The Crystal Structure Study of CaSrFe0.75Co0.75Mn0.5O6−δ by Neutron Diffraction

The crystal structure of CaSrFe0.75Co0.75Mn0.5O6−δ is investigated through neutron diffraction techniques in this study. The material is synthesized using a solid-state synthesis method at a temperature of 1200˚C. Neutron diffraction data is subjected to Rietveld refinement, and a comparative analysis with X-ray diffraction (XRD) data is performed to unravel the structural details of the material. The findings reveal that the synthesized material exhibits a cubic crystal structure with a Pm-3m phase. The neutron diffraction results offer valuable insights into the arrangement of atoms within the lattice, contributing to a comprehensive understanding of the material’s structural properties. This research enhances our knowledge of CaSrFe0.75Co0.75Mn0.5O6−δ, with potential implications for its applications in various technological and scientific domains.

Synthesis and Crystal Structure of the Derivative of Hydroquinone from Mannich Reaction

The regioselective Mannich-type aminomethylation of hydroquinone afforded a nitrogen-containing compound, 2,5-bis-(morpholinomethyl)hydroquinone A, and its crystal structure was determined by single-crystal X-ray diffraction. Crystal data for A: C16H24N2O4, Mr = 308.37, orthorhombic, space group Pbca, a = 10.479(4), b = 10.298(4), c = 14.865(5) ?, V = 1604.3(11) ?3, Z = 4, Dc = 1.277 g/cm3, F(000) = 664, μ = 0.092 mm-1, GOF = 1.078, the final R = 0.0508 and wR = 0.1075 for 1416 observed reflections with I > 2σ(I). There exist two intramolecular O–H…N hy- drogen bonds between the phenolic O atoms and the morpholine N donors and the morpholino rings assume the preferred chair conformation.

Crystal Structure of Derivative of H_4′-NOBIN and the Applications in Hetero-Diels-Alder Reaction

Novel Schiff bases of H4＇-NOBIN 5a and 5b were synthesized by condensation of 3 with aldehydes. Compound 5b was structurally characterized by single-crystal X-ray diffraction. The asymmetric hetero-Diels-Alder reactions were carried out with high yields and good enantioselectivities in the presence of Ti-（S）-5a complex as catalyst. Crystallographic data for 5b： C27H22BrNO, Mr = 456.37, triclinic, space group P1 with a = 9.1618（2）, b = 10.3836（2）, c = 12.7718（2） А,α=105.4860（10）,β= 94.6360（10）, γ= 108.4610（10）°, V= 1092.32（4）А^3, Z=2, Dc= 1.388 g/cm^3, μ= 1.900 mm^-1, F（000） = 468, R = 0.0476 and wR = 0.1248 for 3092 observed reflections （I〉 2σ（I））.

STUDIES ON SOLID STATE REACTIONS OF COORDINATION COMPOUNDS(LXⅡ)Solid state synthesis and crystal structure of the complex ICu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)CIJ·0.5CS_2

[Cu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)Cl]·0.5CS_2=,Mr=895.79,monoclinic,space group P2_1/a,a=17.231(3),b=14.611(2),c=18.000(3) ,β=105.56(2)°,V=4365(1) ~3, Z=4,D_c=1.37g/cm^3.,λ(MoK_α)=0.71073 ,μ=12.15cm^(-1),F(000)=1855,R=0.052, R_W=0.045 for 3930 observed reflections with Ⅰ>1.5σ(Ⅰ).The central metal atom has a dis. torted tetrahedral geometry with bond lengths Cu-S=2.384(2) (Au-S=2.389(4)), Cu-Cl=2.481(3)(Au-Cl=2.474(1))and Cu-P=2.269(2)-2.289(2)(Au-P=2.270(4)-2.279(4)) .

Synthesis and Crystal Structure of a N,N,N′-tri(2-hydroxy-5-methylbenzyl)-1,2-ethanediamine

An aminophenol ligand, N,N,N＇-tri（2-hydroxy-5-methylbenzyl）-l,2-ethanediamine, was prepared through the Marmich reaction, and structurally characterized by NMR, IR, MS and single-crystal X-ray diffraction. The title compound （C26H32N2O3, Mr = 420.54） belongs to the monoclinic system, space group P21/n with a = 8.6233（14）, b = 10.2655（16）, c = 26.017（4） A, β = 95.797（2）°, V = 2291.3（6） A^3, Z = 4, the final R = 0.0461 and wR = 0.1139 for 4267 unique reflections （Rint = 0.028） with 11691 observed ones （I〉 2a（I））.

