Synthesis and Crystal Structure of a 1D Coordination Polymer:{[Cu(HSSA)(py)_3]·H_2O}_n (H_3SSA =5-Sulfosalicylic Acid,py = Pyridine)

The title compound [Cu（HSSA）（py）3H2O]n （H3SSA = 5-sulfosalicylic acid, py = pyridine） I has been synthesized and structurally determined by single-crystal X-ray diffraction. I was further characterized by elemental analyses, thermogravimetric analyses, IR and UV-visible spectroscopy. The crystal belongs to the monoclinic system, space group P21/c with a = 9.4564（10）, b = 18.2679（19）, c = 15.7284（12） A,β= 126.045（4）°, V= 2196.9（4）A^3, Z= 4, Dc = 1.618 g/cm^3, Mr = 535.02,μ = 1.141 mm^-1, F（000） = 1100, 2（MoKα） = 0.71073 A, the final R = 0.0429 and wR = 0.1044 for all observed reflections. In the structure, every two Cu（II） atoms are bridged by a bivalent 5-sulfosalicylic anion to form a 1D chain-like coordination polymer. Lattice waters between chains link them to form 2D layers which are further linked by C-H…O hydrogen bonds to form a three-dimensional supramolecular network.

Structure, Growth and Characterization of Ammonium 5-Sulfosalicylic Acid Monohydrate Crystal

Ammonium 5-sulfosalicylic acid monohydrate （NH4·C7H5O6S·H2O, ASSA） was synthesized and optical grade crystal with dimensions of 45ram × 20mm × 18mm was obtained from aqueous solution by the cooling solution method. The crystal structure was confirmed by X-ray single-crystal diffraction method and the empirical composition is C7HIINO7S with formula weight 253.23. The crystal belongs to monoclinic space group P21/c with a = 1 1.884（9）, b = 7.306（5）, c = 12.152（9） A, β = 104.851（13）°, V= 1019.8（13） A3, Z = 4, Dc = 1.649 g/cm3,μ = 0.340 mm-1, F（000） =528, the final R= 0.0307 and wR= 0.0866 for 7494 observed reflections （I〉 2σ（I））, Elemental analysis, 1R and 1H-NMR spectrum were used to characterize the compound. Thermal analysis showed that one coordination water molecule was contained and dehydration temperature of ASSA crystal was 106℃. Optical transmission and fluorescence spectrum revealed that the ASSA crystal exhibited a strong absorption in ultraviolet region with the sharp absorption edge located at 340 nm and a significant blue fluorescent emission band at 442 nm.

SINGLE AND BINARY ADSORPTION PERFORMANCE OF SALICYLIC ACID AND 5-SULFOSALICYLIC ACID ONTO HYPERCROSSLINKED POLYMERIC ADSORBENTS

Single and binary adsorption behaviors of salicylic acid and 5-sulfosalicylic acid onto hypercrosslinked polymeric adsorbents,i.e.NDA-101 and NDA-99 were investigated.The Freundlich model can successfully describe all the adsorption isotherms tested,which indicates a favorable and exothermic adsorption process.The adsorption of salicylic acid relies on π-π interaction,while the electrostatic interaction further influences the adsorption of 5-sulfosalicylic acid onto NDA-99.The adsorptive capacity of salicylic acid on NDA-99 decreases but increases on NDA-101 with 5-sulfosalicylic acid as the background component in a binary solute system.The amount of 5-sulfosalicylic acid adsorbed was decreased with the increase in initial concentration of salicylic acid on both adsorbents.The competition for the adsorption sites is considered to be predominant in the solid-to-liquid interaction process.The adsorption selectivity of salicylic acid onto NDA-101 is higher than onto NDA-99 by more than an order of magnitude.Thus,combination technique involving NDA-101 followed by NDA-99 can be effectively applied to separate and recover salicylic acid and 5-sulfosalicylic acid from wastewater.

