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The crystal structure of the title compound, bis­[(dibenzo-18-crown-6)­sodium] tetra­thio­cyanato­palladium(II), [Na(C20H24O6)]2[Pd(SCN)4], features an ion-pair-type species consisting of two [Na(dibenzo-18-crown-6)]+ cations and a [Pd(SCN)4]2− dianion which occupies a special position on the inversion centre. The Pd atom has a square-planar coordination formed by four S atoms [Pd—S 2.3241 (9) and 2.3319 (8) Å, S—Pd—S 90.15 (3)°]; the ion pairs are held together through Na...N interactions [2.423 (3) Å] involving the N atoms of two (out of four) thio­cyanate groups. The Na+...π interactions reaching out to the aromatic nucleus of the neighbouring ion pair [Na...C 3.077 (4) and 3.082 (4) Å] are responsible for the formation of infinite chains stretching along the [1\overline 10] direction of the crystal.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801001416/ya6003sup1.cif
Contains datablocks pddb18c6, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801001416/ya6003Isup2.hkl
Contains datablock I

CCDC reference: 159837

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.028
  • wR factor = 0.080
  • Data-to-parameter ratio = 11.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

General Notes

FORMU_01 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: C44 H48 N4 Na2 O12 Pd1 S4 Atom count from _chemical_formula_moiety:C44 H48 N4 Na2 O6 Pd1 S4 ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.879 Tmax scaled 0.777 Tmin scaled 0.733

Comment top

Cation–π interactions have attracted considerable attention as an important non-covalent binding force. Studies in the gas phase (Sunner et al., 1981), aqueous media (Petti et al., 1988; Forman et al., 1995), solid state (Clark et al., 1992; Beer et al., 1994; Werner et al., 1996), biological systems (Ma & Dougherty, 1997; Dougherty & Stauffer, 1990), as well as theoretical calculations (Mecozzi et al., 1996; Jiang et al., 1998, 1999) established the broad scope and significance of these interactions. We have reported the first examples of crown ether complexes, [K(DB18C6)]2[Pd(SCN)4] (DB18C6 is dibenzo-18-crown-6) (Dou et al., 2000) and [K(DB18C6)]2[Pt(SCN)4] (Li et al., 2000), which exhibit cation–π interactions responsible for the formation of infinite chains in crystals. However, in spite of the growing interest, the X-ray evidence for the existence of the analogous Na+···π interaction is still limited. Bock and co-workers synthesized two compounds containing interactions of this kind, namely [(C6H5)2C CHC(C6H5)2]-[Na+O(C2H5)2] (Bock et al., 1990) and [(C6H5)2CC(C6H5)2]2-2[Na+O(C2H5)2] (Bock et al., 1989). In the present paper, we report the synthesis and crystal structure of the complex of DB18C6 with Na2[Pd(SCN)4], (I), which provides a new example of Na+···π interaction.

The structure of the title complex (Fig. 1) features an ion-pair-type species consisting of two [Na(DB18C6)]+ cations and a [Pd(SCN)4]2- dianion. The Pd atom occupies a special position in the inversion center and has a square-planar coordination environment formed by four S atoms [Pd1—S1 2.3241 (9) and Pd1—S2 2.3319 (8) Å, S1—Pd1—S2 90.15 (3)°]. The average Pd—S, S—C and C—N bond lengths (2.3270, 1.671 and 1.133 Å, respectively) are consistent with the corresponding values in [K(DB18C6)]2[Pd(SCN)4] (Dou et al., 2000) and [K(DB18C6)]2[Pd(SCN)4]·H2O (Wu et al., 1991).

