Synthesis and X-ray Crystal Structure of a New Molecular Clip

The synthesis and X-ray crystal structure of a new molecular clip 2 was reported. It （C24H24N4O2, Mr = 400.47） crystallizes in the space group C2/c with a = 15.587（2）, b = 8.5805（12）, c = 15.259（2） A, β = 102.448（3）°, V= 1992.9 （5）A63, Z = 4, Dc = 1.335 g/cm63,μ = 0.087 mm^-1 and F（000） = 848. It remains monomeric in the crystal and a tape-like structure is formed in the crystal structure of molecular clip. The most unusual structural feature of 2 is the boat conformation of its cyclohexyl ring imposed by the ring fusion at C（9）-C（9a）.

Test of a High Throughput Detector on the X-ray Crystal Spectrometer of the EAST

An attempt was made to improve the spatio-temporal resolution of the tangen- tial X-ray crystal spectrometer （XCS） on the Experimental Advanced Superconducting Tokamak （EAST） by evaluating experimentally the applicability of a novel X-ray photon detection tech- nology for measuring the satellite spectra of Ar XVII with a high counting rate. High-resolution experimental data on the profiles of ion temperature and plasma rotation velocity facilitate the studies of the mechanisms underlining important physical phenomena, such as plasma heating, L-H transition and momentum transport. Based on silicon diode array and single-photon counting technology, a relatively small area （83.8 x 33.5 mm~） two-dimensional detector was successfully in- stalled and tested in the recent EAST campaign. X-ray photon counting rate higher than 20 MHz was observed for the first time, and high quality satellite spectra were recorded for ion temperature and plasma rotation measurement, indicating that the new technology is suitable for the next-step high-resolution XCS on EAST, and the deployment of a detector array with a much larger X-ray sensing area is planned for better plasma coverage.

SYNTHESIS, MAGNETIC PROPERTY AND X-RAY CRYSTAL STUCTURE OF MIXED VALENT COBALT COMPLEX SALT [Co~Ⅲ Cl_2(py)_4][Co~Ⅱ Cl_3(py)]

Complex salt Co_2Cl_5(py)_5 (py=pyridine) was obtained by the reaction of CoCl_2·6H_2O with Bu_4NMnO_4 in pyridine in the presence of benzoic acid. It is monoclinic and crystallizes in space group P2_1/n, fw=690.64, a=28.652(5), b=14.108(4), c=7.424(3) ;β=90.09(1); V=3001(2)~3; Z=4, Dc=1.53g/cm^3. Final R factor is 0.041. The structure consists of a discrete cation [Co~ⅢCl_2(py)_4]^+ and an anion [Co~Ⅱ Cl_3(py)]^-. The Co~Ⅲ ion is coordinated by two Cl^- and four pyridine nitrogen atoms to form an octahedral geometry, and Co~Ⅱ is coordinated by three Cl^- and one pyridine nitrogen atom to form the apices of a tetrahedron. The variable-temperature magnetic susceptility measurement shows no magnet-exchange interaction between Co~Ⅲ and Co~Ⅱ ions.

Inversion techniques to obtain local rotation velocity and ion temperature profiles for the x-ray crystal spectrometer on EAST

Inversion techniques are conducted based on the tangential x-ray crystal spectroscopy(TXCS)geometry on EAST to obtain the local profiles of ion temperature(Ti)and toroidal rotation velocity(vt).Firstly,local emissivity profiles of the impurity argon are obtained using the asymmetrical Abel inversion.Then,the local vt and Ti profiles are calculated by considering the local emissivity profiles and the TXCS detailed geometry.In addition,how the changes in the vt profiles affect the accuracy in the Ti profiles is discussed in detail.It is also found that the lineintegrated Ti profiles are becoming less accurate with the increase in the radial gradient in the local vt profiles.Nonetheless,accurate Ti radial profiles are reconstructed after considering the effects of the emissivity and velocity,which are verified by comparing the inverted vt and Ti profiles with those local profile measurements from the Charge eXchange Recombination Spectroscopy(CXRS)on EAST.

THE FIRST BINUCLEAR MOLYBDENUM AND TUNGSTEN COMPLEXES WITH DOUBLY-BRIDGING PYRIDINE-2-THIOLATO LIGANDS.X-RAY CRYSTAL STRUCTURE OF THE COMPLEX[Mo_2(CO)_4(μ-pyS)_2(PPh_3)_2].2C_7H_8

The title complex was obtained by reactions of [Mo(CO)_3(MeCN)_3] with [CuBr(pySH)(PPh_3)_2]or directly with pySH and PPh_3. The latter method can be used to synthesize the corresponding tungsten complex [W_2(CO)_4(μ-pyS)_2(PPh_3)_2].The molecular structure of the title compound was determined by X-ray diffraction method.

