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The crystal and molecular structure of the title compound, [PbCl2(C7H12N2S)4], the first mononuclear lead complex containing a 2-mercapto-1-alkyl­imidazole ligand to be structurally characterized, has been determined by single-crystal X-ray diffraction. The six-coordinate Pb atom displays a distorted octahedral geometry and is surrounded by four thione groups and two cis chloro ligands, with average Pb-S and Pb-Cl bond distances of 2.946 (3) and 3.058 (2) Å, respectively.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680301064X/ac6039sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680301064X/ac6039Isup2.hkl
Contains datablock I

CCDC reference: 214792

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.011 Å
  • R factor = 0.047
  • wR factor = 0.130
  • Data-to-parameter ratio = 17.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Comment top

The coordination chemistry of lead with sulfur-donor ligands is surprisingly underdeveloped despite the purported thiophilicity of this metal. According to a recent survey, only about 16% of all PbII compounds in the Cambridge Structural Database (CSD; Version 5.24, November 2002; Allen, 2002) contain one or more sulfur-donor groups (Claudio et al., 2003). Heterocyclic thione and thionate ligands are no exception, and very few derivatives of lead have been isolated with such donors despite the large number of complexes obtained with them for both transition and main group metals (Raper, 1985; Akrivos, 2001). In view of this imbalance and because of our interest in the coordination chemistry of lead with simple thione-type donor ligands, we set out to prepare new complexes with N-substituted mercaptoimidazoles. We report here the synthesis, characterization and structure of cis-dichlorotetrakis(2-mercapto-1-tert-butylimidazole)lead(II), (I), the first mononuclear lead complex containing a 2-mercapto-1-alkylimidazole ligand.

The crystal and molecular structure of (I) was determined by single-crystal X-ray diffraction (Fig. 1). The Pb atom in cis-Pb(HmimtBu)4Cl2 is coordinated to the thione moieties of four mercaptoimidazole groups and to two adjacent chloro ligands in a distorted octahedral environment, with the trans and cis angles in the approximate ranges 154–170 and 82–112°, respectively. The two Pb—S distances to the thione ligands trans to the chlorides (ca 2.89 Å) are slightly shorter than those for the mutually trans thiones (ca 3.00 Å). While these values are only moderately longer than the corresponding bond lengths to the terminal methimazole groups in the dinuclear derivative Pb2(HmimMe)6(NO3)4 (ca 2.84 Å; Bristow et al., 1987), they are comparable to those found in other PbII complexes with thioureas or heterocyclic thiones (Goldberg & Herbstein, 1972; Herbstein & Kaftory, 1972; Williams et al., 1992). It is also interesting to note that the average C—S bond length in cis-Pb(HmimtBu)4Cl2 (ca 1.71 Å) is very similar to the corresponding averages found for the group 12 metal derivatives (HmimtBu)4MBr2 (M = Zn, Cd, Hg) (ca 1.72 Å) or even in free HmimtBu (1.70 Å; White et al., 2003). The Pb—Cl bond lengths, 3.037 (2) and 3.079 (2) Å, while longer than the mean value found in the CSD for such terminal interactions in six-coordinate PbII (2.87 Å), are still within the range of observed distances for such bonds (2.617–3.348 Å; Allen & Kennard, 1993).

Experimental top

A solution of 2-mercapto-1-tert-butylimidazole (0.150 g, 0.960 mmol) in methanol (1 ml) was added to a stirred solution of PbCl2 (0.067 g, 0.240 mmol) in water (5 ml), resulting in the immediate formation of an off-white precipitate and a pale yellow solution. After stirring the suspension for 30 min, the product was isolated by filtration and dried in vacuo for 14 h (0.126 g, 58%). NMR data (in CD2Cl2): 1H δ 1.74 [s, 36H, C(CH3)3], 6.72 (d, 3JH–H = 2.3 Hz, 4H, imidazole H), 6.84 (d, 3JH–H = 2.3 Hz, 4H, imidazole H), 11.91 (br s, 4H, NH); 13C d 28.5 [q, 1JC–H = 128 Hz, 12 C, C(CH3)3], 59.1 [s, 4 C, C(CH3)3], 114.2 (d, 1JC—H = 176 Hz, 4 C, imidazole C), 116.3 (d, 1JC–H = 167 Hz, 4 C, imidazole C), 156.8 (s, 4 C, CS). IR data (cm−1): 3137 (m), 3096 (s), 3015 (m), 2974 (s), 2917 (m), 2884 (m), 2782 (w), 2729 (w), 1576 (s), 1474 (s), 1455 (m), 1414 (m), 1399 (m), 1369 (m), 1312 (versus), 1264 (w), 1238 (versus), 1225 (s), 1178 (w), 1126 (m), 1118 (m), 1043 (w), 1014 (w), 935 (w), 913 (w), 795 (m), 768 (w), 723 (m), 684 (s), 591 (w), 546 (m), 458 (w). Analysis calculated for C28H48Cl2N8PbS4: C 37.2, H 5.4, N 12.4%; found: C 37.5, H 5.2, N 12.5%.