Crystal Structure of a Tricyclic Compound C_(20)H)(28)O_6 Obtained through IMDA Reaction

The tricyclic compoun d (2) C20H28O6 has been synthesized through thereaction of IMDA. The crystals of the title compound(2A) were crystallized from etherin monoclinic space group C2 with a unit cell: a = 11. 301 (2), b=11-.863 (3 ), c =29. 59 (1) , β= 101. 02(5)°, V=3894. 246, Dc=1.2413 g/cm3, Z=8, F(000)=1568, Mr= 364. 00 R=0.055, R2=0. 055, μ= 535 cm-1, S(GOF) =0. 571. Theconfiguration of C2a-H in the title compound was found to be contrary to what wasexpected and a possible mechanism of reaction was proposed.

Two New Coordination Polymers Assembled with a Functionalized Ligand:Syntheses and Crystal Structures

Two new transition-metal organic coordination polymers [M（mna）2]（M = Cd（1）,Zn（2）;mna = 2-mercaptonicotinic anion） have been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction along with IR and elemental analyses.Compound 1 is generally a one-dimensional linear structure bridged through the sulfur donor of mna ligand,while 2 is a one-dimensional zigzag chain ligated via the oxygen donor of mna ligand.These compounds further result in three-dimensional structures via intermolecular π...π stacking interactions and/or hydrogen bonding interactions.The two compounds were structurally determined by single-crystal X-ray diffraction.Complex 1 crystallizes in monoclinic space group P21/c with a = 3.730（3）,b = 13.973（12）,c = 12.380（11） ,β = 97.953（18）°,V = 639.0（10） 3,Z = 2,CdC12H8O4N2S2,Mr = 420.72,Dc = 2.187 g/cm3,F（000） = 412,Rint = 0.0252,T = 293（2） K,μ = 2.052 mm？1,the final R = 0.0269 and wR = 0.0586 for 1377 observed reflections with I 2σ（I）.Complex 2 belongs to monoclinic space group P21/c with a = 13.376（2）,b = 12.8429（14）,c = 7.4856（10） ,β = 96.190（10）°,V = 1278.5（3） 3,Z = 4,ZnC12H8O4N2S2,Mr = 373.69,Dc = 1.941 g/cm3,F（000） = 752,Rint = 0.0414,T = 293（2） K,μ = 2.264 mm？1,the final R = 0.0418 and wR = 0.0966 for 2396 observed reflections with I 2σ（I）.

Synthesis and Crystal Structure of 2-Ethoxy-3-n-butyl-benzofuro [2,3-d]pyrimidin-4(3H)-one

The crystal structure of the new title compound 2-ethoxy-3-n-butyl- benzofuro[2,3d]pyrimidin-4（3H）-one （C16H18N2O3, Mr = 286.32） has been prepared and determined by singlecrystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 13.7167（14）, b = 13.113（1）, c = 8.378（1） A, β = 98.992（2）^o, V = 1488.4（3） A^3, Z = 4, Dc = 1.278, F（000） = 608, μ = 0.089 mm^-1, MoKa radiation （2 = 0.71073）, R = 0.0498, wR = 0.1238 for 2336 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that all ring atoms in the benzo[4, 5]furo [2,3-d] pyrimi- dinone moieties are almost coplanar.

One-pot Synthesis,Crystal Structures and Antimicrobial Activities of Two New 1,4-Disubstituted 1,2,3-Triazole-4-Carboxylates

