metal-organic compounds
The title complex, bis[(1,4,7,10,13,16-hexaoxacyclooctadecane-κ6O)(isothiocyanato-κN)lead(II)] tetrakis(thiocyanato-κS)palladate(II), [Pb(NCS)(C12H24O6)]2[Pd(NCS)4], has been synthesized by the reaction of PdCl2 and Pb(SCN)2 with 18-crown-6 in 1,2-dichloroethane. The complex is composed of two [Pb(18-crown-6)(NCS)]+ complex cations and one [Pd(SCN)4]2− complex anion. The Pd atom lies on a centre of symmetry. The cation and anion are associated through a weak interaction between the Pb atom of the cation and an N atom of the anion.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806012530/hy2001sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806012530/hy2001Isup2.hkl |
CCDC reference: 298731
Computing details top
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.
bis[(1,4,7,10,13,16-hexaoxacyclooctadecane-κ6O)(isothiocyanato-
κN)lead(II)] tetrakis(thiocyanato-κS)palladium(II) top
Crystal data top
[Pb(NCS)(C12H24O6)]2[Pd(NCS)4] | Z = 1 |
Mr = 1397.88 | F(000) = 672 |
Triclinic, P1 | Dx = 1.991 Mg m−3 |
a = 8.336 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 11.958 (3) Å | Cell parameters from 2559 reflections |
c = 12.464 (3) Å | θ = 2.5–25.4° |
α = 92.043 (4)° | µ = 7.91 mm−1 |
β = 105.979 (3)° | T = 293 K |
γ = 101.316 (4)° | Block, red |
V = 1165.9 (5) Å3 | 0.39 × 0.37 × 0.33 mm |
Data collection top
Siemens SMART CCD area-detector diffractometer | 4040 independent reflections |
Radiation source: fine-focus sealed tube | 3276 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
φ and ω scans | θmax = 25.0°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −8→9 |
Tmin = 0.148, Tmax = 0.180 | k = −14→10 |
6061 measured reflections | l = −14→14 |
Refinement top
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)] = 0.037 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.094 | H-atom parameters constrained |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0542P)2] where P = (Fo2 + 2Fc2)/3 |
4040 reflections | (Δ/σ)max = 0.001 |
259 parameters | Δρmax = 1.54 e Å−3 |
2 restraints | Δρmin = −1.11 e Å−3 |
Special details top
Experimental. FT—IR (ν, cm-1): 2910 (m), 2818 (m), 2110 (s), 1658 (m), 1457 (m), 1408 (m), 1280 (s), 1126 (s), 958 (m), 836 (m), 530 (w). |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Pb1 | 0.33163 (3) | 0.21010 (2) | 0.74201 (2) | 0.04404 (13) | |
