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Acta Crystallogr Sect E Struct Rep Online. 2009 July 1; 65(Pt 7): m755.
Published online 2009 June 10. doi:  10.1107/S1600536809021370
PMCID: PMC2969246

Tripotassium bis­(acetato-κ2 O,O′)(thio­cyanato-κN)plumbate(II) dithio­cyanate

Abstract

In the crystal structure of the title salt, K3[Pb(CH3COO)2(NCS)](NCS)2, the [Pb(CH3COO)2(NCS)] anion exists as a covalently bonded entity in which the acetate anions chelate in an anisobidentate manner. The Pb atom shows a distorted ψ-octa­hedral coordination to four acetate O atoms and one isocyanate N atom, with the stereochemically active lone pair occupying one of the six sites. When the three longer Pb(...)S inter­actions are considered, the eight-coordinate geometry is based on a dodeca­hedron. The Pb(CH3COO)2(NCS)] anion has mirror symmetry. The potassium cations connect the other constituents into a three-dimensional network through electrostatic K(...)N and K(...)S inter­actions.

Related literature

In [K6Pb6(CH3CO2)12(NCS)2](NCS)4, the acetate groups link the lead(II) atoms into a chain; see: Morsali & Mahjoub (2004 [triangle]).

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Object name is e-65-0m755-scheme1.jpg

Experimental

Crystal data

  • K3[Pb(C2H3O2)2(NCS)](NCS)2
  • M r = 616.82
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-65-0m755-efi1.jpg
  • a = 6.1968 (1) Å
  • b = 19.2499 (3) Å
  • c = 7.6354 (1) Å
  • β = 106.982 (1)°
  • V = 871.10 (2) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 10.77 mm−1
  • T = 140 K
  • 0.25 × 0.20 × 0.08 mm

Data collection

  • Bruker SMART APEX diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996 [triangle]) T min = 0.174, T max = 0.480 (expected range = 0.153–0.422)
  • 6058 measured reflections
  • 2045 independent reflections
  • 2015 reflections with I > 2σ(I)
  • R int = 0.023

Refinement

  • R[F 2 > 2σ(F 2)] = 0.022
  • wR(F 2) = 0.056
  • S = 1.16
  • 2045 reflections
  • 104 parameters
  • H-atom parameters constrained
  • Δρmax = 0.81 e Å−3
  • Δρmin = −2.00 e Å−3

Data collection: APEX2 (Bruker, 2008 [triangle]); cell refinement: SAINT (Bruker, 2008 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: X-SEED (Barbour, 2001 [triangle]); software used to prepare material for publication: publCIF (Westrip, 2009 [triangle]).

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809021370/tk2472sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809021370/tk2472Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

I thank Dr Maryam Ranjbar of the Iranian Research Organization for Science and Technology for providing the crystal, and the University of Malaya for supporting this study.

supplementary crystallographic information

Experimental

2,4-Diamino-6-(1-piperidinyl)-2,4-pyrimidine N-oxide (commercial name: minoxidil) (0.5 mmol, 0.10 g), lead(II) acetate (0.5 mmol, 0.17 g) and potassium thiocyanate (1 mmol, 0.10 g) were dissolved in methanol (100 ml). The solution was concentrated to a smaller volume and this was mixed with a similar volume of chloroform. Colorless prisms separated after several days.

Refinement

Hydrogen atoms were placed at calculated positions (C–H 0.98 Å) and were treated as riding on the carbon atom with U(H) set to 1.5Ueq(C). The final difference Fourier map had a deep hole at 1 Å from N1.

Figures

Fig. 1.
Thermal ellipsoid plot (Barbour, 2001) of a portion of the polymeric structure of K3Pb(NCS)3(CH3CO2)2 at the 70% probability level. Hydrogen atoms are drawn as spheres of arbitrary radius. Symmetry operation i: x, 1.5-y, z.
Fig. 2.
Detail showing the dodecahedral geometry of the Pb(II) atom.

