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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806012530/hy2001sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806012530/hy2001Isup2.hkl
Contains datablock I

CCDC reference: 298731

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.014 Å
  • R factor = 0.037
  • wR factor = 0.094
  • Data-to-parameter ratio = 15.6

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 ..................... 0.41 PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C7 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for S1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C15 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Pd1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C13 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.78 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 15
Alert level G ABSTM02_ALERT_3_G 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 0.408 Tmax scaled 0.073 Tmin scaled 0.061
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

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 = 1397.88F(000) = 672
Triclinic, P1Dx = 1.991 Mg m3
a = 8.336 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 11.958 (3) ÅCell parameters from 2559 reflections
c = 12.464 (3) Åθ = 2.5–25.4°
α = 92.043 (4)°µ = 7.91 mm1
β = 105.979 (3)°T = 293 K
γ = 101.316 (4)°Block, red
V = 1165.9 (5) Å30.39 × 0.37 × 0.33 mm
Data collection top
Siemens SMART CCD area-detector
diffractometer
4040 independent reflections
Radiation source: fine-focus sealed tube3276 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
φ and ω scansθmax = 25.0°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 89
Tmin = 0.148, Tmax = 0.180k = 1410
6061 measured reflectionsl = 1414
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)] = 0.037Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.094H-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 parametersΔρmax = 1.54 e Å3
2 restraintsΔρmin = 1.11 e Å3
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
xyzUiso*/Ueq
Pb10.33163 (3)0.21010 (2)0.74201 (2)0.04404 (13)
Pd10.50000.50001.00000.03721 (19)
N10.8441 (11)0.8176 (7)1.0319 (9)0.097 (3)
N20.1144 (10)0.6239 (7)0.7647 (7)0.080 (3)
N30.3864 (9)0.1284 (6)0.5848 (6)0.0574 (18)
O10.6585 (6)0.1889 (5)0.8419 (4)0.0531 (14)
O20.6003 (6)0.3896 (5)0.7636 (5)0.0567 (14)
O30.3021 (7)0.3809 (5)0.6021 (5)0.0602 (15)
O40.0161 (7)0.2255 (5)0.6065 (5)0.0618 (16)
O50.0684 (7)0.0279 (5)0.7002 (5)0.0589 (15)
O60.3855 (7)0.0111 (4)0.8302 (4)0.0520 (13)
S10.5323 (3)0.67377 (19)0.9214 (2)0.0693 (7)
S20.2177 (2)0.44691 (17)0.89047 (18)0.0546 (5)
S30.4577 (4)0.2157 (2)0.4011 (2)0.0882 (8)
C10.7707 (11)0.2941 (8)0.8959 (8)0.071 (3)
H1A0.88530.28210.92770.085*
H1B0.73190.32290.95590.085*
C20.7705 (10)0.3767 (9)0.8117 (9)0.074 (3)
H2A0.84290.44990.84640.088*
H2B0.81500.34950.75380.088*
C30.5935 (12)0.4663 (8)0.6781 (9)0.071 (3)
H3A0.62360.43350.61590.086*
