• Biomolecules & Therapeutics
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• v.29 no.5
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• pp.527-535
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• 2021

Sclerostin (SOST), a regulator of bone formation in osteocytes, inhibits the canonical Wnt signaling by interacting with low-density lipoprotein receptor-related protein 5/6 (LRP5/6) to prevent Wnt binding. Loss-of-function mutations of the SOST gene caused massive bone outgrowth and SOST-null mouse exhibited a high bone density phenotype. Therefore, SOST has been suggested as a promising therapeutic target for osteoporosis. A few previous studies with X-ray crystallography identified the binding interfaces between LRP6 and SOST, but there are limitations in these studies as they used truncated SOST protein or SOST peptide. Here, we analyzed the conformational dynamics of SOST-LRP6 E1E2 complex using hydrogen/deuterium exchange mass spectrometry (HDX-MS). We examined the effect of the C-terminal tail of SOST on LRP6 conformation upon complex formation. HDX-MS analysis suggested a new potential binding interface for the C-terminal region of SOST that was missing from the previous crystal structure of the SOST-LRP6 E1E2 complex.

• Analytical Science and Technology
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• v.20 no.4
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• pp.355-360
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• 2007

The title complex, $(C_3H_{12}N_2)[\{Cd(H_2O)(C_6H_5O_7)\}_2]{\cdot}6H_2O$, I, has been prepared and its structure characterized by FT-IR, EDS, elemental analysis, ICP-AES, and X-ray single crystallography. It is triclinic system, $P{\bar{1}}$ space group with a = 10.236(2), b = 11.318(2), c = $13.198(2){\AA}$, ${\alpha}=77.95(1)^{\circ}$, ${\beta}=68.10(1)^{\circ}$, ${\gamma}=78.12(1)^{\circ}$, V = $1373.5(3){\AA}^3$, Z = 2. Complex I has constituted by protonated 1,3-diaminopropane cations, citrate coordinated cadmium(II) anions, and free water molecules. The central cadmium atoms have a capped trigonal prism geometry by seven coordination with six oxygen atoms of three different citrate ligands and one water molecule. Citrate ligands are bridged to three different cadmium atoms. Each cadmium atom is linked by carboxylate and hydroxyl groups of citrate ligand to construct an one-dimensional ladder-type assembly structure. The polymeric crystal structure is stabilized by three-dimensional networks of the intermolecular O-H${\cdots}$O and N-H${\cdots}$O hydrogen-bonding interaction.

• Korean Journal of Crystallography
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• v.16 no.1
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• pp.43-53
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• 2005

The dihydrido P-C-P pincer complex, $IrH_2{C_6H_3-2,6-(CH_2PBu_2^t)_2}$ (1), was successfully prepared from the reaction of the hydrochloride complex, $IrClH (C_6H_3-2,6-(CH_2PBu_2^t)_2}$, and super acid $(LiBEt_3H)$ under 1 atm of hydrogen in pentane solution at room temperature and followed by Heating at $130^{\circ}C$ in vacuo. Jensen recently found that the dihydrido P-C-P pincer complex 1 is a highly active homogeneous catalyst for the transfer dehydrogenation of alkanes with unusual longterm stability at temperatures as high as $200^{\circ}C$. The treatment of dihydrido complex 1 with nitrogen, water, carbon dioxide, and carbon monoxide in presence of tert-butylethylene (the) at room temperature in an appropriate solution gave the dinitrogen complex, $[Ir{C-6H_3-2,6-(CH_2PBu_2^t)_2}]_2({\mu}-N_2)$ (2), the hydrido hydroxyl complex, $IrH(OH){C_6H_3-2,6-(CH_2PBu_2^t)_2}$ (3), the carbon dioxide complex, $Ir({\eta}^2-CO_2) {C_6H_3-2,6-(CH_2PBu_2^t)_2}$ (including the bicarbonate complex, $IrH({\kappa}^2-O_2COH){C_6H_3-2,6-(CH_2PBu_2^t)_2}\;(4))$, and the carbonyl complex, $Ir(CO) {C_6H_3-2,6-(CH_2PBu_2^t)_2}\;(5)$ (including the carboxyl complex, $IrH(C(O)OH) {C_6H_3-2,6-(CH_2PBu_2^t)_2}\;(6))$, in good yield, respectively. These P-C-P iridium complexes were isolated and characterized by $^1H,\;^{13}C,\;^{31}P\; NMR$, and IR spectroscopy. In addition, the complexes (1-6) were characterized by a single crystal X-ray crystallography. These complexes account for these small molecules' inhibition of dehydrogenation of alkanes catalyzed by the dihydrido complex 1.

