Tripotassium bis­(acetato-κ2O,O′)(thio­cyanato-κN)plumbate(II) dithio­cyanate

Ng, S.W.

doi:10.1107/S1600536809021370

metal-organic compounds

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Volume 65| Part 7| July 2009| Page m755

doi:10.1107/S1600536809021370

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Tripotassium bis(acetato-κ²O,O′)(thiocyanato-κN)plumbate(II) dithiocyanate

Seik Weng Ng ^a ^*

^aDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
^*Correspondence e-mail: seikweng@um.edu.my

(Received 2 June 2009; accepted 5 June 2009; online 10 June 2009)

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 ).

Experimental

Crystal data

K₃[Pb(C₂H₃O₂)₂(NCS)](NCS)₂
M_r = 616.82
Monoclinic, P 2₁ /m
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 ) 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[F² > 2σ(F²)] = 0.022
wR(F²) = 0.056
S = 1.16
2045 reflections
104 parameters
H-atom parameters constrained
Δρ_max = 0.81 e Å⁻³
Δρ_min = −2.00 e Å⁻³

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

Supporting information

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

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

checkCIF report

Related literature top

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

Experimental top

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.

Computing details top

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

Figures top

	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.

Tripotassium bis(acetato-κ²O,O')(thiocyanato-κN)plumbate(II) dithiocyanate top

Crystal data top

K₃[Pb(C₂H₃O₂)₂(NCS)](NCS)₂	F(000) = 576
M_r = 616.82	D_x = 2.352 Mg m⁻³
Monoclinic, P2₁/m	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yb	Cell parameters from 4971 reflections
a = 6.1968 (1) Å	θ = 2.9–28.3°
b = 19.2499 (3) Å	µ = 10.77 mm⁻¹
c = 7.6354 (1) Å	T = 140 K
β = 106.982 (1)°	Block, colorless
V = 871.10 (2) Å³	0.25 × 0.20 × 0.08 mm
Z = 2

Data collection top

Bruker SMART APEX diffractometer	2045 independent reflections
Radiation source: fine-focus sealed tube	2015 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.023
ω scans	θ_max = 27.5°, θ_min = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −7→8
T_min = 0.174, T_max = 0.480	k = −25→25
6058 measured reflections	l = −9→9

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)] = 0.022	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.056	H-atom parameters constrained
S = 1.16	w = 1/[σ²(F_o²) + (0.03P)² + 1.3438P] where P = (F_o² + 2F_c²)/3
2045 reflections	(Δ/σ)_max = 0.001
104 parameters	Δρ_max = 0.81 e Å⁻³
0 restraints	Δρ_min = −2.00 e Å⁻³

Crystal data top

K₃[Pb(C₂H₃O₂)₂(NCS)](NCS)₂	V = 871.10 (2) Å³
M_r = 616.82	Z = 2
Monoclinic, P2₁/m	Mo Kα radiation
a = 6.1968 (1) Å	µ = 10.77 mm⁻¹
b = 19.2499 (3) Å	T = 140 K
c = 7.6354 (1) Å	0.25 × 0.20 × 0.08 mm
β = 106.982 (1)°

Data collection top

Bruker SMART APEX diffractometer	2045 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	2015 reflections with I > 2σ(I)
T_min = 0.174, T_max = 0.480	R_int = 0.023
6058 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.022	0 restraints
wR(F²) = 0.056	H-atom parameters constrained
S = 1.16	Δρ_max = 0.81 e Å⁻³
2045 reflections	Δρ_min = −2.00 e Å⁻³
104 parameters

