Chiral Ligands Derived from Carbohydrates.21. Crystal Structure of Methyl-4,6-O-benzylidene-3-deoxy-3-(salicylideneamino)-α-D-altropyranoside

A new chiral Schiff base derived from carbohydrate, methyl-4,6-O-benzylidene-3- deoxy-3-（salicylideneamino）-α-D-altropyranoside, has been synthesized by reacting methyl 3-amino-4,6-O-benzylidene-3-deoxy-α-D-altropyranoside with salicylaldehyde in methanol and characterized by IR, ^1H NMR, 13C NMR, MS, elemental analysis, and X-ray crystal structure analysis. The crystal belongs to orthorhombic, space group P212121 with a = 8.0856（16）, b = 10.786（2）, c = 22.690（5）A, V = 1978.8（7）A^3, Z = 4, Mr = 385.40, Dc = 1.294 g/cm^3, p = 0.095 mm^-1, F（000） = 816, the final R = 0.0379 and wR = 0.0811 for 2597 independent reflections. In the title compound, the pyrano-ring adopts a twisted ^1C4 chair conformation.

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.

Analyses of Reaction Mechanisms among Different Sulfonation Reagents and m-Diphenylamine and Crystal Structures of the Formed Compounds

In the traditional process, m-phenylenediamine reacts with fuming sulfuric acid at high temperature to get intermediates, and then after dehydration occurs intramolecular rearrangement to get 2,4-diaminobenzenesulfonic acid. Traditional methods need to consume a lot of fuming sulfuric acid or concentrated sulfuric acid, resulting in high industrial large-scale production cost, more waste, and posing a serious environmental pollution risk. In this thesis, three different sulfonation reagents were used for the sulfonation reaction of m-phenylenediamine, and the reaction mechanisms and crystal structures of the three pathways were investigated. The three routes are: 1) one-step synthesis of monosulfonated compound 1 from raw material and sulfur trioxide (SO3);2) rapid reaction of raw material and chlorosulfonic acid to synthesize bisulfonated compound 2;3) direct eutectic crystallization of raw material and ordinary sulfuric acid to obtain compound 3. The crystal structure of the compounds synthesized by three paths was analyzed by X-ray single crystal diffraction, and compound 1 was characterized by NMR, Fourier infrared spectra, UV-visible spectrum and Mass spectrometry. The one-step synthesis of SO3 as a sulfonation reagent has the advantages of mild reaction conditions, simple operation and low cost.

Chiral Phosphine Ligands Derived from Sugars 4.Crystal Structure of Methyl 4,6-O-Benzylidene-3-Deoxy-3-(Diphenylphosphino)-α-D-Altropyranoside (3-MBPA)

The crystal structure of the title compound 3--MBPA, C26H27O5P (Mr.= 450. 44 ). has been determined by single--crystal X-ray diffraction. The crystal ismonoclinic with space group P21, a= 9. 294(l), b= 7. 999(1), c= 15. 925(2) A,β=96. 17(5)°, V= 1176. 9 A 3, Dc=l. 271 g/cm3, F(000)=476, μ=12. 99 cm-1,Z=', Z=2, and final R = 0. 045 and Ru= 0. 057 for 1882 reflections (I≥3a(I) ). Structureanalysis revealed that the pyranose and 4, 6--O--benzylidene ring of the title compoundadopt a distorted chair conformation and the diphenylphosphino, OH and OMe groupsare in pseudo--axial position.

Investigation on the crystal structure and mechanical properties of the ternary compound Mg_(11-x)Zn_(x)Sr combined with experimental measurements and first-principles calculations

A new ternary compound,Mg_(11-x)Zn_(x)Sr in the Mg-Zn-Sr system was observed and studied using Scanning Electron Microscopy(SEM),Energy-Dispersive Spectroscope(EDS),X-Ray Diffraction(XRD)and Transmission Electron Microscopy(TEM).The XRD patterns were refined by the Rietveld refinement method and the results revealed that the crystallized Mg_(11-x)Zn_(x)Sr phase belonged to tetragonal I41/amd space group and had the Cd_(11)Ba prototype.The Mg atoms were successfully doped into Zn_(11)Sr crystal lattice by occupying Zn atomic sites.Moreover,the Rietveld refinement and computational results demonstrated a gradual decrease in the a-axis and c-axis lattice parameters with decreasing concentration levels of Mg coordination substitution in the lattice of Mg_(11-x)Zn_(x)Sr compound.The elastic constants and modulus of the Mg_(11-x)Zn_(x)Sr compounds calculated by first-principles calculations(FPC)indicated they were increased with the increasing of Zn content.The variation of hardness,D-band widths and the total density of states for Mg_(11-x)Zn_(x)Sr compounds with Zn content was discussed.