Synthesis, Characterization and X-ray Crystal Structure of 4-Fluoro-N-(2-methyl-5-((2-(p-tolyloxy)acetamido)- methyl)pyrimidin-4-yl)benzamide

A new crystal of 4-fluoro-N-（2-methyl-5-（（2-（p-tolyloxy）acetamido）methyl）pyrimi- din-4-yl）benzamide has been prepared at room temperature and characterized by 1H NMR, 13C- NMR, IR, MS, elemental analysis and X-ray single-crystal determination. The compound crystallizes in monoclinic, space group P21 /c with a = 17.226（5）, b = 13.934（4）, c = 17.262（5）, μ= 92.180（5）°, V = 4140（2） ？3, Dc = 1.311 g/cm3, Z = 8, F（000） = 1712 and ？？= 0.095 mm-1. The molecular packing in the crystal is the result of N-H…ydrogen bonds.

Synthesis and X-ray Crystal Structure of a Methylene-bridged Glycoluril Dimer

The synthesis and X-ray crystal structure of a methylene-bridged glycoluril dimer 2 was reported.The methylene-bridged glycoluril dimer 2（C38H36Br4N8O12,Mr=1116.35） crystallizes in space group P1 with a=10.5802（6）,b=16.8469（9）,c=24.7673（14） ,α=98.00,β=96.263（1）,γ=101.606（1）o,V=4239.3（4）3,Z=4,Dc=1.749 g/cm3,μ=3.869 mm-1 and F（000）=2224.It crystallizes in an S-shaped conformation that displays two ethoxycarbonyl groups on each face of the molecule.

Synthesis,Characterization and X-ray Crystal Structure of 2-Methylpropan-2-aminium Methyl ((4-Fluorobenzamido)(4-fluorophenyl)methyl) phosphonate·H_2O

A new crystal of 2-methylpropan-2-aminium methyl （（4-fluorobenzamido）（4- fluorophenyl）methyl）phosphonate has been prepared at room temperature and characterized by ZH- NMR, 13C NMR, IR, MS, elemental analysis and X-ray single-crystal determination. The compound crystallizes in monoclinic space, group C2/c with a = 20.719（2）, b = 11.8559（13）, c = 18.176（2） A,β = 94.434（2）°, V= 4451.4（9） A3, Dc = 1.317 Mg/m3, Z= 8, F（000） = 1864 and μ= 0.174 mm-1. The crystal packing is stabilized by intermolecular N-H……O and O-H……O hydrogen bonds, as well as by weak π-π stacking interactions.

Synthesis, Characterization and X-ray Crystal Structure of O,O~ˊ-Dipropyl α-（2,4-Dichlorolphenoxyacylamido）-α-（4-methoxyphenyl） Methylphosphonates

A new crystal of O,Oˊ-dipropyl-α-（2,4-dichlorolphenoxyacylamido）-α-（4-methoxyphenyl） methylphosphonates has been prepared at room temperature and characterized by elemental analysis and IR,MS,1H NMR spectra,13C NMR spectra and X-ray single-crystal determination.The complex crystallizes in triclinic,space group P1 with a = 7.858（2）,b = 12.621（4）,c = 12.621（4）,α = 96.17（3）,β = 90.960（3）,γ = 90.960（3）°,V = 1243.9（7）3,Dc = 1.346 Mg/m3,Z = 2,μ = 0.362 mm-1and F（000） = 528.

Optical 2-benzyl-5-hydroxy-4-oxopentanoic acids against carboxypeptidase A:Synthesis,kinetic evaluation and X-ray crystallographic study

2-Benzyl-5-hydroxy-4-oxopentanoic acid 1 and its enantiomers were designed,synthesized and assayed for inhibitory activity against carboxypeptidase A(CPA,EC 3.4.17.1).To verify the role of the terminal hydroxyl group in 1 binding to CPA,2-benzyl-5- benzyloxy-4-oxopentanoic acid 2 was also synthesized and evaluated.The inhibition constants show that both L-1 and D-1 were shown to have strong binding affinity with L-1 being more potent than its enantiomer by 165-fold.On the other hand,the inhibition constant ...

