Synthesis and Crystal Structure of Organic Salt (H_2Bpy)(cda)_2 (cda = Carbamyldicyano-methanide Anion; H_2bpy = Hydrogen 4,4'-Bipyridyl Divalent Cation)

The organic salt, (H2Bpy)(cda)2, was synthesized by the reaction of sodium car- bamyldicyanomethanide, 4,4-bipyridyl and manganese(II) perchlorate in water solution. The crystal belongs to monoclinic, space group C2/c with a = 20.333(7), b = 6.177(2), c = 15.566(5) ? b = 116.860(5), V = 1744(1) ?, Z = 4, C18H14N8O2 (Mr = 374.37), Dc = 1.426 g/cm3, F(000) = 776, m = 0.100 mm-1 and l = 0.71073 ? The structure was refined to R = 0.0560 and wR = 0.1072 for 590 observed reflections (I > 2s(I)). Two nitrogen atoms of the 4,4?bipyridyl molecule bonded to two hydrogen ions, resulting this neutral molecule into a divalent cation. Through the interaction of colorless H2bpy cation and colorless cda anion the red neutral organic salt was formed.

Synthesis and Crystal Structure of a Magnesium Metal-organic Framework

A magnesium metal organic framework, [N-H2（CH3）2][-N（CH3）4][Mgs（bpdc）3（O2CH）6]· 3H2O （1, bpdcH2 = 4,4＇-biphenyldicarboxylic acid）, has been solvothermally synthesized and structurally characterized. 1 crystallizes in the trigonal system, space group R-3, with a = 11.3427（3）, c = 41.5662（18） A, V = 4631.3（3） A^3, Z = 3 and the final R = 0.0457. Its structure features a pillared-layered three-dimensional network with 8.21 A cavities, in which cationic [NH2（CH3）2]^＋ or [N（CH3）4]^＋ and lattice water molecules are located. Thermal stability of the title compound has also been investigated.

A Novel Organic-Inorganic Complex: Synthesis and Crystal Structure of [Ca(DMSO)_5(H_2O)]_2SiMo_(12)O_(40)

A novel organic-inorganic complex [Ca(DMSO)5(H2O)]2SiMo12O40 was synthesized from CaCl2, DMSO and H4SiMo12O40nH2O in mixed solvent of acetonitrile and water. Its structure was characterized with elemental analysis, IR and X-ray diffraction analysis.

Hydrothermal Synthesis and Crystal Structure of Inorganic-organic Hybrid Compound [H_3NC_2H_4NH_2]VOPO_4

An inorganic-organic hybrid compound, [H_3NC_2H_4NH_2]VOPO_4 was synthesized by means of the hydrothermal method. It was crystallized in a monoclinic system, a space group P2_1/c, with the crystal cell parameters: a=0.92285(11) nm, b=0.72994(9) nm, c=0.98495(11) nm, β=101.280(3)°, V=0.65067(13) nm^3, M_r=223.02 g/mol, D_c=2.277 g/cm^3, Z=4, R=0.0315, ωR=0.0865, GOF=1.085. The VO_5N octahedra chains are corner-linked by PO_4 tetrahedra; the VO_5N octahedra are all trans-linked with V—O bonds being alternately short and long. The monoprotonated ethylenediamine was intercalated between the layers with one end coordinating to V and the other end as an H-bond donor interacting with a terminal O atom of PO_4 from a neighboring sheet. The elementary analysis, infrared spectrum characters and thermal stability were also given.

Synthesis and Crystal Structure Analysis of 2-(3,5-Di-tert-butyl-2-hydroxyphenyl)-2-(3,4- dimethylphenyl) Acetic Acid Dimethylamine Salt

A new compound 2-（3,5-di-tert-butyl-2-hydroxyphenyl）-2-（3,4-dimethylphenyl） acetic acid dimethylamine salt （[NH2（CH3）2][C24H31O3]） was synthesized and structurally determined. It is of monoclinic system, space group P21/c with a = 14.731（2）, b = 10.1185（10）, c = 17.065（2） A^°, β = 98.293（10）° ,Z = 4, V = 2517.0（6）A^°^3, Dc = 1.091 g/cm^3, F（000） = 904 and Mr= 413.58. The dihedral angle defined by two benzene rings is 98.23°.

