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 |
R1 = ∑(||Fo|-|Fc||)/∑| Fo |; wR2 = [∑w(|Fo|-|Fc|2)2]/∑w(|Fo|2)]1/2.