In the [Na(DB18C6)]+ cation, the Na—O bond lengths span the range 2.559–2.853 Å. The Na+ ion is also coordinated by the N atom of one of the SCN groups at a distance of 2.423 (3) Å, which is consistent with the Na—N distance [2.472 (8) Å] in [Na(B15C5)]2[Pd(SCN)4] (B15C5 is benzo-15-crown-5) (Zhu et al., 2000). The remainder of its coordination sphere is made up of the Na—C113i 3.077 (4) Å and Na—C114i 3.082 (4) Å [symmetry code: (i) 2 - x, -y, 1 - z] close contacts involving one of the phenylene rings of the DB18C6 ligand of the neighbouring [Na(DB18C6)]2[Pd(SCN)4] ion pair. These interactions give rise to the formation of infinite chains stretching along the [110] direction in the crystal (Fig. 2). Similar infinite chains formed due to Na···π interactions with even shorter Na···C distances were observed in the abovementioned complexes reported by Bock et al. (1989, 1990) (the average Na···C distances are 2.86 and 2.88 Å respectively).

Experimental top

The synthesis of the title complex was effected by adding 10 ml of aqueous mixture of PdCl2 (0.025 M) and NaSCN (2 M) to 10 ml of 0.1 M solution of DB18C6 in 1,2-dichloroethane. The reaction mixture was stirred for 2 h at room temperature and then filtered. The precipitate was dissolved in acetone. M. p. 485–487 K. Found: C 47.51, H 4.25, N 4.72, S 11.23%; C44H48Na2N4O12PdS4 requires: C 47.79, H 4.38, N 5.07, S 11.58%. Selected FT—IR n/cm-1: 2920, 2850, 2111, 1695, 1595, 1504, 1251, 1213, 1125, 960, 940, 751. The single-crystal was obtained from 4:1 diethyl ether/acetone solution.

Refinement top

The H atoms were located in the difference map and were refined isotropically; the C—H bond lengths span the range 0.88–1.08 Å.

