Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536800020146/na6024sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536800020146/na6024Isup2.hkl |
CCDC reference: 155845
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.011 Å
- R factor = 0.053
- wR factor = 0.146
- Data-to-parameter ratio = 35.3
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 33.18 From the CIF: _reflns_number_total 7977 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 8816 Completeness (_total/calc) 90.48% Alert C: < 95% complete PLAT_702 Alert C Angle Calc 122.04(5), Rep 122.10(10), Dev. 1.20 Sigma S2 -PB1 -S3 2.565 1.555 1.555
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check
An excess quantity of carbon disulfide was added dropwise to a solution of lead(II) chloride and ethylcyclohexylamine (1:2 molar ratio) in ethanol. The dithiocarbamate slowly separated from solution; this was collected and air dried to afford crystals (m.p. 421–422 K). Elemental analysis, found (calculated in parenthesis): C 35.37 (35.36), H 4.75 (5.23), N 4.73 (4.58), S 21.44% (20.96%).
The diffraction data are complete to θ = 25°; the overall, slightly low, completeness of the diffraction data is because of the incompleteness in the 25 < θ < 33° range.
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Fig. 1. ORTEPII (Johnson, 1976) plot of (I) at the 50% probability level. H atoms are drawn as spheres of arbitrary radii. |
[Pb(C9H16NS2)2] | Z = 2 |
Mr = 611.89 | F(000) = 600 |
Triclinic, P1 | Dx = 1.763 Mg m−3 |
a = 9.7180 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 10.1871 (2) Å | Cell parameters from 4596 reflections |
c = 11.8751 (3) Å | θ = 2.7–33.2° |
α = 95.586 (1)° | µ = 7.69 mm−1 |
β = 92.978 (1)° | T = 298 K |
γ = 99.142 (1)° | Parallelepiped, yellow |
V = 1152.45 (4) Å3 | 0.48 × 0.28 × 0.24 mm |
Siemens CCD area-detector diffractometer | 7977 independent reflections |
Radiation source: fine-focus sealed tube | 4557 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.030 |
Detector resolution: 8.33 pixels mm-1 | θmax = 33.2°, θmin = 2.7° |
ω scans | h = −11→14 |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | k = −15→15 |
Tmin = 0.073, Tmax = 0.158 | l = −18→14 |
10652 measured reflections |
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)] = 0.053 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.146 | Riding |
