 |
Crystal size (mm) | 0.40 × 0.32 × 0.31 |
Data collection | |
Diffractometer | Siemens SMART CCD |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.710, 0.763 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 13861, 4882, 2717 |
Rint | 0.041 |
(sin θ/λ)max (Å−1) | 0.625 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.044, 0.128, 1.01 |
No. of reflections | 4882 |
No. of parameters | 262 |
No. of restraints | 3 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.59, −0.77 |
Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SAINT, SHELXS97 (Sheldrick, 1997a), SHELXL97 (Sheldrick, 1997a), SHELXTL (Sheldrick, 1997b), SHELXTL.
Ni1—S2 | 2.2101 (10) | K1—O2 | 2.806 (3) |
Ni1—S1 | 2.2170 (10) | K1—O3 | 2.828 (3) |
K1—O6 | 2.727 (3) | K1—N2i | 2.879 (4) |
K1—O1 | 2.793 (3) | K1—N1 | 3.021 (3) |
K1—O4 | 2.794 (3) | ||
S2—Ni1—S1 | 78.29 (4) |
Symmetry code: (i) −x, y−1/2, −z+1/2. |
In recent years, metal coordination complexes with one-dimensional polymeric structures have attracted interest owing to their important applications as materials with unusual properties (Chen &Suslick, 1993). The complexes formed by crown ethers, alkali metal cations, and transition metal bis(dithiolate) anions, in which the bis(dithiolate) ligands include i-mnt (Long et al., 1998) have attracted widespread interest due to their unusual crystal structures and nusual electrical, magnetic and optical properties (Nakamura et al., 1998). The title complex consists of two [K(18 C6)]+ complex cations, one centrosymmetric [Ni(i-mnt)2]2- complex anion, and a solvent molecule. The Ni atom is located on an inversion center and does not bond directly to the O atoms of the crown ether. It is coordinated by four S atoms from two i-mnt ligands. The NiS4 group is square planar. In the complex cation [K(18 C6)]+, the potassium ion lies within the crown ether cavity, 0.2038Å out of the plane formed by the six ether oxygen atoms. The K+ ion is also coordinated by two N atoms from i-mnt ligands of different [Ni(i-mnt)2]2- complex anions. Thus the [K(18 C6)]+ cations and [Ni(i-mnt)2]2- complex anions form a two-dimensional network bridged by K—N interactions. The solvent molecule also lies on an inversion center.