Refinement top

The maximum and minimum electron-density peaks in the final difference Fourier map are 1.14 and 0.9 Å, respectively, from the Pb atom.

Computing details top

Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. A view of the title compound, showing 30% probability ellipsoids. H atoms have been obmitted for clarity.
[Figure 2] Fig. 2. A packing diagram of the title compound, viewed down the a axis.
cis-Dichlorotetrakis(2-mercapto-1-tert-butylimidazole)lead(II) top
Crystal data top
[PbCl2(C7H12N2S)4]F(000) = 1808
Mr = 903.07Dx = 1.543 Mg m3
Monoclinic, P21/cMelting point: 155 K
Hall symbol: -P 2ybcCu Kα radiation, λ = 1.5418 Å
a = 10.2683 (11) ÅCell parameters from 25 reflections
b = 10.9843 (13) Åθ = 11.0–20.8°
c = 34.514 (4) ŵ = 11.97 mm1
β = 93.294 (9)°T = 293 K
V = 3886.4 (8) Å3Irregular, yellow
Z = 40.40 × 0.29 × 0.17 mm
Data collection top
Enraf-Nonius CAD-4
diffractometer
5838 reflections with I > 2σ(I)
Radiation source: normal-focus sealed tubeRint = 0.051
Graphite monochromatorθmax = 66.9°, θmin = 2.6°
non–profiled ω/2θ scansh = 1212
Absorption correction: analytical
(Katayama, 1986)
k = 013
Tmin = 0.048, Tmax = 0.214l = 3441
10879 measured reflections3 standard reflections every 60 min
6878 independent reflections intensity decay: none
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.047H-atom parameters constrained
wR(F2) = 0.130 w = 1/[σ2(Fo2) + (0.0906P)2 + 2.6577P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.001
6878 reflectionsΔρmax = 1.68 e Å3
404 parametersΔρmin = 1.50 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00190 (9)
Crystal data top
[PbCl2(C7H12N2S)4]V = 3886.4 (8) Å3
Mr = 903.07Z = 4
Monoclinic, P21/cCu Kα radiation
a = 10.2683 (11) ŵ = 11.97 mm1
b = 10.9843 (13) ÅT = 293 K
c = 34.514 (4) Å0.40 × 0.29 × 0.17 mm
β = 93.294 (9)°
Data collection top
Enraf-Nonius CAD-4
diffractometer
5838 reflections with I > 2σ(I)
Absorption correction: analytical
(Katayama, 1986)
Rint = 0.051
Tmin = 0.048, Tmax = 0.2143 standard reflections every 60 min
10879 measured reflections intensity decay: none
6878 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0470 restraints
wR(F2) = 0.130H-atom parameters constrained
S = 1.03Δρmax = 1.68 e Å3
6878 reflectionsΔρmin = 1.50 e Å3
404 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
Pb10.275402 (19)0.415611 (19)0.120267 (6)0.04968 (13)
Cl10.47136 (16)0.24054 (15)0.08822 (6)0.0708 (4)
Cl20.07031 (18)0.36497 (17)0.05362 (5)0.0702 (4)
S110.10801 (15)0.29085 (17)0.17993 (5)0.0656 (4)
C110.0355 (6)0.2407 (5)0.15933 (16)0.0513 (12)
N120.1413 (4)0.1922 (4)0.17545 (14)0.0541 (11)
C120.1592 (6)0.1763 (6)0.21807 (19)0.0628 (15)
