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Lanthanum 3,5-pyridinedicarboxylate, La2[NC5H3(CO2)2]3·3H2O, was prepared in a simple, one-step reaction. The as-synthesized material formed under hydrothermal conditions at 165 °C for 3 days, in which the final reaction mixture had a molar ratio of 308 H2O:1.0 La(NO3)3·6H2O:0.41 LiOH·H2O:0.31 pyridine-3,5-dicarboxylic acid (PDCA, All chemicals were purchased and used as-received. In a typical reaction, 16.0 mL of deionized H2O and 2.5 g of La(NO3)3·5H2O (Fluka, ≥ 99, were added to a Nalgene beaker. To a separate Nalgene beaker, 16.0 mL of deionized H2O, 0.10 g of LiOH·H2O (Alfa Aesar) and 0.30 g of PDCA Aldrich, 95, were added. After ca. 10 min stirring, the latter solution was added dropwise to the former using a plastic pipette and allowed to
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2O (Alfa Aesar) and 0.30 g of PDCA (Aldrich, 95%) were added. After ca. 10 min stirring, the latter solution was added dropwise to the former using a plastic pipette and allowed to stir for another 10 min. The solution was then transferred to a 45 mL capacity Teflon-lined stainless steel autoclave. The autoclave was sealed and heated at 165 °C for 3 days. The crystals were collected by vacuum filtration, rinsed with deionized water and allowed to air-dry overnight. The crystal product weighed ca. 0.288 g (yield: 58.1%). Elemental analysis agrees very well with the structural formula. Analyzed percentages of C, H, and N were 30.84%, 1.77%, and 5.09%, compared with the values of 30.49%, 1.83%, and 5.08% calculated from the molecular formula, respectively.
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A fragment of a colorless block-like crystal of La2[NC5H3(CO2)2]3·3H2O having approximate dimensions of 0.10 × 0.07 × 0.04 mm was mounted on a Kapton loop using Paratone N hydrocarbon oil. All measurements were collected on a Bruker APEX-II [25a] CCD area detector with channel-cut Si-<111> crystal monochromated synchrotron radiation. Crystallographic data were collected at Beamline 11.3.1 at the Advanced Light Source (ALS, Lawrence Berkeley National Laboratory (λ, 0.77490 Å, The data were collected at a temperature of 150(2) K giving μ(Mo-Kα, 4.631 mm-1, R1, 0.0451, wR2, 0.1235 for 5055 data with I>2σ(I) and R1, 0.0487, wR2, 0.1268 for all 5729 data. Frames corresponding to an arbitrary sphere of data were collected using ω-scans of 0.3° counted for a total of 1 second pe
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2 = 0.1268 for all 5729 data. Frames corresponding to an arbitrary sphere of data were collected using ω-scans of 0.3° counted for a total of 1 second per frame. Data were integrated by the program SAINT [25b] to a maximum θ-value of 31.17°. The data were corrected for Lorentz and polarization effects. Data were analyzed for agreement and possible absorption using XPREP [25c]. An empirical absorption correction based on comparison of redundant and equivalent reflections was applied using SADABS [25d]. The structure was solved by direct methods [25e] and expanded using Fourier techniques [25f].
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Program for the Solution of X-ray Crystal Structures
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Bruker Analytical X-ray Systems Inc, Madison, WI
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XS. Program for the Solution of X-ray Crystal Structures. Part of the SHELXTL Crystal Structure Determination Package (1995-99), Bruker Analytical X-ray Systems Inc, Madison, WI
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(1995)
Part of the SHELXTL Crystal Structure Determination Package
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XS1
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Program for the Refinement of X-ray Crystal Structure
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Bruker Analytical X-ray Systems Inc, Madison, WI
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XL. Program for the Refinement of X-ray Crystal Structure. Part of the SHELXTL Crystal Structure Determination Package (1995-99), Bruker Analytical X-ray Systems Inc, Madison, WI
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(1995)
Part of the SHELXTL Crystal Structure Determination Package
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XL1
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