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DOE OSTI2017

Synthesis and Structural Analysis of 2-Cyanophenyl Phenacyl Ether

Molecular and crystal structure of 2-cyanophenyl phenacyl ether, C{sub 15}H{sub 11}O{sub 2}N, have been determined by single crystal X-ray diffraction study. The title compound is monoclinic, with a = 4.4334(4) Å, b = 10.7677(11) Å, c = 12.7779(11) Å, β = 99.806(8)°, Z = 2, sp. gr. P2{sub 1}. The crystal structure is stabilized by C–H···O inter-molecular interactions. In order to clarify the electron delocalization on the whole molecule and determine the active sites of the title compound, DFT calculations and NBO analysis were performed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Synthesis, Spectroscopy, and α-Glucosidase Inhibitory Activity of 3-Substituted Hydrazone Derivatives and Crystal Structure of (1E,2E)-1,2-Bis[1-(3-methoxyphenyl)ethylidene]hydrazone

Six 3-substituted hydrazone derivatives [R = −OCH{sub 3} (1), −NH{sub 2} (2), −NO{sub 2} (3), −F (4), −Cl (5), and −Br (6)] were synthesized by condensation reaction. Their structures were elucidated by {sup 1}H NMR, FT-IR and UV-Vis spectroscopy. The synthesized compounds were further evaluated for their α-glucosidase inhibitory activity. Strong activity was found for 1 and 3. The crystal structure of 1 was determined by single crystal X-ray diffraction: a = 6.9743(1) Å, b = 18.3627(3) Å, c = 12.0207(2) Å, β = 96.087(1)o, sp. gr. P2{sub 1}/c, Z = 4. The molecule of 1 is twisted with the dihedral angle between the two phenyl rings being 51.91(4)°. In the crystal packing, the molecules are linked into chains by C–H···π interactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Synthesis and Molecular Structure of 2-(4-Chlorophenyl)-3-(phenyl-amino)-5-(thiophen-2-ylmethylidene)-3,5-dihydro-4H-imidazol-4-one

2-(4-Chlorophenyl)-3-(phenylamino)-5-(thiophen-2-ylmethylidene)-3,5-dihydro-4H-imidazol-4-one, C{sub 20}H{sub 14}N{sub 3}OSCl was synthesized and its crystal structure was determined by single crystal X-ray diffraction. The crystals are triclinic, sp. gr. P1, Z = 2. All three rings are planar, and imidazole ring is almost perpendicular to the phenyl ring with the dihedral angle of 88.65(2)°. In the crystal, pairs of O–H···O hydrogen bonds link molecules into inversion dimers, featuring R{sub 22}(10) graph set motif. Crystal structure is further stabilized by π···π interactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Hydrothermal Synthesis and Characterization of a New Strandberg-type Diphosphopentamolybdate (C{sub 6}N{sub 3}H{sub 18}){sub 2}[P{sub 2}Mo{sub 5}O{sub 23}] · 6H{sub 2}O

An inorganic-organic hybrid material formulated as (C{sub 6}N{sub 3}H{sub 18}){sub 2}[P{sub 2}Mo{sub 5}O{sub 23}] · 6H{sub 2}O, has been hydrothermally synthesized and characterized by single crystal X-ray diffraction technique, IR spectrum, thermogravimetric analysis and UV-visible spectroscopy. The structure consists of diphosphopentamolybdate Strandberg type polyoxoanions [P{sub 2}Mo{sub 5}O{sub 23}]{sup 6–}, protonated 1-(2-aminoethyl)piperazine cations and six crystallization water molecules. These anions are connected with the organic amine through hydrogen bonding interactions between the hydrogen atoms of the organic molecules and the oxygen atoms of the polyoxoanion and water molecules which generate a three-dimensional network.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

New Diphosphopentamolybdate K{sub 5}[HP{sub 2}Mo{sub 5}O{sub 23}] · 10H{sub 2}O: Synthesis, Structure, and Characterization