Multifunctional Perovskite Photodetectors: From Molecular-Scale Crystal Structure Design to Micro/Nano-scale Morphology Manipulation

Multifunctional photodetectors boost the development of traditional optical communication technology and emerging artificial intelligence fields, such as robotics and autonomous driving. However, the current implementation of multifunctional detectors is based on the physical combination of optical lenses, gratings, and multiple photodetectors, the large size and its complex structure hinder the miniaturization, lightweight, and integration of devices. In contrast, perovskite materials have achieved remarkable progress in the field of multifunctional photodetectors due to their diverse crystal structures, simple morphology manipulation, and excellent optoelectronic properties. In this review, we first overview the crystal structures and morphology manipulation techniques of perovskite materials and then summarize the working mechanism and performance parameters of multifunctional photodetectors. Furthermore, the fabrication strategies of multifunctional perovskite photodetectors and their advancements are highlighted, including polarized light detection, spectral detection, angle-sensing detection, and selfpowered detection. Finally, the existing problems of multifunctional detectors and the perspectives of their future development are presented.

Experimental Investigation of Crystal Structure of Zr 0.98 NiGe 2.94 and Phase Equilibria in Zr-Ni-Ge System

Based on the results of electron probe microanalysis(EPMA)and X-ray diffraction(XRD),the isothermal sections of Zr-Ni-Ge ternary system at 973 K and 1173 K were constructed through alloy sampling approach.It is worth noting that the crystallographic information of the formerly reportedτ2(Zr_(0.98)NiGe_(2.94))was determined,which belongs to the space group Pbcm(No.57).Besides the formerly reported ternary compounds,τ1(Zr_(6)Ni_(16)Ge_(7)),τ_(2)(Zr_(0.98)NiGe_(2.94)),τ_(3)(Zr_(3)Ni_(4)Ge_(4)),τ_(4)(ZrNiGe)andτ_(5)(Zr_(2)Ni_(0.54)Ge_(0.46)),a new ternary phase namedτ_(6)with the composition of Zr_(39)Ni_(18)Ge_(43)was primarily detected in this work.In addition,an invariant reaction Ni_(5)Ge_(3)+τ_(4)τ_(1)+τ_(3)between 973 K and 1173 K was deduced.

Chiral Phosphine Ligands Derived from Sugars8. Crystal and Molecular Structure of Diphenyl (methyl 4', 6'-O-benzylidene-2'-deoxy-α-D-altropyranoside-2-)phosphine Oxide

The crystal structure of the title compound, C26H27O6P, has been determined by single--crystal X-ray diffraction. The crystal is monoclinic with space groupP21, a=16. 193(l), b=5. 804(1), c=12. 512(2) A, β=93. 187(5)°, V=1174. 13A3, Dc=1. 319 g/cm3, F(000) =492, μ= 13. 52 cm-1, Z= 2, and final R= 0. 042and Rw= 0. 040 for 2349 reflections (I≥3σ(I)). Structure analysis revealed that thepyranose and 4, 6-O-benzylidene ring of the title compound adopts a distorted chair conformation.

Chiral Phosphine Ligands Derived fro m Sugars .14 . Crystal Structure of Diphenyl( m ethyl4’,6’-O-benzylidene-3’-deoxy-α- D-altropyranoside-3-)phosphine Oxide

The crystal structure of the title compound, C 26 H 27 O 6P, has been determined by single crystal X ray diffraction analysis. The crystal is orthorhombic with space group P2 12 12 1, a=6.154(4), b=17.199(8), c=22.180(3) , V=2347.6  3, D c=1.32 g/cm 3, F(000)=984, μ=1.5 cm -1 , Z =4, and final R =0.075 and R w =0.080 for 1417 reflections (I≥3σ(I)) . The X ray diffraction analysis revealed that the structure of the title compound s similar to that of its parent phosphine and the pyranose and 4, 6 O benzylidene rings remain distorted chair conformations.