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

	x	y	z	U_iso*/U_eq
Pb1	0.41686 (3)	0.7500	0.47400 (2)	0.01158 (7)
K1	0.85392 (14)	0.59423 (4)	0.42518 (12)	0.01948 (17)
K2	0.74409 (19)	0.7500	0.09371 (15)	0.0160 (2)
S1	1.1475 (2)	0.7500	0.8492 (2)	0.0247 (3)
S2	0.65682 (16)	0.62677 (5)	0.76528 (14)	0.01949 (19)
N1	0.8449 (7)	0.7500	0.4972 (6)	0.0151 (9)
N2	0.2738 (6)	0.54336 (19)	0.6214 (6)	0.0289 (8)
O1	0.4696 (4)	0.66654 (13)	0.2532 (4)	0.0162 (5)
O2	0.1161 (4)	0.66405 (13)	0.2588 (4)	0.0171 (5)
C1	0.2743 (6)	0.63941 (18)	0.2063 (5)	0.0146 (7)
C2	0.2360 (7)	0.5741 (2)	0.0917 (6)	0.0236 (8)
H2A	0.2283	0.5341	0.1689	0.035*
H2B	0.3609	0.5678	0.0388	0.035*
H2C	0.0940	0.5782	−0.0069	0.035*
C3	0.9724 (8)	0.7500	0.6432 (7)	0.0142 (10)
C4	0.4309 (6)	0.57822 (19)	0.6821 (5)	0.0180 (7)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.01294 (11)	0.01291 (10)	0.01004 (11)	0.000	0.00516 (7)	0.000
K1	0.0164 (4)	0.0153 (4)	0.0286 (4)	0.0018 (3)	0.0095 (3)	0.0037 (3)
K2	0.0168 (5)	0.0192 (5)	0.0129 (5)	0.000	0.0058 (4)	0.000
S1	0.0184 (6)	0.0388 (8)	0.0144 (6)	0.000	0.0011 (5)	0.000
S2	0.0194 (4)	0.0185 (4)	0.0210 (5)	−0.0041 (3)	0.0065 (4)	−0.0016 (4)
N1	0.0119 (19)	0.020 (2)	0.013 (2)	0.000	0.0035 (17)	0.000
N2	0.0217 (18)	0.0232 (17)	0.036 (2)	−0.0019 (14)	0.0000 (16)	0.0014 (15)
O1	0.0136 (12)	0.0192 (12)	0.0162 (13)	−0.0004 (9)	0.0050 (10)	−0.0031 (10)
O2	0.0142 (12)	0.0194 (12)	0.0191 (13)	0.0017 (9)	0.0071 (10)	−0.0002 (10)
C1	0.0171 (16)	0.0143 (15)	0.0107 (16)	0.0017 (12)	0.0015 (13)	0.0049 (13)
C2	0.0234 (19)	0.0199 (18)	0.025 (2)	−0.0010 (15)	0.0034 (17)	−0.0079 (16)
C3	0.012 (2)	0.012 (2)	0.020 (3)	0.000	0.008 (2)	0.000
C4	0.0175 (18)	0.0142 (16)	0.0205 (19)	0.0032 (13)	0.0031 (15)	0.0034 (14)

Geometric parameters (Å, º) top

Pb1—O1	2.419 (3)	K2—S2^vi	3.3788 (13)
Pb1—O1ⁱ	2.419 (3)	K2—S2^vii	3.3788 (13)
Pb1—O2	2.669 (3)	S1—C3	1.630 (5)
Pb1—O2ⁱ	2.669 (3)	S2—C4	1.649 (4)
Pb1—N1	2.606 (4)	S2—K2^viii	3.3788 (13)
Pb1—S1ⁱⁱ	3.713 (1)	N1—C3	1.163 (7)
Pb1—S2	3.294 (1)	N1—K1ⁱ	3.0520 (12)
Pb1—S2ⁱ	3.294 (1)	N2—C4	1.162 (5)
K1—O2ⁱⁱⁱ	2.696 (3)	N2—K1^iv	2.757 (4)
K1—O1	2.740 (3)	N2—K1ⁱⁱ	2.774 (4)
K1—N2^iv	2.757 (4)	O1—C1	1.270 (4)
K1—N2ⁱⁱⁱ	2.774 (4)	O2—C1	1.255 (5)
K1—N1	3.0520 (12)	O2—K1ⁱⁱ	2.696 (3)
K1—S2	3.2373 (13)	O2—K2ⁱⁱ	2.818 (3)
K2—O2^v	2.818 (3)	C1—C2	1.509 (5)
K2—O2ⁱⁱⁱ	2.818 (3)	C2—H2A	0.9800
K2—O1	2.858 (3)	C2—H2B	0.9800
K2—O1ⁱ	2.858 (3)	C2—H2C	0.9800
K2—N1	2.959 (5)	C3—K1ⁱ	3.404 (3)