Crystal data

K3[Pb(C2H3O2)2(NCS)](NCS)2F(000) = 576
Mr = 616.82Dx = 2.352 Mg m3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 4971 reflections
a = 6.1968 (1) Åθ = 2.9–28.3°
b = 19.2499 (3) ŵ = 10.77 mm1
c = 7.6354 (1) ÅT = 140 K
β = 106.982 (1)°Block, colorless
V = 871.10 (2) Å30.25 × 0.20 × 0.08 mm
Z = 2

Data collection

Bruker SMART APEX diffractometer2045 independent reflections
Radiation source: fine-focus sealed tube2015 reflections with I > 2σ(I)
graphiteRint = 0.023
ω scansθmax = 27.5°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −7→8
Tmin = 0.174, Tmax = 0.480k = −25→25
6058 measured reflectionsl = −9→9

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.022Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.056H-atom parameters constrained
S = 1.16w = 1/[σ2(Fo2) + (0.03P)2 + 1.3438P] where P = (Fo2 + 2Fc2)/3
2045 reflections(Δ/σ)max = 0.001
104 parametersΔρmax = 0.81 e Å3
0 restraintsΔρmin = −2.00 e Å3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
Pb10.41686 (3)0.75000.47400 (2)0.01158 (7)
K10.85392 (14)0.59423 (4)0.42518 (12)0.01948 (17)
K20.74409 (19)0.75000.09371 (15)0.0160 (2)
S11.1475 (2)0.75000.8492 (2)0.0247 (3)
S20.65682 (16)0.62677 (5)0.76528 (14)0.01949 (19)
N10.8449 (7)0.75000.4972 (6)0.0151 (9)
N20.2738 (6)0.54336 (19)0.6214 (6)0.0289 (8)
O10.4696 (4)0.66654 (13)0.2532 (4)0.0162 (5)
O20.1161 (4)0.66405 (13)0.2588 (4)0.0171 (5)
C10.2743 (6)0.63941 (18)0.2063 (5)0.0146 (7)
C20.2360 (7)0.5741 (2)0.0917 (6)0.0236 (8)
H2A0.22830.53410.16890.035*
H2B0.36090.56780.03880.035*
H2C0.09400.5782−0.00690.035*
C30.9724 (8)0.75000.6432 (7)0.0142 (10)
C40.4309 (6)0.57822 (19)0.6821 (5)0.0180 (7)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Pb10.01294 (11)0.01291 (10)0.01004 (11)0.0000.00516 (7)0.000
K10.0164 (4)0.0153 (4)0.0286 (4)0.0018 (3)0.0095 (3)0.0037 (3)
K20.0168 (5)0.0192 (5)0.0129 (5)0.0000.0058 (4)0.000
S10.0184 (6)0.0388 (8)0.0144 (6)0.0000.0011 (5)0.000
S20.0194 (4)0.0185 (4)0.0210 (5)−0.0041 (3)0.0065 (4)−0.0016 (4)
N10.0119 (19)0.020 (2)0.013 (2)0.0000.0035 (17)0.000
N20.0217 (18)0.0232 (17)0.036 (2)−0.0019 (14)0.0000 (16)0.0014 (15)
O10.0136 (12)0.0192 (12)0.0162 (13)−0.0004 (9)0.0050 (10)−0.0031 (10)
O20.0142 (12)0.0194 (12)0.0191 (13)0.0017 (9)0.0071 (10)−0.0002 (10)
C10.0171 (16)0.0143 (15)0.0107 (16)0.0017 (12)0.0015 (13)0.0049 (13)
C20.0234 (19)0.0199 (18)0.025 (2)−0.0010 (15)0.0034 (17)−0.0079 (16)
C30.012 (2)0.012 (2)0.020 (3)0.0000.008 (2)0.000
C40.0175 (18)0.0142 (16)0.0205 (19)0.0032 (13)0.0031 (15)0.0034 (14)

Geometric parameters (Å, °)

