=1.56 gcm-'; max. 2 0 = 4 4 (Mo,,, i = 0.70930 A. graphite monochromator, w/20-Scan, 7'= 223 K); 4447 reflections measured. 4180 independent, 3950 observed [Fo 3 u(Eo)], Lorentzian polarization and empirical absorption corrections ( p = 21.4 cm-l, $-scan method, min. transmission 84.1 I O h ) ; direct methods (SHELXSX6). refinement with program package SDP (Enrdf-Nonius), positions of hydrogen atoms calculated according to ideal geometry (C-H distance 0.95 A): R = 0.0285, R, = 0.0395; reflexiparameter ratio 12.5, residual electron density +0.582/-0.910 e k 3 . Further details of the X-ray structure analysis are available on request from the FachinformationsLentriim Karlsruhe, Gesellschaft fur wissenschaftlich-technische Information mbH. D-76344 Eggenstein-Leopoldshafen (FRG), on quoting the depository number CSD-57 130, the names of the authors. and the journal citation.
FcI9.67 contains bands and chains as substructures, which are linked together by up to sixfold‐coordinated iodine atoms to form a novel three‐dimensional network (see below). The ferrocenium ions Fc+ are intercalated in the cavities. These cations stabilize crystalline solids that contain not only known polyiodide ions but also FcI9.67, which can be described as the triply charged nonacosaiodide Fc3I29 and is the most iodine‐rich polyiodide known to date.
8 ppm) compared to C-4 and C-6 as C-7 is deshielded due to its allylic An X-ray structure analysis of (6b) is in progress.The silver complex ( 6 4 reacts with dienes at room temperature to give the corresponding cycloadducts (3) and (10)- (33). Gas chromatographically, the sole impurity found in all cases was the cis-olefin (7) (2-13%). The following diastereomeric ratios a / b were determined by capillary gas chromatography: (3): 4.4:l; (11): 2.0:l; (12): 2.4:l. The ratio a/ b = 4.4 : 1 of the furan adducts (3) differs drastically from that found in the trapping of free trans-olefin (2) (a/b = 0.95 : l)l3l and suggests that part of the cycloaddition takes place in the ligand sphere of the silver ion. The insolubility of (64 in solvents suitable for anthracene hinders cycloaddition of the complex. However, (13) (m.p. 122°C) was obtained when ammonia was passed into the stirred suspension of (6a) in the saturated anthracene solution in dichloromethane. Reaction of (6a) with trans-cyclooctene (5) gave tris(trans-cy-c1ooctene)silver perchlorate (4), m. p. 197 "C (decomp.). Preliminary experiments show that cis,trans-cycloheptadienes can also be stabilized as silver complexes.
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