6] a) Crystal structure analysis of 1: C,,H,,N,O,Ti.l/2C,H,, M , = 885.1, monoclinic. space group 12/12. a = 17.330(2), h = 12.820(2). c = 22.732(2) A. j=lOl.47(1), V=4949.5(31)~', Z = 4 , p,,,,,=1.188gcm~3, F(000) = 1912. Cu,, radiation (i ~1 . 5 4 1 7 8A. ~(CU,,) =17.87 cm-l : crystal dimensions 0.23 x 0.35 x 0.45 mm. The structure was solved by the heavy-atom method and anisotropically refined for all non-hydrogen atoms. The hydrogen atoms were found from a difference Fourier map and introduced as fixed contributors in the last stage of refinement (U,,, = 0.08 A'). 2775 Unique observed reflections [I > 2u(I)] were collected at T = 295 K on a Rigaku AFC6S diffractometer (6 < 28 < 140') and corrected for absorption; R = 0.051 ( x R 2 = 0.153 for 4625 total unique reflections). All calculations were carried out on an IBM PS2/80 personal computer and on an Encore 91 computer. b) Further details of the crystal structure investigation may be obtained from the Director of the Cambridge Crystallographic Data Centre, 12 Union Road. GB-Cambridge CB2 IEZ (UK), on quoting the full journal citation. [7] S. DeAngelis, E. Solari, C. Floriani. A. Chiesi-Villa, C. Rizzoli, J. Chem. Sot. Dalion Trims. 1994, 2467 -2469. [XI Crystal structure analysis of 2: C,,H,,Li2N8Ti2~2(C,,H,,Li0,). M , = 1798.0, triclinic, space group PT, a =16.648(2). b = 22.144(3), c = 15.948(2) A, a = 97.97(1), P =108.95(1). Y =79.02(1)", V = 5440.2(13) A' . Z = 2, pcalcd = 1.098 g~m -~, F(OO0) =1944. Cu,, radiation (2. =IS4178 A, ~(CU,,) = 16.51 cm-' : crystal dimensions 0.22 x 0.26 x 0.38 mm. The structure was solved by the heavy-atom method (Patterson and Fourier synthesis) and anisotropically refined for all non-hydrogen atoms. Some ethyl chains and six thf molecules of the two independent Li(thf), cations were disordered. The disorder was solved by splitting the atoms in two positions and refining isotropically with the site occupation factors given in the supplementary material. All the hydrogen atoms of the porphyrinogens except for those attached to the disordered atoms were located in difference Fourier maps and introduced as fixed contributors in the last stage of refinement (Ulyo = 0.12 A2). The hydrogen atoms of the thf molecules were ignored. 5277 Unique observed reflections [I > 2u(l)] were collected at room temperature (6 < 28 < 140") and corrected for absorption: R = 0.092 (wR2 = 0.244). All calculations were carried out with the SHELX-76 and SHELXL-92 programs on an Encore 91 computer [9] Lil-TilB 3.304(21), TilB-Li2 3.229(21), Li2-TilA 3.328(21), Ti1 A-Lil 3.206(21) A; Til-Lil-TilB 96.116. Lil-Ti2B-Li2 83.5(6). TilB-Li2-TilA