C12A0.1471 (9)0.2995 (7)0.2377 (2)0.086 (2)
H12A0.21570.3520.22760.094 (5)*
H12B0.06410.33490.23280.094 (5)*
H12C0.15380.28980.26510.094 (5)*
C12B0.2966 (8)0.1274 (9)0.2225 (3)0.093 (3)
H12D0.35930.18790.21390.094 (5)*
H12E0.30760.10850.24930.094 (5)*
H12F0.30940.05520.20710.094 (5)*
C12C0.0605 (8)0.0856 (6)0.2347 (2)0.0739 (19)
H12G0.06940.07780.26210.094 (5)*
H12H0.02590.11340.23010.094 (5)*
H12I0.07530.0080.22240.094 (5)*
C130.2329 (6)0.1596 (6)0.1461 (2)0.0652 (16)
H130.31320.12320.14960.096 (10)*
C140.1861 (7)0.1895 (7)0.1122 (2)0.0661 (16)
H140.22780.17940.08780.096 (10)*
N150.0644 (5)0.2381 (5)0.12027 (14)0.0563 (11)
H150.01340.26340.10310.073 (11)*
S210.41821 (16)0.62131 (15)0.08922 (5)0.0630 (4)
C210.5368 (6)0.5890 (5)0.05808 (18)0.0527 (13)
N220.6157 (5)0.6656 (5)0.04006 (15)0.0607 (12)
C220.6187 (7)0.8013 (7)0.0433 (2)0.0704 (17)
C22A0.7190 (9)0.8523 (9)0.0162 (3)0.100 (3)
H22A0.80420.82210.02410.094 (5)*
H22B0.71910.93960.01750.094 (5)*
H22C0.69650.82690.010.094 (5)*
C22B0.6584 (10)0.8339 (9)0.0850 (3)0.094 (3)
H22D0.59450.80320.10180.094 (5)*
H22E0.66390.92080.08760.094 (5)*
H22F0.74180.79840.09210.094 (5)*
C22C0.4856 (8)0.8519 (8)0.0307 (3)0.088 (2)
H22G0.46710.83510.00360.094 (5)*
H22H0.48490.93830.03480.094 (5)*
H22I0.42040.81440.04560.094 (5)*
C230.6992 (8)0.5977 (8)0.0185 (2)0.079 (2)
H230.7640.62870.00350.096 (10)*
C240.6701 (8)0.4789 (9)0.0229 (2)0.078 (2)
H240.70990.41270.01170.096 (10)*
N250.5700 (5)0.4760 (5)0.04733 (16)0.0620 (12)
H250.5330.41050.05480.073 (11)*
S310.43764 (16)0.44040 (16)0.19034 (5)0.0622 (4)
C310.5808 (5)0.4869 (5)0.17185 (16)0.0512 (12)
N320.6627 (5)0.5802 (4)0.18264 (15)0.0529 (11)
C320.6423 (6)0.6735 (6)0.21346 (18)0.0589 (14)
C32A0.5161 (7)0.7427 (7)0.2027 (2)0.0693 (17)
H32A0.52650.78920.17950.094 (5)*
H32B0.49670.79660.22340.094 (5)*
H32C0.44580.68580.19820.094 (5)*
C32B0.6390 (8)0.6091 (7)0.2522 (2)0.0690 (17)
H32D0.570.54990.25110.094 (5)*
H32E0.62390.66750.27220.094 (5)*
H32F0.72080.56890.2580.094 (5)*
C32C0.7564 (8)0.7635 (7)0.2148 (2)0.0753 (19)
H32G0.83690.71990.21930.094 (5)*
H32H0.74650.82090.23540.094 (5)*
H32I0.75720.80610.19050.094 (5)*
C330.7672 (6)0.5780 (6)0.1591 (2)0.0617 (15)
H330.83690.63230.16020.096 (10)*
C340.7511 (6)0.4854 (6)0.1345 (2)0.0646 (15)
H340.80660.46320.11530.096 (10)*
N350.6365 (5)0.4286 (4)0.14295 (16)0.0599 (13)
H350.60510.36480.13130.073 (11)*
S410.1170 (2)0.62401 (18)0.13937 (6)0.0732 (5)
C410.1089 (5)0.7028 (6)0.09631 (18)0.0563 (13)
N420.1317 (5)0.8226 (5)0.08930 (14)0.0549 (11)
C420.1618 (7)0.9208 (6)0.1187 (2)0.0640 (16)
C42A0.0488 (9)0.9321 (7)0.1448 (3)0.083 (2)
H42A0.02950.95080.12930.094 (5)*
H42B0.06650.9960.16330.094 (5)*
H42C0.03760.85660.15820.094 (5)*