Pd1 | 0.5000 | 0.5000 | 1.0000 | 0.03721 (19) | |
N1 | 0.8441 (11) | 0.8176 (7) | 1.0319 (9) | 0.097 (3) | |
N2 | 0.1144 (10) | 0.6239 (7) | 0.7647 (7) | 0.080 (3) | |
N3 | 0.3864 (9) | 0.1284 (6) | 0.5848 (6) | 0.0574 (18) | |
O1 | 0.6585 (6) | 0.1889 (5) | 0.8419 (4) | 0.0531 (14) | |
O2 | 0.6003 (6) | 0.3896 (5) | 0.7636 (5) | 0.0567 (14) | |
O3 | 0.3021 (7) | 0.3809 (5) | 0.6021 (5) | 0.0602 (15) | |
O4 | 0.0161 (7) | 0.2255 (5) | 0.6065 (5) | 0.0618 (16) | |
O5 | 0.0684 (7) | 0.0279 (5) | 0.7002 (5) | 0.0589 (15) | |
O6 | 0.3855 (7) | 0.0111 (4) | 0.8302 (4) | 0.0520 (13) | |
S1 | 0.5323 (3) | 0.67377 (19) | 0.9214 (2) | 0.0693 (7) | |
S2 | 0.2177 (2) | 0.44691 (17) | 0.89047 (18) | 0.0546 (5) | |
S3 | 0.4577 (4) | 0.2157 (2) | 0.4011 (2) | 0.0882 (8) | |
C1 | 0.7707 (11) | 0.2941 (8) | 0.8959 (8) | 0.071 (3) | |
H1A | 0.8853 | 0.2821 | 0.9277 | 0.085* | |
H1B | 0.7319 | 0.3229 | 0.9559 | 0.085* | |
C2 | 0.7705 (10) | 0.3767 (9) | 0.8117 (9) | 0.074 (3) | |
H2A | 0.8429 | 0.4499 | 0.8464 | 0.088* | |
H2B | 0.8150 | 0.3495 | 0.7538 | 0.088* | |
C3 | 0.5935 (12) | 0.4663 (8) | 0.6781 (9) | 0.071 (3) | |
H3A | 0.6236 | 0.4335 | 0.6159 | 0.086* | |
H3B | 0.6743 | 0.5382 | 0.7074 | 0.086* | |
C4 | 0.4182 (12) | 0.4865 (7) | 0.6393 (8) | 0.067 (3) | |
H4A | 0.3914 | 0.5245 | 0.7003 | 0.080* | |
H4B | 0.4096 | 0.5357 | 0.5786 | 0.080* | |
C5 | 0.1353 (12) | 0.3945 (9) | 0.5431 (8) | 0.074 (3) | |
H5A | 0.1403 | 0.4351 | 0.4777 | 0.089* | |
H5B | 0.0930 | 0.4395 | 0.5912 | 0.089* | |
C6 | 0.0186 (13) | 0.2819 (9) | 0.5081 (8) | 0.076 (3) | |
H6A | −0.0953 | 0.2910 | 0.4689 | 0.092* | |
H6B | 0.0579 | 0.2371 | 0.4580 | 0.092* | |
C7 | −0.1176 (11) | 0.1231 (9) | 0.5807 (9) | 0.083 (3) | |
H7A | −0.1101 | 0.0760 | 0.5180 | 0.099* | |
H7B | −0.2289 | 0.1428 | 0.5612 | 0.099* | |
C8 | −0.0931 (11) | 0.0606 (9) | 0.6825 (9) | 0.073 (3) | |
H8A | −0.0923 | 0.1096 | 0.7465 | 0.088* | |
H8B | −0.1846 | −0.0066 | 0.6717 | 0.088* | |
C9 | 0.0905 (12) | −0.0638 (7) | 0.7706 (7) | 0.068 (3) | |
H9A | 0.0012 | −0.1314 | 0.7391 | 0.081* | |
H9B | 0.0852 | −0.0415 | 0.8449 | 0.081* | |
C10 | 0.2587 (12) | −0.0881 (7) | 0.7766 (7) | 0.059 (2) | |
H10A | 0.2759 | −0.1533 | 0.8191 | 0.071* | |
