Crystal structure analyses: a) [UO 2 {(calix[4]arene À H)(dmf)}- (calix[4]arene À H)(dmf) 2.7 (dmso) 0.3 ] ´ [calix[4]arene(dmf)] ´1/2 DMF: C 100.2 H 108.2 N 5.2 O 19.5 S 0.3 U, M r 1945.0; monoclinic, space group C2/c, a 29.970(3), b 18.180(3), c 33.802(3) , b 97.073(2)8, V 18277 3 ; Z 4; 1 calcd 1.413 g cm À3 ; crystal dimensions: 0.22 Â 0.14 Â 0.10 mm; m Mo 18.6 cm À1 ; 89 915 measured reflections (Bruker AXS CCD diffractometer, T % 153 K, monochromatic Mo Ka radiation, l 0.71073 ), multiscan absorption correction (min./max. transmission 0.60/0.84; 2q max 588) gave 23 359 unique reflections (R int 0.037), of which 13 875 were considered observed (F b 4s(F)), refinement on j F j (anisotropic thermal parameter refinement for non-H atoms, (x, y, z, U iso ) H included constrained at estimates, phenolic hydrogen atoms located in difference maps), R 0.043, R w 0.043 (statistical weights). [15d] b) [HNEt 3 ] 2 [UO 2 {(p-tBu-tetrathiacalix[4]arene À 4 H)(dmf)}] ´2 DMF: C 61 H 97 N 5 O 9 S 4 U, M r 1410.8; monoclinic, space group P2 1 /n, a 12.309(2), b 21.524(3), c 25.719(3) , b 103.828(2)8, V 6616 3 ; Z 4; 1 calcd 1.416 g cm À3 ; crystal dimensions: 0.40 Â 0.20 Â 0.20 mm; m Mo 26.4 cm À1 ; min./max. transmission 0.51/0.72; 72 054 measured reflections, of which 16 139 were independent (R int 0.027) and 13 760 observed (F b 4s(F)); R 0.025, R w 0.037. [15d] c) [HNEt 3 ] 2 [UO 2 - {(p-tBu-tetrathiacalix[4]arene À 4 H)(MeCN)}] ´$ 1.7 DMSO:
(isomorphous with the DMSO adduct) C 57.46 H 89.38 N 3 O 7.73 S 5.73 U, M r 1367.7; a 11.6912(7), b 21.612(1), c 25.543(2) , b 101.275(1)8, V 6329 3 ; Z 4; 1 calcd 1.435 g cm À3 ; crystal dimensions: 0.45 Â 0.40 Â 0.15 mm; m Mo 28.0 cm À1 ; min./max. transmission 0.48/0.72; 69 598 measured reflections, of which 15 779 were independent (R int 0.044) and 11 866 observed (F b 4s(F)); R 0.050, R w 0.053. Determination c) is less auspicious than b), since the Et 3 NH ion is disordered, with (concomitant) generally higher ªthermal motionº throughout; the DMF solvate is disordered. [15d] d) The structures were solved using the Xtal3.6.1 software package (Xtal3.6.