H3B0.67430.53820.70740.086*
C40.4182 (12)0.4865 (7)0.6393 (8)0.067 (3)
H4A0.39140.52450.70030.080*
H4B0.40960.53570.57860.080*
C50.1353 (12)0.3945 (9)0.5431 (8)0.074 (3)
H5A0.14030.43510.47770.089*
H5B0.09300.43950.59120.089*
C60.0186 (13)0.2819 (9)0.5081 (8)0.076 (3)
H6A0.09530.29100.46890.092*
H6B0.05790.23710.45800.092*
C70.1176 (11)0.1231 (9)0.5807 (9)0.083 (3)
H7A0.11010.07600.51800.099*
H7B0.22890.14280.56120.099*
C80.0931 (11)0.0606 (9)0.6825 (9)0.073 (3)
H8A0.09230.10960.74650.088*
H8B0.18460.00660.67170.088*
C90.0905 (12)0.0638 (7)0.7706 (7)0.068 (3)
H9A0.00120.13140.73910.081*
H9B0.08520.04150.84490.081*
C100.2587 (12)0.0881 (7)0.7766 (7)0.059 (2)
H10A0.27590.15330.81910.071*
H10B0.26610.10590.70180.071*
C110.5546 (11)0.0057 (8)0.8484 (8)0.067 (3)
H11A0.57530.02140.77710.080*
H11B0.56930.07090.89140.080*
C120.6743 (11)0.0959 (8)0.9086 (7)0.063 (2)
H12A0.65100.11310.97880.076*
H12B0.78980.08340.92550.076*
C130.7203 (11)0.7552 (7)0.9872 (8)0.054 (2)
C140.1620 (10)0.5550 (7)0.8173 (7)0.055 (2)
C150.4150 (11)0.1668 (7)0.5127 (7)0.056 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.04155 (18)0.04211 (19)0.04621 (19)0.00963 (12)0.00771 (12)0.01068 (12)
Pd10.0301 (4)0.0327 (4)0.0446 (4)0.0052 (3)0.0044 (3)0.0080 (3)
N10.062 (5)0.049 (5)0.147 (9)0.005 (4)0.015 (5)0.011 (5)
N20.062 (5)0.058 (5)0.097 (6)0.013 (4)0.014 (4)0.021 (5)
N30.068 (5)0.047 (4)0.050 (4)0.012 (3)0.008 (3)0.003 (3)
O10.046 (3)0.060 (4)0.050 (3)0.015 (3)0.005 (2)0.009 (3)
O20.044 (3)0.049 (3)0.073 (4)0.001 (3)0.017 (3)0.014 (3)
O30.068 (4)0.046 (3)0.063 (4)0.018 (3)0.010 (3)0.015 (3)
O40.049 (3)0.062 (4)0.059 (3)0.006 (3)0.007 (3)0.009 (3)
O50.051 (3)0.060 (4)0.060 (3)0.002 (3)0.012 (3)0.018 (3)
O60.057 (3)0.039 (3)0.056 (3)0.011 (3)0.009 (3)0.009 (2)
S10.0495 (12)0.0489 (13)0.0860 (16)0.0046 (10)0.0114 (11)0.0309 (12)
S20.0357 (10)0.0436 (11)0.0718 (14)0.0036 (8)0.0033 (9)0.0166 (10)
S30.118 (2)0.0721 (18)0.0824 (18)0.0109 (16)0.0478 (17)0.0119 (15)
C10.045 (5)0.072 (7)0.077 (6)0.014 (5)0.011 (4)0.008 (5)
C20.036 (5)0.072 (6)0.110 (8)0.012 (4)0.016 (5)0.012 (6)
C30.068 (6)0.059 (6)0.091 (7)0.003 (5)0.034 (5)0.027 (5)
C40.085 (7)0.051 (5)0.071 (6)0.015 (5)0.031 (5)0.027 (5)
C50.080 (7)0.083 (7)0.057 (5)0.034 (6)0.004 (5)0.023 (5)
C60.069 (6)0.081 (7)0.063 (6)0.024 (6)0.015 (5)0.014 (5)
C70.031 (4)0.099 (8)0.113 (8)0.016 (5)0.005 (5)0.036 (7)
C80.040 (5)0.085 (7)0.092 (7)0.000 (5)0.025 (5)0.001 (6)
C90.085 (7)0.050 (5)0.051 (5)0.020 (5)0.013 (5)0.014 (4)
C100.082 (6)0.038 (5)0.059 (5)0.015 (4)0.020 (5)0.012 (4)
C110.073 (6)0.061 (6)0.082 (6)0.038 (5)0.028 (5)0.031 (5)
C120.045 (5)0.089 (7)0.059 (5)0.030 (5)0.007 (4)0.028 (5)
C130.045 (5)0.038 (5)0.075 (6)0.012 (4)0.007 (4)0.011 (4)
C140.039 (4)0.055 (5)0.062 (5)0.007 (4)0.001 (4)0.018 (4)
C150.060 (5)0.046 (5)0.062 (5)0.012 (4)0.018 (4)0.000 (4)
Geometric parameters (Å, º) top
Pb1—N32.353 (7)C1—H1A0.9700
Pb1—O52.692 (5)C1—H1B0.9700
Pb1—O62.721 (5)C2—H2A0.9700
Pb1—O22.727 (5)C2—H2B0.9700