A new diphosphopentamolybdate(VI) K{sub 5}[HP{sub 2}Mo{sub 5}O{sub 23}] · 10H{sub 2}O has been prepared employing solution method and characterized by single crystal X-ray diffraction, energy dispersive analysis, infrared spectroscopy, thermal stability analysis, cyclic voltammetry analysis, and ultraviolet visible spectroscopy. The compound crystallizes in the orthorhombic sp. gr. Pcab: a = 15.9661(10) Å, b = 19.0832(10) Å, c = 20.0970(9) Å, V = 6123.27(10) Å3, Z = 8. The crystal structure contains the polyanion units [HP{sub 2}Mo{sub 5}O{sub 23}]{sup 5–} around the potassium cations and lattice water. The [HP{sub 2}Mo{sub 5}O{sub 23}]{sup 5–} subunits are connected together through K−O−Mo bridges and hydrogen bonds. The crystal shape morphology was simulated using the Bravais–Friedel–Donnay–Harker model.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Crystal Growth and Structural Characterization of a Thiocyanato-Bridged Copper(I/II) Mixed-Valence Coordination Polymer

A new mixed-valence coordination polymer [Cu{sub 3}(SCN){sub 4}(DMSO){sub 2}]{sub n} (SCN{sup –} = thiocyanato and DMSO = dimethyl sulfoxide) was prepared and characterized by single crystal X-ray diffraction method. The in situ formation of thiocyanate during the synthesis induces reduction of a part of Cu(II) to Cu(I). The three-dimensional structure of the binuclear thiocyanato bridged compound provided an example of pseudohalide materials containing two different environments for both copper centers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Synthesis, Crystal Structure, and Luminescent Properties of Ag(I) Coordination Polymer with Tricarboxylic Acid and Flexible N-donor Ligand

The reaction of AgNO{sub 3} with combinations of 1,3-bis(4-pyridyl)propane (bpp) and 1,3,5-benzenetricarboxylic acid (H{sub 3}btc) in aqueous alcohol/ammonia at room temperature produces crystals of {[Ag_6(H_2O)_2(bpp)_6] · (btc)_2 · 25H_2O}{sub n} (Ι). Single crystal X-ray diffraction analysis reveals that the complex Ι consists of 1D infinite cationic chains of [Ag(bpp)]{sub n}{sup n+} and [Ag(H{sub 2}O)(bpp)]{sub n}{sup n+} which are further linked into the cation layer of [Ag(bpp)]{sub n}{sup n+} by Ag···π interactions. The noncoordinated btc{sup 3−} serves as template driving surrounding water molecules to aggregate into the anionic water layer. The neighboring anionic water layer and cationic layer were further alternately joined into a 3D sandwich-like framework by hydrogen bonding. In addition, the luminescent properties of Ι were investigated.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Synthesis, Crystal Structure, and Biological Activity of 1,3,5-Thimethyl-2,4,6-tris(3'-methyl-1'-imidazoliomethylene)Benzene Perchlorate

The title compound, C{sub 24}H{sub 33}C{sub l3}N{sub 6}O{sub 12}(ClO{sub 4}){sub 3}, was synthesized and structurally characterized by elemental analysis, IR, MS, HMR and single crystal X-ray diffraction. The crystals are triclinic, sp. gr. P1, Z = 2. The crystal structure is stabilized by C–H···O hydrogen-bonds forming a three-dimensional network. The preliminary biological test showed that the title compound had anti-Mycobacterium phlei 1180 activity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Bromination of 1,2,3,4-Tetrahydro-1,10-phenanthroline: Synthesis and Crystal Structure of 6-Bromo-1,2,3,4-tetrahydro-1,10-phenanthroline and Its Bromide Salt

The bromination reaction of 1,2,3,4-tetrahydro-1,10-phenanthroline (tphen) is investigated, which can afford a new heterocyclic compound, namely 6-bromo-1,2,3,4-tetrahydro-1,10-phenanthroline (1). The bromide salt of 1, i.e., 1 · (1H) · Br (2), can be isolated from the bromination system. The accurate structures of both compounds are confirmed and investigated by single-crystal X-ray diffraction. The result proves that the bromination reaction of tphen mainly affords its C6-substituted product. In compounds 1 and 2, the N−H···Br hydrogen bonds play an important role in intermolecular connection. Crystal data of 1: Monoclinic system, sp. gr. Pc, a = 4.6628(8) Å, b = 8.7980(15) Å, c = 13.1347(19) Å, β = 101.342(5)°, Z = 2, V = 528.31(15) Å{sup 3}. Crystal data of 2: Monoclinic system, sp. gr. P2{sub 1}/n, a = 16.6171(16) Å, b = 7.8323(8) Å, c = 18.6972(18) Å, β = 113.597(2)°, Z = 4, V = 2230.0(4) Å{sup 3}.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Synthesis and Crystal Structure of a Four-coordinated Cobalt Complex with 1-Methylbenzimidazole

