1
626
Z. Spichal et al. / Polyhedron 30 (2011) 1620–1627
TG /%
00
DSC /(mW/mg)
[1]
1
↓
exo 8
9
8
7
6
5
4
3
0
0
0
0
0
0
0
6
4
2
0
-
-
-
2
4
6
[
1] -8
100
200
300
400
500
600
700
800
900
Temperature /°C
Fig. 6. The TG/DSC traces of 3Pr, in air, heating rate 5 °C/min.
4
.2.2. [Er(dppdO
2
)
2
(NO
3
)
2
]NO
3
Á2MeOH (2Er)
538w, 557m, 582vs, 617vw, 631vw, 694m, 704m, 729m, 752w,
818vw, 852vw, 931vw, 997vw, 1028w, 1090m, 1124s, 1151vs,
1300s, 1385s, 1437s, 1468s, 1591vw, 1630vw, 1730vw, 1768vw,
1826vw, 1907vw, 1977vw, 2295vw, 2426vw, 2503vw, 2712vw,
2993vw, 3028vw, 3059vw, 3423w.
Yield: 204 mg (74.6%). Anal. Calc.: C, 57.03; H, 4.14; N, 2.70.
Found: C, 56.25; H, 3.76; N, 2.70%. IR: 397vw, 419vw, 440vw,
4
7
9
1
1
2
61vw, 500vw, 517w, 550vs, 584vw, 617vw, 625vw, 694m, 710w,
23m, 750w, 802vw, 818vw, 829vw, 881vw, 932vw, 953vw,
97vw, 1032vw, 1078w, 1103m, 1121m, 1134m, 1155vs, 1165s,
236m, 1267w, 1304m, 1385vs, 1439vs, 1462s, 1543vw, 1568w,
591w, 1628vw, 1686vw, 1717vw, 1736vw, 1909vw, 1981vw,
4
.3.3. {[Nd
Yield: 73 mg (47.9%). Anal. Calc.: C, 50.96; H, 3.86; N, 3.83.
Found: C, 50.06; H, 3.50; N, 3.82%. IR: 415vw, 463vw, 478vw,
2
(dppbO
2
)
3
(NO
3
)
6
]Á3MeOH}
n
(3Nd)
324vw, 2426vw, 3057vw, 3424w, 3620vw. ESI-MS m/z ion (rel.
+
int. %): 1432 [Er(dppdO
1
2
)
2
(NO
3
)
2
] (100%), 1295 (25%), 1242 (20%),
5
8
1
1
2
38w, 557m, 582vs, 617vw, 631vw, 694m, 704m, 729m, 752w,
18vw, 852vw, 931vw, 997vw, 1028w, 1092m, 1124s, 1153vs,
302s, 1385s, 1439s, 1470s, 1576vw, 1591vw, 1630vw, 1728vw,
768vw, 1826vw, 1909vw, 1977vw, 2295vw, 2426vw, 2503vw,
713vw, 3028vw, 3059vw, 3423w.
+
+
2 2 2
163 [Na(dppdO ) ] (60%), 970 (15%), 571 [HdppdO ] (50%).
4
.2.3. [Lu(dppdO
Yield: 95 mg (51.1%). Anal. Calc.: C, 55.99; H, 4.45; N, 2.58.
Found: C, 55.62; H, 4.02; N, 2.62%. IR: 397vw, 420vw, 440vw,
2
)
2
(NO
3
)
2
]NO
3
Á3MeOH (2Lu)
4
7
9
1
1
3
59vw, 498vw, 517w, 550vs, 584vw, 617vw, 627vw, 694m,
10m, 723m, 731w, 750w, 800vw, 818vw, 883vw, 932vw,
53vw, 997vw, 1032vw, 1080w, 1103m, 1121m, 1134m, 1157vs,
167vs, 1236m, 1267m, 1310m, 1385vs, 1439vs, 1462s, 1568w,
591w, 1626vw, 1686vw, 1909vw, 1981vw, 2330vw, 2426vw,
057vw, 3422w, 3640vw. ESI-MS m/z ion (rel. int. %): 1439
4
.3.4. {[Sm
Yield: 104 mg (67.9%). Anal. Calc.: C, 50.68; H, 3.84; N, 3.81.
