Solvothermal synthesis and efficient visible light-driven photocatalytic property of 2-D iodoargentate hybrid directed by solvated Fe(III) cation

Solvothermal synthesis and efficient visible light-driven photocatalytic property of 2-D iodoargentate hybrid directed by solvated Fe(III) cation | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Solvothermal synthesis and efficient visible light-driven photocatalytic property of 2-D iodoargentate hybrid directed by solvated Fe(III) cation Hongjin Zhu, Dingxian Jia This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-8885980/v1 This work is licensed under a CC BY 4.0 License Status: Under Review Version 1 posted 4 You are reading this latest preprint version Abstract A Fe(III)-iodoargentate hybrid [Fe(DMSO) 6 ]Ag 10 I 13 ( 1 ) (DMSO = dimethyl sulfoxide) was prepared using a solvated Fe(III) complex cation [Fe(DMSO) 6 ] 3+ formed in-situ as the template under solvothermal conditions. It consists of a [Fe(DMSO) 8 ] 3+ complex cation and a 2-D [Ag 10 I 13 ] n 3n‒ layered anion. The 2-D [Ag 10 I 13 ] n 3n‒ anion is composed of ten crystallographically independent AgI 4 tetrahedral units through corner- and edge-sharing, which contains large circles of Ag 7 I 7 with cross sectional dimensions of 7.285 Å × 8.592 Å. Compound 1 exhibits rapid photocurrent response with steady current density of 4.83 µA·cm − 2 after e under visible light irradiation. It shows high photocatalytic activities in the degradation of MB with degradation ratio of 98.8% after light irradiation of 60 min. Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Introduction Nowadays, the problem of water pollution caused by organic pollutants has drawn growing global attention with the development of economy, industry and agriculture [ 1 , 2 ]. The solar-driven photocatalytic technology is an environmentally friendly method in which sunlight energy is used to convert pollutants into small molecules or nontoxic substances. This method is considered an effective and economical solution for the degradation of organic pollutants in wastewater [ 3 – 5 ]. The design and synthesis of new efficient photocatalysts with greater charge separation under light irradiation has become a key breakthrough to improve the efficiency for the degradation of pollutants [ 6 ]. In recent years, the iodoargentate hybrids, which is an important branch of metal-based inorganic-organic hybrid materials, has attracted increasing attention because of their potential applications in photodegradation of organic pollutants in wastewater treatment. The iodoargentate hybrid with organic counter cation, [Me 3 TPA][Ag 5 I 8 ] (TPA = tri(pyridin-4-yl)amine), exhibited effectively photocatalytic property in the degradation of organic dye methyl violet (MV) with degradation rate of 89% after visible light irradiation of 40 min [ 7 ]. The iodoargentates hybrids containing metal complex cations, [TM(phen) 3 ]Ag 2 I 4 ·DMF, [TM(phen) 3 ] 2 Ag 8 I 12 ·7DMF (TM = Co, Ni, Zn, phen = 1,10-phenanthroline, DMF = N,N-dimethylformamide), [Mn(2,2'-bipy) 2 (DMF) 2 ]Ag 5 I 7 , and [{Zn(DMF) 2 (H 2 O) 2 }(4,4'-bipy) 1.5 ]Ag 5 I 7 ·2DMF (4,4'-bipy = 4,4'-bipyridine) showed catalytic activities in the photodegradation of crystal violet (CV) with approximately degradation rates of 85%-95%, 76–93% and 90–93%, after visible light irradiation of 180 and 360 min, respectively [ 8 , 9 ]. The iodoargentates hybrids containing lanthanide(III) complex cations, [{Nd(DMSO) 8 }(Ag 7 I 10 )] n (DMSO = dimethylsulfoxide) and [Ln(DMA) 7 ] 2 Ag 16 I 22 (Ln = Pr, Sm, DMA = N, N-dimethylacetamide) were catalytically active in the photodegradation of methylene blue (MB) and CV with MB degradation rate of 95.8% after 80 min light irradiation, and CV degradation rates of 80.3% and 86.9% after 210 min light irradiation, respectively [ 10 , 11 ]. The compositions, structures and photocatalytic properties of organic-inorganic halometallate hybridsare influenced by various factors during preparation, such as the structure-directing agents (SDAs), the features and charge distributions of counter cations, and synthetic solvents [ 12 ]. A large number of iodoargentate aggregates with different compositions and structures had been prepared by using organic cations, transition metal (TM) or lanthanide (Ln) metal complex cations as counter cations or SDAs by solvothermal, extracting or diffusing methods in organic solvent. The recent examples include [AgI 2 ] − [ 13 ], [Ag 2 I 3 ] − [ 13 , 14 ], [Ag 2 I 4 ] 2− [ 14 , 15 ], [Ag 3 I 6 ] 3− [ 16 ], [Ag 4 I 7 ] 3− [ 17 ], [Ag 5 I 6 ] − [ 18 ], [Ag 5 I 7 ] 2− [ 19 ] and [Ag 5 I 8 ] 3− [ 7 ]. Considering that the iodoargentates are subtly affected by the organic ligand of and solvent, the reaction of AgI, KI and Fe 2 (SO 4 ) 3 was investigated in a mixed solvent of C 2 H 5 OH/DMSO under solvothermal conditions, and a Fe(III)-iodoargentate hybrid [Fe(DMSO) 6 ]Ag 10 I 13 ( 1 ) was prepared. The [Ag 10 I 13 ] 3− represent a new binary iodoargentate aggregate. Herein, the synthesis, crystal structure, and photoelectric and photocatalytic properties of compound 1 were reported. Experimental Section Materials and physical measurements Chemicals AgI, KI, Fe 2 (SO 4 ) 3 , methylene blue (MB), dimethyl sulfoxide (DMSO), and anhydrous ethanol were purchased from McLean Chemical Reagents Co., Ltd. (Shanghai, China). All of the chemicals in the experimental process were of analytical grade and were used without any further purification. Elemental analyses for C, H and N were carried out on a Perkin-Elmer 2400 analyzer. Fourier transform infrared (FT-IR) spectra were recorded with a Nicolet Magna-IR 550 spectrometer in dry KBr discs over the 4000 − 400 cm − 1 range. Powder X-ray diffraction (PXRD) data of the as-prepared samples were collected on a D/MAX-3 C-type X-ray diffractometer using Cu-Kα radiation ( λ = 1.5406 Å). Optical diffuse reflectance spectra of powder samples were obtained at room temperature using a Shimadzu UV-3150 spectrometer. Absorption ( α / S ) data were calculated from the reflectance using the Kubelka−Munk function α / S = (1 − R ) 2 /2 R [ 20 ]. Syntheses of [Fe(DMSO)]AgI (1) AgI (47 mg, 0.2 mmol), KI (66 mg, 0.40 mmol) and Fe 2 (SO 4 ) 3 (16 mg, 0.04 mmol) were put in a thick-walled Pyrex glass tube with a length of approximately 15 cm, and then 1.0 mL of C 2 H 5 OH and 0.5 mL of DMSO were added to the glass tube. After the mixture was ultrasonically dispersed for 10 min, the glass tube was sealed, heated at 90°C for 3 days. After naturally cooled to room temperature, red block crystals were obtained in the tube. The crystals were collected by filtration, washed with ethanol, and stored in a vacuum dryer. Yield: 44 mg (68% yield based on AgI). Elemental analysis calcd for C 12 H 36 O 6 S 6 FeAg 10 I 13 : C, 4.43; H, 1.12%. Found: C, 4.29; H, 1.08%. IR data (KBr, cm − 1 ): 2987 (w), 2907 (w), 1400 (m), 1004 (vs), 948 (s), 938 (s), 710 (w), 403 (m). X-ray single crystal structure determination The intensity data were collected with a Rigaku Saturn CCD