4208
K. Ding et al. / Journal of Organometallic Chemistry 694 (2009) 4204–4208
Table 5
Crystallographic parameters.
intensity statistics. A direct-methods solution was calculated
which provided most non-hydrogen atoms from the E-map. Full-
matrix least squares/difference Fourier cycles were performed
which located the remaining non-hydrogen atoms. All non-hydro-
gen atoms were refined with anisotropic displacement parameters.
All hydrogen atoms were placed in ideal positions and refined as
riding atoms with relative isotropic displacement parameters. In
the structure of LtBuFeCl(NMP), reflection contributions from highly
disordred solvent were removed using the SQUEEZE function of
PLATON [40], which determined there to be 154 electrons in
683 Å3 removed per unit cell. In LtBuFeCl(NMP), the NMP ligand
was modeled in two orientations, with a ratio of 74:26, and one
isopropyl group of the diketiminate ligand was also disordered
(67:33).
Fe3Cl6NMP8
LtBuFeCl(NMP)ꢂsolvent
C40H62ClFeN3O
692.23
100.0(1)
Monoclinic
P21/n
Empirical formula
Formula weight
T (K)
Crystal system
Space group
Unit cell dimensions
a (Å)
C40H72Cl6Fe3N8O8
1173.31
100.0(1)
Triclinic
ꢀ
P1
8.9811(7)
10.1907(8)
15.0038(12)
84.133(1)
75.260(1)
85.025(1)
1318.42(18)
1
12.5668(15)
9.9966(12)
34.933(4)
90
96.090(2)
90
4363.7(9)
4
1.054
b (Å)
c (Å)
a
(°)
b (°)
(°)
c
V (Å)
Z
DCalc (g/cm3)
1.478
1.173
612
Absorption coefficient (mmꢀ1
F(000)
)
0.436
1496
Appendix A. Supplementary data
Crystal color, morphology
Crystal size (mm)
h range for data collection (°)
Reflections collected
Independent reflections
Observed reflections
Pale purple, block
0.23 ꢃ 0.20 ꢃ 0.15
2.01–32.03
23 235
9045
7318
Yellow-orange, block
0.24 ꢃ 0.16 ꢃ 0.16
1.79–31.51
71 375
14 522
9529
Supplementary data associated with this article can be found, in
References
Completeness to theta = 32.03° 98.6%
99.7%
Maximum and minimum
transmission
Data/restraints/parameters
Goodness-of-fit on F2
0.8437 and 0.7742 0.9335 and 0.9026
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[36]. The data collection was carried out using Mo K
a radiation
(graphite monochromator) with a frame time of 25 (Fe3Cl6NMP8)
or 45 (LtBuFeCl(NMP)) seconds and a detector distance of 5 cm. A
randomly oriented region of reciprocal space was surveyed: four
major sections of frames were collected with 0.50° steps in
four different settings and
x at
u
a
detector position of ꢀ33°
(Fe3Cl6NMP8) or 38° (LtBuFeCl(NMP)) in 2h. The intensity data were
corrected for absorption [37]. Final cell constants were calculated
from the xyz centroids of strong reflections from the actual data
collection after integration [38]. See Table 5 for additional crystal
and refinement information.
The structure was solved and refined using SHELXL-97 [39]. The
space group was determined based on systematic absences and