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Title: Azine Bridged Silver Coordination Polymers: Powder X-ray Diffraction Route to Crystal Structure Determination of Silver Benzotriazole

Authors:
; ; ; ; ; ; ;
Publication Date:
Research Org.:
Brookhaven National Laboratory (BNL) National Synchrotron Light Source
Sponsoring Org.:
Doe - Office Of Science
OSTI Identifier:
914004
Report Number(s):
BNL-78572-2007-JA
DOE Contract Number:
DE-AC02-98CH10886
Resource Type:
Journal Article
Resource Relation:
Journal Name: J. Solid State Chem.; Journal Volume: 179; Journal Issue: 4
Country of Publication:
United States
Language:
English
Subject:
national synchrotron light source

Citation Formats

Rajeswaran,M., Blanton, T., Giesen, D., Whitcomb, D., Zumbulyadis, N., Antalek, B., Neumann, M., and Misture, S.. Azine Bridged Silver Coordination Polymers: Powder X-ray Diffraction Route to Crystal Structure Determination of Silver Benzotriazole. United States: N. p., 2006. Web. doi:10.1016/j.jssc.2006.01.022.
Rajeswaran,M., Blanton, T., Giesen, D., Whitcomb, D., Zumbulyadis, N., Antalek, B., Neumann, M., & Misture, S.. Azine Bridged Silver Coordination Polymers: Powder X-ray Diffraction Route to Crystal Structure Determination of Silver Benzotriazole. United States. doi:10.1016/j.jssc.2006.01.022.
Rajeswaran,M., Blanton, T., Giesen, D., Whitcomb, D., Zumbulyadis, N., Antalek, B., Neumann, M., and Misture, S.. Sun . "Azine Bridged Silver Coordination Polymers: Powder X-ray Diffraction Route to Crystal Structure Determination of Silver Benzotriazole". United States. doi:10.1016/j.jssc.2006.01.022.
@article{osti_914004,
title = {Azine Bridged Silver Coordination Polymers: Powder X-ray Diffraction Route to Crystal Structure Determination of Silver Benzotriazole},
author = {Rajeswaran,M. and Blanton, T. and Giesen, D. and Whitcomb, D. and Zumbulyadis, N. and Antalek, B. and Neumann, M. and Misture, S.},
abstractNote = {},
doi = {10.1016/j.jssc.2006.01.022},
journal = {J. Solid State Chem.},
number = 4,
volume = 179,
place = {United States},
year = {Sun Jan 01 00:00:00 EST 2006},
month = {Sun Jan 01 00:00:00 EST 2006}
}
  • In continuation of our interest in solid-state structures of silver complexes of photographic importance, the structure for silver benzotriazole (AgBZT), has now been obtained. The preferred method for solving crystal structures is via single-crystal X-ray diffraction (XRD). However, for some materials, growing single crystals of appropriate size and quality is often difficult or even impossible. AgBZT is an example of such a silver complex with poor solubility. The usual routes to preparing single crystals using recrystallization from a cooperating solvent resulted in polycrystalline powder samples. We propose a crystal structure for AgBZT, solved from synchrotron X-ray powder diffraction data, usingmore » a direct-space Monte Carlo simulated annealing approach. AgBZT crystals are monoclinic (P2{sub 1} /c), with unit cell dimensions, a=14.8052(3) A, b=3.7498(4) A, c=12.3495(12) A, and {beta}=114.200(6){sup o}. The AgBZT complex is constructed from all three of the Benzotriazole (BZT) nitrogens bonding to a separate silver atom. As a consequence of this bonding mode, the structure is a highly cross-linked, coordination polymer.« less
  • The synthesis of two dimensional (2D) coordination polymer [Pb{sub 2}(µ-I){sub 2}(µ-dpp-N,N,N,N)(µ-dpp-N,N)I{sub 2}]{sub n} (dpp=2,3-bis(2-pyridyl)pyrazine) is reported. As determined by X-ray diffraction of a twinned crystal, the dpp ligand simultaneously adopts a bis–bidentate and bis–monodentate coordination mode in the crystal structure of compound. The electronic band structure along with density of states (DOS) calculated by the DFT method indicates that the compound is an indirect band gap semiconductor. According to the DFT calculations, the observed emission of the compound at 600 nm in solid phase could be attributed to arise from an excited LLCT state (dpp-π{sup ⁎} [C-2p and N-2p states,more » CBs] to I-6p state [VBs]). The linear optical properties of the compound are also calculated by DFT method. The structure of the compound in solution phase is discussed based on the measured {sup 1}H NMR and fluorescence spectra in DMSO. TGA studies indicate that the compound is thermally stable up to 210 °C. - Graphical abstract: The synthesis, crystal structure and emission spectra of [Pb{sub 2}(µ-I){sub 2}(µ-dpp-N,N,N,N)(µ-dpp-N,N)I{sub 2}]{sub n} is presented. The electronic band structure and linear optical properties of the compound are calculated by the DFT method. - Highlights: • Two dimensional [Pb{sub 2}(µ-I){sub 2}(µ-dpp-N,N,N,N)(µ-dpp-N,N)I{sub 2}]{sub n} has been prepared. • The structure of the compound is determined by XRD of a twinned crystal. • DFT calculations indicate that the compound is an indirect band gap semiconductor. • As shown by DFT calculations, the emission band of the compound is LLCT. • Solution phase structure of compound is explored by {sup 1}H NMR and emission spectra.« less
  • The alkaline earth dicyanamides Mg[N(CN){sub 2}]{sub 2}, Ca[N(CN){sub 2}]{sub 2}, Sr[N(CN){sub 2}]{sub 2}, and Ba[N(CN){sub 2}]{sub 2} were synthesized by ion exchange using Na[N(CN){sub 2}] and the respective nitrates or bromides as starting materials. The crystal structures were determined from X-ray powder diffractometry: Mg[N(CN){sub 2}]{sub 2}, Pnnm, Z=2, a=617.14(3), b=716.97(3), and c=740.35(5) pm; Ca[N(CN){sub 2}]{sub 2} and Sr[N(CN){sub 2}]{sub 2}, C2/c, Z=4; Ca[N(CN){sub 2}]{sub 2}, a=1244.55(3), b=607.97(1), and c=789.81(1) pm, {beta}=98.864(2){degree}; Sr[N(CN){sub 2}]{sub 2}, a=1279.63(2), b=624.756(8), and c=817.56(1) pm, {beta}=99.787(1){degree}; Ba[N(CN){sub 2}]{sub 2}, Pnma, Z=4, a=1368.68(7), b=429.07(7), and c=1226.26(2) pm. The dicyanamides consist of the respective alkaline earth cations andmore » bent planar [N(CN){sub 2}]{sup -} ions. The structural features were correlated with vibrational spectroscopic data. The thermal behavior was studied by thermoanalytical experiments.« less
  • No abstract prepared.