diffractometer at 296(2) K using graphite-monochromated Mo- K α radiation (λ = 0.71073 Å) with an ω -scan method to a maximum 2 θ value of 50.70°. An empirical absorption correction was applied for all of the compounds using multi-scan. Structures were solved with direct methods by using the program SHELXS-2015, and refined by a full matrix least-squares technique against F 2 using SHELXL-2015 [ 21 ]. The atoms Ag(2) and Ag(9) are slightly disordered, which both were refined as 90% and 10% occupancies. The disordered atom S3 was refined as 50% and 50% occupancies. All the non-hydrogen atoms were refined anisotropically. The hydrogen atoms were positioned with idealized geometry and refined using the riding model. Technical details of data acquisition and selected refinement results are listed in Table S1 , and the selected bond lengths and angles of 1 are listed in Table S2 the Supplementary Information. Photocurrent response measurement. The photocurrent response behavior of the samples was determined in a standard three-electrode cell using a CHI760E electrochemical workstation, using a platinum wire and a saturated calomel electrode (SCE) as auxiliary and reference electrodes. The sample-coated ITO glass was used as the working electrode. 0.1mol·L − 1 Na 2 SO 4 solution is the support solution. The light source was a 180 W high-pressure xenon lamp, about 20 cm from the surface of the ITO electrode. The prepared pure compounds were coated on ITO glass sheets, and one end was covered with conductive glue as the working electrode. 0.1 mol·L − 1 Na 2 SO 4 solution was used as the support solution. Photocatalytic experiment. The photocatalytic activities of the samples were evaluated by the photodegradation of organic dye methylene blue (MB) in under visible light irradiation of a 180 W Xe lamp with a 400nm cut-off filter. The catalytic reaction was kept at room temperature in a water bath by using circulating water. In the photocatalytic reaction, powder samples (25 mg) were added to 50 mL of aqueous MB solution (1×10 ‒5 mol·L ‒1 ). The mixture was magnetically stirred in the dark for 30 min to establish adsorption equilibrium between the catalyst and solution. Then, the mixture was exposed to visible light irradiation for photodegradation under stirring. Every 10 min, about 5 mL of suspension was taken from the reaction vessel for UV-vis absorption spectra measurement after centrifugation. The UV-Vis-NIR absorption spectra of the resulting solutions were obtained a PE Lambda 35 UV/Vis spectrophotometer. Results and discussion Syntheses and IR spectra Compound 1 was prepared by the reaction of AgI, KI and Fe 2 (SO 4 ) 3 in a mixed solvent of C 2 H 5 OH/DMSO at 90°C for 3 days. The solvated complex cation [Fe(DMSO) 6 ] 3+ acts as the counterion to the iodoargentate anion in the final product. The solvent C 2 H 5 OH played an important role in the crystalization of title compound. In the synthesis of compound 1 , when pure DMSO was used as the solvent instead of the C 2 H 5 OH/DMSO mixed solvent, only a clear solution was obtained and no crystals were produced after solvothermal reaction due to the high solubility of compound 1 in DMSO. In the FT-IR spectrum of 1 , the vibration of the C–H bond is located in the range of 2987–2907 cm -1 . The absorption bands approximately at 1004 cm -1 and 948 cm -1 are attributed to the stretching vibrations S = O and C − S bonds of DMSO (Fig. S1 ), respectively. The PXRD patterns of the bulk phase of 1 were consistent with the simulated