THE CRYSTAL STRUCTURE OF RARE EARTH COMPLEX WITH AMINO ACIDS Ⅱ The Crystal Structure of Gtutamate Comptex of Erbium Perchtorate

The crystat structure of {[Er;（L—Glu）;（H;O）;]（ClO;）;·3H;O);has been studied by X-ray diffraction. The crystal is monoctinic with space group P2;and cell parameters a=19.987（3） , b=16.505（3） , c=11.040（2） , β=104.69（1）;, V=3538（1） , Z=2, Dc=2.29 g. cm;, μ=53.2 cm;, F（000）=2384. The asymmetric unit contains two complex motecules and four centre ions. Each erbium （Ⅲ） is coordinated by five oxygen donors from four different glutamates and four oxygen donors from the aqua ligand to form a nine coordination potyhedron. The mean distances of Er—0 （carboxylate） and Er—Ow are 2.439 and 2.41 respectivety. The finat R and Rw are 0.043 and 0. 058, respectivety.

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）.

Synthesis and Crystal Structure of 2-Amino- 3-ethoxycarbonyl-4-(4-chlorophenyl)-4H, 5H-pyrano-[3,2-c]-benzopyran-5-one

The title compound 2-amino-3-ethoxycarbonyl-4-(4-chlorophenyl)-4H,5H-pyrano- [3,2-c]-benzopyran-5-one (C21H16ClNO5, Mr = 397.80) has been synthesized and characterized by X-ray crystallography. It crystallizes in triclinic, space group P1 with a = 5.756(1), b = 10.099(1), c = 17.106(3) ? a = 80.49(1), b = 83.13(1), g = 80.07(1), V = 961.8(2) ?, Dc = 1.374 g/cm3, = 0.231 mm-1, Z = 2, F(000) = 412, the final R = 0.0369 and wR = 0.0947. In the molecule the pyran ring is of boat conformation. The intermolecular hydrogen bonds of NH…O(5)(x+2, y+1, z+1) and NH…Cl (x+1, y1, z) as well as intramolecular hydrogen bond NH…O(5) are found.

Ionothermal Synthesis, Crystal Structure and Photocatalytic Property of a New Cobalt Coordination Polymer

The reaction of flexible bis（imidazole） ligand and 1,2-bis（imidazol-l＇-yl）methane （bimm） with Co（Ⅱ） salt under ionothermal method resulted in the formation of a new coordination polymer {[Co（bimm）3]·（PF6）2}n （1）. X-ray single-crystal diffraction determination reveals that 1 crystallizes in the triclinic Pi space group, with α = 8.647（6）, b = 12.092（9）, c = 14.967（1 l） A, α = 88.912（8）, β = 81.199（8）, ）, = 89.395（8）°, V= 1546 （2） A3, Z = 2, Mr = 793.39, Dc= 1.704 Mg/m3,μ = 0.768 mm-1 F（000） = 798, the final R = 0.0626 and wR = 0.1634 for 4319 observed reflections with I〉 2σ（I）. In compound 1, the Co（lI） ion is connected to another Co（ll） by two bimm ligands to form 1D double chains which are further linked by bimm ligands to form a 2D wavelike layer. Topologically, the structure of 1 represents a uninodal 2D 4-connected sq1/Shubnikov tetragonal plane net. Moreover, thermogravimetric analyses and photocatalytic property for 1 have also been investigated.

Synthesis, Crystal Structure and Characterization of the Host-guest Type UOF

A new uranium（Ⅵ）-polycarboxylate framework with honeycomb（6,3） nets {[Zn（phen）_2（H_2O）_2][（UO_2）_2（BDC）_3]·2H_2O}n（1, BDC = benzene-1,4-dicarboxylate） was hydrotherrmally synthesized by the reactions of Zn（NO_3）_2·6H_2O with phenanthroine, UO_2（NO_3）_2·6H_2O and benzene-1,4-dicarboxylate. The complex was structurally characterized by FT-IR spectroscopy, powder XRD and X-ray single-crystal diffraction. Crystal data for 1： monoclinic, space group Cc with M_r = 1522.19, a = 14.9385（10）, b = 20.4922（13）, c = 15.9728（10） ？, β = 100.1240（10）°, V = 4813.5（5） ？~3, Z = 4, D_c = 2.100 g？cm^（–3）, μ = 7.293 mm^（–1）, F（000） = 2872, the final R = 0.0224 and w R= 0.0677 for 6522 observed reflections with I 〉 2σ（I）. Hydrogen bonds and π-π stacking interactions contribute to the structural extension and stabilization. Experimental band gap of about 3.57 e V indicates its broad gap semiconductor nature. UV-Vis spectra and solid-state luminescence were discussed in detail. The compound exhibits photocatalytic activities for the degradation of rhodamine B.

