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Cristallisation dans le systeme monoclinique, groupe P2 1 /m et affinement jusqu'a R=0,039. Conformation bateau de l'heterocycle

[Cu(C 7 H 9 N) 2 (C 12 H 8 N 2 )(CH 2 O)] (ClO 4 ) 2 cristallise dans le systeme triclinique avec le groupe d'espace P1. Affinement de la structure jusqu'a 0,040. La coordination autour de Cu est pyramidale carree

Na 4 [Ru(SO 3 ) 2 (HSO 3 ) 2 (NH 3 ) 2 ]•6H 2 O cristallise dans le systeme monoclinique avec le groupe d'espace P2 1 /c. Affinement de la structure jusqu'a 0,044. Le complexe anionique centrosymetrique et pseudo-octaedrique

C7HsC12N3S2, Mr=266.17, triclinic, P), a=6-028(1), b=9-985(2), c=10.157 (3) /~, ct= 117.33 (2), fl= 106.73(2), y=90.31(1) °, V= 513-3(4)/~3, Z=2, D x=1.72gcm -3, 2(MoK~t)= 0.71073 A, /1 = 9.85 cm -1, F(000) = 268, T= 293 K, R = 0.032 for 1547 unique observed reflections. The SNCNS portion of the ring is planar within 0-060 (2)/~ and the third N is displaced 0.336 (2) A from this plane on the side opposite the S-bonded C1 atoms. The S-N distances range from 1.581 (1) to 1.615 (2)/~ and the N-C distances are 1.327 (2) and 1.344 (2) ./k. Experimental. Compound prepared by the reaction of chlorine gas with PhCNsS 3 obtained from the reaction of PhC(NSiMe3) with SaNaC1 a. Crystals obtained from a 50:50 mixture of dichloromethane and hexanes. Air-sensitive parallelpiped data crystal 0.20 × 0.50 × 0.46 mm sealed in a glass capillary. Density not measured. Intensities measured with an Enraf-Nonius CAD-4 diffractometer using 09-20 scans of 4 to 16 ° min -~ in 0. Unit cell determined from least-squares analysis of angle data for 20 reflections with 22 < 20 < 40 °. Analytical absorption correction based on crystal shape varied from 0.67 to 1-00. Data collected to sin0/2 of 0-59/~-~, -7

A one‐film method for orienting single crystals using an oscillation film obtained with a Weissenberg camera is described. Highly precise orientation corrections are obtained by using the curvature of the nonzero lines, which is more sensitive to crystal orientation than the zero layer line curvature used in other methods. The equations used for the corrections are derived, rather than empirical, and a general equation for the shapes of the lines caused by a misoriented crystal is given.