C42B0.2873 (9)0.8913 (8)0.1418 (3)0.087 (2)
H42D0.27770.81560.15520.094 (5)*
H42E0.30670.9550.16030.094 (5)*
H42F0.3570.88450.12460.094 (5)*
C42C0.1768 (9)1.0427 (7)0.0973 (3)0.086 (2)
H42G0.10261.05530.07960.094 (5)*
H42H0.25471.04080.08320.094 (5)*
H42I0.18251.10790.11580.094 (5)*
C430.1163 (7)0.8402 (8)0.0497 (2)0.0741 (18)
H430.1270.91380.03690.096 (10)*
C440.0838 (7)0.7358 (8)0.0328 (2)0.078 (2)
H440.06730.7220.00640.096 (10)*
N450.0796 (5)0.6524 (6)0.06178 (17)0.0703 (15)
H450.06040.57680.05830.073 (11)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.04515 (17)0.04777 (17)0.05645 (18)0.00382 (8)0.00574 (10)0.00037 (8)
Cl10.0649 (9)0.0560 (8)0.0910 (11)0.0060 (7)0.0010 (8)0.0084 (8)
Cl20.0824 (10)0.0735 (10)0.0550 (8)0.0150 (8)0.0060 (7)0.0033 (7)
S110.0577 (8)0.0785 (10)0.0606 (8)0.0171 (7)0.0027 (7)0.0101 (7)
C110.054 (3)0.047 (3)0.053 (3)0.003 (2)0.011 (2)0.003 (2)
N120.053 (3)0.045 (2)0.066 (3)0.004 (2)0.016 (2)0.002 (2)
C120.065 (4)0.055 (3)0.071 (4)0.001 (3)0.029 (3)0.003 (3)
C12A0.119 (6)0.064 (4)0.080 (5)0.007 (4)0.043 (5)0.004 (4)
C12B0.066 (4)0.103 (6)0.112 (7)0.008 (4)0.040 (4)0.017 (5)
C12C0.083 (5)0.066 (4)0.074 (4)0.007 (3)0.017 (4)0.014 (3)
C130.049 (3)0.056 (3)0.090 (5)0.001 (3)0.004 (3)0.007 (3)
C140.060 (3)0.063 (4)0.074 (4)0.007 (3)0.005 (3)0.010 (3)
N150.048 (2)0.063 (3)0.058 (3)0.005 (2)0.004 (2)0.001 (2)
S210.0621 (9)0.0523 (7)0.0775 (10)0.0040 (7)0.0293 (7)0.0078 (7)
C210.049 (3)0.054 (3)0.056 (3)0.001 (2)0.010 (2)0.003 (2)
N220.053 (3)0.064 (3)0.066 (3)0.002 (2)0.015 (2)0.009 (2)
C220.065 (4)0.066 (4)0.082 (4)0.007 (3)0.016 (3)0.015 (3)
C22A0.094 (6)0.094 (6)0.115 (7)0.019 (5)0.040 (5)0.024 (5)
C22B0.110 (7)0.077 (5)0.097 (6)0.026 (5)0.001 (5)0.001 (4)
C22C0.092 (5)0.070 (5)0.104 (6)0.008 (4)0.020 (5)0.027 (4)
C230.064 (4)0.100 (6)0.076 (5)0.007 (4)0.028 (4)0.008 (4)
C240.078 (5)0.093 (6)0.064 (4)0.019 (4)0.024 (3)0.004 (4)
N250.063 (3)0.061 (3)0.064 (3)0.002 (3)0.017 (2)0.001 (2)
S310.0584 (8)0.0706 (9)0.0578 (8)0.0151 (7)0.0056 (6)0.0021 (7)
C310.052 (3)0.047 (3)0.055 (3)0.001 (2)0.001 (2)0.003 (2)
N320.047 (2)0.050 (3)0.061 (3)0.0007 (19)0.001 (2)0.003 (2)
C320.060 (3)0.054 (3)0.062 (3)0.003 (3)0.004 (3)0.000 (3)
C32A0.075 (4)0.061 (4)0.071 (4)0.014 (3)0.002 (3)0.004 (3)
C32B0.078 (4)0.069 (4)0.059 (4)0.003 (3)0.006 (3)0.004 (3)
C32C0.082 (5)0.063 (4)0.079 (4)0.018 (4)0.010 (4)0.004 (3)
C330.046 (3)0.060 (4)0.079 (4)0.001 (3)0.007 (3)0.003 (3)
C340.051 (3)0.063 (4)0.081 (4)0.006 (3)0.012 (3)0.004 (3)
N350.062 (3)0.050 (3)0.067 (3)0.002 (2)0.007 (2)0.010 (2)
S410.0808 (11)0.0669 (10)0.0744 (10)0.0154 (9)0.0275 (9)0.0098 (8)
C410.046 (3)0.062 (3)0.061 (3)0.000 (3)0.003 (2)0.006 (3)
