Effendy et al. / Inorganica Chimica Acta 358 (2005) 763–795
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1035s, 996s, 620s (ClO4), 518m, 504s, 478m, 452m,
433w, 428w, 359w, 325w, 290w, 261w, 223w, 186w,
151w, 99w, 88w, 81w, 73m. ESI MS (+): 534 [100]
[Ag(dppb)]+. Anal. Calc. for C28H28AgClO4P2: C,
53.06; H; 4.45. Found: C, 53.23; H, 4.62%. Km (CH2Cl2,
d 19.0br, 19.5br, 28.0br, 28.5br (CH2dppp), 128.5br,
129.1br, 130.9, 131.1, 132.2, 133.3br (Carom). 31P{1H}
NMR (CDCl3, 293 K): d ꢀ12.9 (br). 31P{1H} NMR
(CDCl3, 218 K): ꢀ12.9. IR (nujol, cmꢀ1): 3072w,
. . .
3052w (CHarom), 1585w, 1571w (C C); 514s, 482s,
•
10ꢀ3 M): 40 Xꢀ1 mol2 cmꢀ1
.
467m, 444m, 432w, 417m, 370w, 345w, 279w, 244w,
185s,. 165br, 119m, 100w, 87w, 77w. ESI MS (+): 490
[20] [Cu2(dppb)2]++; 531 [30] [Cu(dppb)(MeCN)]+; 916
[100] [Cu(dppb)2]+, 1005 [15] [Cu2(Cl)(dppb)2]+. Anal.
Calc. for C28H28CuClP2: C, 64.00; H; 5.37. Found: C,
64.12; H, 5.43%. Km (CH2Cl2, 10ꢀ3 M): 5 Xꢀ1 mol2
2.2.1.14. Synthesis of AgNO3:dppb (1:1)2 (14). Com-
pound 14 has been prepared as a colourless solid in
76% yield, using a similar procedure to that reported
for compound 13, but with a MeCN:EtOH 1:1 mixture
as solvent. It was recrystallised from MeCN; m.p. 272–
276 ꢁC dec. 1H NMR (CDCl3, 293 K): d 1.81br, 1.95 (m
br, 4H, CH2(CH2)2CH2), 2.32br, 2.38br (br, 4H,
CH2(CH2)2CH2), 7.2–7.3, 7.5 (m, 20H, C6H5). 13C
cmꢀ1
.
2.2.1.17. Synthesis of CuBr:dppb (1:1)2 Æ4CHBr3
(17). Compound 17 was obtained as a colourless crys-
talline solid, using a similar procedure to that reported
NMR (CDCl3, 293 K):
128.89d, 130.0d, 130.6d, 133.49s (Carom). 31P{1H}
d 25.5, 28.1 (CH2dppb),
1
for compound 16; m.p. 278 ꢁC dec. H NMR (CDCl3,
1
NMR (CDCl3, 293 K): d 0.80 (d br, J(31P,Ag) = 471
293 K): d 1.9 (m br, 4H, CH2(CH2)2CH2), 2.7 (br, 4H,
CH2(CH2)2CH2), 7.0–7.8 (m br, 20H, C6H5). 13C NMR
(CDCl3, 293 K): d 19.0br, 19.5br, 28.0br, 28.5br
(CH2dppp), 128.5br, 129.1br, 130.9, 131.1, 132.2,
133.3br (Carom). IR (nujol, cmꢀ1): 3072w, 3052w (CHar-
Hz), 2.96 (dd br, 1J(31P,Ag) = 480 Hz). IR (nujol,
cmꢀ1): 3052w (CHarom), 1586w, 1537w (C C); 1455s,
. . .
•
1433s, 1393s, 1312s (NO3); 552w, 512s, 496s, 479s,
451s, 420s, 354w, 332w, 299s, 242w, 204w, 148m,
131m, 120m, 92mbr. ESI MS (+): 534 [100] [Ag(dppb)]+;
960 [90] [Ag(dppb)2]+; 1130 [40] [Ag2(NO3)(dppb)2]+.
Anal. Calc. for C28H28AgNO3P2: C, 56.39; H; 4.73; N,
2.35. Found: C, 56.76; H, 4.72; N, 2.41%. Km (CH2Cl2,
. . .
om), 1585w, 1571w (C C); 514s, 482s, 462m, 445m,
•
427w, 417w, 370w, 347w, 279w, 246w, 189br w, 150w,
133m, 122m, 100w, 87w, 77w. ESI MS (+): 490 [20]
[Cu2(dppb)2]++; 531 [30] [Cu(dppb)(MeCN)]+; 916 [100]
[Cu(dppb)2]+, 1005 [15] [Cu2Br(dppb)2]+. Anal. Calc.
for C28H28CuBrP2: C, 59.01; H; 4.95. Found: C, 58.86;
10ꢀ3 M): 15 Xꢀ1 mol2 cmꢀ1
.
