96
R. Broussier et al. / Journal of Organometallic Chemistry 561 (1998) 85–96
parameters, and interatomic distances and angles for 3,
6 and 15 (11 pages).
(m, meta and meta%); 129.4 (s, para); 130.9 (s, para%);
2
131.5 (pqt, ortho, ꢀ JPC+4iJPCꢀ=15.9 Hz); 135.9 (pqt,
2
ortho%, ꢀ JPC+4JPCꢀ=14.3 Hz); (IV) 86.7 (pt, ipso Cp,
1
3
ꢀ JPC+2JPCꢀ=80.2 Hz); 86.8 (pt, i Cp, ꢀ JPC+3JPCꢀ=
9.0 Hz); 95.2 (pt, h Cp, ꢀ JPC+3JPCꢀ=7.6 Hz); 135.7
2
References
(pdd, ipso phenyl, ꢀ JPC+3JPCꢀ=43.9 Hz); 138.6 (pdd,
1
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ipso% phenyl, ꢀ JPC+3JPCꢀ=46.2 Hz); 198.7 (pt, CO,
1
2
2
ꢀ JPCꢀ=16.2 Hz); 209.0 (pt, CO, ꢀ JPCꢀ=17.1 Hz); 209.4
2
2
(pt, CO, ꢀ JPCꢀ=17.3 Hz); 209.9 (pt, CO, ꢀ JPCꢀ=16.0
P–
Hz). 31P-NMR, CDCl3: +29.4 (s) J(31
W)=232 Hz.
183
3.14. X-ray structure analyses
Crystals suitable for X-ray diffraction studies were
grown from chloroform/hexane (3 and 15) or cold
pentane (6) solutions. The pertinent crystallographic
data are gathered in Table 3. All measurements have
been carried out on an Enraf-Nonius CAD4 diffrac-
tometer at r.t.. The unit cells were determined for each
crystal from 25 reflections selected by the CAD4 rou-
tines. All calculations were carried out by use of the
MOLEN package [23] with neutral-atom scattering fac-
tors [24]. Intensities were corrected for Lorentz and
polarization effects as well as for linear decay. The
C-scan empirical absorption correction was applied for
6.
The structures were solved and refined by conven-
tional Patterson, difference Fourier, and full-matrix
least-squares methods. In the case of 15 a disordered
molecule of chloroform was found. Refinement of this
molecule led to the ratio 0.8/1 (with respect to the
organometallic one) and to an occupation of 0.5 for
one set of three chlorine atoms and 0.3 for a second set
of these atoms. An empirical absorption correction
DIFABS [25] was applied for 3 and 15 after isotropic
refinement. All non-hydrogen atoms of organometallic
molecules were further refined with anisotropic thermal
parameters. The hydrogen atoms were placed in calcu-
lated positions and included in the final cycles of refine-
ments in a riding model.
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4. Supplementary material
Tables of atomic coordinates, anisotropic thermal
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.