Synthesis and Crystal Structure of a Complex Bimetallic Salt [Ni(trans_[14]diene)] [Ni (mnt)_2]

The title compound has been synthesized by the reaction of [Ni(trans[14]diene)]I2 with Na[Ni(mnt)2] in water and THF, where [trans[14]diene]= 5, 7,7, 12, 14, 14-hexamethyl-1, 4, 8, 11-tetraazacyclotetradeca-4, 11-diene and mnt2- = cis-1, 2-dicyano-1,2-ethylenedithiolato. Its crystal structure has been determined by X-raycrystallography analysis with 4827 independent reflections (Fo>4σ(F0). The bimetallic complex salt [Ni (trans [14] diene )] [Ni (mnt )2] (C24 H32N8Ni2S4, Mr = 678. 24 )crystallizes in the triclinic system with space group P1, a = 9. 2911 (9), b= 11. 7075(12), c=15. 799(2) A, α=68. 384(7), β=79. 324(7), γ=67. 581(6)°, V=1474. 9(3) A3, Dc=1. 527 Mg/m3, Z=2, λ=0. 71073 A, μ=1. 589mm-1, F(000) =704,R=0. 0367. The structure consists of slightly distorted Square planar units [Ni(trans[14]diene)]2+ and [Ni(mnt)2]2-.

Synthesis and Crystal Structure of Cis 2-(6- Chloro-3-pyridylmethylamino)-4-chlorophenyl- 5,5-dimethyl-1,3,2-dioxaphosphinane 2-Oxides

The crystal structure of the title compound (C17H19Cl2N2O3P, Mr = 401.21) has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 6.1648(6), b = 19.943(2), c = 15.268(2) ?, β = 99.220(2)°, V = 1852.8(3) ?3, Z = 4, Dc = 1.438 g/cm3, F(000) = 832, μ(MoKα) = 0.456 mm-1, the final R = 0.0622 and wR = 0.1586 for 3986 observed reflections (I > 2σ(I)). X-ray analysis reveals that the product is a thermodynamically stable cis isomer. The intramolecular hydrogen bond N(2)–H(2A)…O(1) is observed in the title compound.

Hydrothermal Synthesis and Characterization of a Novel Organically-templated Tungsten Heteropolyacid with a Microporous Structure

A microporous organically-templated tungsten heteropolyacid, (C2N2H10)2 [H2P2W18O62]?8H2O, with a new type was hydrothermally synthesized by using ethylenediamine as the structure-directing agent. Its structure was determined by single-crystal X-ray diffraction analysis. Crystal data: monoclinic, space group P21/c, a = 14.633(4), b = 19.432(5), c = 26.776(5) ?, β = 117.849(11)o, V = 6732(3) ?3, Z = 4, Mr = 4615.48, Dc = 4.554 g/cm3, μ(MoKα) = 30.781 mm-1, F(000) = 7976, the final R = 0.0678 and wR = 0.1359. The crystal of the title compound is constructed by Dawson anions and organic dications forming a novel “hollow” channel system.

