Crystal structure of bis(2,2'-bipyridine-N, N')carbonatocobalt(III) hydrogencarbonate pentahydrate, [Co(C10H8N2)2(CO3)][HCO3] · 5H2O

H.-M. Guo, B.-S. Zhang
2006 Zeitschrift für Kristallographie - New Crystal Structures  
C22H27C0N4O11, monoclinic, C12/cl (no. 15 ), a = 10.9420(7) A ,b= 16.008(1) A, c = 14.458(1) Ä, β = 101.861(4)°, V= 2478.5 A 3 , Ζ = 4, Rgt(F) = 0.038, wR«f(F 2 ) = 0.095, Τ = 273 Κ. Soiree of material Freshly prepared C0CO3 (0.12 g, 1.01 mmol), 2,2'-bipyridine (0.07 g, 0.45 mmol), 2-iodobenzoic acid (0.20 g, 0.81 mmol), 12 nL CH3OH/H2O (1:2, v/v) were mixed and stirred for ca. 3 h. Subsequently, the resulting suspension was heated in a 23 ml Teflon-lined stainless steel autoclave to 373 Κ and
more » ... clave to 373 Κ and kept at this tem-perature for 7 days. After the autoclave was cooled to room temperature, the solid was filtered off. The resulting orange filtrate was allowed to stand at room temperature and slow evaporation for a month afforded orange block-shaped crystals. Experimental details Η atoms bound to C atoms were placed on calculated positions with d(C-H) = 0.93 A and refined using the riding rigid-body approximation and t/iso= 1.2i/eq(C). Η atoms at Ο atoms were located in Fourier difference maps and refined with an Ο-Η distance restraint of 0.85 A and ί/ύο(Η) = 1.5ί/«,(0). N(hkl) measm i, N(h&l)umquc'·
doi:10.1524/ncrs.2006.0176 fatcat:7wgsqpkg65azdahj2ovsoihkne