Syntheses, Crystal Structures and Antifungal Activities of Two Compounds Containing Pyrazole and Pyrethroid Units

Compounds 1 （C15H17C1F3N303, Mr = 379） and 2 （C14H14C1F3N4OS, Mr = 378） have been synthesized and their crystal structures were determined by single-crystal X-ray diffraction. Crystal 1 belongs to the triclinic system, space group P1 with a = 6.0223（19）, b = 9.324（3）, c = 15.936（5） A, a = 80.687（5）, β= 87.289（5）, ）, = 86.097（5）°, V= 880.4（5） A3, Z = 2, Dc = 1.433 g/cm3,μ（MoKa） = 0.266 mm^-1, F（000） = 392, R = 0.0861 and wR = 0.1999 for 2022 observed reflections with I 〉 2o（/）. Crystal 2 belongs to the triclinic system, space group PI with a = 7.7029（15）, b = 8.3371（16）, c = 14.410（3） A, a = 100.672（3）, β= 103.168（3）, ？ = 98.726（3）°, V = 876.1（3） A3, Z = 2, Dc= 1.451 g/cm^3,μ（MoKa） = 0.379 mm^-1, F（000） = 388, R = 0.0672 and wR = 0.2105 for 2725 observed reflections with I 〉 2σ（I）. Although the two compounds are similar with the same pyrazole and pyrethroid units, X-ray analysis reveals that their structures are completely different.

A New Cd(Ⅱ) Coordination Polymer Constructed by 3-(2-Pyridyl)pyrazole and 5-Nitroisophthalic Acid：Synthesis, Crystal Structure and Theoretical Calculations

A new coordination polymer, [Cd2（NIPH）（L）2（H2O）]n（1, HL = 3-（2-pyridyl）pyrazole and H2NIPH = 5-nitroisophthalic acid）, has been synthesized. The structure of complex 1 has been characterized by X-ray single-crystal diffraction, elemental analysis, IR spectrum analysis, thermogravimetric analysis and fluorescence spectrum analysis. Complex 1 belongs to the triclinic system, space group P1 with a = 8.9539（6）, b = 11.6252（8）, c = 12.2472（8） A^°, α = 80.011（2）, β = 80.3850（10）, γ = 86.773（2）°, V = 1237.37（14） A^°3, Z = 2, Dc = 1.987 g/cm^3, μ = 1.780 mm^-1, Mr = 740.25, F（000） = 724, the final R = 0.0295 and wR = 0.1015 with I 〉 2σ（I）. Two H2NIPH as monodentate and bidentate ligands and two L ligands link four Cd（Ⅱ） ions to form a tetranuclear subunit. Each pair of the tetranuclear subunits is bridged by NIPH ligands to yield a one-dimensional double-chain structure. Furthermore, the 1D chains are linked into a 3D supramolecular framework with hydrogen bonds and π-π interactions. In addition, we analyzed Natural Bond Orbital（NBO） in using the PBE0/LANL2DZ method built in Gaussian 03 Program. The calculation results indicated the obvious covalent interaction between the coordinated atoms and Cd（Ⅱ） ion.