O1—Pb1—O1ⁱ	83.23 (13)	O2^v—K2—S1^ix	143.98 (5)
O1—Pb1—N1	72.87 (9)	O2ⁱⁱⁱ—K2—S1^ix	143.98 (5)
O1ⁱ—Pb1—N1	72.87 (9)	O1—K2—S1^ix	64.83 (6)
O1—Pb1—O2	51.04 (8)	O1ⁱ—K2—S1^ix	64.83 (6)
O1ⁱ—Pb1—O2	101.23 (8)	N1—K2—S1^ix	114.20 (9)
N1—Pb1—O2	123.76 (9)	S2^vi—K2—S1^ix	72.51 (3)
O1—Pb1—O2ⁱ	101.23 (8)	S2^vii—K2—S1^ix	72.51 (3)
O1ⁱ—Pb1—O2ⁱ	51.04 (8)	S1^vi—K2—S1^ix	120.08 (5)
N1—Pb1—O2ⁱ	123.76 (9)	C3—S1—K2^viii	97.79 (19)
O2—Pb1—O2ⁱ	76.62 (11)	C3—S1—K2^x	142.1 (2)
O2ⁱⁱⁱ—K1—O1	94.59 (8)	K2^viii—S1—K2^x	120.08 (5)
O2ⁱⁱⁱ—K1—N2^iv	127.44 (11)	C4—S2—K1	93.34 (15)
O1—K1—N2^iv	104.45 (9)	C4—S2—K2^viii	128.15 (15)
O2ⁱⁱⁱ—K1—N2ⁱⁱⁱ	80.28 (10)	K1—S2—K2^viii	135.65 (4)
O1—K1—N2ⁱⁱⁱ	170.07 (10)	C3—N1—Pb1	117.3 (4)
N2^iv—K1—N2ⁱⁱⁱ	85.36 (11)	C3—N1—K2	151.1 (4)
O2ⁱⁱⁱ—K1—N1	68.92 (10)	Pb1—N1—K2	91.61 (13)
O1—K1—N1	61.85 (10)	C3—N1—K1	97.45 (9)
N2^iv—K1—N1	161.31 (12)	Pb1—N1—K1	93.42 (8)
N2ⁱⁱⁱ—K1—N1	108.25 (11)	K2—N1—K1	79.74 (8)
O2ⁱⁱⁱ—K1—S2	134.60 (6)	C3—N1—K1ⁱ	97.45 (9)
O1—K1—S2	78.90 (6)	Pb1—N1—K1ⁱ	93.42 (8)
N2^iv—K1—S2	97.35 (9)	K2—N1—K1ⁱ	79.74 (8)
N2ⁱⁱⁱ—K1—S2	98.58 (9)	K1—N1—K1ⁱ	158.52 (17)
N1—K1—S2	68.55 (9)	C4—N2—K1^iv	141.4 (3)
O2^v—K2—O2ⁱⁱⁱ	71.90 (11)	C4—N2—K1ⁱⁱ	123.8 (3)
O2^v—K2—O1	130.58 (9)	K1^iv—N2—K1ⁱⁱ	94.64 (11)
O2ⁱⁱⁱ—K2—O1	89.45 (8)	C1—O1—Pb1	99.1 (2)
O2^v—K2—O1ⁱ	89.45 (8)	C1—O1—K1	123.3 (2)
O2ⁱⁱⁱ—K2—O1ⁱ	130.58 (9)	Pb1—O1—K1	106.18 (9)
O1—K2—O1ⁱ	68.41 (10)	C1—O1—K2	138.4 (2)
O2^v—K2—N1	68.78 (9)	Pb1—O1—K2	98.16 (8)
O2ⁱⁱⁱ—K2—N1	68.78 (9)	K1—O1—K2	86.99 (8)
O1—K2—N1	61.80 (9)	C1—O2—Pb1	87.8 (2)
O1ⁱ—K2—N1	61.80 (9)	C1—O2—K1ⁱⁱ	126.6 (2)
O2^v—K2—S2^vi	132.59 (7)	Pb1—O2—K1ⁱⁱ	115.30 (10)
O2ⁱⁱⁱ—K2—S2^vi	81.51 (6)	C1—O2—K2ⁱⁱ	133.8 (2)
O1—K2—S2^vi	86.29 (6)	Pb1—O2—K2ⁱⁱ	104.14 (8)
O1ⁱ—K2—S2^vi	136.45 (7)	K1ⁱⁱ—O2—K2ⁱⁱ	88.66 (8)
N1—K2—S2^vi	135.40 (2)	O2—C1—O1	121.6 (3)
O2^v—K2—S2^vii	81.51 (6)	O2—C1—C2	119.6 (3)
O2ⁱⁱⁱ—K2—S2^vii	132.59 (7)	O1—C1—C2	118.8 (3)
O1—K2—S2^vii	136.45 (6)	C1—C2—H2A	109.5
O1ⁱ—K2—S2^vii	86.29 (6)	C1—C2—H2B	109.5
N1—K2—S2^vii	135.40 (2)	H2A—C2—H2B	109.5
S2^vi—K2—S2^vii	89.19 (4)	C1—C2—H2C	109.5
O2^v—K2—S1^vi	67.87 (6)	H2A—C2—H2C	109.5
O2ⁱⁱⁱ—K2—S1^vi	67.87 (6)	H2B—C2—H2C	109.5
O1—K2—S1^vi	145.78 (5)	N1—C3—S1	179.1 (5)
O1ⁱ—K2—S1^vi	145.78 (5)	N1—C3—K1ⁱ	62.76 (9)
N1—K2—S1^vi	125.72 (9)	S1—C3—K1ⁱ	117.37 (8)
S2^vi—K2—S1^vi	65.92 (3)	N2—C4—S2	178.7 (4)
S2^vii—K2—S1^vi	65.92 (3)