Pb1—O12.419 (3)K2—S2vi3.3788 (13)
Pb1—O1i2.419 (3)K2—S2vii3.3788 (13)
Pb1—O22.669 (3)S1—C31.630 (5)
Pb1—O2i2.669 (3)S2—C41.649 (4)
Pb1—N12.606 (4)S2—K2viii3.3788 (13)
Pb1—S1ii3.713 (1)N1—C31.163 (7)
Pb1—S23.294 (1)N1—K1i3.0520 (12)
Pb1—S2i3.294 (1)N2—C41.162 (5)
K1—O2iii2.696 (3)N2—K1iv2.757 (4)
K1—O12.740 (3)N2—K1ii2.774 (4)
K1—N2iv2.757 (4)O1—C11.270 (4)
K1—N2iii2.774 (4)O2—C11.255 (5)
K1—N13.0520 (12)O2—K1ii2.696 (3)
K1—S23.2373 (13)O2—K2ii2.818 (3)
K2—O2v2.818 (3)C1—C21.509 (5)
K2—O2iii2.818 (3)C2—H2A0.9800
K2—O12.858 (3)C2—H2B0.9800
K2—O1i2.858 (3)C2—H2C0.9800
K2—N12.959 (5)C3—K1i3.404 (3)
O1—Pb1—O1i83.23 (13)O2v—K2—S1ix143.98 (5)
O1—Pb1—N172.87 (9)O2iii—K2—S1ix143.98 (5)
O1i—Pb1—N172.87 (9)O1—K2—S1ix64.83 (6)
O1—Pb1—O251.04 (8)O1i—K2—S1ix64.83 (6)
O1i—Pb1—O2101.23 (8)N1—K2—S1ix114.20 (9)
N1—Pb1—O2123.76 (9)S2vi—K2—S1ix72.51 (3)
O1—Pb1—O2i101.23 (8)S2vii—K2—S1ix72.51 (3)
O1i—Pb1—O2i51.04 (8)S1vi—K2—S1ix120.08 (5)
N1—Pb1—O2i123.76 (9)C3—S1—K2viii97.79 (19)
O2—Pb1—O2i76.62 (11)C3—S1—K2x142.1 (2)
O2iii—K1—O194.59 (8)K2viii—S1—K2x120.08 (5)
O2iii—K1—N2iv127.44 (11)C4—S2—K193.34 (15)
O1—K1—N2iv104.45 (9)C4—S2—K2viii128.15 (15)
O2iii—K1—N2iii80.28 (10)K1—S2—K2viii135.65 (4)
O1—K1—N2iii170.07 (10)C3—N1—Pb1117.3 (4)
N2iv—K1—N2iii85.36 (11)C3—N1—K2151.1 (4)
O2iii—K1—N168.92 (10)Pb1—N1—K291.61 (13)
O1—K1—N161.85 (10)C3—N1—K197.45 (9)
N2iv—K1—N1161.31 (12)Pb1—N1—K193.42 (8)
N2iii—K1—N1108.25 (11)K2—N1—K179.74 (8)
O2iii—K1—S2134.60 (6)C3—N1—K1i97.45 (9)
O1—K1—S278.90 (6)Pb1—N1—K1i93.42 (8)
N2iv—K1—S297.35 (9)K2—N1—K1i79.74 (8)
N2iii—K1—S298.58 (9)K1—N1—K1i158.52 (17)
N1—K1—S268.55 (9)C4—N2—K1iv141.4 (3)
O2v—K2—O2iii71.90 (11)C4—N2—K1ii123.8 (3)
O2v—K2—O1130.58 (9)K1iv—N2—K1ii94.64 (11)
O2iii—K2—O189.45 (8)C1—O1—Pb199.1 (2)
O2v—K2—O1i89.45 (8)C1—O1—K1123.3 (2)
O2iii—K2—O1i130.58 (9)Pb1—O1—K1106.18 (9)
O1—K2—O1i68.41 (10)C1—O1—K2138.4 (2)
O2v—K2—N168.78 (9)Pb1—O1—K298.16 (8)
O2iii—K2—N168.78 (9)K1—O1—K286.99 (8)
O1—K2—N161.80 (9)C1—O2—Pb187.8 (2)
O1i—K2—N161.80 (9)C1—O2—K1ii126.6 (2)
O2v—K2—S2vi132.59 (7)Pb1—O2—K1ii115.30 (10)
O2iii—K2—S2vi81.51 (6)C1—O2—K2ii133.8 (2)
O1—K2—S2vi86.29 (6)Pb1—O2—K2ii104.14 (8)
O1i—K2—S2vi136.45 (7)K1ii—O2—K2ii88.66 (8)
N1—K2—S2vi135.40 (2)O2—C1—O1121.6 (3)
O2v—K2—S2vii81.51 (6)O2—C1—C2119.6 (3)