Cocrystallization of N-donor type compounds with 5-sulfosalicylic acid:The effect of hydrogen-bonding supramolecular architectures

Benzotriazole,N,N'-dimethylpiperazine and N-methylpiperazine were applied to crystallize with 5-sulfosalicylic acid(5-H2SSA),affording three new binary molecular cocrystals [(C6H6N3+).(C7H5O6S-)].H2O(1),[(C6H16N22+)1/2.(C7H5O6S-)].H2O(2) and [(C5H14N22+).(C7H5O6S-)2].3H2O(3) under general conditions.Proton-transferring occurs from acid to nitrogen of N-donor compounds in all compounds 1,2 and 3.Analysis of the hydrogen-bonding synthons and their effects on crystal packing were also presented in the context of crystal engineering and host-guest chemistry.In compound 1,1-D infinite chains are extended to a 2-D layered architecture via strong O-H...O hydrogen bonds and then to a 3-D network by N-H...O interactions.Compound 2 and 3 both have the 1-D chain which is formed by O-H...O bonds and weak C-H...O hydrogen bonds.A common intramolecular S(6) [synthon I] ring is formed by the hydroxyl with the carboxyl group in all three compounds.

Synthesis,Crystal Structure and Luminescence of a Novel Cadmium(Ⅱ) Coordination Polymer with 5-Connected nov Net

A novel interesting coordination polymer,[Cd（HSSA）（2-bimb）2].3H2O（1,H3SSA = 5-sulfosalicylic acid,2-bimb = 1,2-bis（imidazol-1-ylmethyl）-benzene）,has been synthesized and structurally characterized.Compound 1 crystallizes in the monoclinic system,space group P21/n with a = 10.8653（10）,b = 19.4100（17）,c = 17.4414（17） ,β = 91.944（2）°,V = 3676.2（6） 3,Z = 4,C35H38CdN8O9S,Mr = 859.19,Dc = 1.552 g/cm3,μ = 0.717 mm-1,S = 0.999,F（000） = 1760,R = 0.0531 and wR = 0.1078.The compound features a rare three-dimensional（3D） 5-connected nov topology.In addition,compound 1 exhibits strong photoluminescent emission at room temperature.

Supramolecular Assemblies in Salts of 2,2＇-Biimidazole with 5-Sulfosalicylic Acid and 3,4,5-Trihydroxybenzoic Acid

Supramolecular assemblies of 2,2＇-biimidazole with 5-sulfosalicylic acid and 3,4,5-trihydroxybenzoic acid, have been synthesized and characterized by single-crystal X-ray diffraction methods. Both the two proton-transfer compounds of 2,2＇-biimidazole with 3-carboxy-4-hydroxybenzenesulfonic acid （5-sulfosalicylic acid, 5-SSA） [namely bis（2-（2-1H-imidazolyl）-1H-imidazolium） 4-hydroxybenzene-3-carboxylate-1-sulfonate monohydrate, 2（C6HTN4）^＋· CTH4068^2-.H2O, （Ⅰ）] and 3,4,5-trihydroxybenzoic acid [namely 2,2＇-bi-1H-imidazolium bis（3,4,5-trihydroxybenzoate） tetrahydrate, C6H8N4^2＋ ·2（C7H5O5）^-·4（H20）, （Ⅱ）] feature extensively hydrogen-bonded three-dimensional network structures having significant interlayer n-n interactions between the cation and anion species. In Ⅰ, a 5-SSA^2- dianionic species results from deprotonation of both the sulfonic and the carboxylic acid groups, all available O-atom acceptors interact with all cation and water molecule donors by hydrogen bonds. In Ⅱ, the formula unit displays a crystallographic inversion symmetry. The structural information about the two complexes between 2,2＇-biimidazole compound and benzenecarboxylic acids obtained in this work will be particularly important for the rational design of supramolecular organic functional materials.