H10B | 0.2661 | −0.1059 | 0.7018 | 0.071* | |
C11 | 0.5546 (11) | −0.0057 (8) | 0.8484 (8) | 0.067 (3) | |
H11A | 0.5753 | −0.0214 | 0.7771 | 0.080* | |
H11B | 0.5693 | −0.0709 | 0.8914 | 0.080* | |
C12 | 0.6743 (11) | 0.0959 (8) | 0.9086 (7) | 0.063 (2) | |
H12A | 0.6510 | 0.1131 | 0.9788 | 0.076* | |
H12B | 0.7898 | 0.0834 | 0.9255 | 0.076* | |
C13 | 0.7203 (11) | 0.7552 (7) | 0.9872 (8) | 0.054 (2) | |
C14 | 0.1620 (10) | 0.5550 (7) | 0.8173 (7) | 0.055 (2) | |
C15 | 0.4150 (11) | 0.1668 (7) | 0.5127 (7) | 0.056 (2) |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Pb1 | 0.04155 (18) | 0.04211 (19) | 0.04621 (19) | 0.00963 (12) | 0.00771 (12) | 0.01068 (12) |
Pd1 | 0.0301 (4) | 0.0327 (4) | 0.0446 (4) | 0.0052 (3) | 0.0044 (3) | 0.0080 (3) |
N1 | 0.062 (5) | 0.049 (5) | 0.147 (9) | 0.005 (4) | −0.015 (5) | 0.011 (5) |
N2 | 0.062 (5) | 0.058 (5) | 0.097 (6) | 0.013 (4) | −0.014 (4) | 0.021 (5) |
N3 | 0.068 (5) | 0.047 (4) | 0.050 (4) | 0.012 (3) | 0.008 (3) | 0.003 (3) |
O1 | 0.046 (3) | 0.060 (4) | 0.050 (3) | 0.015 (3) | 0.005 (2) | 0.009 (3) |
O2 | 0.044 (3) | 0.049 (3) | 0.073 (4) | −0.001 (3) | 0.017 (3) | 0.014 (3) |
O3 | 0.068 (4) | 0.046 (3) | 0.063 (4) | 0.018 (3) | 0.010 (3) | 0.015 (3) |
O4 | 0.049 (3) | 0.062 (4) | 0.059 (3) | 0.006 (3) | −0.007 (3) | 0.009 (3) |
O5 | 0.051 (3) | 0.060 (4) | 0.060 (3) | 0.002 (3) | 0.012 (3) | 0.018 (3) |
O6 | 0.057 (3) | 0.039 (3) | 0.056 (3) | 0.011 (3) | 0.009 (3) | 0.009 (2) |
S1 | 0.0495 (12) | 0.0489 (13) | 0.0860 (16) | −0.0046 (10) | −0.0114 (11) | 0.0309 (12) |
S2 | 0.0357 (10) | 0.0436 (11) | 0.0718 (14) | 0.0036 (8) | −0.0033 (9) | 0.0166 (10) |
S3 | 0.118 (2) | 0.0721 (18) | 0.0824 (18) | 0.0109 (16) | 0.0478 (17) | 0.0119 (15) |
C1 | 0.045 (5) | 0.072 (7) | 0.077 (6) | 0.014 (5) | −0.011 (4) | −0.008 (5) |
C2 | 0.036 (5) | 0.072 (6) | 0.110 (8) | 0.012 (4) | 0.016 (5) | 0.012 (6) |
C3 | 0.068 (6) | 0.059 (6) | 0.091 (7) | 0.003 (5) | 0.034 (5) | 0.027 (5) |
C4 | 0.085 (7) | 0.051 (5) | 0.071 (6) | 0.015 (5) | 0.031 (5) | 0.027 (5) |
C5 | 0.080 (7) | 0.083 (7) | 0.057 (5) | 0.034 (6) | 0.004 (5) | 0.023 (5) |
C6 | 0.069 (6) | 0.081 (7) | 0.063 (6) | 0.024 (6) | −0.015 (5) | 0.014 (5) |
C7 | 0.031 (4) | 0.099 (8) | 0.113 (8) | 0.016 (5) | 0.005 (5) | 0.036 (7) |
C8 | 0.040 (5) | 0.085 (7) | 0.092 (7) | 0.000 (5) | 0.025 (5) | 0.001 (6) |