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: SHELXS97 (Sheldrick, 1990); 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 [Na(DB18C6)]2[Pd(SCN)4] showing 30% probablity displacement elliposoids. H atoms have been omitted for clarity.
[Figure 2] Fig. 2. A fragment of the infinite chain in the crystal packing of [Na(DB18C6)]2[Pd(SCN)4].
bis[(dibenzo-18-crown-6)sodium] palladium(II)tetrathiocyanate top
Crystal data top
[Na(C20H24O6)]2[Pd(SCN)4]Z = 1
Mr = 1105.48F(000) = 560
Triclinic, P1Dx = 1.487 Mg m3
a = 11.5695 (10) ÅMo Kα radiation, λ = 0.71073 Å
b = 8.568 (3) ÅCell parameters from 25 reflections
c = 12.976 (2) Åθ = 10.5–13.5°
α = 81.58 (2)°µ = 0.63 mm1
β = 104.804 (10)°T = 293 K
γ = 96.85 (2)°Prism, orange
V = 1225.7 (5) Å30.60 × 0.50 × 0.40 mm
Data collection top
Enraf-Nonius CAD-4
diffractometer
3190 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.020
Graphite monochromatorθmax = 25.2°, θmin = 1.6°
θ/2θ scansh = 1313
Absorption correction: ψ scan
(North et al., 1968)
k = 1010
Tmin = 0.834, Tmax = 0.884l = 015
4622 measured reflections3 standard reflections every 200 reflections
4406 independent reflections intensity decay: 5.0%
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)] = 0.028Hydrogen site location: difference Fourier map
wR(F2) = 0.080All H-atom parameters refined
S = 1.0 w = 1/[σ2(Fo2) + (0.0375P)2 + 0.4501P]
where P = (Fo2 + 2Fc2)/3
4406 reflections(Δ/σ)max < 0.001
400 parametersΔρmax = 0.41 e Å3
0 restraintsΔρmin = 0.43 e Å3
Crystal data top
[Na(C20H24O6)]2[Pd(SCN)4]γ = 96.85 (2)°
Mr = 1105.48V = 1225.7 (5) Å3
Triclinic, P1Z = 1
a = 11.5695 (10) ÅMo Kα radiation
b = 8.568 (3) ŵ = 0.63 mm1
c = 12.976 (2) ÅT = 293 K
α = 81.58 (2)°0.60 × 0.50 × 0.40 mm
β = 104.804 (10)°
Data collection top
Enraf-Nonius CAD-4
diffractometer
3190 reflections with I > 2σ(I)
Absorption correction: ψ scan
(North et al., 1968)
Rint = 0.020
Tmin = 0.834, Tmax = 0.8843 standard reflections every 200 reflections
4622 measured reflections intensity decay: 5.0%
4406 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0280 restraints
wR(F2) = 0.080All H-atom parameters refined
S = 1.0Δρmax = 0.41 e Å3
4406 reflectionsΔρmin = 0.43 e Å3
400 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
Pd10.50000.50000.50000.04075 (11)
S10.44659 (8)0.43541 (12)0.32522 (7)0.0645 (2)
S20.68440 (7)0.39662 (11)0.52685 (6)0.0588 (2)
Na10.76645 (10)0.12092 (14)0.27043 (10)0.0570 (3)
N10.6354 (3)0.3245 (4)0.2641 (2)0.0748 (8)
N20.7893 (3)0.3538 (5)0.7474 (3)0.0971 (12)
O10.78730 (18)0.0540 (2)0.47380 (16)0.0538 (5)
O20.93244 (18)0.2640 (2)0.40380 (16)0.0555 (5)
O30.91422 (19)0.3214 (2)0.18705 (16)0.0590 (5)
O40.7735 (2)0.1203 (3)0.05228 (17)0.0663 (6)
O50.6207 (2)0.0745 (3)0.11971 (18)0.0660 (6)
O60.60868 (18)0.0860 (3)0.32723 (18)0.0633 (6)
C10.5615 (3)0.3706 (4)0.2935 (2)0.0559 (8)