Synthesis,Crystal Structure and Photophysical Property of 2-(9H-carbazol-9-yl)-3-(2-(2,4,5-tri-(9H-carbazol-9-yl)-3,6-dicyanophenoxy)phenoxy)dibenzo[b,e][1,4]dioxine-1,4-dicarbonitrile

A purely organic compound 2-（9 H-carbazol-9-yl）-3-（2-（2,4,5-tri-（9 H-carbazol-9-yl）-3,6-dicyanophenoxy）phenoxy）dibenzo[b,e][1,4]dioxine-1,4-dicarbonitrile, C76 H40 N8 O4, was synthesized and characterized by NMR, UV-Vis, photoluminescenceand X-ray single-crystal structure analysis. The compound crystallizes in monoclinic system, space group P21/n with a = 11.6537（3）, b = 34.9738（8）, c = 15.5053（3） ？, β =101.992（2）°, V = 6181.6（2）？3, Z = 4, Mr= 1129.18 g/mol, Dc =1.396 g/cm3, F（000） =2672, μ = 2.239 mm–1, GOOF = 1.019, the final R = 0.0577 and wR= 0.1559 for 11925 observed reflections with I 〉2σ（I）. The UV-vis absorption and fluorescence of the compound were discussed. The compound exhibitsyellow-green luminescence with maximum emission peak at 538 nm, and quantum yields of ф = 0.25 and 0.48 in air-equilibrated and degassed toluene at room temperature. Transient decay spectral studies show that compound 1 displays two component decay fashions with a short decay lifetime of 23 ns for the prompt fluoresce anda long decay lifetime of 3.8ms for thermally activated delayed fluorescence. In air-equilibrated toluene, only a short decay lifetime of 17 ns was observed.The experimental and computational results show thatthe emission of the compound originates from the CT excited states.

Hydrothermal Synthesis and Crystal Structure of a Keggin Polyoxometalate [Co^Ⅱ（2,2′-bipy）2（H2O）]2[SiW^Ⅵ12O40]·2H2O

A Keggin-type tungstosilicate compound [Co^Ⅱ（2,2′-bipy）2（H2O）]2[SiW^Ⅵ12O40]·2H2O 1 （bipy = bipyridine） was prepared by a hydrothermal method for the first time. Single-crystal X-ray diffraction revealed that 1 （C40H40Co2N8O44SiW12） crystallizes in the triclinic system, space group P1 with a = 10.4979（6）, b = 13.3946（7）, c = 13.5756（8）A, α= 70.0769（18）, β = 68.910（3）, γ = 74.186（4）°, V = 1649.84（16）A^3, Mr = 3688.95, Z = 1, Dc = 3.713 mg·m^-3, μ = 21.432 mm^-1, F（000） = 1644, S = 1.058, the final R = 0.0511 and wR =0.1023 for 6523 observed reflections （I 〉 2σ（I））. Compound 1 consists of two coordinated cation fragments [Co^Ⅱ（2,2′-bipy）2（H2O）]^2＋, one normal Keggin polyanion unit [SiW^Ⅵ12O40]^4- and two lattice water molecules. To be noted, each polyanion unit is linked to two cation fragments by its two surface terminal oxygen atoms and two cobalt atoms of two cation fragments forming an organic-inorganic hybrid unit in 1. Furthermore, the compound shows strong photoluminescence property in the solid state at room temperature.

Solvothermal Synthesis and Crystal Structure of a Novel Inorganic-Organic Hybrid Material, Fe_2O(OH)(C_5H_4NCOO)SO_4

A novel inorganic organic hybrid material, Fe 2O(OH)(C 5H 4 ~NCOO)SO 4 was synthesized via solvothermal route using a reaction of FeCl 3·6H 2O, KCNS, and 4 cyanopyridine in aqueous solution of H 2O 2 and ethanol at 130 ℃ for 3 d. The compound crystallized in monoclinic space group P 2 1, with cell parameters a =0 73850(15) nm, b =0 65100(13) nm, c =1 0546(2) nm, β =90 36(3)°, V =0 50700(18) nm 3 and Z =2. The structure is constructed with inorganic layered [Fe 2O(OH)SO 4] + cations linked by organic (C 5H 4NCOO) - anions. The compound is thermally stable up to approximately 240 ℃.

