Diethylformamide Research Articles

Solvent-controlled synthesis of Ti-based porphyrinic metal-organic frameworks for the selective photocatalytic oxidation of amines.

The photocatalytic activity of metal-organic frameworks (MOFs) can be managed by the milieu of synthesis. Herein, N,N'-dimethylacetamide (DMA) and N,N'-diethylformamide (DEF) were employed as solvents for the synthesis of two Ti-based porphyrinic MOFs, namely Ti-PMOF-DMA and Ti-PMOF-DEF, from tetrabutyl orthotitanate and 4,4',4'',4'''-(porphine-5,10,15,20-tetrayl)tetrakis(benzoic acid). Notably, both DMA and DEF were adsorbed onto the Ti-oxo clusters of the two MOFs to shape their properties. Ti-PMOF-DMA was observed with better optoelectronic response and charge transfer than Ti-PMOF-DEF. Moreover, Ti-PMOF-DMA owned a larger pore volume than Ti-PMOF-DEF, imparting more accessible sites to benzyl amines. Ti-PMOF-DMA exhibited better activity in selective photocatalytic aerobic oxidation of benzylamine than Ti-PMOF-DEF. Irradiated by red light-emitting diodes, outstanding results for selective conversion of benzyl amines to imines over Ti-PMOF-DMA were attained. Superoxide radical anion, generated by the electron transfer from porphyrin via Ti-oxo clusters to dioxygen, turned out to be the primary reactive oxygen species. There was generality towards aerobic oxidation of amines to imines and considerable stability for Ti-PMOF-DMA. This work provides a new perspective on the altering MOFs to enhance photocatalytic organic transformations.

Synthesis of 1-[(Aryl)(3-amino-5-oxopyrazolidin-4-ylidene) methyl]-2-oxo-1,2-dihydroquinoline-3-carboxylic Acid Derivatives and Their Breast Anticancer Activity

This research aimed to produce new 1-[(aryl)(3-amino-5-oxopyrazolidin-4-ylidene) methyl]-2-oxo-1,2-dihydroquinoline-3-carboxylic acid derivatives and check their anticancer effect against the breast cancer MCF-7 cell line. The 2-oxo-1,2-dihydroquinoline-3-carboxylic acid (4) compound was obtained by hydrolyzing ethyl 2-oxo-1,2-dihydroquinoline-3-carboxylate (2) with thiourea and anhydrous potassium carbonate ethanol, which was then treated with ethyl 3-substituted 2-cyanoacrylates (6) in the presence of triethylamine in diethyl formamide to give 1-[2-(ethoxy)carbonyl-2-cyano-1-arylvinyl]-2-oxo-1,2-dihydroquinoline-3-carboxylic (7a,d). Cyclization of compound 7 with hydrazine hydrate ethanol inferred the association of 1-[(aryl)(3 amino-5-oxopyrazolidin-4-ylidene)methyl-2-oxo-1,2-dihydroquinol-3-carboxylates (8a,d). Spectroscopic and micro-analytical techniques such as IR, NMR, and elemental analysis were used to validate the structure of the synthesized organic compounds. The anticancer effects of the synthesized compounds 7a–d and 8a–d were tested by using the MTT assay on the MCF-7 cell line. When compared to the reference compound Dox, the compounds 7b,c and 8a–c demonstrated strong anticancer activity against the MCF-7 cell line. The anticancer effects of the synthesized compounds 7a–d and 8a–d were tested against the MCF-7 cell line, using MTT assay. The compounds 7b,c and 8a–c showed significant anticancer activity compared to the reference compound Dox against the MCF-7 cell line.

Solvent Influence in Obtaining Diverse Coordination Symmetries of Dy(III) Metal Centers in Coordination Polymers: Synthesis, Characterization, and Luminescent Properties