C9 | 0.085 (7) | 0.050 (5) | 0.051 (5) | −0.020 (5) | 0.013 (5) | 0.014 (4) |
C10 | 0.082 (6) | 0.038 (5) | 0.059 (5) | 0.015 (4) | 0.020 (5) | 0.012 (4) |
C11 | 0.073 (6) | 0.061 (6) | 0.082 (6) | 0.038 (5) | 0.028 (5) | 0.031 (5) |
C12 | 0.045 (5) | 0.089 (7) | 0.059 (5) | 0.030 (5) | 0.007 (4) | 0.028 (5) |
C13 | 0.045 (5) | 0.038 (5) | 0.075 (6) | 0.012 (4) | 0.007 (4) | 0.011 (4) |
C14 | 0.039 (4) | 0.055 (5) | 0.062 (5) | 0.007 (4) | −0.001 (4) | 0.018 (4) |
C15 | 0.060 (5) | 0.046 (5) | 0.062 (5) | 0.012 (4) | 0.018 (4) | 0.000 (4) |
Geometric parameters (Å, º) top
Pb1—N3 | 2.353 (7) | C1—H1A | 0.9700 |
Pb1—O5 | 2.692 (5) | C1—H1B | 0.9700 |
Pb1—O6 | 2.721 (5) | C2—H2A | 0.9700 |
Pb1—O2 | 2.727 (5) | C2—H2B | 0.9700 |
Pb1—O1 | 2.733 (5) | C3—C4 | 1.478 (12) |
Pb1—O3 | 2.736 (5) | C3—H3A | 0.9700 |
Pb1—O4 | 2.752 (5) | C3—H3B | 0.9700 |
Pd1—S2 | 2.3214 (19) | C4—H4A | 0.9700 |
Pd1—S2i | 2.3214 (19) | C4—H4B | 0.9700 |
Pd1—S1i | 2.329 (2) | C5—C6 | 1.470 (13) |
Pd1—S1 | 2.329 (2) | C5—H5A | 0.9700 |
N1—C13 | 1.133 (11) | C5—H5B | 0.9700 |
N2—C14 | 1.136 (10) | C6—H6A | 0.9700 |
N3—C15 | 1.086 (9) | C6—H6B | 0.9700 |
O1—C12 | 1.417 (9) | C7—C8 | 1.481 (13) |
O1—C1 | 1.429 (10) | C7—H7A | 0.9700 |
O2—C2 | 1.422 (10) | C7—H7B | 0.9700 |
O2—C3 | 1.427 (10) | C8—H8A | 0.9700 |
O3—C4 | 1.407 (10) | C8—H8B | 0.9700 |
O3—C5 | 1.426 (10) | C9—C10 | 1.469 (13) |
O4—C6 | 1.423 (10) | C9—H9A | 0.9700 |
O4—C7 | 1.444 (11) | C9—H9B | 0.9700 |
O5—C8 | 1.437 (10) | C10—H10A | 0.9700 |
O5—C9 | 1.437 (10) | C10—H10B | 0.9700 |
O6—C11 | 1.420 (9) | C11—C12 | 1.443 (12) |
O6—C10 | 1.427 (10) | C11—H11A | 0.9700 |
S1—C13 | 1.648 (9) | C11—H11B | 0.9700 |
S2—C14 | 1.675 (8) | C12—H12A | 0.9700 |
S3—C15 | 1.629 (9) | C12—H12B | 0.9700 |
C1—C2 | 1.466 (13) | ||
N3—Pb1—O5 | 84.3 (2) | C4—C3—H3A | 110.0 |
N3—Pb1—O6 | 84.2 (2) | O2—C3—H3B | 110.0 |
O5—Pb1—O6 | 60.90 (16) | C4—C3—H3B | 110.0 |
N3—Pb1—O2 | 90.3 (2) | H3A—C3—H3B | 108.3 |
O5—Pb1—O2 | 174.34 (16) | O3—C4—C3 | 109.2 (7) |
O6—Pb1—O2 | 120.10 (16) | O3—C4—H4A | 109.8 |
N3—Pb1—O1 | 81.6 (2) | C3—C4—H4A | 109.8 |
O5—Pb1—O1 | 120.97 (17) | O3—C4—H4B | 109.8 |
O6—Pb1—O1 | 60.80 (16) | C3—C4—H4B | 109.8 |
O2—Pb1—O1 | 59.39 (16) | H4A—C4—H4B | 108.3 |
N3—Pb1—O3 | 78.8 (2) | O3—C5—C6 | 110.1 (8) |