S = 0.99 | w = 1/[σ2(Fo2) + (0.065P)2] where P = (Fo2 + 2Fc2)/3 |
7977 reflections | (Δ/σ)max < 0.001 |
226 parameters | Δρmax = 1.32 e Å−3 |
0 restraints | Δρmin = −2.09 e Å−3 |
[Pb(C9H16NS2)2] | γ = 99.142 (1)° |
Mr = 611.89 | V = 1152.45 (4) Å3 |
Triclinic, P1 | Z = 2 |
a = 9.7180 (2) Å | Mo Kα radiation |
b = 10.1871 (2) Å | µ = 7.69 mm−1 |
c = 11.8751 (3) Å | T = 298 K |
α = 95.586 (1)° | 0.48 × 0.28 × 0.24 mm |
β = 92.978 (1)° |
Siemens CCD area-detector diffractometer | 7977 independent reflections |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | 4557 reflections with I > 2σ(I) |
Tmin = 0.073, Tmax = 0.158 | Rint = 0.030 |
10652 measured reflections |
R[F2 > 2σ(F2)] = 0.053 | 0 restraints |
wR(F2) = 0.146 | Riding |
S = 0.99 | Δρmax = 1.32 e Å−3 |
7977 reflections | Δρmin = −2.09 e Å−3 |
226 parameters |
x | y | z | Uiso*/Ueq | ||
Pb1 | 0.26984 (2) | 0.58470 (2) | 0.01673 (2) | 0.06438 (12) | |
S1 | 0.2738 (2) | 0.6822 (2) | 0.2377 (2) | 0.0620 (4) | |
S2 | 0.0133 (2) | 0.6614 (2) | 0.0908 (1) | 0.0527 (4) | |
S3 | 0.3307 (2) | 0.8183 (2) | −0.0739 (2) | 0.0670 (5) | |
S4 | 0.5590 (2) | 0.6878 (2) | 0.0151 (2) | 0.0589 (4) | |
N1 | 0.0238 (5) | 0.6901 (5) | 0.3178 (4) | 0.048 (1) | |
N2 | 0.5912 (5) | 0.8659 (5) | −0.1366 (4) | 0.046 (1) | |
C1 | 0.0955 (6) | 0.6786 (6) | 0.2237 (5) | 0.047 (1) | |
C2 | −0.1298 (6) | 0.6725 (6) | 0.3106 (5) | 0.045 (1) | |
C3 | −0.1934 (7) | 0.5330 (7) | 0.3345 (7) | 0.063 (2) | |
C4 | −0.3511 (8) | 0.5127 (9) | 0.3260 (9) | 0.082 (2) | |
C5 | −0.4042 (8) | 0.6166 (9) | 0.4025 (7) | 0.076 (2) | |
C6 | −0.3440 (8) | 0.7535 (9) | 0.3749 (7) | 0.073 (2) | |
C7 | −0.1849 (8) | 0.7787 (7) | 0.3862 (6) | 0.064 (2) | |
C8 | 0.0969 (8) | 0.705 (1) | 0.4313 (6) | 0.077 (2) | |
C9 | 0.164 (1) | 0.849 (1) | 0.4694 (7) | 0.107 (4) | |
C10 | 0.5050 (6) | 0.7973 (6) | −0.0719 (5) | 0.048 (1) | |
C11 | 0.7372 (5) | 0.8396 (6) | −0.1447 (5) | 0.042 (1) | |
C12 | 0.7452 (7) | 0.7291 (6) | −0.2378 (6) | 0.056 (2) | |
C13 | 0.8931 (8) | 0.6965 (8) | −0.2398 (7) | 0.067 (2) | |
C14 | 0.9985 (7) | 0.8210 (8) | −0.2514 (6) | 0.064 (2) | |
C15 | 0.9891 (6) | 0.9292 (7) | −0.1576 (6) | 0.061 (2) | |
C16 | 0.8413 (7) | 0.9647 (6) | −0.1588 (6) | 0.055 (1) | |
C17 | 0.5429 (7) | 0.9666 (7) | −0.2039 (6) | 0.061 (2) | |
