organic compounds
Table 2
Selected geometric parameters (A, ) for (II).
for phenyl H atoms were set at 1.2Ueq(C) of the bonded C atoms,
whilst the methyl H atoms were given a common re®ned Uiso(H)
value. The largest peak and trough in the difference electron-density
ꢀ
Ê
P1ÐC1
P1ÐC7
P1ÐC13
P1ÐC31
1.814 (2)
1.801 (2)
1.789 (2)
1.787 (2)
P2ÐC2
P2ÐC19
P2ÐC25
C1ÐC2
1.858 (2)
1.838 (2)
1.834 (2)
1.406 (3)
Ê
map for [o-C6H4(PMe2)(PMe3)]I were less than 1 A from the I atom.
For compounds (I) and (II), data collection: COLLECT (Hooft,
1998) and DENZO (Otwinowski & Minor, 1997); cell re®nement:
COLLECT and DENZO; data reduction: COLLECT and DENZO.
For compound (III), data collection: MSC/AFC Diffractometer
Control Software (Molecular Structure Corporation, 1988); cell
re®nement: MSC/AFC Diffractometer Control Software; data reduc-
tion: TEXSAN (Molecular Structure Corporation, 1995). For all
compounds, program(s) used to solve structure: SHELXS97 (Shel-
drick, 1997); program(s) used to re®ne structure: SHELXL97
(Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976);
software used to prepare material for publication: SHELXL97.
C31ÐP1ÐC13
C31ÐP1ÐC7
C13ÐP1ÐC7
C31ÐP1ÐC1
C13ÐP1ÐC1
C7ÐP1ÐC1
111.96 (11)
106.12 (11)
109.57 (10)
111.19 (11)
107.57 (10)
110.46 (10)
C25ÐP2ÐC19
C25ÐP2ÐC2
C19ÐP2ÐC2
C2ÐC1ÐP1
C1ÐC2ÐP2
104.26 (10)
100.67 (10)
101.50 (10)
120.79 (16)
121.29 (17)
Compound (III)
The authors thank the EPSRC for access to the Chemical
Database Service at Daresbury and Dr N. J. Hill for data
collections.
Crystal data
+
C11H19P2 ÁI
Z = 4
Dx = 1.532 Mg m
Mo Kꢂ radiation
ꢅ = 2.36 mm
T = 150 (2) K
Rhomb, colourless
0.2 Â 0.2 Â 0.05 mm
3
Mr = 340.10
Monoclinic, P21=c
1
Ê
a = 9.2002 (16) A
Supplementary data for this paper are available from the IUCr electronic
archives (Reference: FA3012). Services for accessing these data are
described at the back of the journal.
Ê
b = 11.846 (3) A
Ê
c = 13.566 (2) A
ꢃ = 94.312 (14)ꢀ
Ê
V = 1474.3 (5) A
3
Data collection
References
Rigaku AFC-7S diffractometer
!/2ꢆ scans
Absorption correction: scan
(North et al., 1968)
Tmin = 0.596, Tmax = 0.890
5375 measured re¯ections
2587 independent re¯ections
1772 re¯ections with I > 2ꢀ(I)
Rint = 0.120
Blessing, R. H. (1997). J. Appl. Cryst. 30, 421±426.
Davis, M. F., Levason, W., Reid, G. & Webster, M. (2006). Polyhedron, 25, 930±
936.
Dunne, B. J., Morris, R. B. & Orpen, A. G. (1991). J. Chem. Soc. Dalton Trans.
pp. 653±661.
ꢆmax = 25.0ꢀ
3 standard re¯ections
every 150 re¯ections
intensity decay: none
Genge, A. R. J., Hill, N. J., Levason, W. & Reid, G. (2001). J. Chem. Soc. Dalton
Trans. pp. 1007±1012.
Hart, R., Levason, W., Patel, B. & Reid, G. (2001). Eur. J. Inorg. Chem.
pp. 2927±2933.
Hill, N. J., Levason, W. & Reid, G. (2002). J. Chem. Soc. Dalton Trans.
pp. 1188±1192.
Hooft, R. W. W. (1998). COLLECT. Nonius BV, Delft, The Netherlands.
Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National
Laboratory, Tennessee, USA.
Kyba, E. P., Liu, S. T. & Harris, R. L. (1983). Organometallics, 2, 1877±1879.
Levason, W. (1990). Comments Inorg. Chem. 9, 331±361.
Levason, W., Matthews, M. L., Patel, B., Reid, G. & Webster, M. (2004). Dalton
Trans. pp. 3305±3312.
McFarlane, H. C. E. & McFarlane, W. (1983). Polyhedron, 2, 303±304.
Molecular Structure Corporation (1988). MSC/AFC Diffractometer Control
Software. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381,
USA.
Molecular Structure Corporation (1995). TEXSAN. Version 1.7-1. MSC, 3200
Research Forest Drive, The Woodlands, TX 77381, USA.
North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351±
359.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M.
Sweet, pp. 307±326. New York: Academic Press.
Roberts, N. K., Skelton, B. W. & White, A. H. (1980). J. Chem. Soc. Dalton
Trans. pp. 1567±1571.
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of
Re®nement
Re®nement on F2
R[F2 > 2ꢀ(F2)] = 0.046
wR(F2) = 0.121
S = 0.97
2587 re¯ections
128 parameters
H-atom parameters constrained
w = 1/[ꢀ2(F2o) + (0.0668P)2]
where P = (F2o + 2Fc2)/3
(Á/ꢀ)max = 0.001
3
Ê
Áꢇmax = 2.21 e A
3
Ê
2.89 e A
Áꢇmin
=
Table 3
Selected geometric parameters (A, ) for (III).
ꢀ
Ê
P1ÐC1
P1ÐC7
P1ÐC8
P1ÐC9
1.820 (5)
1.794 (6)
1.795 (6)
1.792 (5)
P2ÐC2
P2ÐC10
P2ÐC11
C1ÐC2
1.858 (5)
1.832 (6)
1.843 (7)
1.390 (8)
C9ÐP1ÐC8
C9ÐP1ÐC7
C8ÐP1ÐC7
C9ÐP1ÐC1
C8ÐP1ÐC1
C7ÐP1ÐC1
110.4 (3)
106.4 (3)
106.5 (3)
111.4 (3)
112.2 (3)
109.6 (3)
C10ÐP2ÐC11
C10ÐP2ÐC2
C11ÐP2ÐC2
C2ÐC1ÐP1
C1ÐC2ÐP2
100.4 (3)
101.3 (3)
100.5 (3)
123.3 (4)
121.4 (4)
È
Gottingen, Germany.
Sigl, M., Schier, A. & Schmidbaur, H. (1998a). Eur. J. Inorg. Chem. pp. 203±
210.
Sigl, M., Schier, A. & Schmidbaur, H. (1998b). Z. Naturforsch. Teil B, 53,
1313±1315.
Warren, L. F. & Bennett, M. A. (1976). Inorg. Chem. 15, 3126±3140.
H atoms were placed in calculated positions [CÐH = 0.95
Ê
(aromatic) and 0.98 A (methyl)]. For (I) and (II), a common re®ned
Uiso(H) value was used for all the H atoms. For (III), Uiso(H) values
+
+
ꢁ
o440 Levason et al. C30H24P2, C31H27P2 ÁI and C11H19P2 ÁI
Acta Cryst. (2006). C62, o438±o440