Synthesis and Structural Characterizations of a New Lithium Salt for Lithium-ion Batteries

A novel crystal [（CH3O）2CO]3Li2[C2BF2O4]2 was synthesized and fully characterized by FT-IR and single-crystal X-ray diffraction analysis. It crystallizes in monoclinic system, P2Jn space group, with a = 8.1749（2）, b = 10.7449（2）, c = 12.8665（3） A, βl = 94.654（2）°, V= 1126.45（4） A3, Z = 2, Dc = 1.644 g/cm, F（000） = 568, p = 1.498 mm^-1, Mr= 557.77 g/mol, the final R = 0.0334 and wR = 0.0903. The structure analysis revealed that each Li atom is three-coordinated and adopts 1.5 O atoms of two different dimethyl carbonates and one O atom of C2BF2O4-. Thermal stability and infrared spectra analysis were studied and discussed.

Synthesis and Structural Chemistry of Two Novel Transition Metal Organic Phosphonates

Two novel transition metal phosphonate compounds, [Co（H2BDPP）（phen）]n 1 （BDPP = p-O3PCH2（C6H4）CH2PO3, phen = 1,10-phenanthroline） and [Pb3（BCP）2]n 2 （BCP = OOC（C6H4）CH2PO3）, have been synthesized and structurally determined by X-ray single-crystal diffraction. Compound 1 crystallizes in the monoclinic system, space group C2/c with a = 21.169（4）, b = 12.001（2）, c = 7.6211（15）A, β = 98.03（3）°, V= 1917.2（6）A^3, C20H18N2O6P2Co, Mr = 505.22, Z = 8, De= 1.737 g/cm^3, p = 1.107 mm^-1, F（000） = 1020, the final R= 0.0450 and wR = 0.1306 for 2072 observed reflections （I 〉 2σ（I）. Compound 2 crystallizes in the monoclinic system, space group C2/c with a = 4.7167（9）, b = 18.753（2）, c = 22.781（3）A, β = 91.07（3）°, V= 2014.7（14）A^, C8H6O5PPb1.5, Mr = 523.88, Z = 8, Dc = 3.454 g/cm^3, p = 25.222 mm^-1, F（000） = 1856, the final R = 0.0441 and wR = 0.1906 for 2259 observed reflections （I 〉 2σ（I）. In compound 1, the 1D chain running along the c axis is bridged by four ligands （trans- HO3PCH2C6H4CH2PO3H） in four different directions to extend the structure into a three- dimensional network. In compound 2, the Pb（II） displays 4- and 5-coordination modes. There is a one-dimensional P-O-Pb band along the a axis formed by PO3 groups and Pb（II） cations. These bands are joined by μ2-O of -COO to yield two-dimensional inorganic P-O-Pb layers which are pillared by the OOCC6HaCH2PO3 ligands to form a three-dimensional network. Moreover, compound 2 displays a strong emission band attributed to the ligand-centered （LC） transition.

Synthesis and Characterization of a New Metal-organic Framework with Nou Topology

A new compound, [H2N（CH3）2]2[Zn（btec）]H20 （1, H4btec = 1,2,4,5-benzenetetra- carboxylic acid） has been solvothermally synthesized and structurally characterized by single- crystal X-ray diffraction. The crystal structure is of monoclinic, space group P21/c with a = 9.5741（3）, b = 14.5044（4）, c = 13.7329（5） A,β = 100.582（4）°, V = 1874.61（10） As, C14H20N2O9Zn, Mr = 425.7, Z = 4, Dc = 1.387 g/cm3,μ = 1.349 mm^-1, F（000） = 776, R = 0.0560 and wR = 0.1684 for 2834 observed reflections （1 〉 2a（I））. Compound 1 based onμ4-btec and tetrahedral building unit features a three-dimensional （3D） anionic framework with mixed connected nou topology. The luminescent property and thermogravimetric analysis of compound 1 are investigated.