Six new Dy(III)-containing coordination polymers (CPs) have been synthesized emphasizing the role of solvent molecules in directing the formation of the Dy(III) coordination sphere which in turn influences the dimensionality of the coordination polymer, thermal stability, and emission properties. An isophthalate-based flexible ligand 5-[(anthracen-9-ylmethyl)-amino]-isophthalic acid (H2L) with different solvents such as dimethylformamide (DMF), dimethylacetamide (DMA), dimethyl sulfoxide (DMSO), diethylformamide (DEF), and N-donor linkers phen (1,10-phenanothroline) and pyridine (py) was employed to obtain six different coordination polymers, viz., [Dy2(L)2(HCOO)3(DMF)·Me2NH2·H2O]n (1), [Dy4(L)6(DMA)2(H2O)4·4DMA·4H2O]n (2), [Dy2(L)3(DMSO)3(H2O)2·2DMSO·2H2O]n (3), [{Dy(L)(DEF)}2(μ2-OH)]n (4), [Dy2(L)3(phen)2·DMA·7H2O]n (5), and [Dy(L)(NO3)(py)2·py]n (6), respectively. All the compounds were characterized by IR spectroscopy and thermogravimetric analysis, and unambiguously characterized by single crystal X-ray crystallography. The bulky anthracenyl group of the linker H2L in combination with the solvent molecules significantly alters the coordination symmetry of the Dy(III) coordination sphere in the polymers in the manner: D2d in 1, C2v and D4d in 2, C4v and Cs in 3, C5v in 4, D4d in 5, and D2d in 6. The coordination symmetry plays an interesting role in sensitization of lanthanide emission. The emission maxima of compounds 1–6 vary from the blue region to the yellow region significantly due to coordination symmetry expressed by the Dy(III) centers, which in turn depends upon the coordinated solvent molecule. The thermogravimetric profile indicates the thermal stability of the solvent free compounds up to 300 °C.

Unconventional Pyridyl Ligand Inclusion within a Flexible Metal-Organic Framework Bearing an N,N'-Diethylformamide (DEF)-Solvated Cd5 Cluster Secondary Building Unit.

A cationic three-dimensional (3D) metal-organic framework (MOF) sustained by an N,N'-diethylformamide (DEF)-solvated zigzag-shaped Cd5 cluster secondary building unit (SBU), [Et2 NH2 ]2 [Cd5 (BTB)4 (DEF)2 ] ⋅ 4.75DEF (1 a, H3 BTB=benzene-1,3,5-tribenzoic acid) shows flexible framework behavior and undergoes solvate exchange with CHCl3 to yield [Et2 NH2 ]2 [Cd5 (BTB)4 (DEF)2 ] ⋅ xCHCl3 (1 b) accompanied by changes to pore sizes and shapes. Unexpectedly, the DEF solvates coordinated to the central Cd2+ could not be replaced by strongly donor pyridyl and dipyridyl ligands. Additionally, more electron-deficient pyridyls preferentially coordinated to the flanking Cd2+ of the Cd5 SBU, as exemplified by [Et2 NH2 ]2 [Cd5 (BTB)4 (DEF)2 (PyCHO)2 ] ⋅ xSol (2 a, PyCHO=4-pyridinealdehyde) and [Et2 NH2 ]2 [Cd5 (BTB)4 (DEF)2 (PyAc)2 ] ⋅ xSol (2 b, PyAc=4-acetylpyridine). Density functional theory (DFT) calculations were used to understand these counterintuitive observations.

Self-Assembly of Ag+/[PW11NbO40]4- Complexes in Nonaqueous Solutions.

Self-assembly between Ag+ and [PW11NbO40]4- in N- and O-donor solvents (nitriles and amides) has been studied. In the case of dimethylformamide (DMF), formation of a yellow [Ag4(DMF)12][PW11NbO40] (1a) metastable phase and a colorless [Ag4(DMF)10][PW11NbO40] (1) stable phase was observed. In acetonitrile (CH3CN), the product was [Ag(CH3CN)4]2{[Ag(CH3CN)3]2[PW11NbO40]} (2a). By contrast, [SiW12O40]4- of the same size and charge as [PW11NbO40]4- produces [Ag(CH3CN)3]4[SiW12O40] (3a). Partial desolvation of 2a and 3a leads to Ag4[PW11NbO40]·7.5CH3CN (2) and Ag4[SiW12O40]·7.5CH3CN (3), respectively. The CH3CN molecules in the structure of 2 are labile, and this compound was used as the starting material to study solvent-exchange processes in N-methyl-2-pyrrolidone (NMP), dimethylacetamide (DMA), diethylformamide (DEF), and benzonitrile (PhCN) solutions. These solvent reactions yield [Ag(DMA)4][Ag3(DMA)6][PW11NbO40] (4), [Ag2(NMP)4(CH3CN)]2[PW11NbO40]·1.3NMP (5a), [Ag2(NMP)5]2[PW11NbO40] (5b), Ag4[PW11NbO40]·9.5DEF (6), and [Ag(PhCN)4]2[{Ag(PhCN)3}2PW11NbO40] (7). All products were isolated and characterized by single-crystal X-ray diffraction (except for 2 and 3), IR, elemental analysis, and thermogravimetric analysis techniques. The O-donor solvents favor polynuclear, solvent-bridged cationic aggregates. In the case of DMF, DMA, and DEF discrete, tri- and tetranuclear polycations are observed, while in the case of NMP, the formation of infinite polycationic structures takes place. By contrast, the N-donor solvents (CH3CN and PhCN) favor mononuclear cations, which can exist either as distorted tetrahedral, isolated [Ag(Solv)4]+ cations or as pseudotriangular {Ag(Solv)3}+ units, additionally coordinated to a polyoxometalate. Screening of the luminescent properties for solid samples of 1-7 revealed that only 5a/5b and 7 are emissive. In particular, the sample containing 5a and 5b demonstrates long-lived phosphorescence with a 30 ms lifetime.