O2ⁱⁱⁱ—K1—S2—C4	150.92 (15)	O1ⁱ—Pb1—O1—C1	−114.5 (2)
O1—K1—S2—C4	65.45 (14)	N1—Pb1—O1—C1	171.4 (2)
N2^iv—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—C4	129.38 (15)	O1ⁱ—Pb1—O1—K1	116.73 (7)
O2ⁱⁱⁱ—K1—S2—K2^viii	−9.98 (11)	N1—Pb1—O1—K1	42.61 (10)
O1—K1—S2—K2^viii	−95.45 (7)	O2—Pb1—O1—K1	−132.90 (14)
N2^iv—K1—S2—K2^viii	161.19 (9)	O2ⁱ—Pb1—O1—K1	164.73 (9)
N2ⁱⁱⁱ—K1—S2—K2^viii	74.80 (9)	O1ⁱ—Pb1—O1—K2	27.51 (11)
N1—K1—S2—K2^viii	−31.52 (10)	N1—Pb1—O1—K2	−46.61 (9)
O1—Pb1—N1—C3	−135.98 (7)	O2—Pb1—O1—K2	137.88 (13)
O1ⁱ—Pb1—N1—C3	135.98 (7)	O2ⁱ—Pb1—O1—K2	75.51 (9)
O2—Pb1—N1—C3	−131.78 (8)	O2ⁱⁱⁱ—K1—O1—C1	145.2 (3)
O2ⁱ—Pb1—N1—C3	131.78 (8)	N2^iv—K1—O1—C1	14.7 (3)
O1—Pb1—N1—K2	44.02 (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—K2	48.22 (8)	O2ⁱⁱⁱ—K1—O1—Pb1	−101.92 (10)
O2ⁱ—Pb1—N1—K2	−48.22 (8)	N2^iv—K1—O1—Pb1	127.50 (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—Pb1	32.68 (7)
O2—Pb1—N1—K1	−31.60 (15)	O2ⁱⁱⁱ—K1—O1—K2	−4.30 (8)
O2ⁱ—Pb1—N1—K1	−128.03 (8)	N2^iv—K1—O1—K2	−134.88 (10)
O1—Pb1—N1—K1ⁱ	123.83 (13)	N1—K1—O1—K2	58.82 (11)
O1ⁱ—Pb1—N1—K1ⁱ	35.79 (10)	S2—K1—O1—K2	130.30 (6)
O2—Pb1—N1—K1ⁱ	128.03 (8)	O2^v—K2—O1—C1	158.4 (3)
O2ⁱ—Pb1—N1—K1ⁱ	31.60 (15)	O2ⁱⁱⁱ—K2—O1—C1	−136.3 (3)
O2^v—K2—N1—C3	−39.03 (6)	O1ⁱ—K2—O1—C1	89.0 (3)
O2ⁱⁱⁱ—K2—N1—C3	39.03 (6)	N1—K2—O1—C1	157.7 (4)
O1—K2—N1—C3	140.36 (6)	S2^vi—K2—O1—C1	−54.7 (3)
O1ⁱ—K2—N1—C3	−140.36 (7)	S2^vii—K2—O1—C1	30.2 (4)
S2^vi—K2—N1—C3	90.78 (10)	S1^vi—K2—O1—C1	−89.4 (4)
S2^vii—K2—N1—C3	−90.78 (10)	S1^ix—K2—O1—C1	17.7 (3)
S1^vi—K2—N1—C3	0.000 (2)	O2^v—K2—O1—Pb1	44.69 (13)
S1^ix—K2—N1—C3	180.000 (3)	O2ⁱⁱⁱ—K2—O1—Pb1	110.02 (9)
O2^v—K2—N1—Pb1	140.97 (6)	O1ⁱ—K2—O1—Pb1	−24.68 (10)
O2ⁱⁱⁱ—K2—N1—Pb1	−140.97 (6)	N1—K2—O1—Pb1	43.94 (8)
O1—K2—N1—Pb1	−39.64 (6)	S2^vi—K2—O1—Pb1	−168.45 (8)
O1ⁱ—K2—N1—Pb1	39.64 (6)	S2^vii—K2—O1—Pb1	−83.54 (10)