C20.7444 (3)0.3723 (4)0.6585 (3)0.0618 (9)
C30.8901 (3)0.0918 (4)0.5487 (2)0.0516 (7)
C40.9705 (3)0.2065 (4)0.5094 (2)0.0512 (7)
C51.0079 (3)0.3870 (4)0.3608 (3)0.0597 (8)
C60.9386 (3)0.4480 (4)0.2522 (3)0.0637 (9)
C70.8642 (4)0.3736 (5)0.0779 (3)0.0795 (12)
C80.8562 (4)0.2399 (6)0.0159 (3)0.0816 (12)
C90.7500 (3)0.0184 (5)0.0064 (2)0.0648 (9)
C100.6663 (3)0.1251 (4)0.0440 (2)0.0613 (8)
C110.5300 (3)0.1745 (5)0.1586 (3)0.0732 (10)
C120.5021 (3)0.0968 (5)0.2421 (3)0.0720 (10)
C130.5856 (3)0.0474 (5)0.4219 (3)0.0644 (9)
C140.6979 (3)0.0548 (4)0.5094 (3)0.0616 (8)
C1120.9188 (4)0.0279 (5)0.6542 (3)0.0659 (9)
C1131.0262 (4)0.0779 (6)0.7219 (3)0.0797 (12)
C1141.1050 (4)0.1858 (5)0.6840 (3)0.0758 (11)
C1151.0785 (3)0.2522 (5)0.5776 (3)0.0640 (9)
C1210.8011 (5)0.0554 (7)0.0702 (3)0.0870 (13)
C1220.7706 (5)0.2001 (8)0.1086 (4)0.1013 (16)
C1230.6900 (6)0.3057 (7)0.0710 (3)0.0957 (16)
C1240.6355 (4)0.2698 (5)0.0046 (3)0.0807 (12)
H11.026 (3)0.485 (4)0.405 (2)0.063 (9)*
H21.083 (3)0.337 (4)0.353 (3)0.071 (10)*
H30.863 (4)0.486 (4)0.254 (3)0.088 (12)*
H40.983 (3)0.534 (4)0.219 (3)0.061 (9)*
H50.782 (4)0.413 (5)0.069 (3)0.097 (14)*
H60.911 (3)0.459 (4)0.053 (3)0.065 (10)*
H70.823 (3)0.268 (5)0.058 (3)0.089 (12)*
H80.938 (4)0.181 (4)0.031 (3)0.086 (12)*
H90.461 (3)0.193 (4)0.102 (3)0.071 (10)*
H100.470 (3)0.019 (4)0.214 (3)0.064 (10)*
H110.561 (3)0.282 (4)0.191 (3)0.068 (10)*
H120.445 (3)0.166 (4)0.276 (3)0.074 (10)*
H130.559 (3)0.066 (4)0.400 (3)0.065 (9)*
H140.523 (3)0.126 (4)0.441 (2)0.059 (9)*
H150.681 (3)0.017 (4)0.573 (3)0.076 (11)*
H160.725 (3)0.162 (4)0.523 (3)0.070 (10)*
H1120.870 (3)0.053 (4)0.674 (2)0.050 (9)*
H1131.047 (3)0.035 (4)0.795 (3)0.084 (12)*
H1141.179 (4)0.214 (5)0.727 (3)0.087 (12)*
H1151.128 (3)0.326 (4)0.547 (2)0.052 (9)*
H1210.857 (4)0.012 (5)0.092 (3)0.093 (15)*
H1220.810 (4)0.237 (6)0.162 (4)0.132 (18)*
H1230.667 (4)0.403 (6)0.087 (4)0.120 (19)*
H1240.578 (3)0.334 (5)0.035 (3)0.081 (13)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.03754 (17)0.04263 (19)0.04051 (18)0.00244 (12)0.00870 (13)0.00607 (13)
S10.0550 (5)0.0935 (7)0.0476 (5)0.0151 (4)0.0045 (4)0.0237 (4)
S20.0434 (4)0.0789 (6)0.0549 (5)0.0117 (4)0.0079 (3)0.0125 (4)
Na10.0530 (7)0.0594 (7)0.0609 (7)0.0007 (6)0.0214 (6)0.0049 (6)
N10.073 (2)0.095 (2)0.0640 (19)0.0219 (17)0.0190 (16)0.0170 (16)
N20.0637 (19)0.156 (4)0.058 (2)0.016 (2)0.0078 (16)0.023 (2)
O10.0520 (12)0.0596 (12)0.0502 (12)0.0016 (10)0.0177 (10)0.0037 (10)
O20.0507 (11)0.0590 (13)0.0549 (13)0.0069 (10)0.0130 (10)0.0095 (10)
O30.0681 (14)0.0531 (12)0.0517 (12)0.0008 (10)0.0140 (10)0.0012 (10)
O40.0652 (14)0.0805 (16)0.0532 (13)0.0068 (12)0.0191 (11)0.0099 (12)
O50.0658 (14)0.0654 (14)0.0666 (14)0.0078 (11)0.0198 (12)0.0109 (11)
O60.0478 (12)0.0802 (15)0.0658 (14)0.0072 (11)0.0242 (11)0.0133 (12)