N420.052 (2)0.052 (3)0.061 (3)0.011 (2)0.005 (2)0.003 (2)
C420.058 (4)0.054 (3)0.081 (4)0.006 (3)0.007 (3)0.013 (3)
C42A0.096 (6)0.062 (4)0.093 (5)0.019 (4)0.035 (5)0.009 (4)
C42B0.087 (5)0.081 (5)0.090 (6)0.014 (4)0.017 (4)0.024 (4)
C42C0.091 (5)0.052 (4)0.116 (7)0.007 (4)0.016 (5)0.003 (4)
C430.076 (4)0.080 (5)0.066 (4)0.013 (4)0.003 (3)0.011 (4)
C440.076 (4)0.088 (5)0.070 (4)0.012 (4)0.012 (3)0.004 (4)
N450.059 (3)0.071 (4)0.081 (4)0.001 (3)0.001 (3)0.016 (3)
Geometric parameters (Å, º) top
Pb1—S312.8698 (16)C24—N251.366 (9)
Pb1—S412.9057 (19)C24—H240.93
Pb1—S212.9299 (16)N25—H250.86
Pb1—Cl13.0374 (18)S31—C311.714 (6)
Pb1—Cl23.0787 (17)C31—N351.341 (8)
Pb1—S113.0790 (16)C31—N321.364 (7)
S11—C111.691 (6)N32—C331.384 (8)
C11—N121.358 (7)N32—C321.500 (8)
C11—N151.364 (7)C32—C32B1.516 (9)
N12—C131.388 (8)C32—C32C1.531 (9)
N12—C121.503 (8)C32—C32A1.531 (9)
C12—C12C1.511 (9)C32A—H32A0.96
C12—C12A1.515 (10)C32A—H32B0.96
C12—C12B1.526 (9)C32A—H32C0.96
C12A—H12A0.96C32B—H32D0.96
C12A—H12B0.96C32B—H32E0.96
C12A—H12C0.96C32B—H32F0.96
C12B—H12D0.96C32C—H32G0.96
C12B—H12E0.96C32C—H32H0.96
C12B—H12F0.96C32C—H32I0.96
C12C—H12G0.96C33—C341.328 (9)
C12C—H12H0.96C33—H330.93
C12C—H12I0.96C34—N351.379 (8)
C13—C141.333 (10)C34—H340.93
C13—H130.93N35—H350.86
C14—N151.373 (8)S41—C411.717 (7)
C14—H140.93C41—N451.333 (8)
N15—H150.86C41—N421.361 (8)
S21—C211.707 (6)N42—C431.381 (8)
C21—N221.344 (8)N42—C421.500 (8)
C21—N251.345 (8)C42—C42B1.511 (10)
N22—C231.386 (9)C42—C42A1.515 (10)
N22—C221.496 (9)C42—C42C1.540 (10)
C22—C22C1.517 (10)C42A—H42A0.96
C22—C22B1.516 (11)C42A—H42B0.96
C22—C22A1.537 (10)C42A—H42C0.96
C22A—H22A0.96C42B—H42D0.96
C22A—H22B0.96C42B—H42E0.96
C22A—H22C0.96C42B—H42F0.96
C22B—H22D0.96C42C—H42G0.96
C22B—H22E0.96C42C—H42H0.96
C22B—H22F0.96C42C—H42I0.96
C22C—H22G0.96C43—C441.321 (11)
C22C—H22H0.96C43—H430.93
C22C—H22I0.96C44—N451.359 (10)
C23—C241.350 (11)C44—H440.93
C23—H230.93N45—H450.86
S31—Pb1—S4192.26 (6)N22—C23—H23126
S31—Pb1—S2187.51 (5)C23—C24—N25105.9 (7)
S41—Pb1—S2176.93 (5)C23—C24—H24127.1
S31—Pb1—Cl190.14 (5)N25—C24—H24127.1
S41—Pb1—Cl1166.54 (5)C21—N25—C24111.1 (6)
S21—Pb1—Cl189.95 (5)C21—N25—H25124.5
S31—Pb1—Cl2170.34 (5)C24—N25—H25124.5
S41—Pb1—Cl286.79 (6)C31—S31—Pb1100.6 (2)
S21—Pb1—Cl2101.62 (5)N35—C31—N32106.3 (5)
Cl1—Pb1—Cl293.01 (5)N35—C31—S31123.1 (4)
S31—Pb1—S1178.34 (4)N32—C31—S31130.6 (5)
S41—Pb1—S1181.82 (5)C31—N32—C33108.3 (5)
S21—Pb1—S11153.93 (5)C31—N32—C32126.8 (5)
Cl1—Pb1—S11111.64 (5)C33—N32—C32124.9 (5)
Cl2—Pb1—S1192.01 (4)N32—C32—C32B108.5 (5)
C11—S11—Pb1111.7 (2)N32—C32—C32C109.0 (5)
N12—C11—N15105.3 (5)C32B—C32—C32C109.3 (5)
N12—C11—S11130.8 (5)N32—C32—C32A108.5 (5)
N15—C11—S11123.9 (4)C32B—C32—C32A112.7 (6)
