Materials and Measurements.
All chemicals used in the synthesis were of reagent grade and used without further purification.
pmide) was prepared according to literature procedures.
UV/Vis absorption spectra were recorded with a SCINCO S-2100 spectrophotometer. Infrared spectra were recorded with a Thermo Fisher Scientific IR200 spectrophotometer (± 1 cm
) using KBr disk. Elemental analyses were carried out using a Fissons/Carlo Erba EA1108 instrument. X-ray powder diffraction (XRPD) patterns were measured on a Bruker AXS D2 Phaser X-ray Diffractometer with increments of degree and time step of 0.02° and 0.2 sec/step in 2𝛳. Luminescence spectra were obtained with a SINCO FS-2 fluorescence spectrometer.
Preparation of 1.
To an MeCN solution (2 mL) of H
pmide (100 mg, 0.51 mmol) was added an MeCN/MeOH (v/v, 2:1) mixture solution (3 mL) of Ni(NO
O (74 mg, 0.25 mmol), and the color became light violet, and the solution was stirred for 30 min at room temperature. After filtrating, pink crystals were obtained by slow diffusion of diethyl ether into the mixture solution of
, collected by filtration, and washed with acetonitrile and dried in air. Yield: 129 mg (88%). FT-IR (KBr, cm
): 3392, 3085, 2975, 1609, 1384, 1068, 1027, 769. UV/Vis (diffuse reflectance spectrum):λ
= 264, 308 (sh), 544, 917 nm. Anal. calcd for C
: C, 41.76; H, 5.61; N, 14.61. Found: C, 41.60; H, 5.64; N, 14.37.
Preparation of 2.
This complex was obtained as blue crystals in a manner similar to the synthesis of
except that NiCl
O (61 mg, 0.25 mmol) instead of Ni(NO
O was used. Yield: 122 mg (91%). FT-IR (KBr, cm
): 3357, 3046, 2968, 1609, 1433, 1066, 1028, 780. UV/Vis (diffuse reflectance spectrum):λ
= 264, 304 (sh), 360 (sh), 579, 796 (sh, forbidden), 989 nm. Anal. calcd for C
: C, 46.01; H, 6.18; N,10.73. Found: C, 45.86; H, 6.24; N, 10.79.
Crystal Structure Determination.
Single crystals of
were coated with paratone-
oil and the diffraction data measured at 100(2) K with synchrotron radiation (λ = 0.70000 Å) on an ADSC Quantum-210 detector at 2D SMC with a silicon (111) double crystal monochromator (DCM) at the Pohang Accelerator Laboratory, Korea. The ADSC Q210 ADX program
was used for data collection (detector distance is 63 mm, omega scan; Δω= 1°, exposure time is 1 sec per frame) and HKL3000sm (Ver. 703r)
was used for cell refinement, reduction and absorption correction. The crystal structures of
were solved by direct methods,
and refined by full-matrix least-squares refinement using the SHELXL-97 computer program.
The positions of all nonhydrogen atoms were refined with anisotropic displacement factors. All hydrogen atoms were placed using a riding model, and their positions were constrained relative to their parent atoms using the appropriate HFIX command in SHELXL-97, except the hydrogen atoms of coordinated hydroxyl groups. The crystallographic data and the result of refinements of
are summarized in
Summary of the Crystallographic Data for1and2
aR1 = ∑||Fo| − |Fc||/∑ |Fo|. bwR2 = [∑w(Fo2 −Fc2)2/∑w(Fo2)2]1/2.
This work was supported under the framework of international cooperation program managed by the National Research Foundation of Korea (NRF- 2012K2A2A4012500). X-ray crystallography at PLS-II 2DSMC beamline was supported in part by MEST and POSTECH.Supporting Information.Powder and simulated XRPD patterns and extended 2-D structures of1and2. Crystallographic data (excluding structure factors) for the structures reported in this paper have been deposited with the Cambridge Crystallographic Data Centre as supplementary publication nos. CCDC-955898 (for1) and CCDC-955899 (for2). Copies of the data can be obtained free of charge on application to CCDC, 12 Union Road, Cambridge CB2 1EZ, UK [Fax (internat.) +44-1223/336-033; E-mail: email@example.com].
Huheey J. E.
Keiter E. A.
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Inorganic Chemistry, Chap. 12
Infrared and Raman Spectra of Inorganic and Coordination Compounds, Part B
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DOI : 10.1021/ic2009368
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Hitchman M. A.
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Poway, CA, USA
in Methods in Enzymology, Carter, C. W., Jr., Sweet, R. M., Eds., vol. 276, part A
Sheldrick G. M.
Acta Crystallogr., Sect. A
Sheldrick G. M.
University of Göttingen