metal-organic compounds
Table 4
Selected bond lengths (A) for (III).
molecules could be determined; thus, in (I), a full hydration water
molecule was treated as split into three partially occupied sites, and
was re®ned with an overall isotropic displacement parameter and
occupations restrained to sum to unity, and in (III), one of the three
methanol solvent molecules was treated as split over two sites, re®ned
with occupation factors summing to unity. In addition, a PLATON
(Spek, 2003) run detected in this latter structure (void) solvent-
Ê
Cu1ÐO1
Cu2ÐO1
Cu3ÐO1
Cu4ÐO1
Cu1ÐCu2
1.913 (3)
1.907 (3)
1.916 (3)
1.914 (3)
3.1144 (9)
Cu1ÐCu3
Cu1ÐCu4
Cu2ÐCu3
Cu2ÐCu4
Cu3ÐCu4
3.1375 (9)
3.1354 (9)
3.1146 (9)
3.0945 (9)
3.1436 (9)
3
Ê
accessible regions of 35 A , in which the electron density was hardly
distinguishable from background. A PLATON SQUEEZE re®ne-
ment, however, did not signi®cantly improve the re®nement. The
rather high R indices obtained are probably the result of poor data
quality. However, the large number of parameters might also have
played a non-negligible role [see Krebs (2000) for a detailed analysis].
For all compounds, data collection: SMART (Bruker, 2001); cell
re®nement: SAINT (Bruker, 2000); data reduction: SAINT;
program(s) used to solve structure: SHELXS97 (Sheldrick, 1997);
program(s) used to re®ne structure: SHELXL97 (Sheldrick, 1997);
molecular graphics: XP in SHELXTL (Bruker, 2000); software used
to prepare material for publication: SHELXL97.
Table 5
Hydrogen-bond geometry (A, ) for (III).
ꢁ
Ê
DÐHÁ Á ÁA
DÐH
HÁ Á ÁA
DÁ Á ÁA
DÐHÁ Á ÁA
N21ÐH21Á Á ÁCl3i
N22ÐH22Á Á ÁCl5ii
N23ÐH23Á Á ÁO1A
N23ÐH23Á Á ÁO2A
N24ÐH24Á Á ÁO1B
O1BÐH1BÁ Á ÁO1Ciii
O1CÐH1CÁ Á ÁCl4iv
O1AÐH1AÁ Á ÁCl6v
O2AÐH2AÁ Á ÁCl2vi
0.86
0.86
0.86
0.86
0.86
0.82
0.82
0.82
0.82
2.36
2.49
1.97
2.15
1.87
2.19
2.56
2.47
2.74
3.220 (5)
3.304 (5)
2.813 (10)
2.935 (10)
2.727 (7)
2.655 (9)
3.274 (7)
3.223 (9)
3.416 (9)
174
159
167
152
175
116
146
153
141
The authors acknowledge CONICYT±FONDAP (grant No.
11980002) and FONDECYT (grant No. 1020122). PC thanks
CONICYT, for a doctoral scholarship, and the Departamento
de Posgrado y Postitulo, Universidad de Chile (Beca PG/87/02).
1
2
Symmetry codes: (i) x
1
;
y 12; z 12; (ii) x 23; y 21; z 12; (iii) x 2, y,
z 1; (iv) x
;
y 12; z 12; (v) x 1; y 1; z 1; (vi) x 1; y; z.
2
Table 6
Comparison of mean bond distances in the Cu4OCl6 cores (A).
Ê
Supplementary data for this paper are available from the IUCr electronic
archives (Reference: DN3008). Services for accessing these data are
described at the back of the journal.
hCuÐOi
hCuÐCli
Literature*
(I)
(II)
1.909 (17)
1.909 (17)
1.90 (3)
1.90 (2)
1.913 (5)
2.41 (5)
2.41 (5)
2.41 (8)
2.42 (11)
2.42 (4)
(II0)
References
(III)
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Allen, F. H. (2002). Acta Cryst. B58, 380±388.
*Average of 52 structures in the 2005 version of the CSD.
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Inorg. Chem. 38, 5681±5685.
Bertrand, J. A. (1967). Inorg. Chem. 6, 495±498.
Bruker (2000). SAINT (Version 6.02a) and SHELXTL (Version 6.10). Bruker
AXS Inc., Madison, Wisconsin, USA.
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Ê
Ê
positions (NÐH = 0.86 A, aromatic CÐH = 0.93 A and methyl CÐ
Ê
H = 0.96 A) and allowed to ride. Even though located in a rather
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were treated by use of the AFIX 147 instruction in SHELXL97,
subject to orientational restraint. H atoms bound to the disordered
water molecule in (I) were not included in the model. All H atoms
were assigned a Uiso(H) value of xUeq(carrier), with x = 1.2 for
aromatic H atoms, and x = 1.5 for methyl and hydroxy H atoms. In
spite of the heavy atoms present, the crystals used for data collection
were poorly diffracting, and only with measurement times of 20, 20
and 15 s per frame for (I), (II) and (III), respectively, was it possible
to account for an observed/unique ratio of re¯ections of ca 0.5. A
residual effect of this was the uncertainty with which some solvent
È
Gottingen, Germany.
È
Sheldrick, G. M. (2001). SADABS. University of Gottingen, Germany.
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ꢀ
Â
m314 Cortes et al. Three [Cu4(ꢀ2-Cl)6(ꢀ4-O)] complexes
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Cortes, Piedad