A four-coordinated complex, L{sub 2}Co(NCO){sub 2}, (L = 1-methylbenzimidazole) has been synthesized and characterized by IR spectroscopy, elemental analyses, and single crystal X-ray diffraction. The crystal is monoclinic, a = 14.522(2) Å, b = 14.610(2) Å, c = 8.6850(13) Å, β = 92.037(3)°, Z = 4, sp. gr. P2{sub 1}/c. Bond lengths Co–N(L) are equal to 2.0165(16) and 2.0174(15) Å, Co–O(NCO) are 1.944(2) and 1.945(2) Å. Intermolecular C–H···O, C–H···N, and C–H···π interactions link the molecules into three-dimensional networks in the crystal.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Crystal and Molecular Structure of 3,5-Diphenyl-4,5-dihydro-2-phenylcarboxamide-1H-pyrazole

Crystal structure of the title compound C{sub 22}H{sub 19}N{sub 3}O is determined by single crystal X-ray diffraction (sp. gr. P2{sub 1}/c, Z = 4). The molecule as a whole, is not planar: phenyl cycles are rotated relative to the plane of pyrazole ring. N−H···N intramolecular hydrogen bond forms five-membered ring fused to pyrazole ring. There are also intramolecular C−H···O and C−H···π interactions. Intermolecular C−H···O hydrogen bond links the molecules into a C(7) chain along the a axis. The crystal structure is stabilized also by C–H···π and π···π intermolecular hydrogen bonds.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Synthesis, Crystal Structure, and Free Radical Scavenging Activity of 4-Aminopyridinium 3,5-Dinitrobenzoate

The crystal structure of 4-aminopyridinium 3,5-dinitrobenzoate, C{sub 12}H{sub 10}O{sub 6}N{sub 4}, has been determined by single-crystal X-ray diffraction technique. The title compound crystallizes in the monoclinic sp. gr. P21/n with the unit cell parameters: a = 7.4726(3) Å, b = 23.0898(9) Å, c = 8.0744(4) Å, V = 1338.64(10) Å{sup 3}, Z = 4. The asymmetric unit of the compound consists of one 3,5-dinitrobenzoate anion and 4-aminopyridine cation. The adjacent anions and cations are linked through two N−H···O hydrogen bonds, N2−H2A···O5 and N{sub 2}−H2B···O6, to form an infinite chain of anions and cations, extended along the [010] direction.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Absolute Configuration of Andrographolide and Its Proliferation of Osteoblast Cell Lines

Andrographolide, C{sub 20}H{sub 30}O{sub 5}, is a labdane diterpenoid which was isolated from the leave of Andrographis paniculata. Its crystal structure is determined by single crystal X-ray diffraction: monoclinic, sp. gr. P2{sub 1}, Z = 2. Absolute configuration is determined by the refinement of the Flack parameter to 0.21(19). In the crystal, molecules are linked by O–H···O hydrogen bonds and C–H···O interactions into two dimensional network parallel to the (001) plane. Its proliferation of osteoblast cell lines is reported.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Synthesis, Structure, and Band Gap of a Novel Inorganic–Organic Hybrid Material Based on Antimony Halide and Organoamine

Using an organoamine, 2,5-bis (1-imidazoly) pyridine (L), a novel inorganic-organic hybrid material based on antimony halide formulated as {(CH_3)_2L}{sup 2+}{(Sb_4Cl_8I_8)"0"."5}{sup 2–}(1) was synthesized in situ via solvothermal technique and characterized by the single-crystal X-ray diffraction. During the synthesis, the organoamine L was transformed in situ into the imidazolium ion, {(CH_3)_2L}{sup 2+}. In the compound 1, four Sb(III) ions are linked by two u{sub 3{sup −}}I{sup –} and four uu{sub 2{sup −}}I{sup –} ligands into a (Sb{sub 4}I{sub 8}Cl{sub 8}){sup 4–}unit, in which eight Cl{sup –}ions and two I{sup –}ions act as the terminal ligands. The uncoordinated {(CH_3)_2L}{sup 2+} organoamine moieties are linked with the (Sb{sub 4}I{sub 8}Cl{sub 8}){sup 4–} clusters via H bonds into three-dimensional (3D) supramolecular architecture. The band structure calculation shows that the compound has an indirect band gap of 2.253 eV.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Molecular and Crystal Structure of 2-{(E)-[(5-Chloro-2-methoxyphenyl)imino]methyl}-4-nitrophenol