PXRD patterns based on the single-crystal XRD data (Fig. S2 ), indicating that the bulk phase of the as-prepared compound 1 was pure. Crystal structure X-ray single-crystal structure determination showed that compound 1 crystallizes in the monoclinic space group P 2 1 / c with four molecular units in the unit cell (Table S1 ). It consists of octahedral complex cation [Fe(DMSO) 6 ] 3+ and 2-D polymeric iodoargentate anion [Ag 10 I 13 ] n 3n– . The Fe 3+ ion was solvated by six DMSO molecules to form a hexakis-DMSO Fe(III) complex cation [Fe(DMSO) 6 ] 3+ to act the counter ion of the polymeric anion [Ag 10 I 13 ] n 3n– in the solvothermal synthesis (Fig. 2 a). The atom S3 is disordered, which was refined as 50% and 50% occupancies. The complex cation [Fe(DMSO) 6 ] 3+ is in a distorted octahedral geometry with equatorial and axial O−Fe−O angles in the range of 87.7(2)−91.7(2)° and 176.5(2)−179.0(2)° (Table S2 ), respectively. The Fe–O bond lengths are in the range of 1.981(6)−2.032(6) Å, which are consistent with those of reported Fe(III) complexes of DMSO ligands [ 22 ]. The 2-D polymeric anion [Ag 10 I 13 ] n 3n– is composed of ten crystallographically independent Ag + and thirteen I − ions (Fig. 2 b). All of the Ag + ions are coordinated by four I − ions with Ag–I distances ranging from 2.7424(10) Å to 3.234(11) Å, forming AgI 4 acting as the primarily building units (PBUs). All these AgI 4 PBUs are in approximately tetrahedral geometries with I–Ag–I angles in the range of 91.14(3)–123.80(3)° (Table S2 ). The Ag–I lengths and I–Ag–I angles are consistent with the corresponding values observed in 2-D iodoargentate anions [Ag 6 I 11 ] n 5n– and [Ag 7 I 10 ] n 3n– [ 23 , 24 ]. The ten crystallographically independent AgI 4 PBUs are connected via corner- or edge-sharing, forming the asymmetric structural unit Ag 10 I 13 . The Ag 10 I 13 units are interconnected via sharing I2, I7, I11 and I13 atoms to form the 2-D layered anion [Ag 10 I 13 ] n 3n– (Fig. 2 b). In the [Ag 10 I 13 ] n 3n– layer, large circles of Ag 7 I 7 with cross sectional dimensions of 7.285 Å × 8.592 Å are formed (Fig. S3 ). In the [Ag 10 I 13 ] n 3n– anion, the I atoms adopt µ 2 -I (I3, I8, I9, I12), µ 3 -I (I2, I5, I7, I13) and µ 4 -I (I1, I4, I6, I10, I11) bridging coordination modes. As expected, the Ag–I bond distances fall in the decreasing order of Ag–µ 4 -I (2.9189 Å) > Ag–µ 3 -I (2.8403 Å) > Ag–µ 2 -I (2.7688 Å). Short Ag⋯Ag distances in the range of 2.912(15)‒3.295(2) Å are observed in the [Ag 10 I 13 ] n 3n– anion. The Ag⋯Ag distances are less than the sum of the van der Waals radii of Ag − Ag (3.44 Å) [ 25 ], indicating metal–metal interactions [ 26 ]. The [Ag 10 I 13 ] n 3n– layers are stacked parallel to form channels running along the a -axis (Fig. 3 a). The [Fe(DMSO) 8 ] 3+ cations are located between the [Ag 10 I 13 ] n 3n– layers, and are arranged in arrays along the channels (Fig. 3 b). The characteristic of iodoargentates is that the AgI 4 and/or AgI 3 PBUs can easily copolymerize to form various iodoargentate aggregates in the presence of different kinds of structural directing agents (SDAs) because of the strong affinity of Ag(I) for the iodide ion. The structures of iodoargentate aggregates can be further tuned by the nature of the metal ion and the organic ligands to the metal ion when metal complex cation was used as the SDA. Using the hexakis solvated transition metal(TM) complex cations as the SDAs, a series of binary iodoargentate anions with Ag/I molar ratios in the range of 