• Korean Journal of Crystallography
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• v.7 no.2
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• pp.105-112
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• 1996

The structure of the tetra-tert-butyl-dipropionyloxy-dihydroxycalis[4]arene (C50H64O6) has been determined by X-ray diffraction methods. The crystal is monoclinic, space group C2/c, unit cell constant a=16.067(2), b=26.391(17), c=10.335(1)Å, β=94.26(1)°, Z=4, V=4370.2(29)Å3, Dc=1.16, Dm=1.2 gcm-3. The intensity data were collected on an Enraf-Nonius CAD-4 Diffractometer with a graphite monochromated Cu-Kα radiation (λ=1.5418Å). The structure was solved by direct methods and refined by least-squares methods. The final R value was 0.07 for 2354 observed reflections. The molecule has the 1, 3-alternate conformation with own two-fold symmetry axis, : two propionyloxy phenyl groups are up and the other two hydroxy phenyl groups are down.

• Analytical Science and Technology
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• v.12 no.5
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• pp.421-427
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• 1999

Two shapes of crystals have been isolated by the interdiffusion of $Co(NCS)_2$ dissolved in methanol with 1,2-bis(2,2'-bipyridyl-6-yl)ethane (bbpe) dissolved in chloroform. The two crystals have been elucidated as $trans-Co^{II}(NCS)_2(bbpe)$ and $trans-Co^{II}(NCS)_2(bbpe){\cdot}2CHCl_3$, by X-ray crystallography, elemental analysis, IR, and thermal analysis. The two molecular structures are very similar except for the absence or presence of chloroform solvate molecules. The bbpe ligand coordinates to the cobalt(II) ion in an open-ended tetradentate mode, resulting in discrete mononuclear cobalt(II) complex. The cobalt atom adopts a typical octahedral arrangement with six nitrogen donating atoms with two NCS groups in trans positions. A significant solid-to-solid phase transition occurs presumably due to the change of conformationally flexible bbpe ligand. The formation of both crystals oeeurs in a successive two-step process, the formation of $trans-Co^{II}(NCS)_2(bbpe)$ and its transformation into $trans-Co^{II}(NCS)_2(bbpe){\cdot}2CHCl_3$. The thermal stability and favorable formation of the solvate crystals may be ascribed to the interaction between S atom of NCS group and Cl of chloroform.

• Journal of the Korean Chemical Society
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• v.47 no.6
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• pp.553-558
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• 2003

The crystal structure of $[n-Bu_4N]_2[Mo_6O_{19}]$(TBAM) (n-Bu4N=tetrabutylammonium) has been determined by X-ray crystallography. It crystallizes in the monoclinic system, space group C2/c, with lattice parameters ${\alpha}$=16.314(5), b=17.288(5), c=17.776(4)${\AA}$ ${\beta}$=101.47(3), and Z=4. In $[Mo_6O{19}]^{2-}$ anion, Mo atoms occupy six vertices of octahedron and each Mo atom is coordinated by six oxygen atoms to adopt distorted octahedral coordination geometry. The average bond distance of Mo-Ot (terminal), Mo-Ob (bridged) and Mo-Oc (central) are 1.680 ${\AA}$, 1.931 ${\AA}$ and 2.325 ${\AA}$ respectively. In $[n-Bu_4N]^+$ cation, the N atom possesses a slightly distorted tetrahedral geometry. There are some potential extensive C-H ${\cdots}$ O hydrogen bonds in the lattice, by which connecte molecules and stabilize the crystal structure. Thermogravimetric analysis suggests that thermal decomposition of the title compound includes two transitions and it loses weight at 356.0 and 803.5 $^{\circ}$, respectively, and the residue presumable be $Mo_2O_2$. Accordingly, the title compound has high thermal stability.