Hydrothermal Synthesis, Crystal Structure and Thermal Analyses of Pyrazine-2,3-dicarboxylic Acid Bridged Co(II) Coordination Polymer of _∞~2[Co(phen)(μ-L)_(3/3)]·H_2O (H_2L = Pyrazine-2,3-dicarboxylic Acid)

A novel pyrazine-2,3-dicarboxylic acid bridged Co(II) phen complex 2 ∞ [Co- (phen)(μ-L)3/3]?H2O (H2L = pyrazine-2,3-dicarboxylic acid) has been hydrothermally synthesized, and X-ray single-crystal diffraction analysis shows that it crystallizes in the monoclinic system, space group P21/n with a = 11.480(2), b = 11.885(2), c = 12.939(3) ?, β = 110.55(3)°, V = 1653.1(6) ?3, Mr = 423.25, Dc = 0.425 g/cm3, Z = 4, R = 0.0361 and wR = 0.1011. The title complex consists of 2D 2 ∞ [Co(phen)(μ-L)3/3] layers and crystal water molecules. Each Co atom is octahedrally coordinated by three N atoms and three O atoms to form 2D 2 ∞ [Co(phen)(μ-L)3/3] polymeric layers. Furthermore, such 2D layers are stacked into 3D supramolecular frameworks via Van der Waals’ intermolecular forces, strong and weak hydrogen-bond interactions. The coordination phen and crystal water molecules are resided into cavities of the frameworks.

Syntheses and Crystal Structures of Cd(Ⅱ) and Ni(Ⅱ) Complexes Containing Flexible Sulfide and Nitrogen Heterocyclic Ligands

Two new coordination polymers [Cd（EBLA）（ip）（H2O）] （1） and [Ni（EBSA） （im）2（H2O）], （2） were synthesized by hydrothermal and solution methods using 2,2＇-dithio- salicylicacid （EBSA）, lH-imidazo[4,5-f][1,10]phenanthroline （ip）, imidazole （im）, Cd（NO3）2-4H2O and Ni（NOa）z＇6H20. The complexes were characterized by elemental analysis and FT-IR. Meanwhile, the crystal structures, fluorescence properties of complex 1 and thermogravimetrie analysis of complex 2 have been studied. In complex 1, 2,2＇-dicarboxydiphenylthioether （EBLA） was prepared with 2,2＇-dithiosalicylicacid （EBSA） in situ reaction by hydrothermal method. Complex 1 is a dinuclear structure and Cd2＋ is five-coordinated in a distorted trigonal bipyramidal geometry. Complex 2 is a one-dimensional infinite linear chain and Ni2＋ is six-coordinated to form a distorted octahedral geometry. Hydrogen bonding and π-π interactions are observed in these complexes.

Synthesis and Crystal Structure of a Novel Ca(Ⅱ) Coordination Polymer Containing Dipyridine Dicarboxylic Ligand

The novel alkaline metal complex Ca（BPDCH）2 （1, BPDCH2 = 2,2＇-bipyri- dine-5,5＇-dicarboxylic acid） has been synthesized by the hydrothermal reaction of Ca（NO3）2·4H2O with 2,2＇-bipyridine-5,5＇-dicarboxylic acid. The molecular and crystal structures of complex 1 have firstly been characterized by FTIR, elemental analysis, and X-ray single-crystal diffraction. The 3D MOF structure of complex 1 was interpreted by the versatile binding modes-the intermolecular hydrogen bonds and π-π stacking interactions of 2,2＇-bipyridine-5,5＇-dicarboxylic acid ligand. The analysis results show complex 1 belongs to a coordination polymer with 3D MOF structure. The results of thermogravimetric analysis and solubility demonstrate complex 1 is a thermostable compound and does not dissolve in water and traditional organic solvents.

Solvent-free Synthesis and Crystal Structure of 2,2＇-Dialkyl Bis(3-methyl-6,7- dihydrobenzofuran-4(5H)-one) Derivatives

A series of 2,2＇-dialkyl bis（3-methyl-6,7-dihydrobenzofuran-4（5H）-one） derivatives was prepared through H2SO4·SiO2 catalyzed condensation reaction under solvent-free conditions as potential anti-tumor agents. All of them were characterized by ESI-MS, IR and NMR spectra. Meanwhile, the single crystal of the target compound （4b）, C24H28O4, was also obtained and determined by X-ray crystallography. Crystal data： triclinic system, space group P , a = 8.463（10）, b = 9.612（11）, c = 13.828（15） , α = 74.29（5）, β = 80.93（5）, γ = 69.90（3）°, V = 1014（2） 3, Z = 2, F（000） = 408, Dc = 1.246 g/cm3, μ = 0.084 mm？1, R = 0.0883 and wR = 0.2440 for 4616 independent reflections （Rint = 0.1200） and 3490 observed ones （I 〉 2σ（I））.