The molecular structure of the title compound, C{sub 14}H{sub 11}ClN{sub 2}O{sub 4}, was determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic sp. gr. P2{sub 1}/c with Z = 4. The title compound, C{sub 14}H{sub 11}ClN{sub 2}O{sub 4}, is a Schiff base which adopts the phenol-imine tautomeric form in the solid state.The molecule is almost planar and the dihedral angle between the planes of two aromatic ring is 2.2(1)°. The molecular structure is stabilized by intramolecular O–H···N hydrogen bond which generates a six-membered ring. In the crystal structure, the molecules are linked together by intermolecular C–H···O interactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Crystal Structure of 2-((E)-(5-Bromo-2- hydroxybenzylidene)hydrazono)-1,2-diphenylethanone

The molecular structure of the title compound, C{sub 21}H{sub 15}Br{sub 1}N{sub 2}O{sub 2}, was characterized by single crystal X-ray diffraction. The compound crystallizes in the triclinic sp. gr. P1̄ with Z = 2. The molecule is not planar: the dihedral angle between the planes of two aromatic rings [C1/C6] and [C16/C21] is 84.9(2)°. The other dihedral angle between two aromatic rings [C9/C14] and [C16/C21] is 88.8(2)°. The title compound exists as a phenol-imine tautomer, in which a strong intramolecular O–H···N hydrogen bond is formed. This study verifies the preference of the phenol-imine tautomeric form in the solid state. A π–π stacking interactions are also observed, which may influence crystal stability: the distance between centroids is 3.702(2) Å.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Synthesis, Crystal Structure, Antioxidant, and α-Glucosidase Inhibitory Activities of Methoxy-substituted Benzohydrazide Derivatives

Eight methoxy substituted at the benzylidene moiety benzohydrazide derivatives [R = 2-OCH{sub 3} (1), 3-OCH{sub 3} (2), 4-OCH{sub 3} (3), 2,3-(OCH{sub 3}){sub 2} (4), 3,4-(OCH{sub 3}){sub 2} (5), 2,4,5-(OCH{sub 3}){sub 3} (6), 2,4,6-(OCH{sub 3}){sub 3} (7), and 3,4,5-(OCH{sub 3}){sub 3} (8)] were synthesized and characterized by {sup 1}H NMR, FT-IR and UV-Vis spectroscopy. The crystal structure of 4 was determined by single crystal X-ray diffraction (sp. gr. Pbca, Z = 8). The molecule is slightly twisted with the dihedral angle between the two phenyl rings being 9.33(14)°. The methoxy group at the ortho position is twisted [C–O–C–C angle is–109.2(3)°] whereas the other at meta position is co-planar with the attached benzene ring. In the crystal packing, the molecules are linked into two-dimensional network parallel to the (001) plane by O–H···O, O–H···N, and N–H···O hydrogen bonds. Compounds 1–8 were evaluated for an antioxidant and α-glucosidase inhibitory activities and the results suggested that the −OCH{sub 3} substituent was ineffective for bioactivity enhancement.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

A Two-Dimensional Coordination Polymer Based on 1,1':4',1''-Terphenyl-2',4,4'',5'-tetracarboxylate

The coordination polymer, [MnL{sub 0.5}(H{sub 2}O)(phen)]{sub n} (H{sub 4}L = 1,1':4',1''-terphenyl-2',4,4'',5'-tetracarboxylic acid, phen = 1,10-phenanthroline), has been solvothermal synthesized and structurally characterized by single-crystal X-ray diffraction. Complex crystallizes in triclinic sp. gr.P1̄ with Z = 2. Two carboxylate oxygen atoms in the central phenyl rings from two μu{sub 6{sup −}}L{sup 4–} ligands doubly-bridge two Mn(II) ions to form the dinuclear Mn{sub 2}(O{sub COO{sup −}}){sub 2} unit. Each dinuclear Mn{sub 2}(O{sub COO{sup −}}){sub 2} unit links four L{sup 4–} ligands and each L{sup 4–}ligand bridges four dinuclear Mn{sub 2}(O{sub COO{sup −}}){sub 2} units to generate a 2D coordination network, which can be rationalized as a binodal (4,4) topological network by considering the dinuclear Mn{sub 2}(O{sub COO{sup −}}){sub 2} units and L{sup 4–} ligands as 4-connected nodes.

36 MATERIALS SCIENCE↗