• Bulletin of the Korean Chemical Society
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• v.34 no.10
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• pp.2889-2894
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• 2013

A new complex [$Ni(phen)(C_9H_8Br_2NO_3)_2{\cdot}2CH_3OH{\cdot}2H_2O$] [phen: 1,10-phenanthroline $C_9H_8Br_2NO_3$: 3,5-dibromo-L-tyrosine] was synthesized and characterized by IR, elemental analysis and single crystal X-ray diffraction. X-ray crystallography shows that Ni(II) ion is six-coordinated. The Ni(II) ion coordinates with four nitrogen atoms and two oxygen atoms from three ligands, forming a mononuclear Ni(II) complex. The crystal crystallizes in the Orthorhombic system, space group $P2_12_12$ with a = 12.9546 ${\AA}$, b = 14.9822 ${\AA}$, c = 9.9705 ${\AA}$, V = 1935.2 ${\AA}$, Z = 1, F(000) = 1008, S = 0.969, ${\rho}_{calcd}=1.742g{\cdot}cm^{-3}$, ${\mu}=4.688mm^{-1}$, $R_1$ = 0.0529 and $wR_2$ = 0.0738 for 3424 observed reflections (I > $2{\sigma}(I)$). Theoretical study of the title complex was carried out by density functional theory (DFT) method and the B3LYP method employing the $6-3l+G^*$ basis set. The energy gap between HOMO and LUMO indicates that this complex is prone to interact with DNA. CCDC: 908041.

• Korean Journal of Crystallography
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• v.16 no.1
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• pp.38-42
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• 2005

The crystal structure of Bis(ethylenediamine) cuprate(II)$\cdot$dichromate, $Cu(C_2H_8N_2)_2{\cdot}Cr_2O_7$, has been determined by X-ray crystallography. Crystal data: a=5.682(2), b=8.567(3), c=14.839(3) ${\AA},\;{\alpha}=97.50(2),\;{\beta}=101.06(1),\;{\gamma}=109.38(2)^{\circ}$ Triclinic, P-1 (SG No=2), Z=2, V=653.9(2) ${\AA}^3,\;D_c=2.030gcm^{-3},\;{\mu}=3.273mm^{-1}$. The structure was solved by Patterson method and refined by full matrix least-square methods uslng unit weights. The final R and S values were $R_1=0.0256,\;R_w=0.0708,\;R_{all}=0.0316,\;S=1.151$ for the observed 2291 reflections. The two cupper complex ion has the usual distorted octahedral structure with mean four Cu-N distances of 2.010(3) $\AA$ and the longer mean Cu-O distance of 2.525(2) $\AA$. The Cu-complex and dichromate ions are linked to form infinite chain arranged alternatively along the [111]-direction. The neighboring chains in the (0-11) plane are connected with N1-O5 and N3-O1 hydrogen bonds.

• Korean Journal of Crystallography
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• v.17 no.2
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• pp.41-45
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• 2006

The complex $cis-[Co(13-aneN_4)(N_3)_2]Cl\cdot H_2O$ (1) (13-ane$N_4$ = 1,4,7,10-tetraazacyclotridecane) has been synthesized and structurally characterized by X-ray crystalloaraphy. It crystallizes in the orthorhombic system Pbca, a = 7.8282(4) ${\AA}$, b = 14.3197(7) ${\AA}$, c = 29.9021(15) ${\AA}$, V = 3351.9(3) ${\AA}^3$, Z = 8. The cobalt(III) ion in 1 is coordinated to four nitrogen atoms from the macrocycle and two azide ligands of cis position in a distorted octahedral environment, which forms the 1D polymer through hydrogen bonding contacts involving the cation, chloride anion and solvent water molecules.

• Bulletin of the Korean Chemical Society
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• v.27 no.7
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• pp.1005-1008
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• 2006

The reaction of $AgClO_{4}$ with acyclic potential tridentate N,N,N',N',N''-pentamethyldiethylenetriamine (pmdeta) has given colorless crystals suitable for X-ray crystallography. The crystal structure ($P2_{1}$/n, a = 14.413(1) $\AA$, b = 25.270(2) $\AA$, c = 16.130(1) $\AA$, b = $103.012(1){^{\circ}}$, V = 5723.7(8) A$\AA^{3}$, Z = 4, R = 0.0349) has been solved and refined. Three silver(I) ions connect four pmdeta ligands to produce discrete complex of $[Ag_3(pmdeta)_4](ClO_4)_3$. A pmdeta ligand is bridged to three silver(I) ions, and three other pmdeta ligands are chelated to each silver(I) center in a tridentate mode. Thus, the product is a rare tri-nuclear silver(I) complex with two different chemical environments. $^{13}C$ NMR and $MAS\;^{13}$C NMR indicate that the tri-nuclear silver(I) complex is not rigid in solution. The contact angles and thermal analyses of the complex are measured and discussed.