Synthesis,Characterization and X-ray Crystal Structure of N,N'-Bis(4-nitrophenylcarba-mothioyl)-isophthalamide·DMF

A new crystal of N,N＇-bis（4-nitrophenylcarbamothioyl）isophthalamide DMF solva-te has been prepared at room temperature and characterized by elemental analysis and IR,MS,1H NMR spectra and X-ray single-crystal determination.The complex crystallizes in monoclinic,space group P21/c with a = 11.2093（12）,b = 22.081（2）,c = 13.9640（15） ,β= 112.128（2）°,V = 3201.8（6） 3,C28H30N8O8S2,Mr = 670.72,Dc = 1.391 Mg/m3,Z = 4,μ= 0.228 mm-1,F（000） = 1400,the final R = 0.0483 and wR = 0.1411（I 2σ（I））.The molecular packing in the crystal is the result of N-H…O hydrogen bonding.

X-ray Crystallinity Studies of Palladium Polyacrylate

Free radical polymerized palladium polyacrylate was characterized by X-ray diffraction. Various parameters including mean crystallite size, interchain separation and radius of gyration have been calculated and discussed with respect to the concentration of Pd in the polymeric salt. The results show that polymer is predominantly amorphous in nature.

Synthesis, Characterization, X-ray Crystal Structure and Herbicidal Activity of(E)-2-(2,4-Dichlorophenoxy)-1-(5,5-dimethyl-2-oxido-1,3,2-dioxaphosphinan-2-yl)vinyl 2-(2,4-Dichlorophenoxy)acetate

A new crystal of（E）-2-（2,4-dichlorophenoxy）-1-（5,5-dimethyl-2-oxido-1,3,2-dioxaphosphinan-2-yl）vinyl 2-（2,4-dichlorophenoxy）acetate has been determined by single-crystal X-ray diffraction. The compound crystallizes in triclinic, space group P1 with a = 7.9393（17）, b = 11.974（3） ？, c = 13.532（3） ？, α = 90.937（4）, β = 101.998（3）, γ = 101.363（4）°, V = 1231.5（5） ？3, Dc = 1.500 Mg/m3, Z = 2, F（000） = 568 and μ = 0.585 mm^（-1）. The molecular packing in the crystal is the result of C（10）–H（10）···O（5） hydrogen bond, as well as weak π-π stacking interactions. The herbicidal activity results indicated that the title compound 3 showed 80~100% inhibitory activities against all of the tested weeds at a dosage of 150 g×ai/ha.

Synthesis, X-ray Crystallographic Analysis and Bioactivities of α-Aminophosphonates Featuring Pyrazole and Fluorine Moieties

A series of novel -aminophosphonates containing pyrazole and fluorine moieties was designed and synthesized through ultrasonic-assisted condensation and solvent-free addition reactions. Their structures were verified by IR, ^1H NMR, ^13C NMR and elemental analysis. The crystal structure of diethyl[（4-cyano-1H-pyrazol-3-ylamino）（3,5-difluorophenyl）methyl]phosphonate（4a, C15H17F2N4O3P） was determined by single-crystal X-ray diffraction. Compound 4a crystallizes in the triclinic system, space group P1 with a = 8.381（3）, b = 10.103（5）, c = 11.268（3） A, α= 83.772（19）, β= 74.726（19）, γ= 70.964（18）, V = 869.9（6） 3, Mr = 370.30, Dc = 1.414 g/cm^3, Z = 2, F（000） = 384, = 0.200 mm^-1, MoKa radiation（ = 0.71073 ）, the final R = 0.0487 and w R = 0.0823 for 1582 observed reflections with I 〉 2（I）. X-ray diffraction analysis reveals that there are two planes in 4a, and the dihedral angle is 71.51°. Two intermolecular hydrogen bonds and a face-to-face … stacking interaction are observed in the crystal structure. The compounds were evaluated for their antifungal, antiviral and antitumor activities, respectively. Among them, 4b, 4c, 4g and 4h exhibit good activities on Sclerotium rolfsii Sacc at 200 μg/m L, while 4b, 4c, 4f and 4g possess good anti-TMV activities at 500 μg/m L. Unfortunately, all of the compounds showed weak antitumor activities.

Reinvestigation on the Reaction of Salicylic Chloride with Salicylic Amide and X-ray Crystal Structure of a New Macrocyclic Polyester

The reaction of salicylic chloride and salicylic amide at 170 ℃ gave benzoxazine and a new macrocyclic polyester 3, whose crystal structure has been determined by single-crystal X-ray diffraction analysis. Compound 3: C28H16O8, Mr = 480.41, monoclinic, space group P21/n, a = 15.353(3), b = 14.196(3), c = 21.147(4) ? b = 103.32(3), V = 4485(2) ?, Z = 8, F(000) = 1984, Dc = 1.423 g/cm3 and m = 0.106 mm-1. The final R = 0.0535 and wR = 0.1275 for 7903 observed reflections (I ≥ 2(I)). In the asymmetric unit of the compound there exist two independent molecules which are connected by weak aromatic CH…O hydrogen bonding between C(47)?H(47) and atom O(7) of the carbonyl group.