C11—N12—C13109.1 (5)C32C—C32—C32A108.8 (6)
C11—N12—C12126.3 (5)C32—C32A—H32A109.5
C13—N12—C12124.6 (5)C32—C32A—H32B109.5
N12—C12—C12C109.3 (5)H32A—C32A—H32B109.5
N12—C12—C12A108.8 (5)C32—C32A—H32C109.5
C12C—C12—C12A112.6 (7)H32A—C32A—H32C109.5
N12—C12—C12B107.7 (6)H32B—C32A—H32C109.5
C12C—C12—C12B109.5 (6)C32—C32B—H32D109.5
C12A—C12—C12B108.8 (6)C32—C32B—H32E109.5
C12—C12A—H12A109.5H32D—C32B—H32E109.5
C12—C12A—H12B109.5C32—C32B—H32F109.5
H12A—C12A—H12B109.5H32D—C32B—H32F109.5
C12—C12A—H12C109.5H32E—C32B—H32F109.5
H12A—C12A—H12C109.5C32—C32C—H32G109.5
H12B—C12A—H12C109.5C32—C32C—H32H109.5
C12—C12B—H12D109.5H32G—C32C—H32H109.5
C12—C12B—H12E109.5C32—C32C—H32I109.5
H12D—C12B—H12E109.5H32G—C32C—H32I109.5
C12—C12B—H12F109.5H32H—C32C—H32I109.5
H12D—C12B—H12F109.5C34—C33—N32108.4 (6)
H12E—C12B—H12F109.5C34—C33—H33125.8
C12—C12C—H12G109.5N32—C33—H33125.8
C12—C12C—H12H109.5C33—C34—N35106.8 (6)
H12G—C12C—H12H109.5C33—C34—H34126.6
C12—C12C—H12I109.5N35—C34—H34126.6
H12G—C12C—H12I109.5C31—N35—C34110.3 (5)
H12H—C12C—H12I109.5C31—N35—H35124.9
C14—C13—N12108.3 (6)C34—N35—H35124.9
C14—C13—H13125.9C41—S41—Pb1101.6 (2)
N12—C13—H13125.9N45—C41—N42106.0 (6)
C13—C14—N15106.7 (6)N45—C41—S41124.2 (5)
C13—C14—H14126.7N42—C41—S41129.8 (5)
N15—C14—H14126.7C41—N42—C43107.5 (6)
C11—N15—C14110.7 (5)C41—N42—C42127.3 (5)
C11—N15—H15124.7C43—N42—C42125.1 (6)
C14—N15—H15124.7N42—C42—C42B109.8 (5)
C21—S21—Pb1117.4 (2)N42—C42—C42A109.0 (6)
N22—C21—N25106.3 (5)C42B—C42—C42A111.3 (7)
N22—C21—S21129.2 (5)N42—C42—C42C108.9 (6)
N25—C21—S21124.5 (5)C42B—C42—C42C109.5 (7)
C21—N22—C23108.7 (6)C42A—C42—C42C108.4 (6)
C21—N22—C22126.8 (5)C42—C42A—H42A109.5
C23—N22—C22124.4 (6)C42—C42A—H42B109.5
N22—C22—C22C109.2 (6)H42A—C42A—H42B109.5
N22—C22—C22B108.1 (6)C42—C42A—H42C109.5
C22C—C22—C22B112.0 (7)H42A—C42A—H42C109.5
N22—C22—C22A109.2 (7)H42B—C42A—H42C109.5
C22C—C22—C22A108.4 (7)C42—C42B—H42D109.5
C22B—C22—C22A109.9 (7)C42—C42B—H42E109.5
C22—C22A—H22A109.5H42D—C42B—H42E109.5
C22—C22A—H22B109.5C42—C42B—H42F109.5
H22A—C22A—H22B109.5H42D—C42B—H42F109.5
C22—C22A—H22C109.5H42E—C42B—H42F109.5
H22A—C22A—H22C109.5C42—C42C—H42G109.5
H22B—C22A—H22C109.5C42—C42C—H42H109.5
C22—C22B—H22D109.5H42G—C42C—H42H109.5
C22—C22B—H22E109.5C42—C42C—H42I109.5
H22D—C22B—H22E109.5H42G—C42C—H42I109.5
C22—C22B—H22F109.5H42H—C42C—H42I109.5
H22D—C22B—H22F109.5C44—C43—N42109.1 (7)
H22E—C22B—H22F109.5C44—C43—H43125.4
C22—C22C—H22G109.5N42—C43—H43125.4
C22—C22C—H22H109.5C43—C44—N45106.2 (7)
H22G—C22C—H22H109.5C43—C44—H44126.9
C22—C22C—H22I109.5N45—C44—H44126.9
H22G—C22C—H22I109.5C41—N45—C44111.3 (6)
H22H—C22C—H22I109.5C41—N45—H45124.3
C24—C23—N22108.0 (6)C44—N45—H45124.3
C24—C23—H23126