• Applied Biological Chemistry
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• v.48 no.3
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• pp.189-200
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• 2005

Biological nitrogen fixation is an important process for academic and industrial aspects. This review will briefly compare industrial and biological nitrogen fixation and cover the characteristics of biological nitrogen fixation studied in Azotobacter vinelandii. Various organisms can carry out biological nitrogen fixation and recently the researches on the reaction mechanism were concentrated on the free-living microorganism, A. vinelandii. Nitrogen fixation, which transforms atmospheric $N_2$ into ammonia, is chemically a reduction reaction requiring electron donation. Nitrogenase, the biological nitrgen fixer, accepts electrons from biological electron donors, and transfers them to the active site, FeMo-cofactor, through $Fe_4S_4$ cluster in Fe protein and P-cluster in MoFe protein. The electron transport and the proton transport are very important processes in the nitrogenase catalysis to understand its reaction mechanism, and the interactions between FeMo-cofactor and nitrogen molecule are at the center of biological nitrogen fixation mechanism. Spectroscopic studies including protein X-ray crystallography, EPR and $M{\ddot{o}}ssbauer$, biochemical approaches including substrate and inhibitor interactions as well as site-directed mutation study, and chemical approach to synthesize the FeMo-cofactor model compounds were used for biological nitrogen fixation study. Recent research results from these area were presented, and finally, a new nitrogenase reaction mechanism will be proposed based on the various research results.

• Applied Biological Chemistry
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• v.38 no.4
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• pp.359-363
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• 1995

New ten N-[1-(benzotriazol-1-yl)alkyl]aniline(4) derivatives were synthesized and the crystal structure of 4h was shown by X-ray crystallography and the absolute configuration has been assigned as S form. The molecule crystallizes in the monoclinic system, space group $P2_{1}/n$. And the molecules in the crystal are linked with each other through the hydrogen bond $(N_{11}-H_{11}{\cdots}N3)$ with distance $2.300(11){\AA}$ The fungicidal activity($pI_{50}$) in-vitro against Botrytis cineria (BC), Phytophthora casici (PC) and Sclerotium cepinorum (SC) were determined by the agar dilution method. The structure activity ralationships (SAR) between structure of 4 and the activity were studied using a physicochemical parameters of substituents and multiple regression technique. Among these compounds, only the bromo group substituent(4f) showed higher activity, which depend on the hydrophobic(${\pi}$) of substituents. The relative orders of the activity are SC>BC> and PC, respectively. This implies that the activity is affected by the hydrophobic(${\pi}$) nature of the Z group rather than the X group. Linear free energy relationships(LFER) on the fungicidal activity with substituents has been also discussed.

• Analytical Science and Technology
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• v.18 no.5
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• pp.391-395
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• 2005

The title complex, $[Cd(N_3)_2(2-ethylimidazole)_2]$, I, has been prepared and characterized by X-ray single crystallography. The complex I crystallizes in the monoclinic system, Cc space group with a = 16.200(3), b = 12.926(3), $c=7.007(1){\AA}$, ${\beta}=102.29(3)^{\circ}$, $V=1433.7(5){\AA}^3$, Z = 4, $R_1=0.0239$ and ${\omega}R_2=0.0604$ for 1874 independent reflections. Cd(II) atom has a slightly distorted octahedral coordination geometry, with four end-on (${\mu}-1$,1) bridging azido ligands and two 2-ethylimidazole ligands bonding through nitrogen atom. The central cadmium(II) atoms are run in parallel to the c-axis and are doubly bridged with neighboring cadmium(II) atoms by the end-on (${\mu}-1$,1) bridging azido ligands. Thus, this complex has a one-dimensional zigzag chain structure in which the 2-ethylimidazole is in the cis conformation.