• BMB Reports
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• v.49 no.12
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• pp.681-686
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• 2016

Fructose 1,6-bisphosphate aldolase (FBA) is important for both glycolysis and gluconeogenesis in life. Class II (zinc dependent) FBA is an attractive target for the development of antibiotics against protozoa, bacteria, and fungi, and is also widely used to produce various high-value stereoisomers in the chemical and pharmaceutical industry. In this study, the crystal structures of class II Escherichia coli FBA (EcFBA) were determined from four different crystals, with resolutions between $1.8{\AA}$ and $2.0{\AA}$. Native EcFBA structures showed two separate sites of Zn1 (interior position) and Zn2 (active site surface position) for $Zn^{2+}$ ion. Citrate and TRIS bound EcFBA structures showed $Zn^{2+}$ position exclusively at Zn2. Crystallographic snapshots of EcFBA structures with and without ligand binding proposed the rationale of metal shift at the active site, which might be a hidden mechanism to keep the trace metal cofactor $Zn^{2+}$ within EcFBA without losing it.

• Bulletin of the Korean Chemical Society
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• v.27 no.5
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• pp.687-693
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• 2006

Chromium(III) complexes, cis-[Cr([14]-decane)$(HOC _6H _4COO) _2$]$ClO _4$ I and cis-[Cr([14]-decane)(OH) $(OC _6H _4NO _2)$]$ClO _4{\cdot}H _2O$ II ([14]-decane = rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-teraazacyclotetradecane) are synthesized and structurally characterized by a combination of elemental analysis, conductivity, IR and VIS spectroscopy, and X-ray crystallography. The complexes crystallizes in the monoclinic space groups, $C2 _1$/a in I and $P2 _1$/n in II. Analysis of the crystal structure of complex I reveals that central chromium(III) ion has a distorted octahedral coordination environment and two hydrogensalicylato ligands are unidentate to the chromium(III) ion via the carboxyl groups in the cis-position. For monomeric complex I the hydrogensalicylato coordination geometry is as follows: Cr-O(average) = 1.984(3) $\AA$;Cr-N range = 2.105(3)-2.141(4) $\AA$;C(24)-O(4) = 1.286(5) $\AA$;N(2)-Cr-N(4) (equatorial position) = 96.97(15)${^{\circ}}$; N(1)-Cr-N(3) (axial position) = 168.27(15)${^{\circ}}$; O(1)-Cr-O(4) = 85.70(13)${^{\circ}}$. The crystal structure of II has indicated that chromium(III) ion is six-coordinated by four secondary amines of the macrocycle, hydroxide anion and nitrophenolate anion.

• Molecules and Cells
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• v.41 no.4
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• pp.301-310
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• 2018

LysR-type transcriptional regulators (LTTRs) contain an N-terminal DNA binding domain (DBD) and a C-terminal regulatory domain (RD). Typically, LTTRs function as homotetramers. VV2_1132 was identified in Vibrio vulnificus as an LTTR that is a homologue of HypT (also known as YjiE or QseD) in Escherichia coli. In this study, we determined the crystal structure of full-length VV2_1132 at a resolution of $2.2{\AA}$, thereby revealing a novel combination of the domains in the tetrameric assembly. Only one DBD dimer in the tetramer can bind to DNA, because the DNA binding motifs of the other DBD dimer are completely buried in the tetrameric assembly. Structural and functional analyses of VV2_1132 suggest that it might not perform the same role as E. coli HypT, indicating that further study is required to elucidate the function of this gene in V. vulnificus. The unique structure of VV2_1132 extends our knowledge of LTTR function and mechanisms of action.