Experimental details

Crystal data
Chemical formula[PbCl2(C7H12N2S)4]
Mr903.07
Crystal system, space groupMonoclinic, P21/c
Temperature (K)293
a, b, c (Å)10.2683 (11), 10.9843 (13), 34.514 (4)
β (°) 93.294 (9)
V3)3886.4 (8)
Z4
Radiation typeCu Kα
µ (mm1)11.97
Crystal size (mm)0.40 × 0.29 × 0.17
Data collection
DiffractometerEnraf-Nonius CAD-4
diffractometer
Absorption correctionAnalytical
(Katayama, 1986)
Tmin, Tmax0.048, 0.214
No. of measured, independent and
observed [I > 2σ(I)] reflections
10879, 6878, 5838
Rint0.051
(sin θ/λ)max1)0.597
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.047, 0.130, 1.03
No. of reflections6878
No. of parameters404
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.68, 1.50

Computer programs: CAD-4 EXPRESS (Enraf-Nonius, 1994), CAD-4 EXPRESS, XCAD4 (Harms & Wocadlo, 1995), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).

Selected geometric parameters (Å, º) top
Pb1—S312.8698 (16)Pb1—Cl13.0374 (18)
Pb1—S412.9057 (19)Pb1—Cl23.0787 (17)
Pb1—S212.9299 (16)Pb1—S113.0790 (16)
S31—Pb1—S4192.26 (6)S21—Pb1—Cl2101.62 (5)
S31—Pb1—S2187.51 (5)Cl1—Pb1—Cl293.01 (5)
S41—Pb1—S2176.93 (5)S31—Pb1—S1178.34 (4)
S31—Pb1—Cl190.14 (5)S41—Pb1—S1181.82 (5)
S41—Pb1—Cl1166.54 (5)S21—Pb1—S11153.93 (5)
S21—Pb1—Cl189.95 (5)Cl1—Pb1—S11111.64 (5)
S31—Pb1—Cl2170.34 (5)Cl2—Pb1—S1192.01 (4)
S41—Pb1—Cl286.79 (6)
 

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