The reaction of
As a continuation of our work on the synthesis and solid-state structures of phosphorus(III) ligands containing direct P–N bonds and derivatives [
All experiments were carried out under purified dry nitrogen using standard Schlenk and vacuum line techniques. Solvents were dried and freshly distilled under nitrogen [
A solution of
Crystallographic data are given in Table
Crystal data and structure refinement for
Formula | C38H27CrNO4P2 |
|
4 |
|
675.55 |
|
1.342 |
Temp [K] | 150(2) |
|
1392 |
Crystal system | Monoclinic | Abs coeff [mm−1] | 4.053 |
Space group |
|
No. of rflns coll. | 24513 |
|
12.209(5) | No. of indep rflns | 6488 |
|
20.003(5) |
|
0.0223 |
|
13.954(5) | No. of params | 415 |
|
90 |
|
0.0313 |
|
101.085(5) | w |
0.0869 |
|
90 |
|
0.200 |
|
3344(2) |
|
−0.323 |
Complex
Yellow colored crystals of
Selected bond lengths (Å) and bond angles (deg.) for
Cr1−C11 | 1.883(2) | C14−Cr1−C11 | 175.52(8) |
Cr1−C12 | 1.859(2) | P1−Cr1−C12 | 100.26(7) |
Cr1−C13 | 1.865(2) | P1−Cr1−C13 | 166.57(7) |
Cr1−C14 | 1.881(2) | P1−Cr1−C14 | 88.05(6) |
Cr1−P1 | 2.347(1) | P2−Cr1−C11 | 93.51(6) |
Cr1−P2 | 2.347(1) | P2−Cr1−C12 | 168.99(6) |
P1−N1 | 1.719(1) | P2−Cr1−C13 | 97.99(7) |
P2−N1 | 1.722(1) | P2−Cr1−C14 | 90.89(6) |
P1−C15 | 1.829(2) | P1−N1−P2 | 100.70(7) |
P1−C21 | 1.818(2) | P1−Cr1−P2 | 68.74(3) |
P2−C27 | 1.819(2) | P1−Cr1−C11 | 92.79(6) |
P2−C33 | 1.830(2) | N1−P1−Cr1 | 94.26(5) |
N1−C1 | 1.443(2) | N1−P2−Cr1 | 94.19(5) |
C11−O1 | 1.136(2) | N1−P1−C15 | 105.49(7) |
C12−O2 | 1.147(2) | N1−P1−C21 | 109.46(8) |
C13−O3 | 1.140(2) | N1−P2−C27 | 106.55(8) |
C14−O4 | 1.146(2) | N1−P2−C33 | 109.00(7) |
C12−Cr1−C11 | 86.43(9) | C15−P1−C21 | 100.97(8) |
C12−Cr1−C13 | 93.02(9) | C27−P2−C33 | 101.42(8) |
C12−Cr1−C14 | 89.09(8) |
|
359.91(9) |
C13−Cr1−C11 | 90.05(9) | P2−Cr1−P1−N1 | −9.66(5) |
C13−Cr1−C14 | 90.15(9) | C3−C2−C1−N1 | −177.61(2) |
An
The crystal structure of
The ability of the
To the best of our knowledge, there are other three structurally characterized monocyclic four-membered ring complexes of bidentate
A comparison of the structural data of the P–Cr–P and P–N–P bond angles in
The P–N–P [100.70(7)°] bond angle is significantly smaller than those in the free diphosphinoamine ligands [
The C-napthyl skeleton in
The average P–N bond distance in
The two Cr–P bond distances [2.347(1) and 2.347(1) Å] in
The Cr–C bond distances are 1.859(2)–1.883(2) Å for
In conclusion, we have shown the synthesis and molecular structure of
The author declares that there is no conflict of interests regarding the publication of this paper.