• Analytical Science and Technology
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• v.18 no.5
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• pp.381-385
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• 2005

The title compound, $\{H_2NCH_2CH_2NH_2CH_2CH_2\}\{Cu(H_2O)_6\}(SO_4)_2$, I, has been synthesized under solvo/hydrothermal conditions and their crystal structure analyzed by X-ray single crystallography. Compound I crystallizes in the monoclinic system, $P2_1/n$ space group with a = 6.852(1), b = 10.160(2), $c=11.893(1){\AA}$, ${\beta}=92.928(8)^{\circ}$, $V=826.9(2){\AA}^3$, Z = 2, $D_x=1.815g/cm^3$, $R_1=0.031$ and ${\omega}R_2=0.084$. The crystal structure of the piperazine templated Cu(II)-sulfate demonstrate zero-dimensional compound constituted by doubly protonated piperazine cations, hexahydrated copper cations and sulfate anions. The central Cu atom has a elongated octahedral coordination geometry. The crystal structure is stabilized by three-dimensional networks of the intermolecular $O_{water}-H{\cdots}O_{sulfate}$ and $N_{pip}-H{\cdots}O_{sulfate}$ hydrogen bonds between the water molecules and sulfate anions and protonated piperazine cations. Based on the results of thermal analysis, the thermal decomposition reaction of compound I was analyzed to have three distinctive stages.

• Korean Journal of Crystallography
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• v.5 no.2
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• pp.78-84
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• 1994

The crystal structure of N-11-(benzotriazol-1-yl)butyl]-P-nitroaniline ( C16H17N502) has been determinedfromsingle crystal x-ray diffractionstudy:C16H17N502 monoclinic, P21/n, a=17542(2)A, b=10.755(3)A, c=8.891(1)A, β=104.58(1)˚, V=1623.4(5)A3, 7=293(2)K, Z=4, Cuka(A = 1.5418A) , The molecular structure was solved was by direct meshed refined by full-matrix least squares to a final R =0.0411 for 2248 unique observed [F≥4o(p) ] reflections and 255 Parameters. The crystal structure is stabilized by intermolecular N (11) -Hl 1 (Nl 1) ‥‥N (3) hydrogen bond with N(11) ‥‥ N(3) =3.136(2)A and N(11)-Hll(Nll)‥‥N(3) =164.1(15) ˚.

• Korean Journal of Crystallography
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• v.18 no.1_2
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• pp.1-6
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• 2007

An Organometallic compound, $C_{16}H_{35}B_{10}IrS_2Si$, was synthesized from o-carborane, $Cp^*Ir(S_2C_2B{10}H_{10})$, and $Me_3SiCHN_2$. The molecular structure of this complex has been determined by X-ray diffraction. Crystallographic data : monoclinic, space group $P2_1/n$, $a=10.1986(12)\;{\AA}$, $b=14.834(5)\;{\AA}$, $c=17.139\;{\AA}$, ${\beta}=92.24(2)^{\circ}$, Z=4, $V=2591.0(14)\;{\AA}^3$. The structure was solved by direct methods and refined by full-matrix leat-squares methods to give a model with a reliability factor R=0.053 for 5080 reflections.

• Korean Journal of Crystallography
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• v.15 no.1
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• pp.24-28
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• 2004

The structure of $C_{12}H_{15}N_3O_3$ has been determined by X-ray diffraction methods. The crystal system is monoclinic, space group $P2_1/c$, unit cell constants, a = 12.9955(9) ${\AA}$, b = 7.7137(5) ${\AA}$, c = 13.4699(11) ${\AA}$, ${\beta}$ = 107.86(1)$^{\circ}$, V = 1285.2(1) ${\AA}^3$, T = 296 K, Z = 4, $D_c$ = 1.350 $Mgm^{-3}$. The intensity data were collected on an Enraf-Nonius CAD-4 Diffractometer with graphite monochromated Mo $K{\alpha}$ radiation (${\lambda}$ = 1.71073 ${\AA}$). The molecular structure was solved by direct methods and refined by full-matrix least squares to a final R = 4.19% for 1644 unique observed $F_0\;>\;4{\sigma}(F_0)$ reflections 193 parameters.