Two new 1,4-disubstituted 1,2,3-triazoles-4-carboxylates were synthesized via click reaction. Compound 1a was synthesized by the interaction of 6-nitro-tetrazolo[1.5-a]-pyridine with ethyl propynoate at room temperature in the presence of Cu（OAc）2 as a catalyst and THF as solvent. Compound 1b was also synthesized by the same manner except that tert-butyl propionate, instead of ethyl propynoate, was used. The compounds were characterized by IR, 1H-NMR, 13C-NMR and single-crystal X-ray diffraction analysis. Compound 1a（C10H9N5O4） crystallizes in the triclinic system, space group P1 with a = 5.0894（9）, b = 8.9834（13）, c = 13.089（2） ？, α= 83.041（7）, β= 80.256（7）, γ=87.296（8）°, V = 585.24（16）？3, Z = 2, Mr = 263.22, crystal size（mm） = 0.37 × 0.20 ×0.18,（I 〉 2σ（I）） = 8557, 2493, 1229, Rint = 0.057. Compound 1b（C12H13N5O4） crystallizes in the monoclinic system, space group P21/c with a = 6.8854（5）, b = 21.783（2）, c = 9.3986（8） ？,β = 93.239（4）°, V = 1407.4（2）？3, Z = 4, Mr = 291.27, crystal size（mm） = 0.38 × 0.22 × 0.20,（I 〉 2σ（I）） = 11842, 3172, 1866, Rint = 0.047. Antimicrobial assay results showed that the title compounds display excellent activities to different bacterial and fungal strains.

A New Cadmium(Ш) Polymer Based on 3,5-Pyrazoledicarboxylic Acid:Hydrothermal Synthesis and Crystal Structure

The reaction of CdCl3.2.5H2O with 3,5-pyrazoledicaiboxylic acid under hydrother-mal conditions produce a novel three-dimensional（3-D） coordination polymer [Cd2（C5H2O4N2）2.2H2O]n.The title compound crystallizes in the monoclinic system,space group P21/c with a = 6.422（4）,b = 12.334（7）,c = 8.936（6） ,β = 104.793（7）°,V = 684.4（7） 3,Z = 4,Dc = 2.761 g/cm3,μ = 3.181 mm-1,F（000） = 544,R = 0.0248 and wR = 0.0624.In the crystal structure of the title compround,molecules are linked through N-H...O hydrogen bonds,forming chains running along the a axis.Every Cd（Ш） coordinates with four molecules of ligand and one water molecule,forming a pentagomal-bipyramidal geometry.

Crystal Structure and Magnetic Property of a Quaternary Sulfide, Al_(0.36)Sm_3Ge_(0.98)S_7

A new quaternary sulfide, Al0.36Sm3Ge0.98S7 1, has been prepared by a facile solidstate reaction, and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in the hexagonal space group P63 with a = 9.964（1）, c = 5.768（2）A, V = 495.9（1）A^3 and Z = 2. In the crystal structure of 1, Al^3＋ and Ge^4＋ occupy the octahedral and tetrahedral interspaces of the 3-D main-framework constructed by SmS8 bicapped trigonal prisms, respectively. The investigation of optical and magnetic properties of 1 indicates that its optical band gap is 2.18 eV and it shows antiferromagnetic-like interaction.

6,8-Di-tert-butyl-3-(2,4-dimethyl-quinolin-7-yl)-3,4-dihydro-2H-benzo[e][1,3]oxazine: Synthesis, Crystal Structure and Luminescent Properties

6,8-Di-tert-butyl-3-（2,4-dimethyl-quinolin-7-yl）-3,4-dihydro-2H-benzo[e][1,3]oxa- zine（1） was obtained by one-pot reaction starting from 2,4-di-tert-butylphenol, 7-amino-2,4- dimethyl-quinoline and paraformaldehyde. The compound was structurally characterized by NMR, IR and single-crystal X-ray diffraction along with the elemental analysis. Compound 1 crystallizes as solvate with chloroform. The solvate 1·CHCl3（C28 H35 Cl3 N2 O, Mr = 521.93） belongs to the triclinic system, space group P1 with a = 10.852（2）, b = 11.352（2）, c = 13.050（3）, α = 101.95（3）, β = 92.94（3）, γ = 114.64（3）o, V = 1412.4（5）3, Z = 2, Dc = 1.227 g/cm3, F（000） = 552, μ = 0.347 mm–1, R = 0.0959 and wR = 0.2725（I 〉 2？（I））. The chloroform molecule displays a rotational disorder as one chloro atom can be located at two different positions. The packing of 1·CHCl3 was further stabilized by intramolecular C–H…O interactions, intermolecular C–H…N interactions, C–H…π interactions, and π…nteractions. The luminescent properties of compound 1 in both methylene chloride solution and the solid state were studied.