Found: C, 49.93; H, 3.49; N, 3.73%. IR: 417vw, 463vw, 478vw,
38w, 557m, 582vs, 617vw, 631vw, 694m, 704m, 729m, 752w,
16vw, 852vw, 931vw, 997vw, 1028w, 1092w, 1124s, 1155vs,
2
(dppbO
2
)
3
(NO
3
)
6
]Á3MeOH}
n
(3Sm)
5
8
+
+
1306s, 1385s, 1439s, 1473s, 1576vw, 1591vw, 1630vw, 1730vw,
1768vw, 1826vw, 1907vw, 1977vw, 2297vw, 2426vw, 2505vw,
2
[
Lu(dppdO
2
)
2
3
(NO )
2
]
2 2
(60%), 1259 (20%), 1163 [Na(dppdO ) ]
+
(
100%), 1015 (12%), 974 (15%), 571 [HdppdO
2
] (30%).
713vw, 3028vw, 3059vw, 3425w.
4
.3. Reactions of 3
4
.3.5. {[Er(dppbO
Yield: 57 mg (39.7%). Anal. Calc.: C, 54.19; H, 4.11; N, 3.06. Found:
C, 53.72; H, 3.75; N, 3.04%. IR: 424vw, 463vw, 476vw, 538w, 557s,
80vs, 617vw, 631vw, 694m, 704m, 729m, 752w, 816vw, 852vw,
30vw, 997vw, 1018vw, 1030vw, 1093w, 1122s, 1157vs, 1300m,
385vs, 1437m, 1483m, 1591vw, 1630vw, 1726vw, 1776vw,
826vw, 1911vw, 1979vw, 2426vw, 2993vw, 3059vw, 3425w.
2
)
2
(NO
3
)
2
]NO
3
Á2MeOH}
n
(3Er)
Ligand 3 (100 mg, 0.209 mmol) was dissolved in a mixture of
mL dichloromethane and 10 mL methanol (3 is insoluble in
5
5
9
1
1
methanol). Lanthanide nitrate salt (0.139 mmol) was added and
the mixture was stirred shortly and left to evaporate at ambient
temperature. First crystals usually appeared after 24 h and the
crystalline solid was isolated after the solvent was evaporated to
approximately 1/3 of the initial volume.
4
.3.6. {[Lu(dppbO
Yield: 30 mg (20.8%). Anal. Calc.: C, 53.88; H, 4.08; N, 3.04.
Found: C, 53.10; H, 3.69; N, 3.10%. IR: 424vw, 447vw, 463vw,
2
)
2
(NO
3
)
2
]NO
3
Á2MeOH}
n
(3Lu)
4
.3.1. {[Ce
Yield: 51 mg (33.6%). Anal. Calc.: C, 51.15; H, 3.88; N, 3.85.
Found: C, 50.59; H, 3.54; N, 3.80%. IR: 415vw, 447vw, 463vw,
2
(dppbO
2
)
3
(NO
3
)
6
]Á3MeOH}
n
(3Ce)
4
7
1
1
2
76vw, 538w, 555m, 580vs, 619vw, 631vw, 694m, 704m, 729m,
52w, 816vw, 852vw, 930vw, 997vw, 1018vw, 1030vw, 1093w,
122s, 1159vs, 1302m, 1385vs, 1439m, 1485m, 1591vw,
630vw, 1726vw, 1778vw, 1826vw, 1911vw, 1979vw, 2322vw,
426vw, 2511vw, 2607vw, 2993vw, 3059vw, 3427w.
4
7
1
1
2
78vw, 538w, 555m, 582vs, 617vw, 631vw, 694m, 704m, 731m,
52w, 818vw, 852vw, 931vw, 997vw, 1028w, 1090m, 1124s,
151vs, 1302s, 1385s, 1437s, 1466s, 1475s, 1576vw, 1591vw,
630vw, 1730vw, 1765vw, 1826vw, 1905vw, 1977vw, 2293vw,
426vw, 2499vw, 2605vw, 2713vw, 2993vw, 3059vw, 3423vw.
Acknowledgements
4
.3.2. {[Pr
Yield: 83 mg (57.2%). Anal. Calc.: C, 51.74; H, 3.47; N, 4.02.
Found: C, 52.53; H, 3.56; N, 3.69%. IR: 415vw, 463vw, 478vw,
2 2 3 3 6 n
(dppbO ) (NO ) ]} (3Pr)
This work was supported by the Ministry of Education of the
Czech Republic (MSM0021622410) and by the Czech Science