S2^vi—K2—N1—Pb1	−89.22 (10)	S1^vi—K2—O1—Pb1	156.87 (8)
S2^vii—K2—N1—Pb1	89.22 (10)	S1^ix—K2—O1—Pb1	−96.05 (8)
S1^vi—K2—N1—Pb1	180.0	O2^v—K2—O1—K1	−61.24 (11)
S1^ix—K2—N1—Pb1	0.0	O2ⁱⁱⁱ—K2—O1—K1	4.10 (8)
O2^v—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—K1	53.55 (7)	S2^vi—K2—O1—K1	85.63 (6)
O1ⁱ—K2—N1—K1	132.82 (11)	S2^vii—K2—O1—K1	170.54 (5)
S2^vi—K2—N1—K1	3.96 (16)	S1^vi—K2—O1—K1	50.94 (14)
S2^vii—K2—N1—K1	−177.60 (6)	S1^ix—K2—O1—K1	158.03 (8)
S1^vi—K2—N1—K1	−86.82 (7)	O1—Pb1—O2—C1	4.13 (19)
S1^ix—K2—N1—K1	93.18 (7)	O1ⁱ—Pb1—O2—C1	75.8 (2)
O2^v—K2—N1—K1ⁱ	47.79 (8)	N1—Pb1—O2—C1	−1.0 (2)
O2ⁱⁱⁱ—K2—N1—K1ⁱ	125.85 (11)	O2ⁱ—Pb1—O2—C1	120.85 (18)
O1—K2—N1—K1ⁱ	−132.82 (11)	O1—Pb1—O2—K1ⁱⁱ	134.06 (15)
O1ⁱ—K2—N1—K1ⁱ	−53.55 (7)	O1ⁱ—Pb1—O2—K1ⁱⁱ	−154.31 (10)
S2^vi—K2—N1—K1ⁱ	177.60 (6)	N1—Pb1—O2—K1ⁱⁱ	128.90 (11)
S2^vii—K2—N1—K1ⁱ	−3.96 (16)	O2ⁱ—Pb1—O2—K1ⁱⁱ	−109.23 (8)
S1^vi—K2—N1—K1ⁱ	86.82 (7)	O1—Pb1—O2—K2ⁱⁱ	−130.64 (13)
S1^ix—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—C3	152.1 (4)	O2ⁱ—Pb1—O2—K2ⁱⁱ	−13.92 (12)
N2^iv—K1—N1—C3	106.4 (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—C3	63.5 (3)	K2ⁱⁱ—O2—C1—O1	100.3 (4)
O2ⁱⁱⁱ—K1—N1—Pb1	141.70 (14)	Pb1—O2—C1—C2	170.0 (3)
O1—K1—N1—Pb1	34.03 (9)	K1ⁱⁱ—O2—C1—C2	49.7 (4)
N2^iv—K1—N1—Pb1	−11.7 (4)	K2ⁱⁱ—O2—C1—C2	−82.5 (4)
N2ⁱⁱⁱ—K1—N1—Pb1	−146.82 (12)	Pb1—O1—C1—O2	8.0 (4)
S2—K1—N1—Pb1	−54.57 (9)	K1—O1—C1—O2	124.4 (3)
O2ⁱⁱⁱ—K1—N1—K2	50.68 (9)	K2—O1—C1—O2	−105.3 (4)
O1—K1—N1—K2	−56.99 (9)	Pb1—O1—C1—C2	−169.2 (3)
N2^iv—K1—N1—K2	−102.7 (4)	K1—O1—C1—C2	−52.9 (4)
N2ⁱⁱⁱ—K1—N1—K2	122.16 (11)	K2—O1—C1—C2	77.4 (4)
S2—K1—N1—K2	−145.59 (10)	Pb1—N1—C3—K1ⁱ	−97.76 (12)
O2ⁱⁱⁱ—K1—N1—K1ⁱ	33.4 (4)	K2—N1—C3—K1ⁱ	82.24 (12)
O1—K1—N1—K1ⁱ	−74.3 (4)	K1—N1—C3—K1ⁱ	164.5 (2)
N2^iv—K1—N1—K1ⁱ	−120.0 (5)	K2^viii—S1—C3—K1ⁱ	97.27 (19)
N2ⁱⁱⁱ—K1—N1—K1ⁱ	104.8 (4)	K2^x—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.