C18 | 0.491 (1) | 0.912 (1) | −0.3226 (8) | 0.107 (3) | |
H2a | −0.1598 | 0.6821 | 0.2322 | 0.054* | |
H3a | −0.1623 | 0.4678 | 0.2808 | 0.076* | |
H3b | −0.1608 | 0.5180 | 0.4100 | 0.076* | |
H4a | −0.3844 | 0.5173 | 0.2483 | 0.099* | |
H4b | −0.3876 | 0.4246 | 0.3465 | 0.099* | |
H5a | −0.5054 | 0.6040 | 0.3930 | 0.091* | |
H5b | −0.3780 | 0.6073 | 0.4809 | 0.091* | |
H6a | −0.3785 | 0.8197 | 0.4254 | 0.088* | |
H6b | −0.3755 | 0.7638 | 0.2979 | 0.088* | |
H7a | −0.1500 | 0.8666 | 0.3644 | 0.076* | |
H7b | −0.1525 | 0.7762 | 0.4645 | 0.076* | |
H8a | 0.1688 | 0.6494 | 0.4305 | 0.093* | |
H8b | 0.0309 | 0.6749 | 0.4855 | 0.093* | |
H9a | 0.2095 | 0.8544 | 0.5436 | 0.160* | |
H9b | 0.0925 | 0.9050 | 0.4718 | 0.160* | |
H9c | 0.2305 | 0.8794 | 0.4170 | 0.160* | |
H11a | 0.7649 | 0.8079 | −0.0730 | 0.050* | |
H12a | 0.7179 | 0.7567 | −0.3104 | 0.068* | |
H12b | 0.6806 | 0.6497 | −0.2254 | 0.068* | |
H13a | 0.9165 | 0.6596 | −0.1704 | 0.080* | |
H13b | 0.8975 | 0.6297 | −0.3030 | 0.080* | |
H14a | 1.0920 | 0.7989 | −0.2485 | 0.077* | |
H14b | 0.9807 | 0.8530 | −0.3241 | 0.077* | |
H15a | 1.0560 | 1.0082 | −0.1671 | 0.073* | |
H15b | 1.0125 | 0.8992 | −0.0851 | 0.073* | |
H16a | 0.8363 | 1.0336 | −0.0974 | 0.066* | |
H16b | 0.8190 | 0.9987 | −0.2298 | 0.066* | |
H17a | 0.6194 | 1.0398 | −0.2063 | 0.073* | |
H17b | 0.4684 | 1.0023 | −0.1663 | 0.073* | |
H18a | 0.4612 | 0.9816 | −0.3620 | 0.160* | |
H18b | 0.4137 | 0.8407 | −0.3211 | 0.160* | |
H18c | 0.5648 | 0.8783 | −0.3611 | 0.160* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pb1 | 0.0459 (1) | 0.0562 (2) | 0.0867 (2) | 0.0016 (1) | 0.0234 (1) | −0.0127 (1) |
S1 | 0.0356 (7) | 0.077 (1) | 0.074 (1) | 0.0031 (7) | 0.0074 (7) | 0.0165 (9) |
S2 | 0.0407 (7) | 0.0666 (9) | 0.0471 (8) | 0.0019 (6) | 0.0098 (6) | −0.0058 (7) |
S3 | 0.0411 (8) | 0.090 (1) | 0.076 (1) | 0.0244 (8) | 0.0148 (8) | 0.012 (1) |
S4 | 0.0452 (8) | 0.069 (1) | 0.070 (1) | 0.0149 (7) | 0.0187 (7) | 0.0269 (8) |
N1 | 0.040 (2) | 0.060 (3) | 0.042 (3) | 0.000 (2) | 0.004 (2) | 0.015 (2) |
N2 | 0.039 (2) | 0.047 (3) | 0.053 (3) | 0.011 (2) | 0.005 (2) | 0.007 (2) |
C1 | 0.039 (3) | 0.038 (3) | 0.063 (4) | 0.000 (2) | 0.011 (3) | 0.005 (2) |
C2 | 0.041 (3) | 0.054 (3) | 0.040 (3) | 0.008 (2) | 0.013 (2) | 0.006 (2) |
C3 | 0.051 (4) | 0.050 (3) | 0.090 (5) | 0.006 (3) | 0.010 (3) | 0.012 (3) |