An ionic 2D inorganic-organic hybrid of tris[((1H-tetrazol-5-yl)methyl)morpholine] dodecatungstophosphate(Ⅴ) pentahydrate:Synthesis X-ray crystal structure and spectroscopic characterizations

A unique ionic hybrid material[C_6H_(12)N_5O]_3[(PO_4)W__(12)O_(36)]·5H_2O has been synthesized from the reaction of((1H-tetrazole-5- yl)methyl)morpholine andα-H_3[(PO_4)W_(12)O_(36)]·21H_2O.It has successfully been characterized by elemental analysis,IR and ~1H NMR spectroscopies,TGA and single-crystal X-ray diffraction method.The title compound is constructed from the three [C_6H_(12)N_5O]^+ cations andα-Keggin[(PO_4)W_(12)O_(36)]^(3-) polyoxoanion.The most remarkable structural feature of this hybrid can...

Measurement of tungsten impurity spectra with a two-crystal X-ray crystal spectrometer on EAST

Spectral measurement of tungsten(W)impurity is essential to study impurity transport.Therefore,an X-ray crystal spectrometer(XCS)on EAST was used to measure the line spectra from highly ionized W ions.On EAST,both poloidal XCS and tangential XCS have been developed to measure the plasma temperature as well as the rotation velocity.Recently,He-like and H-like argon spectra have also been obtained using a two-crystal setup.W lines are identified in this study.Through a careful analysis,the W lines of 3.9336,3.9321,and 3.664(A)are found to be diffracted by He-like or H-like crystals.The lines are confirmed with the NIST database.We also calculated the ion temperature with Doppler broadening of these lines.The ion temperature from the W lines is entirely consistent with that from Ar line spectra.The measurement of these W line spectra could be used to study W impurity transport in future work.

A High-Efficiency X-Ray Crystal Spectrometer for X-Ray Thomson Scattering

Highly oriented pyrolitic graphite （HOPG） has high X-ray diffraction efficiency due to its unique mosaic crystal structure, and thus is very suitable for its application to X-ray Thomson scattering measurement of solid-density plasmas. In this article, by using the K-shell X-ray source from laser-produced Ti plasma, the properties of the HOPG spectrometer are characterized and compared with those of the flat Pentaerythritol （PET） spectrometer. The results show that the diffraction efficiency of the HOPG spectrometer under focusing condition is an order higher than that of the PET spectrometer, while the spectral resolution of the HOPG is about 320, high enough to be used in the measurement of X-ray Thomson scattering spectra.

Synthesis and X-ray Crystal Structure of a New Manganese 18-Metallacrown-6

A new hexanuclear manganese (III) azametallacrown, [Mn6 (anhz)6 (DMF)2 (H2O)4]·8DMF was synthesized using trianionic pentadentate ligand, N-acetyl-3-hydroxy-2-naphthoic acid hydrazide (anhz3?), and characterized by X-ray single crystal diffraction. The deprotonated ligand bridges the metal ions using the N?N group of hydrazide to form an 18-membered-ring that has M?N?N repeating units and a cavity in the center. The stereochemistry of the compound has an alternating Δ/Λ propeller configuration. Key words azametallacrown - manganese - crystal structure - pentadentate - hydrazide - synthesis CLC number O 614.7 Foundation item: Supported by the National Natural Science Foundation of China (20171035), The Natural Science Foundation of Hubei ProvinceBiography: Han Dong-dong (1977-), female, Master, research direction: inorganic chemistry

x-ray Crystal Structure of a Dinuclear Zinc(Ⅱ) Complex with Unusual Two Monodentate O-coordination of Carboxylate Group of Isonicotinate

Reaction of Zn(ClO4)2·6H2O with septadentate 2,6-bis[bis(2-benzimidazolylme-thyl)amino methyl]-4-methylphenol (Hbbap) and sodium isonicotinate yielded a dinuclear zinc complex[Zn2(bbap) (Iso) (Hiso)] (ClO4)2·[Zn2 (bbap) (Iso) (H2O)] (ClO4)2·4H2O(1a·1b·4H2O). Hiso isisonicotinic acid and Iso is isonicotinate anion. The structure has been established by X-raycrystallography and shows that the two zinc ions are bridged by the phenoxy unit of bbap- ligand,and the presence of unusual monodentate O-coordination of carboxylate group from isonicotinicacid. The coordination geometry around the zinc ion is approximately trigonal bipyramidal.