Experimental details

Crystal data
Chemical formula	K₃[Pb(C₂H₃O₂)₂(NCS)](NCS)₂
M_r	616.82
Crystal system, space group	Monoclinic, P2₁/m
Temperature (K)	140
a, b, c (Å)	6.1968 (1), 19.2499 (3), 7.6354 (1)
β (°)	106.982 (1)
V (Å³)	871.10 (2)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	10.77
Crystal size (mm)	0.25 × 0.20 × 0.08

Data collection
Diffractometer	Bruker SMART APEX diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.174, 0.480
No. of measured, independent and observed [I > 2σ(I)] reflections	6058, 2045, 2015
R_int	0.023
(sin θ/λ)_max (Å⁻¹)	0.650

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.022, 0.056, 1.16
No. of reflections	2045
No. of parameters	104
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.81, −2.00

Computer programs: APEX2 (Bruker, 2008), SAINT (Bruker, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2009).

Acknowledgements

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.

References

Barbour, L. J. (2001). J. Supramol. Chem. 1, 189–191. CrossRef CAS Google Scholar
Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Morsali, A. & Mahjoub, A. R. (2004). Helv. Chim. Acta, 87, 2717–2722. Web of Science CSD CrossRef CAS Google Scholar
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Westrip, S. P. (2009). publCIF. In preparation. Google Scholar