C4 | 0.055 (4) | 0.074 (5) | 0.111 (7) | −0.009 (4) | 0.016 (4) | 0.005 (5) |
C5 | 0.046 (4) | 0.104 (6) | 0.081 (5) | 0.010 (4) | 0.016 (3) | 0.024 (5) |
C6 | 0.074 (5) | 0.088 (5) | 0.068 (4) | 0.040 (4) | 0.025 (4) | 0.012 (4) |
C7 | 0.071 (4) | 0.061 (4) | 0.059 (4) | 0.012 (3) | 0.018 (3) | 0.001 (3) |
C8 | 0.053 (4) | 0.126 (7) | 0.054 (4) | 0.004 (4) | 0.009 (3) | 0.028 (4) |
C9 | 0.089 (6) | 0.149 (9) | 0.056 (5) | −0.043 (6) | −0.002 (4) | −0.012 (5) |
C10 | 0.037 (3) | 0.057 (3) | 0.050 (3) | 0.014 (2) | 0.009 (2) | −0.001 (3) |
C11 | 0.033 (2) | 0.050 (3) | 0.042 (3) | 0.005 (2) | 0.005 (2) | 0.007 (2) |
C12 | 0.051 (3) | 0.049 (3) | 0.064 (4) | 0.003 (3) | 0.004 (3) | −0.009 (3) |
C13 | 0.057 (4) | 0.066 (4) | 0.079 (5) | 0.019 (3) | 0.015 (3) | −0.007 (4) |
C14 | 0.052 (4) | 0.092 (5) | 0.056 (4) | 0.022 (4) | 0.020 (3) | 0.016 (4) |
C15 | 0.039 (3) | 0.074 (4) | 0.068 (4) | 0.001 (3) | 0.011 (3) | 0.010 (3) |
C16 | 0.054 (3) | 0.047 (3) | 0.062 (4) | 0.001 (3) | 0.009 (3) | 0.001 (3) |
C17 | 0.051 (4) | 0.056 (4) | 0.077 (5) | 0.012 (3) | 0.001 (3) | 0.016 (3) |
C18 | 0.132 (9) | 0.106 (7) | 0.088 (7) | 0.037 (7) | −0.026 (6) | 0.028 (6) |
Pb1—S1 | 2.710 (2) | C3—H3a | 0.9700 |
Pb1—S2 | 2.883 (2) | C3—H3b | 0.9700 |
Pb1—S2i | 3.508 (2) | C4—H4a | 0.9700 |
Pb1—S3 | 2.700 (2) | C4—H4b | 0.9700 |
Pb1—S4 | 2.841 (2) | C5—H5a | 0.9700 |
Pb1—S4ii | 3.457 (2) | C5—H5b | 0.9700 |
S1—C1 | 1.726 (6) | C6—H6a | 0.9700 |
S2—C1 | 1.712 (6) | C6—H6b | 0.9700 |
S3—C10 | 1.740 (6) | C7—H7a | 0.9700 |
S4—C10 | 1.714 (6) | C7—H7b | 0.9700 |
N1—C1 | 1.353 (7) | C8—H8a | 0.9700 |
N1—C2 | 1.472 (7) | C8—H8b | 0.9700 |
N1—C8 | 1.473 (9) | C9—H9a | 0.9600 |
N2—C10 | 1.329 (7) | C9—H9b | 0.9600 |
N2—C17 | 1.478 (8) | C9—H9c | 0.9600 |
N2—C11 | 1.492 (7) | C11—H11a | 0.9800 |
C2—C3 | 1.517 (8) | C12—H12a | 0.9700 |
C2—C7 | 1.520 (8) | C12—H12b | 0.9700 |
C3—C4 | 1.51 (1) | C13—H13a | 0.9700 |
C4—C5 | 1.50 (1) | C13—H13b | 0.9700 |
C5—C6 | 1.50 (1) | C14—H14a | 0.9700 |
C6—C7 | 1.52 (1) | C14—H14b | 0.9700 |
C8—C9 | 1.52 (1) | C15—H15a | 0.9700 |
C11—C12 | 1.513 (8) | C15—H15b | 0.9700 |
C11—C16 | 1.524 (8) | C16—H16a | 0.9700 |
C12—C13 | 1.527 (9) | C16—H16b | 0.9700 |
C13—C14 | 1.52 (1) | C17—H17a | 0.9700 |
C14—C15 | 1.51 (1) | C17—H17b | 0.9700 |
C15—C16 | 1.535 (9) | C18—H18a | 0.9600 |
C17—C18 | 1.50 (1) | C18—H18b | 0.9600 |