Investigating the role of amides on the textural and optical properties of mesoporous-nanostructured $$\uptheta $$-$$\hbox {Al}_{{2}}\hbox {O}_{{3}}$$

Mesoporous-nanostructured $$\uptheta $$-$$\hbox {Al}_{{2}}\hbox {O}_{{3}}$$ was synthesized by an autoclaving technique using different amides i.e., formamide (F), dimethyl formamide (DMF) and diethyl formamide (DEF) at $$150^{\circ }\hbox {C}/24\,\hbox {h}$$ followed by calcination at $$1000^{\circ }\hbox {C}$$. Crystallization and structural behaviour of the as-synthesized materials were characterized by X-ray diffraction and Fourier transform infrared spectroscopy. The porosity study was carried out by $$\hbox {N}_{{2}}$$ adsorption–desorption (BET) technique. Microstructural features were measured by transmission electron microscopy (TEM). The amide-based solvents played a deliberate role in microstructural and textural features of $$\uptheta $$-$$\hbox {Al}_{{2}}\hbox {O}_{{3}}$$. The DMF-based solvent showed an enhanced surface area of $$158\,\hbox {m}^{2}\,\hbox {g}^{-1}$$. The as-prepared $$\uptheta $$-$$\hbox {Al}_{{2}}\hbox {O}_{{3}}$$ rendered a nano-sheet, nano-rod and nano-flake like morphology for F, DMF and DEF derived products, respectively. From the UV–Vis spectroscopic measurement, the estimated band-gap of $$\uptheta $$-$$\hbox {Al}_{{2}}\hbox {O}_{{3}}$$ was found to be 5.16–5.40 eV. Photoluminescence investigation further revealed blue emission particularly for excitation at a wavelength of 252 nm. A DMF-derived sample rendered the lowest band gap due to its smaller crystallite size and higher surface area compared to that of F- and DEF-derived samples.

Al–Mg–Ca-Layered Double Oxides for Efficient Removal of As(V) from Water: The Role of Amides

Al–Mg–Ca-layered double oxides (LDO) were synthesized by solvothermal process at 160 °C/24 h in the presence of formamide (F), dimethylformamide (DMF), and diethylformamide (DEF), followed by calci...

Porous Uranium Diphosphonate Frameworks with Trinuclear Units Templated by Organic Ammonium Hydrolyzed from Amine Solvents.

By varying solvent systems, the solvothermal treatment of uranyl nitrate and methylenediphosphonic acid (H4PCP) afforded three new porous uranyl-organic frameworks (UOFs). All were structurally characterized by single-crystal X-ray diffraction and formulated as (Et2NH2)2[(UO2)3(PCP)2](H2O)2.5 (1), (MeNH3)(H3O)[(UO2)3(PCP)2(H2O)3] (2), and [Na(H2O)4](H3O)[(UO2)3(PCP)2(H2O)2](H2O)5 (3). These compounds crystallize with three-dimensional anionic frameworks containing U(VI) and distinct cationic species due to in situ solvent hydrolysis. The solvent systems diethylformamide (DEF), N-methyl-2-pyrrolindone (NMP), and the additive sodium vanadate (Na3VO4) significantly impact the resultant structures, affording diethyl ammonium, methyl ammonium, and sodium cations captured in channels of the anionic frameworks of 1-3. In 1, a trinuclear U3O18 unit formed by three uranyl polyhedra that share edges is connected into a three-dimensional framework. Compound 2 has a three-dimensional framework formed from a uranyl-methylenediphosphonate layer that is pillared by UO7 pentagonal bipyramids. With the inclusion of sodium cations, 3 is a porous framework containing UO7 pentagonal bipyramids within a layer, with sodium cations and UO6 square bipyramids linking the adjacent layers. Compounds 1-3 feature the uranyl/ligand ratio of 3:2, but present diverse structural building units ranging from edge-shared trinuclear to heteronuclear assemblies. The compounds have been characterized by infrared (IR), Raman, and UV-vis spectroscopies, X-ray diffraction, and thermogravimetric analysis.

