Table 3 Crystal data and refinement parameters for complexes 1-5
Complex 1 | Complex 2 | Complex 3 | Complex4 | Complex5 | |
|---|---|---|---|---|---|
Empirical formula | C20H12N2O4Cl2S2Pb | C22H16Cl2N2O4S2Pb | C44H24Cl4N4O8S4Pb2 | C22H16Br2N2O4PbS2 | C38H26Br2N4O8Pb2S2 |
Formula weight | 686.56 | 714.61 | 1421.15 | 803.51 | 1304.97 |
Temp, K | 296 | 296 | 296 | 296 | 296 |
λ (Å) | 0.71073 | 0.71073 | 0.71073 | 0.71073 | 0.71073 |
Crystal system | Triclinic | Triclinic | Triclinic | Triclinic | Monoclinic |
Space group | P-1 | P-1 | P-1 | P-1 | P21/c |
a (Å) | 9.0760(1) | 10.6261(3) | 10.2998(1) | 10.710(5) | 8.918(5) |
b (Å) | 12.0102(2) | 10.9835(2) | 11.3830(1) | 10.973(5) | 23.841(5) |
c (Å) | 12.0754(2) | 11.4710(2) | 11.4287(1) | 11.623(5) | 12.744(5) |
α(º) | 116.441(1) | 115.441(1) | 100.292(1) | 115.592(5) | 90 |
β (º) | 93.682(1) | 98.773(1) | 103.011(1) | 98.676(5) | 133.39(2) |
γ (º) | 106.176(1) | 96.052(1) | 115.391(1) | 96.238(5) | 90 |
V (Å3) | 1104.46(3) | 1172.71(5) | 1120.29(2) | 1194.5(9) | 1969.0(16) |
Z | 2 | 2 | 1 | 2 | 2 |
ρ calcd (g/cm3) | 2.065 | 2.024 | 2.106 | 2.234 | 2.201 |
μ (mm-1) | 8.099 | 7.632 | 7.989 | 10.615 | 10.732 |
F(000) | 652 | 684 | 676 | 756 | 1224 |
Crystal size (mm) | 0.04 × 0.05 × 0.05 | 0.05 x 0.05 × 0.06 | 0.04 × 0.05 × 0.06 | 0.08 × 0.09 × 0.06 | 0.09 × 0.05 × 0.06 |
No of reflections collected | 7170 | 8554 | 7529 | 8114 | 6592 |
Number restraints | 0 | 0 | 0 | 0 | 0 |
Goodness-of-fit on F2 | 1.026 | 1.03 | 1.00 | 1.02 | 0.98 |
Final R1 index [I > 2σ(I)] | 0.0239 | 0.0240 | 0.0303 | 0.0290 | 0.0309 |
wR2 (all data) | 0.0541 | 0.0556 | 0.0635 | 0.0633 | 0.0690 |
Largest difference in peak and hole (e Å-3) | −0.61, 1.14 | −0.63, 1.27 | −0.45, 1.18 | −1.08, 1.13 | −1.05, 0.88 |
CCDC number | 821366 | 821367 | 821365 | 920520 | 920521 |