C2—H2a | 0.9800 | C18—H18c | 0.9600 |
S1—Pb1—S2 | 64.0 (1) | C6—C5—H5b | 109.7 |
S1—Pb1—S2i | 117.3 (1) | C4—C5—H5b | 109.7 |
S1—Pb1—S3 | 98.9 (1) | H5a—C5—H5b | 108.2 |
S1—Pb1—S4 | 90.0 (1) | C5—C6—H6a | 109.2 |
S1—Pb1—S4ii | 111.4 (1) | C7—C6—H6a | 109.2 |
S2—Pb1—S2i | 70.4 (1) | C5—C6—H6b | 109.2 |
S2—Pb1—S3 | 89.9 (1) | C7—C6—H6b | 109.2 |
S2—Pb1—S4 | 140.9 (1) | H6a—C6—H6b | 107.9 |
S2—Pb1—S4ii | 141.6 (1) | C2—C7—H7a | 109.7 |
S2i—Pb1—S3 | 122.1 (1) | C6—C7—H7a | 109.7 |
S2i—Pb1—S4 | 148.0 (1) | C2—C7—H7b | 109.7 |
S2i—Pb1—S4ii | 80.8 (1) | C6—C7—H7b | 109.7 |
S3—Pb1—S4 | 64.6 (1) | H7a—C7—H7b | 108.2 |
S3—Pb1—S4ii | 127.5 (1) | N1—C8—H8a | 109.1 |
S4—Pb1—S4ii | 73.3 (1) | C9—C8—H8a | 109.1 |
C1—S1—Pb1 | 90.0 (2) | N1—C8—H8b | 109.1 |
C1—S2—Pb1 | 84.6 (2) | C9—C8—H8b | 109.1 |
C10—S3—Pb1 | 88.9 (2) | H8a—C8—H8b | 107.8 |
C10—S4—Pb1 | 84.9 (2) | C8—C9—H9a | 109.5 |
C1—N1—C2 | 121.4 (5) | C8—C9—H9b | 109.5 |
C1—N1—C8 | 120.4 (5) | H9a—C9—H9b | 109.5 |
C2—N1—C8 | 117.9 (5) | C8—C9—H9c | 109.5 |
C10—N2—C17 | 120.6 (5) | H9a—C9—H9c | 109.5 |
C10—N2—C11 | 120.3 (4) | H9b—C9—H9c | 109.5 |
C17—N2—C11 | 119.0 (5) | N2—C11—H11a | 107.0 |
N1—C1—S2 | 121.4 (4) | C12—C11—H11a | 107.0 |
N1—C1—S1 | 119.4 (5) | C16—C11—H11a | 107.0 |
S2—C1—S1 | 119.2 (3) | C11—C12—H12a | 109.5 |
N1—C2—C3 | 111.3 (5) | C13—C12—H12a | 109.5 |
N1—C2—C7 | 112.7 (5) | C11—C12—H12b | 109.5 |
C3—C2—C7 | 111.2 (5) | C13—C12—H12b | 109.5 |
C4—C3—C2 | 112.0 (6) | H12a—C12—H12b | 108.1 |
C5—C4—C3 | 111.2 (7) | C14—C13—H13a | 109.5 |
C6—C5—C4 | 109.9 (6) | C12—C13—H13a | 109.5 |
C5—C6—C7 | 112.3 (6) | C14—C13—H13b | 109.5 |
C2—C7—C6 | 109.6 (6) | C12—C13—H13b | 109.5 |
N1—C8—C9 | 112.5 (7) | H13a—C13—H13b | 108.0 |
N2—C10—S4 | 122.4 (4) | C15—C14—H14a | 109.5 |
N2—C10—S3 | 119.5 (4) | C13—C14—H14a | 109.5 |
S4—C10—S3 | 118.0 (3) | C15—C14—H14b | 109.5 |
N2—C11—C12 | 111.2 (5) | C13—C14—H14b | 109.5 |
N2—C11—C16 | 113.1 (5) | H14a—C14—H14b | 108.1 |
C12—C11—C16 | 111.1 (5) | C14—C15—H15a | 109.5 |
C11—C12—C13 | 110.7 (5) | C16—C15—H15a | 109.5 |
C14—C13—C12 | 110.9 (6) | C14—C15—H15b | 109.5 |
C15—C14—C13 | 110.7 (5) | C16—C15—H15b | 109.5 |
C14—C15—C16 | 110.7 (6) | H15a—C15—H15b | 108.1 |
C11—C16—C15 | 109.0 (5) | C11—C16—H16a | 109.9 |
N2—C17—C18 | 113.3 (6) | C15—C16—H16a | 109.9 |
N1—C2—H2a | 107.1 | C11—C16—H16b | 109.9 |