Pb1—O12.733 (5)C3—C41.478 (12)
Pb1—O32.736 (5)C3—H3A0.9700
Pb1—O42.752 (5)C3—H3B0.9700
Pd1—S22.3214 (19)C4—H4A0.9700
Pd1—S2i2.3214 (19)C4—H4B0.9700
Pd1—S1i2.329 (2)C5—C61.470 (13)
Pd1—S12.329 (2)C5—H5A0.9700
N1—C131.133 (11)C5—H5B0.9700
N2—C141.136 (10)C6—H6A0.9700
N3—C151.086 (9)C6—H6B0.9700
O1—C121.417 (9)C7—C81.481 (13)
O1—C11.429 (10)C7—H7A0.9700
O2—C21.422 (10)C7—H7B0.9700
O2—C31.427 (10)C8—H8A0.9700
O3—C41.407 (10)C8—H8B0.9700
O3—C51.426 (10)C9—C101.469 (13)
O4—C61.423 (10)C9—H9A0.9700
O4—C71.444 (11)C9—H9B0.9700
O5—C81.437 (10)C10—H10A0.9700
O5—C91.437 (10)C10—H10B0.9700
O6—C111.420 (9)C11—C121.443 (12)
O6—C101.427 (10)C11—H11A0.9700
S1—C131.648 (9)C11—H11B0.9700
S2—C141.675 (8)C12—H12A0.9700
S3—C151.629 (9)C12—H12B0.9700
C1—C21.466 (13)
N3—Pb1—O584.3 (2)C4—C3—H3A110.0
N3—Pb1—O684.2 (2)O2—C3—H3B110.0
O5—Pb1—O660.90 (16)C4—C3—H3B110.0
N3—Pb1—O290.3 (2)H3A—C3—H3B108.3
O5—Pb1—O2174.34 (16)O3—C4—C3109.2 (7)
O6—Pb1—O2120.10 (16)O3—C4—H4A109.8
N3—Pb1—O181.6 (2)C3—C4—H4A109.8
O5—Pb1—O1120.97 (17)O3—C4—H4B109.8
O6—Pb1—O160.80 (16)C3—C4—H4B109.8
O2—Pb1—O159.39 (16)H4A—C4—H4B108.3
N3—Pb1—O378.8 (2)O3—C5—C6110.1 (8)
O5—Pb1—O3117.61 (17)O3—C5—H5A109.6
O6—Pb1—O3162.98 (17)C6—C5—H5A109.6
O2—Pb1—O359.58 (16)O3—C5—H5B109.6
O1—Pb1—O3115.16 (17)C6—C5—H5B109.6
N3—Pb1—O488.6 (2)H5A—C5—H5B108.1
O5—Pb1—O460.22 (17)O4—C6—C5107.6 (7)
O6—Pb1—O4121.09 (17)O4—C6—H6A110.2
O2—Pb1—O4118.31 (17)C5—C6—H6A110.2
O1—Pb1—O4169.88 (17)O4—C6—H6B110.2
O3—Pb1—O459.78 (17)C5—C6—H6B110.2
S2—Pd1—S2i180.0 (1)H6A—C6—H6B108.5
S2—Pd1—S1i89.19 (7)O4—C7—C8106.8 (8)
S2i—Pd1—S1i90.81 (7)O4—C7—H7A110.4
S2—Pd1—S190.81 (7)C8—C7—H7A110.4
S2i—Pd1—S189.19 (7)O4—C7—H7B110.4
S1i—Pd1—S1180.0C8—C7—H7B110.4
C15—N3—Pb1130.7 (7)H7A—C7—H7B108.6
C12—O1—C1113.1 (6)O5—C8—C7106.5 (7)
C12—O1—Pb1115.4 (4)O5—C8—H8A110.4
C1—O1—Pb1113.6 (5)C7—C8—H8A110.4
C2—O2—C3110.7 (7)O5—C8—H8B110.4
C2—O2—Pb1120.3 (5)C7—C8—H8B110.4
C3—O2—Pb1119.4 (5)H8A—C8—H8B108.6
C4—O3—C5112.4 (6)O5—C9—C10107.2 (7)
C4—O3—Pb1117.0 (4)O5—C9—H9A110.3
C5—O3—Pb1118.6 (5)C10—C9—H9A110.3
C6—O4—C7110.6 (7)O5—C9—H9B110.3
C6—O4—Pb1115.1 (5)C10—C9—H9B110.3
C7—O4—Pb1117.5 (5)H9A—C9—H9B108.5
C8—O5—C9114.7 (7)O6—C10—C9107.9 (7)
C8—O5—Pb1112.4 (5)O6—C10—H10A110.1
C9—O5—Pb1116.7 (5)C9—C10—H10A110.1
C11—O6—C10112.8 (6)O6—C10—H10B110.1
C11—O6—Pb1114.6 (4)C9—C10—H10B110.1
C10—O6—Pb1114.6 (4)H10A—C10—H10B108.4
C13—S1—Pd1109.6 (3)O6—C11—C12109.3 (7)
C14—S2—Pd1110.0 (3)O6—C11—H11A109.8
O1—C1—C2108.0 (7)C12—C11—H11A109.8
O1—C1—H1A110.1O6—C11—H11B109.8
C2—C1—H1A110.1C12—C11—H11B109.8
O1—C1—H1B110.1H11A—C11—H11B108.3
C2—C1—H1B110.1O1—C12—C11109.2 (7)
H1A—C1—H1B108.4O1—C12—H12A109.8
O2—C2—C1108.9 (7)C11—C12—H12A109.8
O2—C2—H2A109.9O1—C12—H12B109.8
C1—C2—H2A109.9C11—C12—H12B109.8
O2—C2—H2B109.9H12A—C12—H12B108.3
C1—C2—H2B109.9N1—C13—S1175.2 (8)
H2A—C2—H2B108.3N2—C14—S2175.7 (8)
O2—C3—C4108.6 (7)N3—C15—S3176.0 (9)
O2—C3—H3A110.0
Symmetry code: (i) x+1, y+1, z+2.
 

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