O5—Pb1—O3 | 117.61 (17) | O3—C5—H5A | 109.6 |
O6—Pb1—O3 | 162.98 (17) | C6—C5—H5A | 109.6 |
O2—Pb1—O3 | 59.58 (16) | O3—C5—H5B | 109.6 |
O1—Pb1—O3 | 115.16 (17) | C6—C5—H5B | 109.6 |
N3—Pb1—O4 | 88.6 (2) | H5A—C5—H5B | 108.1 |
O5—Pb1—O4 | 60.22 (17) | O4—C6—C5 | 107.6 (7) |
O6—Pb1—O4 | 121.09 (17) | O4—C6—H6A | 110.2 |
O2—Pb1—O4 | 118.31 (17) | C5—C6—H6A | 110.2 |
O1—Pb1—O4 | 169.88 (17) | O4—C6—H6B | 110.2 |
O3—Pb1—O4 | 59.78 (17) | C5—C6—H6B | 110.2 |
S2—Pd1—S2i | 180.0 (1) | H6A—C6—H6B | 108.5 |
S2—Pd1—S1i | 89.19 (7) | O4—C7—C8 | 106.8 (8) |
S2i—Pd1—S1i | 90.81 (7) | O4—C7—H7A | 110.4 |
S2—Pd1—S1 | 90.81 (7) | C8—C7—H7A | 110.4 |
S2i—Pd1—S1 | 89.19 (7) | O4—C7—H7B | 110.4 |
S1i—Pd1—S1 | 180.0 | C8—C7—H7B | 110.4 |
C15—N3—Pb1 | 130.7 (7) | H7A—C7—H7B | 108.6 |
C12—O1—C1 | 113.1 (6) | O5—C8—C7 | 106.5 (7) |
C12—O1—Pb1 | 115.4 (4) | O5—C8—H8A | 110.4 |
C1—O1—Pb1 | 113.6 (5) | C7—C8—H8A | 110.4 |
C2—O2—C3 | 110.7 (7) | O5—C8—H8B | 110.4 |
C2—O2—Pb1 | 120.3 (5) | C7—C8—H8B | 110.4 |
C3—O2—Pb1 | 119.4 (5) | H8A—C8—H8B | 108.6 |
C4—O3—C5 | 112.4 (6) | O5—C9—C10 | 107.2 (7) |
C4—O3—Pb1 | 117.0 (4) | O5—C9—H9A | 110.3 |
C5—O3—Pb1 | 118.6 (5) | C10—C9—H9A | 110.3 |
C6—O4—C7 | 110.6 (7) | O5—C9—H9B | 110.3 |
C6—O4—Pb1 | 115.1 (5) | C10—C9—H9B | 110.3 |
C7—O4—Pb1 | 117.5 (5) | H9A—C9—H9B | 108.5 |
C8—O5—C9 | 114.7 (7) | O6—C10—C9 | 107.9 (7) |
C8—O5—Pb1 | 112.4 (5) | O6—C10—H10A | 110.1 |
C9—O5—Pb1 | 116.7 (5) | C9—C10—H10A | 110.1 |
C11—O6—C10 | 112.8 (6) | O6—C10—H10B | 110.1 |
C11—O6—Pb1 | 114.6 (4) | C9—C10—H10B | 110.1 |
C10—O6—Pb1 | 114.6 (4) | H10A—C10—H10B | 108.4 |
C13—S1—Pd1 | 109.6 (3) | O6—C11—C12 | 109.3 (7) |
C14—S2—Pd1 | 110.0 (3) | O6—C11—H11A | 109.8 |
O1—C1—C2 | 108.0 (7) | C12—C11—H11A | 109.8 |
O1—C1—H1A | 110.1 | O6—C11—H11B | 109.8 |
C2—C1—H1A | 110.1 | C12—C11—H11B | 109.8 |
O1—C1—H1B | 110.1 | H11A—C11—H11B | 108.3 |
C2—C1—H1B | 110.1 | O1—C12—C11 | 109.2 (7) |
H1A—C1—H1B | 108.4 | O1—C12—H12A | 109.8 |
O2—C2—C1 | 108.9 (7) | C11—C12—H12A | 109.8 |
O2—C2—H2A | 109.9 | O1—C12—H12B | 109.8 |
C1—C2—H2A | 109.9 | C11—C12—H12B | 109.8 |
O2—C2—H2B | 109.9 | H12A—C12—H12B | 108.3 |
C1—C2—H2B | 109.9 | N1—C13—S1 | 175.2 (8) |
H2A—C2—H2B | 108.3 | N2—C14—S2 | 175.7 (8) |
O2—C3—C4 | 108.6 (7) | N3—C15—S3 | 176.0 (9) |
O2—C3—H3A | 110.0 |
Symmetry code: (i) −x+1, −y+1, −z+2. |