C10.063 (2)0.0587 (19)0.0423 (16)0.0036 (15)0.0064 (15)0.0067 (14)
C20.0376 (16)0.076 (2)0.067 (2)0.0036 (15)0.0131 (15)0.0077 (17)
C30.0582 (18)0.0510 (17)0.0503 (17)0.0180 (14)0.0127 (14)0.0109 (14)
C40.0507 (16)0.0554 (18)0.0525 (17)0.0143 (14)0.0111 (14)0.0171 (14)
C50.0540 (19)0.0524 (18)0.073 (2)0.0080 (15)0.0187 (16)0.0138 (16)
C60.066 (2)0.0453 (18)0.077 (2)0.0071 (16)0.0199 (19)0.0033 (17)
C70.097 (3)0.071 (3)0.058 (2)0.013 (2)0.018 (2)0.0178 (19)
C80.091 (3)0.104 (3)0.044 (2)0.012 (2)0.023 (2)0.008 (2)
C90.065 (2)0.086 (3)0.0388 (17)0.0132 (18)0.0014 (15)0.0082 (16)
C100.065 (2)0.069 (2)0.0451 (17)0.0145 (17)0.0036 (15)0.0134 (15)
C110.058 (2)0.074 (3)0.079 (3)0.0173 (19)0.0087 (19)0.013 (2)
C120.0433 (18)0.089 (3)0.080 (3)0.0150 (18)0.0181 (17)0.009 (2)
C130.0566 (19)0.071 (2)0.072 (2)0.0082 (18)0.0353 (18)0.0046 (18)
C140.065 (2)0.063 (2)0.064 (2)0.0025 (17)0.0347 (18)0.0028 (17)
C1120.080 (3)0.064 (2)0.057 (2)0.023 (2)0.0179 (19)0.0030 (17)
C1130.094 (3)0.092 (3)0.051 (2)0.045 (3)0.001 (2)0.009 (2)
C1140.069 (2)0.086 (3)0.071 (3)0.030 (2)0.007 (2)0.031 (2)
C1150.056 (2)0.067 (2)0.070 (2)0.0102 (17)0.0066 (18)0.0246 (18)
C1210.091 (3)0.121 (4)0.051 (2)0.012 (3)0.015 (2)0.021 (2)
C1220.123 (4)0.136 (5)0.052 (2)0.040 (4)0.013 (3)0.025 (3)
C1230.140 (5)0.090 (3)0.050 (2)0.035 (3)0.009 (3)0.019 (2)
C1240.103 (3)0.077 (3)0.053 (2)0.012 (2)0.001 (2)0.013 (2)
Geometric parameters (Å, º) top
Pd1—S1i2.3241 (9)C6—H40.96 (3)
Pd1—S12.3241 (9)C7—C81.474 (6)
Pd1—S22.3319 (8)C7—H51.02 (4)
Pd1—S2i2.3319 (8)C7—H60.93 (4)
S1—C11.663 (4)C8—H70.95 (4)
S2—C21.664 (4)C8—H81.08 (4)
Na1—N12.423 (3)C9—C1211.368 (5)
Na1—O12.572 (2)C9—C101.383 (5)
Na1—O22.559 (2)C10—C1241.383 (5)
Na1—O32.597 (2)C11—C121.471 (6)
Na1—O42.853 (2)C11—H90.95 (3)
Na1—O52.841 (3)C11—H111.02 (3)
Na1—O62.559 (2)C12—H101.08 (3)
Na1—C113ii3.077 (4)C12—H120.98 (4)
Na1—C114ii3.082 (4)C13—C141.492 (5)
N1—C11.151 (4)C13—H131.03 (3)
N2—C21.133 (4)C13—H140.98 (3)
O1—C31.368 (4)C14—H151.00 (4)
O1—C141.428 (4)C14—H160.99 (4)
O2—C41.364 (4)C112—C1131.388 (6)
O2—C51.428 (4)C112—H1120.89 (3)
O3—C71.413 (4)C113—C1141.350 (6)
O3—C61.430 (4)C113—Na1ii3.077 (4)
O4—C91.374 (4)C113—H1130.94 (4)
O4—C81.430 (4)C114—C1151.385 (6)
O5—C101.370 (4)C114—Na1ii3.082 (4)
O5—C111.420 (4)C114—H1140.92 (4)
O6—C131.413 (4)C115—H1150.91 (3)
O6—C121.434 (4)C121—C1221.378 (7)
C3—C1121.370 (5)C121—H1210.89 (4)
C3—C41.403 (4)C122—C1231.352 (8)
C4—C1151.384 (4)C122—H1221.02 (5)
C5—C61.486 (5)C123—C1241.381 (7)
C5—H11.06 (3)C123—H1230.88 (5)
C5—H21.05 (4)C124—H1240.94 (4)
C6—H30.98 (4)
S1i—Pd1—S1180.0O3—C6—H3109 (2)
S1i—Pd1—S290.15 (3)C5—C6—H3112 (2)
S1—Pd1—S289.85 (3)O3—C6—H4108.5 (19)
S2—Pd1—S2i180.0C5—C6—H4111.7 (19)
O2—Na1—O364.23 (7)H3—C6—H4107 (3)
O2—Na1—O159.40 (7)O3—C7—C8107.9 (3)
O3—Na1—O459.83 (7)O3—C7—H5110 (2)
O5—Na1—O452.46 (7)C8—C7—H5112 (2)
O6—Na1—O164.00 (7)O3—C7—H6111 (2)