O2iii—K2—S2vii132.59 (7)O1—C1—C2118.8 (3)
O1—K2—S2vii136.45 (6)C1—C2—H2A109.5
O1i—K2—S2vii86.29 (6)C1—C2—H2B109.5
N1—K2—S2vii135.40 (2)H2A—C2—H2B109.5
S2vi—K2—S2vii89.19 (4)C1—C2—H2C109.5
O2v—K2—S1vi67.87 (6)H2A—C2—H2C109.5
O2iii—K2—S1vi67.87 (6)H2B—C2—H2C109.5
O1—K2—S1vi145.78 (5)N1—C3—S1179.1 (5)
O1i—K2—S1vi145.78 (5)N1—C3—K1i62.76 (9)
N1—K2—S1vi125.72 (9)S1—C3—K1i117.37 (8)
S2vi—K2—S1vi65.92 (3)N2—C4—S2178.7 (4)
S2vii—K2—S1vi65.92 (3)
O2iii—K1—S2—C4150.92 (15)O1i—Pb1—O1—C1−114.5 (2)
O1—K1—S2—C465.45 (14)N1—Pb1—O1—C1171.4 (2)
N2iv—K1—S2—C4−37.91 (15)O2—Pb1—O1—C1−4.14 (19)
N2iii—K1—S2—C4−124.30 (15)O2i—Pb1—O1—C1−66.5 (2)
N1—K1—S2—C4129.38 (15)O1i—Pb1—O1—K1116.73 (7)
O2iii—K1—S2—K2viii−9.98 (11)N1—Pb1—O1—K142.61 (10)
O1—K1—S2—K2viii−95.45 (7)O2—Pb1—O1—K1−132.90 (14)
N2iv—K1—S2—K2viii161.19 (9)O2i—Pb1—O1—K1164.73 (9)
N2iii—K1—S2—K2viii74.80 (9)O1i—Pb1—O1—K227.51 (11)
N1—K1—S2—K2viii−31.52 (10)N1—Pb1—O1—K2−46.61 (9)
O1—Pb1—N1—C3−135.98 (7)O2—Pb1—O1—K2137.88 (13)
O1i—Pb1—N1—C3135.98 (7)O2i—Pb1—O1—K275.51 (9)
O2—Pb1—N1—C3−131.78 (8)O2iii—K1—O1—C1145.2 (3)
O2i—Pb1—N1—C3131.78 (8)N2iv—K1—O1—C114.7 (3)
O1—Pb1—N1—K244.02 (7)N1—K1—O1—C1−151.6 (3)
O1i—Pb1—N1—K2−44.02 (7)S2—K1—O1—C1−80.2 (3)
O2—Pb1—N1—K248.22 (8)O2iii—K1—O1—Pb1−101.92 (10)
O2i—Pb1—N1—K2−48.22 (8)N2iv—K1—O1—Pb1127.50 (12)
O1—Pb1—N1—K1−35.79 (10)N1—K1—O1—Pb1−38.80 (11)
O1i—Pb1—N1—K1−123.83 (13)S2—K1—O1—Pb132.68 (7)
O2—Pb1—N1—K1−31.60 (15)O2iii—K1—O1—K2−4.30 (8)
O2i—Pb1—N1—K1−128.03 (8)N2iv—K1—O1—K2−134.88 (10)
O1—Pb1—N1—K1i123.83 (13)N1—K1—O1—K258.82 (11)
O1i—Pb1—N1—K1i35.79 (10)S2—K1—O1—K2130.30 (6)
O2—Pb1—N1—K1i128.03 (8)O2v—K2—O1—C1158.4 (3)
O2i—Pb1—N1—K1i31.60 (15)O2iii—K2—O1—C1−136.3 (3)
O2v—K2—N1—C3−39.03 (6)O1i—K2—O1—C189.0 (3)
O2iii—K2—N1—C339.03 (6)N1—K2—O1—C1157.7 (4)
O1—K2—N1—C3140.36 (6)S2vi—K2—O1—C1−54.7 (3)
O1i—K2—N1—C3−140.36 (7)S2vii—K2—O1—C130.2 (4)
S2vi—K2—N1—C390.78 (10)S1vi—K2—O1—C1−89.4 (4)
S2vii—K2—N1—C3−90.78 (10)S1ix—K2—O1—C117.7 (3)
S1vi—K2—N1—C30.000 (2)O2v—K2—O1—Pb144.69 (13)
S1ix—K2—N1—C3180.000 (3)O2iii—K2—O1—Pb1110.02 (9)
O2v—K2—N1—Pb1140.97 (6)O1i—K2—O1—Pb1−24.68 (10)
O2iii—K2—N1—Pb1−140.97 (6)N1—K2—O1—Pb143.94 (8)
O1—K2—N1—Pb1−39.64 (6)S2vi—K2—O1—Pb1−168.45 (8)
O1i—K2—N1—Pb139.64 (6)S2vii—K2—O1—Pb1−83.54 (10)
