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See the Supporting Information for details
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See the Supporting Information for details.
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38349019663
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Crystal data for L1 (C25H20N 2O3, Mr, 198.2, colorless crystal, crystal dimensions 0.40 x 0.40 x 0.25 mm3, orthorhombic, space group Pbcn (no. 60, Z, 8, ρcalcd, 1.39 g cm -3, F(000, 831.9, 2θmax, 55.8° were a, 7.1974(5, b, 6.4495(5, c, 40.935(3) Å, and V, 1900.16(2) Å3. The intensity data were collected on a Bruker SMART APEX CCD diffractometer (MoKα radiation, λ, 0.71073 Å) at 103 K. A total of 10 678 reflections were collected of which 2243 reflections were independent Rint, 0.0254, The crystal structure was solved by direct methods using the SHELXS-97 program[18] and refined by successive differential Fourier syntheses and full-matrix least-squares procedures using the SHELXL-97 program, 19] Anis
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-3..
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38349073444
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Crystallization of 1 from DMF or DMSO solutions gave only crystals of 2. We have reasoned that during crystallization, 1 was gradually converted into the thermodynamically more stable 2. See text for details
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Crystallization of 1 from DMF or DMSO solutions gave only crystals of 2. We have reasoned that during crystallization, 1 was gradually converted into the thermodynamically more stable 2. See text for details.
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4243992753
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A. K. Rappe, K. S. Colwell, C. J. Casewit, Inorg. Chem. 1993, 32, 3438-3450.
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e signal of 1 was not observed at the lowest possible temperature for the solvent.
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e signal of 1 was not observed at the lowest possible temperature for the solvent.
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38349019662
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2ν symmetry with a planar conformation in the complexes and a box shape for 1 was pointed out by one of the referees. PM6 calculations suggested that benzophenone with a planar conformation has a higher heat of formation than the other conformations because of the steric repulsion between hydrogen atoms of neighboring phenyl rings.
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2ν symmetry with a planar conformation in the complexes and a box shape for 1 was pointed out by one of the referees. PM6 calculations suggested that benzophenone with a planar conformation has a higher heat of formation than the other conformations because of the steric repulsion between hydrogen atoms of neighboring phenyl rings.
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38349052154
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Crystal data for 2 (Pd(C25H20N 2O3)2(DMF, Mr, 972.4, colorless crystal, crystal dimensions 0.11 x 0.10 x 0.04 mm3, tetragonal, space group P4/n (no. 85, Z, 8, ρcalcd, 0.90 g cm-3, F(000, 4015.4, 2θmax, 54.4° were a, 20.8580(8, b, 20.8580(8, c, 33.150(2) Å, and V, 14 421.1(1) Å3. The intensity data were collected on a Rigaku Saturn-724 CCD diffractometer (MoKα radiation, λ, 0.71073 Å) at 103 K. A total of 145 124 reflections were collected of which 16 491 reflections were independent Rint, 0.0791, The crystal structure was solved by direct methods using the SIR-2004 program[20] and refined by successive differential Fourier syntheses and full-matrix least-squares procedures using the SHELXL-97 pro
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1) and 652007 contain the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/ data_request/cif.
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[17]
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[17]
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0004048804
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University of Glasgow, Glasgow Scotland
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A. L. Spek, PLATON, University of Glasgow, Glasgow (Scotland), 1998.
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(1998)
PLATON
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Spek, A.L.1
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37
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0004150157
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Program for X-ray Crystal Structure Solution, University of Göttingen, Göttingen Germany
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G. M. Sheldrick, SHELXS-97: Program for X-ray Crystal Structure Solution, University of Göttingen, Göttingen (Germany), 1997.
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(1997)
SHELXS-97
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Sheldrick, G.M.1
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38
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0004150157
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Program for X-ray Crystal Structure Refinement, University of Göttingen, Göttingen Germany
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G. M. Sheldrick, SHELXL-97: Program for X-ray Crystal Structure Refinement, University of Göttingen, Göttingen (Germany), 1997.
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(1997)
SHELXL-97
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Sheldrick, G.M.1
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39
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84860013705
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A program for automatic solution and refinement of crystal structures
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M. C. Burla, R. Caliandro, M. Camalli, B, Carrozzini, G. L. Cascararo, L. De Caro, C. Giacovazzo, G. Polidori, R. Spagna, SIR-2004: A program for automatic solution and refinement of crystal structures.
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SIR-2004
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Burla, M.C.1
Caliandro, R.2
Camalli, M.3
Carrozzini, B.4
Cascararo, G.L.5
De Caro, L.6
Giacovazzo, C.7
Polidori, G.8
Spagna, R.9
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