Green synthesis of multi metal- citrate complexes and their characterization

Four new multi metal-citrate complexes have been synthesized through green synthetic pathways. Their synthesis by hydrothermal route in the present research is decorated with features such as, a simple one pot synthesis, cost effectiveness, easy to scale up for commercial production, efficient synthesis conditions like mild temperature and shorter duration which further rules out the possibility of forming byproducts which may cause damage to the environment and being environmental benign as it eliminates the use and recovery of harmful organic solvents such as N, N- dimethyl formamide and N, N- diethyl formamide, used by the researchers in the past during the synthesis of similar metal- organic framework complexes. All four complexes are well defined crystalline materials with polynuclear multi metal-citrate framework having cubic crystal structure as indicated by their Powder X-ray Diffraction patterns. These complexes have been characterized by Fourier Transform Infrared Spectroscopy, Scanning Electron Microscopy, Energy Dispersive X-ray Spectroscopy, Thermogravimetric analysis and Powder XRD techniques.

Syntheses, Crystal Structure, Luminescence, Porosity and Magnetic Properties of Three‐Dimensional Lanthanide Coordination Polymers with 2‐Aminoterepthalic Acid

AbstractTen isomorphous coordination polymers (CPs) with the formula [Ln2(ATPA)3(DEF)2]n Ln=Ce (1), Pr(2), Nd (3), Eu (5), Gd (6) and [Ln(ATPA)1.5(DEF)]n Ln=Sm (4), Tb (7), Dy (8), Ho (9) and Y(10) (H2ATPA=2‐aminoterepthalic acid and DEF=diethyl formamide) have been synthesized by the self assembly of Ln(III) ions, 2‐aminoterepthalate and DEF under solvothermal condition. These polymers have been systematically characterized by single‐crystal X‐ray diffraction, FTIR, PXRD, thermogravimetric (TGA) and elemental analyses. Structure analyses of CPs 1–10 reveal that all CPs crystallize in the monoclinic space group C2/c system and form 3D framework with difference in coordination numbers. The CPs 1 & 2 exhibit eight coordination numbers whereas CPs 3–10 show seven coordination number with different geometries. TGA indicate thermal stability and robustness of the synthesized CPs. The Sm (4), Eu (5), Tb (7) and Dy (8) polymers emit strong ligand sensitized characteristic f‐f luminescence. Analyses of magnetic susceptibility data of CPs 4, 6, 7 & 8 at variable temperatures and applied magnetic fields reveal weak ferromagnetic interactions at low temperatures.

Solvothermal synthesis and structure of 3D frameworks of Nd(III) and Y(III) with thiophene-2,5-dicarboxylate and N,N′-diethylformamide

Two new 3D MOFs [Nd2(TDA)3(DEF)2(H2O)]n (1) and [Y4(TDA)6(DEF)4]n (2) [Thiophene-2,5-dicarboxylic acid (H2TDA) and N,N′-diethylformamide (DEF)] were synthesized by solvothermal method. They were characterized by elemental analyses, infrared spectroscopy and single crystal X-ray diffraction studies. The two MOFs (1) and (2) belong to the monoclinic system with space group P21/n and C 2 respectively. Structural characterizations by single-crystal X-ray crystallography reveal that 1 and 2 adopt three-dimensional frameworks constructed by cross-linking of rod shaped infinite chain secondary building unit (SBU) by thiophene-2,5-dicarboxylates as linker. These frameworks feature rhomboidal channels, inside which coordinated DEF/H2O solvent molecules are located. DEF plays pivotal role in reaction and design of MOFs. Thermogravimetric analysis shows that both MOFs are thermally robust.