O6—Na1—O560.17 (7)C8—C7—H6110 (2)
C113ii—Na1—C114ii25.32 (11)H5—C7—H6106 (3)
S1i—Pd1—S2i89.85 (3)O4—C8—C7106.4 (3)
S1—Pd1—S2i90.15 (3)O4—C8—H7106 (2)
C1—S1—Pd1111.05 (11)C7—C8—H7112 (2)
C2—S2—Pd1107.44 (12)O4—C8—H8104 (2)
N1—Na1—O289.57 (10)C7—C8—H8115 (2)
N1—Na1—O688.79 (10)H7—C8—H8113 (3)
O2—Na1—O6123.36 (8)C121—C9—O4125.9 (4)
N1—Na1—O190.25 (9)C121—C9—C10120.1 (4)
N1—Na1—O392.12 (10)O4—C9—C10114.0 (3)
O6—Na1—O3172.38 (9)O5—C10—C9114.8 (3)
O1—Na1—O3123.55 (8)O5—C10—C124125.5 (4)
N1—Na1—O5101.98 (10)C9—C10—C124119.6 (4)
O2—Na1—O5168.18 (8)O5—C11—C12107.0 (3)
O1—Na1—O5122.25 (8)O5—C11—H9112 (2)
O3—Na1—O5112.27 (8)C12—C11—H9112 (2)
N1—Na1—O4104.56 (10)O5—C11—H11110.0 (19)
O2—Na1—O4122.44 (8)C12—C11—H11110 (2)
O6—Na1—O4112.63 (8)H9—C11—H11107 (3)
O1—Na1—O4164.91 (8)O6—C12—C11107.6 (3)
N1—Na1—C113ii167.78 (14)O6—C12—H10110.3 (18)
O2—Na1—C113ii81.18 (10)C11—C12—H10114.0 (18)
O6—Na1—C113ii102.95 (12)O6—C12—H12104 (2)
O1—Na1—C113ii91.88 (10)C11—C12—H12110 (2)
O3—Na1—C113ii76.70 (12)H10—C12—H12111 (3)
O5—Na1—C113ii87.03 (10)O6—C13—C14109.0 (3)
O4—Na1—C113ii74.27 (9)O6—C13—H13103.6 (18)
N1—Na1—C114ii165.47 (13)C14—C13—H13112.1 (18)
O2—Na1—C114ii93.38 (10)O6—C13—H14107.3 (18)
O6—Na1—C114ii77.70 (12)C14—C13—H14110.4 (18)
O1—Na1—C114ii79.10 (10)H13—C13—H14114 (3)
O3—Na1—C114ii101.98 (12)O1—C14—C13107.4 (3)
O5—Na1—C114ii76.06 (10)O1—C14—H15108 (2)
O4—Na1—C114ii85.82 (10)C13—C14—H15107 (2)
C1—N1—Na1150.4 (3)O1—C14—H16109 (2)
C3—O1—C14117.6 (2)C13—C14—H16110 (2)
C3—O1—Na1123.03 (17)H15—C14—H16115 (3)
C14—O1—Na1118.08 (19)C3—C112—C113120.1 (4)
C4—O2—C5117.3 (2)C3—C112—H112117 (2)
C4—O2—Na1123.30 (18)C113—C112—H112122 (2)
C5—O2—Na1117.51 (18)C114—C113—C112120.6 (4)
C7—O3—C6112.0 (3)C114—C113—Na1ii77.5 (2)
C7—O3—Na1111.9 (2)C112—C113—Na1ii113.3 (2)
C6—O3—Na1104.05 (19)C114—C113—H113119 (2)
C9—O4—C8118.0 (3)C112—C113—H113121 (2)
C9—O4—Na1120.53 (19)Na1ii—C113—H11378 (2)
C8—O4—Na1114.3 (2)C113—C114—C115120.6 (4)
C10—O5—C11118.2 (3)C113—C114—Na1ii77.1 (2)
C10—O5—Na1120.59 (19)C115—C114—Na1ii115.1 (2)
C11—O5—Na1114.1 (2)C113—C114—H114121 (3)
C13—O6—C12112.4 (3)C115—C114—H114118 (3)
C13—O6—Na1108.73 (19)Na1ii—C114—H11477 (2)
C12—O6—Na1110.9 (2)C4—C115—C114119.6 (4)
N1—C1—S1174.9 (3)C4—C115—H115116 (2)
N2—C2—S2177.3 (3)C114—C115—H115125 (2)
O1—C3—C112126.0 (3)C9—C121—C122120.0 (5)
O1—C3—C4114.5 (3)C9—C121—H121119 (3)
C112—C3—C4119.6 (3)C122—C121—H121120 (3)
O2—C4—C115125.6 (3)C123—C122—C121120.1 (5)
O2—C4—C3114.8 (3)C123—C122—H122117 (3)
C115—C4—C3119.5 (3)C121—C122—H122123 (3)
O2—C5—C6107.1 (3)C122—C123—C124120.9 (5)
O2—C5—H1111.6 (17)C122—C123—H123128 (4)
C6—C5—H1105.0 (17)C124—C123—H123111 (4)
O2—C5—H2108.1 (18)C123—C124—C10119.2 (5)
C6—C5—H2108.7 (19)C123—C124—H124128 (2)
H1—C5—H2116 (2)C10—C124—H124113 (2)
O3—C6—C5107.8 (3)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+2, y, z+1.