Synthesis, Crystal Structure and Catalytic Activity of a Dinuclear Aluminum Alkyl Complex

Treatment of indolyl-3-aldimines（3-~tBuN=CH）C8H5NH with AlMe3 afforded the deprotonated indolyl aluminum complex cis-[（μ-η~1：η~1-3-~tBuN=CH）C8H5NAlMe2]2,and its crystal structure was determined by X-ray single-crystal diffraction.The crystal belongs to the orthorhombic system,space group P21212 with a = 14.590（9）,b = 15.860（2）,c = 13.266（8） A,μ=0.118 mm^（-1）,Mr = 512.64,V= 3069.5（3） A^3,Z = 4,Dc= 1.109 g/cm^3,F（000） = 1104,R= 0.0451 and wR = 0.0937 for 4978 observed reflections with I 2σ（I）.In addition,the title compound exhibited a high catalytic activity toward the addition of amines to carbodiimide to form guanidines.

Synthesis, Crystal Structure and Property of Cu Pb_2(OH)_2Cl_3

A new copper（1）-lead（Ⅱ） oxyhalide, CuPb2（OH）2Cl3, has been prepared by hydrothermal reaction and structurally characterized by single-crystal X-ray analysis. The compound crystallizes in tetragonal, space group 14（1）/acd with a = b = 13.77（1）, c = 15.38（1） A, V = 2916.2（2）, Z = 4, Mr = 618.29, Dc = 5.633 g/cm^3,μ = 49.97（2） mm^-1, F（000） = 4192, the final R = 0.0204 and wR = 0.0452 for 757 observed reflections with I 〉 2σ（I）. The structure of CuPb2（OH）2Cl3 contains one-dimensional helical chains built by CuCl4 tetrahedra with comer-sharing along the c-axis, in which the Pb^2＋ and OH^- ions are located at the voids between chains. Optical reflectance spectrum measurements indicate that it is a semiconductor with a band-gap of 3.23 eV.

Facile Synthesis and Crystal Structure of a Novel Cyanopyridine

The title compound 2-amino-4-（4-hydroxy-3,5-dimethoxyphenyl）-5-methyl-6- phenyl nicotinonitrile, C21H19N3O3, was synthesized via four-component reactions between propiophenone, malononitrile, syringaldehyde and ammonium acetate in ethanol under reflux without catalyst and characterized by IR, 1H NMR, 13C NMR, MS, EA and single-crystal X-ray diffraction. Single-crystal X-ray diffraction analysis shows that the compound is of monoclinic system, space group P21/n with a = 8.4600（17）, b = 17.139（3）, c = 13.408（3） A, β= 107.06（3）°, V= 1858.6（6） A3, Z = 4, Mr = 361.39, F（000） = 760, μ（MoKa） = 0.088 mm^-1 Dc = 1.292 g/cm3, 2 = 0.71073 A, the final R = 0.0751 and wR = 0.0938 for 3333 observed reflections with I〉 2σ（I）. The crystal packing of the title compound is stabilized by intermolecular hydrogen bonds.

Synthesis and Crystal Structure of (E)-ethyl 6-benzyl-2-[(cyclopropylmethylamino)(4-fluorophenylamino)-methyleneamino]-4,5,6,7-tetrahydrothieno[2,3-c]pyridine-3-carboxylate ethanol monosolvate

The crystal structure of the new title compound （E）-ethyl 6-benzyl-2-[（cyclopropylmethylamino）（4-fluorophenylamino）methyleneamino]-4,5,6,7-tetrahydrothieno[2,3-c]pyridine-3-carboxylate ethanol monosolvate （C28H31FN 4O2S·C2H6O, Mr=552.70） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic system, space group P21/c with a=13.806（10）, b=10.850（7）, c=19.938（14）, β=98.842（9）° , V=2951（4）3 , Z=4, Dc=1.244g/cm 3 , F（000）=1176, μ=0.153 mm-1 , MoKα radiation （λ=0.71073）, R=0.0758 and wR=0.2234 for 4262 observed reflections with I 〉 2σ（I）. Intramolecular N-H…S and C-H…N interactions as well as intermolecular N-H…O and O-H…N hydrogen bonds help to stabilize the crystal structure. X-ray diffraction analysis reveals that the asymmetric unit contains one title molecule and one ethanol molecule.

