A solution and solid state study of niobium complexes University of ...
A solution and solid state study of niobium complexes University of ... A solution and solid state study of niobium complexes University of ...
Chapter 4 Table 4.7: Selected bond lengths for [NbCl(phacac-κ 2 -O,O’)(OMe)3] and [NbCl2(phacac-κ 2 - O,O’)(OMe)2]. Atoms Bond length (Å) Atom Bond length (Å) Nb – O1 2.094 (3) Nb – Cl2 2.412 (8) Nb – O2 2.077 (3) O1 – C1 1.276 (6) Nb – O3 1.830 (2) O2 – C3 1.281 (5) Nb – O4 1.837 (4) O3 – C5 1.491 (8) Nb – O5 1.839 (4) O4 – C6 1.402 (8) Nb – Cl1 2.432 (2) O5 – C7 1.404 (6) Table 4.8: Selected bond angles for [NbCl(phacac-κ 2 -O,O’)(OMe)3] and [NbCl2(phacac-κ 2 - O,O’)(OMe)2]. Atoms Bond angles (°) Atoms Bond angles (°) O1 – Nb – O3 94.30 (8) O4 – Nb – O3 92.70 (8) O1 – Nb – O4 170.27 (17) O4 – Nb – O5 73 101.22 (17) O1 – Nb – O2 80.65 (13) O5 – Nb – O1 85.23 (15) O2 – Nb – O3 88.80 (8) O1 – Nb – Cl2 84.83 (16) O2 – Nb – O4 92.76 (16) O1 – Nb – Cl1 84.42 (12) O3 – Nb – O5 92.50 (7) O3 – Nb – Cl1 171.85 (10) O3 – Nb – O2 80.03 (10) Cl1 – Nb – Cl2 163.87 (11) The distortion in the two molecules are further illustrated in Figures 4.12 and 4.13. A plane was constructed through O1, O2, C1 and C3 of the phacac ligand (purple) as well as through C11, C12, C13, C14, C15 and C16 of the phenyl ring (pink) on C1, as indicated in Figure 4.12. The dihedral angle between the phenyl ring and the acetylacetone backbone is -7.33 (8) °.
Chapter 4 Figure 4.12: The phacac plane constructed through O1, O2, C1 and C3 (purple) illustrating the angle of the phenyl ring (pink) at C1. A plane was constructed through O1, O2, O4 and O5 as indicated in Figure 4.13. The niobium metal centre is slightly elevated above this plane by 0.071 (4) Å. This illustrates the distorted octahedral geometry of the molecule. Figure 4.13: Side view of the equatorial plane through O1, O2, O4 and O5. 74
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Chapter 4<br />
Table 4.7: Selected bond lengths for [NbCl(phacac-κ 2 -O,O’)(OMe)3] <strong>and</strong> [NbCl2(phacac-κ 2 -<br />
O,O’)(OMe)2].<br />
Atoms Bond length (Å) Atom Bond length (Å)<br />
Nb – O1 2.094 (3) Nb – Cl2 2.412 (8)<br />
Nb – O2 2.077 (3) O1 – C1 1.276 (6)<br />
Nb – O3 1.830 (2) O2 – C3 1.281 (5)<br />
Nb – O4 1.837 (4) O3 – C5 1.491 (8)<br />
Nb – O5 1.839 (4) O4 – C6 1.402 (8)<br />
Nb – Cl1 2.432 (2) O5 – C7 1.404 (6)<br />
Table 4.8: Selected bond angles for [NbCl(phacac-κ 2 -O,O’)(OMe)3] <strong>and</strong> [NbCl2(phacac-κ 2 -<br />
O,O’)(OMe)2].<br />
Atoms Bond angles (°) Atoms Bond angles (°)<br />
O1 – Nb – O3 94.30 (8) O4 – Nb – O3 92.70 (8)<br />
O1 – Nb – O4<br />
170.27 (17) O4 – Nb – O5<br />
73<br />
101.22 (17)<br />
O1 – Nb – O2 80.65 (13) O5 – Nb – O1 85.23 (15)<br />
O2 – Nb – O3 88.80 (8) O1 – Nb – Cl2 84.83 (16)<br />
O2 – Nb – O4 92.76 (16) O1 – Nb – Cl1<br />
84.42 (12)<br />
O3 – Nb – O5 92.50 (7) O3 – Nb – Cl1 171.85 (10)<br />
O3 – Nb – O2 80.03 (10) Cl1 – Nb – Cl2 163.87 (11)<br />
The distortion in the two molecules are further illustrated in Figures 4.12 <strong>and</strong> 4.13. A<br />
plane was constructed through O1, O2, C1 <strong>and</strong> C3 <strong>of</strong> the phacac lig<strong>and</strong> (purple) as<br />
well as through C11, C12, C13, C14, C15 <strong>and</strong> C16 <strong>of</strong> the phenyl ring (pink) on C1,<br />
as indicated in Figure 4.12. The dihedral angle between the phenyl ring <strong>and</strong> the<br />
acetylacetone backbone is -7.33 (8) °.
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