Experimental details

Crystal data
Chemical formula[Na(C20H24O6)]2[Pd(SCN)4]
Mr1105.48
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)11.5695 (10), 8.568 (3), 12.976 (2)
α, β, γ (°)81.58 (2), 104.804 (10), 96.85 (2)
V3)1225.7 (5)
Z1
Radiation typeMo Kα
µ (mm1)0.63
Crystal size (mm)0.60 × 0.50 × 0.40
Data collection
DiffractometerEnraf-Nonius CAD-4
diffractometer
Absorption correctionψ scan
(North et al., 1968)
Tmin, Tmax0.834, 0.884
No. of measured, independent and
observed [I > 2σ(I)] reflections
4622, 4406, 3190
Rint0.020
(sin θ/λ)max1)0.599
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.028, 0.080, 1.0
No. of reflections4406
No. of parameters400
H-atom treatmentAll H-atom parameters refined
Δρmax, Δρmin (e Å3)0.41, 0.43

Computer programs: CAD-4 Manual (Enraf-Nonius, 1988), CAD-4 Manual, SDP-Plus (Frenz, 1985), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1996), SHELXL97.

Selected geometric parameters (Å, º) top
Pd1—S12.3241 (9)Na1—O42.853 (2)
Pd1—S22.3319 (8)Na1—O52.841 (3)
S1—C11.663 (4)Na1—O62.559 (2)
S2—C21.664 (4)Na1—C113i3.077 (4)
Na1—N12.423 (3)Na1—C114i3.082 (4)
Na1—O12.572 (2)N1—C11.151 (4)
Na1—O22.559 (2)N2—C21.133 (4)
Na1—O32.597 (2)
S1ii—Pd1—S290.15 (3)O5—Na1—O452.46 (7)
O2—Na1—O364.23 (7)O6—Na1—O164.00 (7)
O2—Na1—O159.40 (7)O6—Na1—O560.17 (7)
O3—Na1—O459.83 (7)C113i—Na1—C114i25.32 (11)
Symmetry codes: (i) x+2, y, z+1; (ii) x+1, y+1, z+1.
 

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