C3—C2—H2a | 107.1 | C15—C16—H16b | 109.9 |
C7—C2—H2a | 107.1 | H16a—C16—H16b | 108.3 |
C4—C3—H3a | 109.2 | N2—C17—H17a | 108.9 |
C2—C3—H3a | 109.2 | C18—C17—H17a | 108.9 |
C4—C3—H3b | 109.2 | N2—C17—H17b | 108.9 |
C2—C3—H3b | 109.2 | C18—C17—H17b | 108.9 |
H3a—C3—H3b | 107.9 | H17a—C17—H17b | 107.7 |
C5—C4—H4a | 109.4 | C17—C18—H18a | 109.5 |
C3—C4—H4a | 109.4 | C17—C18—H18b | 109.5 |
C5—C4—H4b | 109.4 | H18a—C18—H18b | 109.5 |
C3—C4—H4b | 109.4 | C17—C18—H18c | 109.5 |
H4a—C4—H4b | 108.0 | H18a—C18—H18c | 109.5 |
C6—C5—H5a | 109.7 | H18b—C18—H18c | 109.5 |
C4—C5—H5a | 109.7 | ||
S3—Pb1—S1—C1 | 94.1 (2) | N1—C2—C3—C4 | −179.3 (6) |
S4—Pb1—S1—C1 | 158.4 (2) | C7—C2—C3—C4 | 54.2 (9) |
S2—Pb1—S1—C1 | 8.7 (2) | C2—C3—C4—C5 | −56 (1) |
S4ii—Pb1—S1—C1 | −129.6 (2) | C3—C4—C5—C6 | 57 (1) |
S2i—Pb1—S1—C1 | −39.1 (2) | C4—C5—C6—C7 | −58.3 (9) |
S3—Pb1—S2—C1 | −108.7 (2) | N1—C2—C7—C6 | −179.6 (5) |
S1—Pb1—S2—C1 | −8.8 (2) | C3—C2—C7—C6 | −53.8 (7) |
S4—Pb1—S2—C1 | −61.8 (2) | C5—C6—C7—C2 | 56.8 (8) |
S4ii—Pb1—S2—C1 | 83.3 (2) | C1—N1—C8—C9 | 82.7 (9) |
S2i—Pb1—S2—C1 | 126.9 (2) | C2—N1—C8—C9 | −104.1 (7) |
S1—Pb1—S3—C10 | 96.7 (2) | C17—N2—C10—S4 | −175.5 (5) |
S4—Pb1—S3—C10 | 11.0 (2) | C11—N2—C10—S4 | 6.2 (8) |
S2—Pb1—S3—C10 | 160.3 (2) | C17—N2—C10—S3 | 4.3 (8) |
S4ii—Pb1—S3—C10 | −29.0 (2) | C11—N2—C10—S3 | −174.0 (4) |
S2i—Pb1—S3—C10 | −133.1 (2) | Pb1—S4—C10—N2 | −162.3 (5) |
S3—Pb1—S4—C10 | −11.2 (2) | Pb1—S4—C10—S3 | 17.9 (3) |
S1—Pb1—S4—C10 | −111.0 (2) | Pb1—S3—C10—N2 | 161.4 (5) |
S2—Pb1—S4—C10 | −65.1 (2) | Pb1—S3—C10—S4 | −18.8 (3) |
S4ii—Pb1—S4—C10 | 136.7 (2) | C10—N2—C11—C12 | 88.0 (7) |
S2i—Pb1—S4—C10 | 99.2 (2) | C17—N2—C11—C12 | −90.4 (6) |
C2—N1—C1—S2 | 7.3 (8) | C10—N2—C11—C16 | −146.2 (5) |
C8—N1—C1—S2 | −179.7 (5) | C17—N2—C11—C16 | 35.4 (7) |
C2—N1—C1—S1 | −173.0 (4) | N2—C11—C12—C13 | −176.1 (5) |
C8—N1—C1—S1 | −0.1 (8) | C16—C11—C12—C13 | 57.0 (7) |
Pb1—S2—C1—N1 | −166.1 (5) | C11—C12—C13—C14 | −55.4 (8) |
Pb1—S2—C1—S1 | 14.3 (3) | C12—C13—C14—C15 | 56.2 (8) |
Pb1—S1—C1—N1 | 165.2 (5) | C13—C14—C15—C16 | −58.2 (8) |
Pb1—S1—C1—S2 | −15.1 (3) | N2—C11—C16—C15 | 176.0 (5) |
C1—N1—C2—C3 | 98.6 (7) | C12—C11—C16—C15 | −58.1 (7) |
C8—N1—C2—C3 | −74.5 (8) | C14—C15—C16—C11 | 58.7 (7) |
C1—N1—C2—C7 | −135.6 (6) | C10—N2—C17—C18 | −93.5 (9) |