Morphologically Tuned Aluminum Hydrous Oxides and Their Calcined Products

Aluminum hydrous oxides and their derivatives were prepared by a facile solvothermal process in the presence of formamide, dimethyl formamide, and diethyl formamide as solvents at 150°C/24 h. The as‐synthesized products were calcined at 500°C/1 h to obtain γ‐Al2O3. The crystallization behavior and microstructure of the pre‐ and postcalcination products were studied by X‐ray diffraction and transmission electron microscopy, respectively. The surface textural properties of the calcined samples were investigated by N2 adsorption–desorption analysis. The formamide and its derivatives played a significant role in tuning textural properties of the calcined products. The diethyl formamide based sample exhibited enhanced Brunauer–Emmett–Teller surface area and pore volume of 517 m2 g−1 and 2 cm3 g−1, respectively. Both the as‐prepared and calcined samples showed variable morphologies and crystallinity using different solvents. The trend in morphological changes as nanosheet → nanorod → nanowire bundles occurred in the presence of formamide, dimethylformamide, and diethylformamide, respectively. A tentative mechanism has been illustrated for the formation of the products.

Sensitive chemosensing of nitro group containing organophosphate pesticides with MOF-5

A luminescent metal–organic framework, MOF-5 [Zn4O (BDC)3 (BDC=1,4-benzenedicarboxylate)] has been synthesized by the reaction of zinc nitrate and terephthalic acid in diethylformamide (DEF) medium. The obtained fluorescent porous material has been characterized by X-ray diffraction, transmission electron microscopy, confocal microscopy, UV–vis spectroscopy, photoluminescence spectroscopy and surface area analysis. The synthesized MOF exhibits reasonably good fluorescence characteristics (excitation wavelength=330nm, emission wavelength=493nm). The potential of above Zn based MOF for the sensing of nitro group containing organophosphate pesticides (OPs), namely parathion, methyl parathion, paraoxon and fenitrothion, is demonstrated. It has been possible to detect the above four OPs separately in the concentration range of 5–600ppb. The detection limit of the proposed method for all the said OPs is 5ppb. Interestingly, their mixture also shows the above characteristic data. The proposed method for the sensing of nitro OPs is selective towards other OPs e.g., malathion, dichlorvos and monocrotophos.

Assay of Desmopressin in nasal spray by HPLC – UV detector with one Isocratic pump and system set – up

The aim of this study was to apply high performance liquid chromatography – UV detector to determine desmopressin in pharmaceutical preparation using one pump (isocratic pump) and ODS, 5um column. And Mobil phase acetonitrile: N, N diethyl formamide in ratio of 85:15 which show good quantitative and qualitative analysis in desmopressin acetate nasal spray (Cipla LTD INDIA) New controlled condition for setting-up the system to get a result with high resolution was shown in this study. Keywordsdesmopressin, HPLC method , isocratic pump and system set-up

Solvent-Dependent Formation of Cd(II) Coordination Polymers Based on a C2-Symmetric Tricarboxylate Linker

Three novel solvent-dependent Cd(II) coordination architectures [Cd3(BPT)2(DMF)2]·2H2O [1], [Cd3(BPT)2(DMA)2] [2], and [(CH3CH2)2NH2]·[Cd(BPT)]·2H2O [3] were obtained by the hydrothermal reaction of a C2-symmetric tricarboxylate linker, biphenyl-3,4′,5-tricarboxylic acid (H3BPT), with cadmium nitrate in the mixed solvents of water with N,N-dimethylformamide (DMF), N,N-dimethylacetamide (DMA), diethylformamide (DEF), respectively. Single-crystal X-ray diffraction analyses reveal that complex 1 is a three-dimensional (3D) network containing infinite Cd–O–Cd chains with the solvent DMF molecule bridging the neighboring Cd1 and Cd2 centers. Though complex 2 also has a 3D network containing infinite metal-carboxylate chains, the solvent DMA molecule only coordinates to one of the Cd(II) centers as a terminated solvent molecule. Complex 3 possesses a two-dimensional (2D) (6, 3) honeycomb type net formed by the mononuclear metal ion and the BPT ligand, which are further stacked in ABAB fashion through π–π intera...

Quantitative Analysis of Dimethyl Formamide Residues in Acrylic Fiber by GC

In this article, acrylic fiber which was from factory production lines was chosen as samples. The method consisted of extraction of Diethyl Formamide (DMF) via using solid-liquid extraction technique and Gas Chromatograph (GC) analysis. DMF in acrylic fiber were extracted by distilled water, separated though DB-17 capillary column and detected by Flame Ionization Detector (FID). By means of external standard method quantitative analysis was accurately investigated. Detection limit was 3 ppm and recovery rate of DMF was in the range of 94% and 98%. These results showed that this test method was of high precision and sensitivity, which achieved the enterprise production requirements.