Hydrothermal Synthesis, Crystal Structure and Photoluminescence of [Sm(PCA)_3(H_2O)_2]_n·6nH_2O

A new one-dimensional （1-D） compound [Sm（PCA）3（H2O）2]n·6nH2O （1, HPCA=pyrazinecarboxylic acid） has been synthesized via hydrothermal reaction and structurally characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the Pbca space group of orthorhombic system with a=19.465（3）, b=12.034（4）, c=19.842（4） , V=4648（2）3, C15H25N6O14Sm, Mr=663.76, Dc=1.897 g/cm3, S=1.023, μ（MoKα）=2.610 mm-1, F（000）=2648, R=0.0239 and wR=0.0616. Compound 1 is characteristic of an infinite 1-D chain-like structure with the samarium atoms locating at an environment of a monocapped square antiprism. The [Sm（PCA）3（H2O）2]n chains and the lattice water molecules interconnect together through π-π interactions and hydrogen bonding interactions to yield a 3-D supramolecular framework. Photoluminescent investigation reveals that the title compound displays an emission in the greenish blue region.

Synthesis and Crystal Structure of an Incomplete Cubane-type Mo_3S_4 Cluster with the N-N-O Type Tridentate Ligand: {Mo_3S_4[NH_2CH_2CH(O)CH_2NH_2]_3}(DTP)·(H_2O)_2·(DMF)

A new cluster {Mo3S4[NH2CH2CH(O)CH2NH2]3}(DTP)?(H2O)2?(DMF) (DTP = diethyldithiophosphate) has been synthesized via ligand substitution reaction of Mo3S4(DTP)4(H2O) with an alkaline ligand 1,3-diamino-2-propanol(DAPROH) in a mixed organic solvent, and its crys- tal structure was determined with the following data: Mo3S6PC16H48O8N7, Mr = 977.76, triclinic, space group P1, Z = 2, a = 10.319(2), b = 12.843(3), c = 15.335(3) ?, α = 65.26(3), β = 82.18(3), γ = 70.67(3)o, V = 1741.7(6) ?3, Dc = 1.864 g/cm3, μ = 1.517 mm-1, F(000) = 988, the final R = 0.0794 and wR = 0.2111 for 6318 observed reflections (I>2σ(I)). The structure analysis indicates that all DTP ligands of Mo3S4(DTP)4(H2O) are replaced and each DAPRO molecule acts as a tri- dentate ligand chelating to each Mo atom of the Mo3S4 core. Different from the precursor, the clus- ter symmetry is elevated to C3. In addition, the UV-spectrum of the title compound was measured.

Synthesis and Crystal Structure of a Novel 14,20-Annulated Pentacyclic Steroid 17(S)-Methyl-13β-hydroxyl-14(R),20(S)-epoxy-pregn-4-en-3-one

The title compound 17（S）-methyl-13β-hydroxyl-14（R）,20（S）-epoxy-pregn-4-en-3-one was synthesized by an improved tandem reaction, and its structure was determined by IR, NMR, HR MS and X-ray single-crystal diffraction. The crystal belongs to orthorhombic, space group P212121 with a = 10.55248（15）, b = 12.14700（16）, c = 14.56841（18） ？, V = 1867.39（4） ？3, Z = 4, Dc= 1.175 g/cm3, μ= 0.604 mm-1, F（000） = 720, the final R = 0.0400 and w R = 0.1072 for 3610 observed reflections with I 〉 2σ（I）.

Synthesis and Crystal Structure of FeCo_2(CO)_8(μ_3-S)〔P(OCH_2Ph)_3〕

The title compound FeCo2 (CO)8 (μ3-S) [P (OCH2Ph )3] was synthe-sized by the reaction of P (OCH2Ph)3 with FeCo2 (CO)9 (μ3-S) at room temperature.Crystal data: C29H21 O11 PSCo2Fe, Mr=782. 23, monoclinic, space group P21/n(14), a= l5. 123(4), b=14. 580(4), c=15. 942(3)A, g=115. 66(1), V=3168293K, final R= 0. 032, R= 0. 037 for 3010 observed reflections with I>3. 00(I).The monosubstituted ligand P (OCH2Ph )3 in FeCo2 (CO)8 (μ3-S ) [P (OCH2Ph )3] islinked to one cobalt atom of the tetrahedron FeCo2S framework.