C8—N1—C2—C7 | 51.3 (8) | C11—N2—C17—C18 | 84.8 (8) |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y+1, −z. |
Experimental details
Crystal data | |
Chemical formula | [Pb(C9H16NS2)2] |
Mr | 611.89 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 298 |
a, b, c (Å) | 9.7180 (2), 10.1871 (2), 11.8751 (3) |
α, β, γ (°) | 95.586 (1), 92.978 (1), 99.142 (1) |
V (Å3) | 1152.45 (4) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 7.69 |
Crystal size (mm) | 0.48 × 0.28 × 0.24 |
Data collection | |
Diffractometer | Siemens CCD area-detector diffractometer |
Absorption correction | Empirical (using intensity measurements) (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.073, 0.158 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10652, 7977, 4557 |
Rint | 0.030 |
(sin θ/λ)max (Å−1) | 0.770 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.053, 0.146, 0.99 |
No. of reflections | 7977 |
No. of parameters | 226 |
H-atom treatment | Riding |
Δρmax, Δρmin (e Å−3) | 1.32, −2.09 |
Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), SHELXL97.
Pb1—S1 | 2.710 (2) | Pb1—S3 | 2.700 (2) |
Pb1—S2 | 2.883 (2) | Pb1—S4 | 2.841 (2) |
Pb1—S2i | 3.508 (2) | Pb1—S4ii | 3.457 (2) |
S1—Pb1—S2 | 64.0 (1) | S2—Pb1—S4ii | 141.6 (1) |
S1—Pb1—S2i | 117.3 (1) | S2i—Pb1—S3 | 122.1 (1) |
S1—Pb1—S3 | 98.9 (1) | S2i—Pb1—S4 | 148.0 (1) |
S1—Pb1—S4 | 90.0 (1) | S2i—Pb1—S4ii | 80.8 (1) |
S1—Pb1—S4ii | 111.4 (1) | S3—Pb1—S4 | 64.6 (1) |
S2—Pb1—S2i | 70.4 (1) | S3—Pb1—S4ii | 127.5 (1) |
S2—Pb1—S3 | 89.9 (1) | S4—Pb1—S4ii | 73.3 (1) |
S2—Pb1—S4 | 140.9 (1) |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y+1, −z. |
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Several lead(II) dithiocarbamates have been reported in the literature, e.g. bis(dimethyldithiocarbamato)lead (Iwasaki, 1980), bis(diethyldithiocarbamato)lead (Zvonkova et al., 1967), bis(diisopropyldithiocarbamato)lead (Ito & Iwasaki, 1980) and bis(N-ethyl-N-isopropyldithiocarbamato)lead(II) (Trindade, 1997; Ng, 1999). These compounds, as well as the title dithiocarbamate, (I), have the Pb atoms in a distorted tetrahedral geometry, and adjacent molecules are linked by Pb···S interactions into chains. The bond dimensions as well as the interactions in the title compound are similar to those found in other dithiocarbamates, and the size of the cyclohexyl ring does not appear to affect the packing.