Inorganic Chemistry
ARTICLE
pellet): 2922, 2427, 2361, 2342, 1637, 1587, 1571, 1454, 1421, 1384,
1196, 1083, 1046, 813, 752, 708, 678 cmꢀ1. Anal. Calcd for [C19H23-
CuN3O6S4]: C, 39.27; H, 3.99. Found: C, 39.55; H, 3.92%.
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S. S. Inorg. Chem. 2010, 49, 7510. (k) Lee, S. Y.; Lee, S. S. CrystEngComm
2010, 12, 3471. (l) Kim, H. J.; Sultana, K. F.; Lee, J. Y.; Lee, S. S.
CrystEngComm 2010, 12, 1494. (m) Park, S.; Lee, S. Y.; Lee, S. S. Inorg.
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Preparation of 3, {[Cu(L)(NO3)Hg2I5] CH2Cl2}n. Mercury(II)
3
iodide (11.5 mg, 0.025 mmol) and copper(II) nitrate trihydrate (6.14
mg, 0.025 mmol) in methanol (4 mL) were added to a solution of L
(10.0 mg, 0.025 mmol) in dichloromethane (2 mL). Slow evaporation of
the solution afforded green crystalline 3 that proved suitable for X-ray
analysis. Mp: 195ꢀ197 ꢀC (decomp). IR (KBr pellet): 2910, 2361,
2341, 1603, 1491, 1464, 1384, 1283, 1025, 999, 731, 708, 697, 669,
652 cmꢀ1. Anal. Calcd for [C19H23CuHg2I5N2O3S4]: C, 14.68; H, 1.49.
Found: C, 14.21; H, 1.45%.
X-ray Crystallographic Analysis. All data were collected on a
Bruker SMART APEX II ULTRA diffractometer equipped with graphite
monochromated Mo KR radiation (λ = 0.710 73 Å) generated by a
rotating anode. The cell parameters for the compounds were obtained
from a least-squares refinement of the spot (from 36 collected frames).
Data collection, data reduction, and semiempirical absorption correction
were carried out using the software package APEX2.11 All of the
calculations for the structure determination were carried out using the
SHELXTL package.12 In all cases, all nonhydrogen atoms were refined
anisotropically, and all hydrogen atoms except coordinated water
molecules were placed in idealized positions and refined isotropically
in a riding manner along with the their respective parent atoms. In the
cases of coordinated water molecules, the initial positions of the
hydrogen atoms were obtained from difference electron density maps
and refined with riding constraints. Relevant crystal data collection and
refinement data for the crystal structures of L, 1, 2, and 3 are summarized
in Tables 1, 2, 3, and 4.
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(11) APEX2 Version 2009.1ꢀ0 Data Collection and Processing Software;
Bruker AXS Inc.: Madison, WI, 2008.
(12) SHELXTL-PC Version 6.22 Program for Solution and Refinement
of Crystal Structures; Bruker AXS Inc.: Madison, WI, 2001.
’ ASSOCIATED CONTENT
S
Supporting Information. X-ray data in CIF format, and
b
crystal packing and NMR spectrum of L as noted in the text. This
acs.org.
’ AUTHOR INFORMATION
Corresponding Author
*E-mail: sslee@gnu.ac.kr.
’ ACKNOWLEDGMENT
This work was supported by WCU project (R32-20003) and
NRF (2010-0022499), S. Korea.
’ REFERENCES
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dx.doi.org/10.1021/ic200684x |Inorg. Chem. 2011, 50, 5803–5807