2.2.1.15. Synthesis of Ag(tfa):dppb (1:1)2 (15). Com-
pound 15 has been prepared in 65% yield as a colourless
solid, using a similar procedure to that reported for
compound 13. It was recrystallised from MeCN; m.p.
H, 4.81%. Km (CH2Cl2, 10ꢀ3 M): 5 Xꢀ1 mol2 cmꢀ1
.
2.2.1.18. Synthesis of AgCl:dppn (1:1)(1/1) ÆpyÆH2O
(18). dppn (0.44 g, 0.1 mmol) was added to a pyridine
(py) solution of AgCl (0.14 g, 0.1 mmol). Slow evapora-
tion of the solution yielded colourless crystals of com-
pound 18 in 75% yield after 8 days; m.p. 162–165 ꢁC
1
230–234 ꢁC dec. H NMR (CDCl3, 293 K): d 1.9 (m
br, 4H, CH2(CH2)2CH2), 2.4 (br, 4H, CH2(CH2)2CH2),
7.2–7.3, 7.5 (m, 20H, C6H5). 13C NMR (CDCl3, 293 K):
d 25.4, 27.2 (CH2dppb), 128.8br, 129.9br, 133.3br (Car-
om). 31P{1H} NMR (CDCl3, 293 K): d 0.01 (d br,
1J(31P,Ag) = 480 Hz), 1.94 (dd br, 1J(31P,Ag) = 480
Hz). IR (nujol, cmꢀ1): 3052w (CHarom), 1660sbr, 1460s
1
dec. H NMR (CDCl3, 295 K): d 1.6, 1.8, 2.5 (m br,
10H, (CH2)5), 7.2–7.4 (m, 20H, C6H5). 13C NMR
(CDCl3, 293 K): d 24.37s, 27.18s, 29.42s (CH2dppn),
128.71, 129.46, 133.30, 134.36 (Carom). 31P{1H} NMR
1
(CDCl3, 293 K): d ꢀ3.0 (d br, J(31P,Ag) = 361 Hz).
. . .
(CO), 1586w, 1537w (C C); 552w, 509s, 485s, 478s,m
•
463m, 447m, 438w, 424w, 399w, 381w, 352w, 295w,
277wm, 260m, 224w br, 175wbr, 151w, 100w, 89w,
77w, 71w. ESI MS (+): 534 [100] [Ag(dppb)]+; 960 [40]
[Ag(dppb)2]+; 1104 [95] [Ag2Cl(dppb)2]+, 1181 [20]
[Ag2(tfa)(dppb)2]+. Anal. Calc. for C30H28AgF3O2P2:
C, 55.66; H; 4.36. Found: C, 55.30; H, 4.18%. Km
IR (nujol, cmꢀ1): 3400br (OH), 3045w (CHarom),
. . .
1582w, (C C); 552w, 514s, 493m, 481br, 450w, 438w,
•
280w, 180m, 169w, 121w, 100w, 92w, 78w. ESI MS
(+): 548 [55] [Ag(dppn)]+; 1131 [100] [Ag2(Cl)(dppn)2]+.
Anal. Calc. for C34H37AgClNOP2: C, 59.97; H; 5.48; N,
2.06 Found: C, 60.12; H, 5.48; N, 1.96%. Km (CH2Cl2,
(CH2Cl2, 10ꢀ3 M): 2 Xꢀ1 mol2 cmꢀ1
.
10ꢀ3 M): 2 Xꢀ1 mol2 cmꢀ1
.
2.2.1.16. Synthesis of CuCl:dppb (1:1)2 Æ4CHBr3
(16). Compound 16 deposited in 80% yield as a colour-
less crystalline solid from a CHCl3 solution containing
dppb (0.43 g, 1.0 mmol) and CuCl (0.10 g, 1.0 mmol)
over 72. Recrystallisation from CHBr3 yielded 16; m.p.
278 ꢁC dec. H NMR (CDCl3, 293 K): d 1.8 (m br,
4H, CH2(CH2)2CH2), 2.6 (br, 4H, CH2(CH2)2CH2),
7.0–7.8 (m br, 20H, C6H5). 13C NMR (CDCl3, 293 K):
2.2.1.19. Synthesis of AgBr:dppn (1:1)2 (19). Com-
pound 19 has been prepared in 56% yield, using a similar
procedure to that reported for compound 1, using
MeCN as solvent. Crystals for the diffraction study were
obtained from 2-methylpyridine solution; m.p. 135–137
1
1
ꢁC dec. H NMR (CDCl3, 295 K): d 1.5, 2.2 (m br,
10H, (CH2)5), 7.2–7.4 (m, 20H, C6H5). 13C NMR
(CDCl3, 293 K): d 24.4br, 27.3br, 30.3br (CH2dppn),