Influence of structure on exchange strength and relaxation barrier in a series of FeIIReIV(CN)2 single-chain magnets

Cyano-bridged single-chain magnets of the type L4FeReCl4(CN)2, where L = diethylformamide (DEF) (1), dibutylformamide (DBF) (2), dimethylformamide (DMF) (3), dimethylbutyramide (DMB) (4), dimethylpropionamide (DMP) (5), and diethylacetamide (DEA) (6), have been synthesized to enable a systematic study of the influence of structural perturbations on magnetic exchange and relaxation barrier. Across the series, varying the amide ligand leads to Fe–N–C bond angles ranging from 154.703(7)° in 1 to 180° in 6. Variable-temperature dc magnetic susceptibility data indicate ferromagnetic exchange coupling in all compounds, with the strength of exchange increasing linearly, from J = +4.2(2) cm−1 to +7.2(3) cm−1, with increasing Fe–N–C bond angle. Ac magnetic susceptibility data collected as a function of frequency reveal that the relaxation barrier of the chain compounds rises steeply with increasing exchange strength, from 45 cm−1 to 93 cm−1. This examination demonstrates that subtle tuning of orbital overlap, and thus exchange strength, can engender dramatic changes in the relaxation barrier. Indeed, the perfectly linear Fe–N–C bond angle in 6 leads to one of the highest barriers and coercive fields yet observed for a single-chain magnet.

Solvothermal synthesis, structure and properties of a new 3-D anionic porous framework

A new three-dimensional porous Zinc(II) metal-organic framework [NH 2 Et 2 ][Zn(BTC)]·H 2 O ( 1 ) was synthesized by the self-assembly of 1,3,5-benzenetricarboxy acid (H 3 BTC) and Zn(II) salt in diethylformamide (DEF), and characterized by single-crystal X-ray structure determination, thermogravimetric analysis and X-ray powder diffraction studies. The adsorption behavior shows that compound 1 has selective adsorption capacities of CO 2 over N 2 after the removal of the water molecules within the pores. A novel 3D Zn(II) coordination polymer, [NH 2 Et 2 ][Zn(BTC)]·0.5H 2 O ( 1 ) [BTC = 1,3,5-benzenetricarboxylate], has been solvothermally synthesized and characterized. Complex 1 shows a rare rtl topology net with selective adsorption capacities of CO 2 over N 2 . ► Three-dimensional anionic coordination framework. ► Solvothermal synthesis effect on formation and structure of the anionic metal-organic framework. ► Selective sorption behavior of CO 2 over N 2 .

Desorption of dimethylformamide from Zn4O(C8H4O4)3 framework

Both dimethylformamide (DMF) and diethylformamide (DEF) are important solvents for the synthesis of Zn4O(C8H4O4)3 framework (MOF-5). It is generally recognized that DMF molecules can be completely displaced by CH2Cl2 during the synthesis of MOF-5. Herein, however, it was found that the DMF molecules inside the pores of the MOF-5 framework cannot be displaced by CH2Cl2. The desorption of the DMF molecules from the pores, which requires a temperature of 100°C or above, is the first order with activation energy of 56.38kJ/mol. In contrast, DEF molecules can be completely displaced by CH2Cl2 during the synthesis of MOF-5, because DEF molecules cannot penetrate into the pores of the MOF-5 paste.

Facile synthesis of MOF-177 by a sonochemical method using 1-methyl-2-pyrrolidinone as a solvent

High quality MOF-177 crystals in the size range of 5-20 microm were successfully synthesized via a sonochemical route in a substantially reduced synthesis time (40 min) in the presence of low-cost NMP (1-methyl-2-pyrrolidone) as a solvent. Microwave heating in NMP also produced MOF-177 under similar conditions (35 min, 5-50 microm) but exhibited inferior crystallinity. In comparison, a conventional solvothermal route in DEF (diethylformamide) took 48 h to produce MOF-177 crystals 0.5-1.5 mm in size. The BET surface areas of the MOF-177 samples decreased in the order of sonochemical (4898 m(2) g(-1)) > conventional (4833 m(2) g(-1)) > microwave route (4197 m(2) g(-1)). In line with this trend, MOF-177 prepared via the sonochemical route resulted in the highest CO(2) adsorption capacity, 1315 mg g(-1) at 30 bar and 298 K. The product yield of MOF-177 synthesized via the sonochemical route was 95.6%, and was significantly higher than the product yields of other methods.