Adsorption selectivity of salicylic acid and 5-sulfosalicylic acid onto hypercrosslinked polymeric adsorbents

Both bottle-point and column-feeding experi-ments involving different solutes and sorbents were carried out to investigate the adsorption selectivity and separation performance of salicylic acid and 5-sulfosalicylic acid.Their adsorption isotherms onto such hypercrosslinked polymeric adsorbents as NDA-100 and NDA-99 could be well described by the Freundlich equations whose characteristics describe extrathermic and favorable adsorption processes.The adsorp-tion towards NDA-100 mainly depended on the p-p interac-tion,while that towards NDA-99 was extremely influenced by the static-electric interaction.Additionally,the adsorptive capacity of salicylic acid on NDA-99 decreased while it increased on NDA-100 with the presence of 5-sulfosalicylic acid in the adsorptive environment as the competitive component.Comparatively,the adsorption capacity of 5-sulfosalicylic acid decreased on both resins with salicylic acid as the competitive component.In fact,the difference in the interaction between adsorbent and adsorbate resulted in the straight antagonism on the effective adsorption sites on the adsorbent.In conclusion,the adsorption selectivity of salicylic acid onto NDA-100 was obviously larger than that onto NDA-99 with the existence of 5-sulfosalicylic acid in the adsorptive environment.A satisfactory separation and recovery of tested solutes in aqueous phase could be foresee-ably achieved by the sequencing adsorption technique involving NDA-100 as well as NDA-99.

~1H and ^(13)C NMR studies of lanthanide complex with 5-sulfosalicylic acid

In this paper, paramagnetic shifts have been measured for all ~1H and ^(13)C nuclei of 5-sulfo- salicylic acid (SSA) in the presence of the lanthanide ions in the second half of the series. The ligand forms isostructural complexes with these ions in aqueous solution. The separation of LISs was carried out by the use of the Reilley method and the calculated dipolar shifts were used to simulate the coordination structure of the complex. The result reveals that SSA is coordinated to lanthanide ion via two oxygens, one from the carboxylic group and the other from the phenolic group with Ln—O bond lengths equal to 2.47 . The lanthanide ion lies on the benzene plane and the carboxylic group is twisted 20°from the benzene ring. Of all the nuclei examined, those in the six-membered chelate ring experience significant dipolar interactions and contact interactions. Small |G/A| ratios were obtained for two protons five bonds away from the central lanthanide ion, which shows that the number of bonds alone cannot be used as a criterion for neglecting contact shifts in aromatic ligand.

Hierarchical porous nanosheets of Co-Mn bimetallic oxide from deep eutectic solvent for highly efficient peroxymonosulfate activation

The development of highly active catalysts is the key to the successful application of sulfate radical(SO_(4)^(·-))-based advanced oxidation processes(AOPs)to wastewater treatment.Herein,bimetallic oxide CoMn_(2)O_(4)hierarchical porous nanosheets(CoMn_(2)O_(4)HPNSs)were constructed using glucose/urea deep eutectic solvent(DES)as sustainable solvent and self-formed sacrificial carbon templates.The prepared CoMn_(2)O_(4)HPNS exhibited outstanding peroxymonosulfate(PMS)activation performance,achieving the rapid degradation of refractory organic compounds in wastewater,including 5-sulfosalicylic acid(100%),acetaminophen(100%),oxtetracycline(100%),and sulfamethoxazole(91%)within 20 min.This excellent performance was attributed not only to the synergistic catalytic effect of Co-Mn bimetals,but also to the hierarchical porous structure which exposes more active sites and accelerates the migration of PMS and organic pollutants.In addition,CoMn_(2)O_(4)HPNS also showed excellent reusability and high stability in multiple cycles of degradation.The active species quenching results and electron paramagnetic resonance measurements revealed that SO_(4)^(·-)greatly contributed to organic degradation,while^(1)O_(2)and·OH also involved.Moreover,a series of other transition metal oxides(Co_(3)O_(4),Fe_(2)O_(3),Mn_(3)O_(4),NiO,and CoFe_(2)O_(4))with hierarchical porous nanosheet structures were successfully fabricated with this method.This study provides a simple,general,and low-cost strategy for fabricating hierarchical porous transition metal oxides,which are promising for the environmental remediation or many other applications in the future.