S2vi—K2—N1—Pb1−89.22 (10)S1vi—K2—O1—Pb1156.87 (8)
S2vii—K2—N1—Pb189.22 (10)S1ix—K2—O1—Pb1−96.05 (8)
S1vi—K2—N1—Pb1180.0O2v—K2—O1—K1−61.24 (11)
S1ix—K2—N1—Pb10.0O2iii—K2—O1—K14.10 (8)
O2v—K2—N1—K1−125.85 (11)O1i—K2—O1—K1−130.60 (4)
O2iii—K2—N1—K1−47.79 (8)N1—K2—O1—K1−61.98 (8)
O1—K2—N1—K153.55 (7)S2vi—K2—O1—K185.63 (6)
O1i—K2—N1—K1132.82 (11)S2vii—K2—O1—K1170.54 (5)
S2vi—K2—N1—K13.96 (16)S1vi—K2—O1—K150.94 (14)
S2vii—K2—N1—K1−177.60 (6)S1ix—K2—O1—K1158.03 (8)
S1vi—K2—N1—K1−86.82 (7)O1—Pb1—O2—C14.13 (19)
S1ix—K2—N1—K193.18 (7)O1i—Pb1—O2—C175.8 (2)
O2v—K2—N1—K1i47.79 (8)N1—Pb1—O2—C1−1.0 (2)
O2iii—K2—N1—K1i125.85 (11)O2i—Pb1—O2—C1120.85 (18)
O1—K2—N1—K1i−132.82 (11)O1—Pb1—O2—K1ii134.06 (15)
O1i—K2—N1—K1i−53.55 (7)O1i—Pb1—O2—K1ii−154.31 (10)
S2vi—K2—N1—K1i177.60 (6)N1—Pb1—O2—K1ii128.90 (11)
S2vii—K2—N1—K1i−3.96 (16)O2i—Pb1—O2—K1ii−109.23 (8)
S1vi—K2—N1—K1i86.82 (7)O1—Pb1—O2—K2ii−130.64 (13)
S1ix—K2—N1—K1i−93.18 (7)O1i—Pb1—O2—K2ii−59.01 (10)
O2iii—K1—N1—C3−100.2 (4)N1—Pb1—O2—K2ii−135.80 (10)
O1—K1—N1—C3152.1 (4)O2i—Pb1—O2—K2ii−13.92 (12)
N2iv—K1—N1—C3106.4 (5)Pb1—O2—C1—O1−7.2 (3)
N2iii—K1—N1—C3−28.7 (4)K1ii—O2—C1—O1−127.5 (3)
S2—K1—N1—C363.5 (3)K2ii—O2—C1—O1100.3 (4)
O2iii—K1—N1—Pb1141.70 (14)Pb1—O2—C1—C2170.0 (3)
O1—K1—N1—Pb134.03 (9)K1ii—O2—C1—C249.7 (4)
N2iv—K1—N1—Pb1−11.7 (4)K2ii—O2—C1—C2−82.5 (4)
N2iii—K1—N1—Pb1−146.82 (12)Pb1—O1—C1—O28.0 (4)
S2—K1—N1—Pb1−54.57 (9)K1—O1—C1—O2124.4 (3)
O2iii—K1—N1—K250.68 (9)K2—O1—C1—O2−105.3 (4)
O1—K1—N1—K2−56.99 (9)Pb1—O1—C1—C2−169.2 (3)
N2iv—K1—N1—K2−102.7 (4)K1—O1—C1—C2−52.9 (4)
N2iii—K1—N1—K2122.16 (11)K2—O1—C1—C277.4 (4)
S2—K1—N1—K2−145.59 (10)Pb1—N1—C3—K1i−97.76 (12)
O2iii—K1—N1—K1i33.4 (4)K2—N1—C3—K1i82.24 (12)
O1—K1—N1—K1i−74.3 (4)K1—N1—C3—K1i164.5 (2)
N2iv—K1—N1—K1i−120.0 (5)K2viii—S1—C3—K1i97.27 (19)
N2iii—K1—N1—K1i104.8 (4)K2x—S1—C3—K1i−82.73 (19)
S2—K1—N1—K1i−162.9 (5)

Symmetry codes: (i) x, −y+3/2, z; (ii) x−1, y, z; (iii) x+1, y, z; (iv) −x+1, −y+1, −z+1; (v) x+1, −y+3/2, z; (vi) x, y, z−1; (vii) x, −y+3/2, z−1; (viii) x, y, z+1; (ix) x−1, y, z−1; (x) x+1, y, z+1.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: TK2472).

References

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  • Westrip, S. P. (2009). publCIF In preparation.

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