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Programs used for centering reflections, autoindexing, refinement of cell parameters and axial photographs are those described in: Sparks, R. A. Nicolet P3/R3 Operations Manual; Syntex Analytical Instruments: Cupertino, CA, 1978.
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Programs used for centering reflections, autoindexing, refinement of cell parameters and axial photographs are those described in: Sparks, R. A. Nicolet P3/R3 Operations Manual; Syntex Analytical Instruments: Cupertino, CA, 1978.
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45
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77949389642
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SHELXTL uses scattering factors and anomalous dispersion terms taken from: International Tables of X-Ray Crystallography; Kynoch: Birmingham, England, 1968; IV.
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SHELXTL uses scattering factors and anomalous dispersion terms taken from: International Tables of X-Ray Crystallography; Kynoch: Birmingham, England, 1968; Vol. IV.
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47
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77949393668
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The NMR spectra for 1 can be compared with data for the acid and base fragment molecules (Me3Si)3Al-OEt21H NMR (C6D6, <5 0.24 (27 H, SiMe, 0.73 (6H, OCH 2CH3, 3.34(4H, OCH2CH3, 13C{1H) NMR(C6D6, δ2.84 (SiMe, 13.19 (OCH2CH3, 69.63 (OCH2CH 3, Me3N3B3Me2(NH 2) 1H NMR (C6D6, δ 0.47 (6 H, B-4, 6 Me, 1.93 (2 H, NH2, 2.56 (6 H, N-1,3 Me, 2.77 (3 H, N-5 Me, 13C{1H) NMR (C6D6, δ -0.10 (B-4,6 Me, 31.75 (N-1,3 Me, 34.53 (N-5 Me, 11B( 1H) NMR (C6D6, δ 26.2 (B-2, 36.3 B-4,6
-
6): δ 26.2 (B-2), 36.3 (B-4,6).
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77949351382
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The descrepandes in CHN analytical data result from incomplete combustion of the samples as noted in analysis reports from commercial sources. This is likely due to formation of ceramic residues. Similar observations were made with analyses of, Me3Si2AlNH2]2. 11a
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