THE PHENOMENON OF CONGLOMERATE CRYSTALLIZATION .25. SPONTANEOUS RESOLUTION IN COORDINATION-COMPOUNDS - THE CRYSTAL-STRUCTURE OF [CIS-CO(EN)2(NH3)BR]BR2

Br3CoN5C4H19, (1), crystallizes in the monoclinic system, space group C2/c, with cell constants a = 24.579(9), b = 8.665(3), c = 14.409(5) angstrom, and beta = 92.69(3)-degrees; V = 2988.87 angstrom3 and d (MW = 435.875, Z = 8) = 2.097 gm cm-3. Data were collected in the range 4-degrees less-than-or-equal-to 2theta less-than-or-equal-to 50-degrees, for a total of 2823 reflections, of which 1409 were independent and had I greater-than-or-equal-to 3sigma(I). The structure factors were corrected for absorption (mu = 90.882 cm-1) using psi scan curves obtained from reflections near X = 90-degrees. The transmission coefficients ranged from 0.68 to 0.99. The structure was solved by direct methods and refinement converged to final discrepancy indices of R(F) = 0.0601 and R(w)(F) = 0.0663. The cobalt configuration and chelate ring conformations for (1) were found to be the preferred (lel)2-DELTA(deltadelta) and DELTA(lambdalambda). The Co-N distances to the en rings are 1.961(6), 1.960(6), 1.977(6), 1951(6) angstrom, while that to the -NH3 ligand is 1.963(6) angstrom. The C-C distances are 1.52(1) and 1.50(1) angstrom; finally, the Co-Br distance is 2.403(1) angstrom.