Hydrothermal synthesis and characterization of two novel inorganic-organic hybrid materials

By using different organic ligands, two 3D inorganic-organic hybrid compounds Co(C4H4N2)(VO3)2 1 and Co(C12H12N2)(VO3)2 2 were synthesized by hydrothermal reaction and characterized by X-ray crystallography. Crystal data: 1. crystal system orthorhombic, space group Pnna, a=10.188(2), b=11.497(2), c=7.3975(15), V=866.5(3)3, Z=4, Dcalcd= 2.705 g/cm3; 2. crystal system triclinic, space group P1– (No. 2), a=8.3190(17), b=8.4764(17), c=11.183(2), α=95.48(3)°, β=92.03(3)°, γ=107.24(3)°, V=748.0(3)3, Z=2, Dcalcd=1.958 g/cm3. The framework of compound 1 contains both {Co(C4H4N2)} and infinite metavanadate chains. Crystal structure of compound 2 is constructed with inorganic {CoV2O6} layers across-linked by organic 1,2-bis(4-pyridyl) ethane ligands. The two compounds are thermally stable to approximately 410 °C and 350 °C, respec- tively. Their optical band gaps are determined to be 2.13 eV and 2.12 eV by UV-VIS-NIR diffuse reflectance spectra, which revealed their nature of semiconductor and optical absorption features.

Synthesis, structure and biological activity of 3,7-dinitrodibenzobromonium salt

3,7-Dinitrodibenzobromonium bisulfate 3 was prepared directly by the reaction of4,4’ -dinitrobiphenyl with sodium bromide and potassium persulfate in the concentrated sulphuric acid. Metathetical reactions of 3 gave 3, T-dinitrodibenzobromonium chloride 4, bromide 5 and iodide 6, respectively. Crystal structure of 3a obtained by crystallization of 3 in formic acid showed that each molecule of 3a consists of two dibenzobromonium ions, two bisulfate anions and a formic acid. The dibenzobromonium ion is nearly coplanar. Compound 3 can dramatically increase mice’s immunofunction.

Synthesis and Structure of a Novel Organic-Inorganic Hybrid Polyoxovanadate, [Ni（bpp）2]2（V4O12） （bpp= 1,3-bi-4-pyridylpropane）

A novel organic-inorganic hybrid polyoxovanadate, [Ni（bpp）2]2（V4O12） （bpp= 1,3-bi-4-pyridylpropane）, was hydrothermally synthesized from a mix.ture of NiCl2＊6H2O, NH4VO3, bpp, EtOH and H2O. The crystal structure consists of ∞^2[Ni（bpp）2]^2＋, two-dimensional networks interpenetrating perpendicularly with each other, and （V4O12）^4-, cyclic tetranuclear clusters linking the ∞^2[Ni（bpp）2]^2＋ networks to form a three-dimensional coordination framework. The crystal belongs to tetragonal space group I41/a with unit cell parameters, a= 2.14705 nm, c= 1.29293 nm. UV-Vis-NIR reflectance spectroscopy study revealed insulator nature for the crystal with an optical energy gap of 2.70 eV.

Recent advances in single-crystalline two-dimensional polymers:Synthesis,characterization and challenges

Two-dimensional polymers(2DPs)are emerging crystalline 2D organic material comprising free-standing,single-atom/monomer-thick,planar,and covalent networks with long-ranging structural order.Benefiting from their intrinsic porosity,crystallinity,and electrical properties,2DPs have displayed great potential for separation,energy conversion and electronic fields.In this mini review,we aim to provide the recent progress in crystalline 2DPs films form synthesis strategies to characterization methods,as well as the future trends.We first present the synthesis strategy of single-crystalline 2DPs films including crystal engineering approaches and surface science.Also,we summarize the characterization methods of 2DPs films and highlight the advantages and limitations of different methods focusing on chemical bonding,morphology,and crystal structure.Finally,we will present the current challenges and trends regarding the future developments of crystallinity,monomer design,synthesis strategy and characterization.