0.667–0.750 and different dimensions had been prepared (Table 1 ). The [Ni(DMSO) 6 ] 2+ complex cation resulted in the 1-D anion [Ag 5 I 7 ] 2– in DMSO/H 2 O solvent, while the hexakis complex cation [V(DMSO) 5 (H 2 O)] 2+ with mixed solvation ligand led to formation of a 3-D anion [Ag 6 I 8 ] 2– in the same solvent [ 27 ]. The trivalence [Cr(DMSO) 6 ] 3+ produced a 1-D polymric anion [Ag 6 I 9 ] n 2n– under the same synthetic conditions [ 27 ]. The DMSO-solvated lanthanide complex cations, which led to formation of iodoargentate anions with Ag/I molar ratios in the range of 0.400–0.700 (Table 1 ), exhibited different structural directing effect from the TM complex cations on the formation of iodoargentate aggregates. The trivalence lanthanide complex cations [Ln(DMSO) 8 ] 3+ (Ln = La, Ce), [Ln(DMSO) 8 ] 3+ (Ln = Eu, Tb, Dy) and [Yb(DMSO) 7 ] 3+ led to the iodoargentate anions of 0-D cluster [Ag 22 I 34 ] 12− , 2-D layer [Ag 7 I 10 ] 3– , and 1-D chain [Ag 5 I 8 ] 3– , respectively [ 28 ], whileas the [Tb(DMSO) 8 ] 3+ gave a iodoargentate that contains both 0-D [Ag 2 I 5 ] 3– and 2-D [Ag 5 I 8 ] 3– anions [ 24 , 29 ]. In this work, the hexakis Fe(III) complex cation [Fe(DMSO) 6 ] 3+ afforded a novel 2-D iodoargentate anion [Ag 10 I 13 ] 3– with a higher Ag/I ratio of 0.769, which is a new member of iodoargentate anion with layered structure. As a result, the compositions and dimensions of the iodoargentates are affected by the ionic radius, valence state, and type of the metal ions when the metal-DMOS complex cations were used as the templates in the syntheses of iodoargentate hybrids. Table 1 A summary of the dimensions and Ag/I molar ratios of the iodoargentate anions templated by DMSO-solvated metal complex cations Compound Iodoargentate Dimension Ag/I ratio Ref. [Ni(DMSO) 6 ]Ag 5 I 7 [Ag 5 I 7 ] 2– 1-D 0.714 27 [Cr(DMSO) 6 ]Ag 6 I 9 ·H 2 O [Ag 6 I 9 ] 3– 1-D 0.667 [V(DMSO) 5 (H 2 O)]Ag 6 I 8 [Ag 6 I 8 ] 2– 3-D 0.750 [Fe(DMSO) 6 ]Ag 10 I 13 [Ag 10 I 13 ] 3– 2-D 0.769 this work [Yb(DMSO) 7 ]Ag 5 I 8 [Ag 5 I 8 ] 3– 1-D 0.625 28 [Ln(DMSO) 8 ]Ag 7 I 10 (Ln = Eu, Tb, Dy) [Ag 7 I 10 ] 3– 1-D 0.700 [La(DMSO) 8 ] 4 Ag 22 I 34 ·2H 2 O [Ag 22 I 34 ] 12– 0-D 0.647 [Ln(DMSO) 8 ](Ag 2 I 5 )(Ag 5 I 8 ) (Ln = Eu, Tb) [Ag 2 I 5 ] 3– 0-D 0.400 24, 29 [Ag 5 I 8 ] 3– 2-D 0.625 Solid-state UV-vis reflectance spectra and optical band gaps The solid-state UV-Vis-NIR diffuse reflectance spectrum showed that compound 1 exhibited sensitive light reflection properties in the visible light range. It had almost no diffuse reflection signals in near-infrared region (Fig. 4 a). The reflectance data were converted to absorption spectrum by the Kubelka-Munk function F ( R ) = (1– R ) 2 /2 R [ 20 ], which was shown in Fig. 4 b. Compound 1 exhibited steep absorption edge. Extrapolating the tangent drawn from the steep absorption edge to the energy axis yielded the intercept value of 1.80 eV (Fig. 4 b), which is corresponding to the band gap ( E g ) of compound 1 . Compound 1 exhibited distinct redshift in the absorption edges in comparison with bulk AgI (zinc-blend structure, E g : ~2.40 eV) [ 30 ]. The band gap of compound 1 is comparable to those of the iodoargentate hybrids with organic cations [(BV) 2 (Ag 5 I 9 )] n (BV 2+ = benzyl viologen) ( E g = 1.76 eV) [ 31 ], (H 2 dpe) 0.5 (β-AgI 2 ) (dpe = 1,2-di(4-pyridyl)ethylene) ( E g = 1.99 eV) [ 32 ]. It is smaller than those of the TM(II)-containing iodoargentate hybrids [Cr(DMSO) 6 ]Ag 6 I 9 ·H 2 O ( E g = 3.33 eV), [Ni(DMSO) 6 ]Ag 5 I 7 ( E g = 2.73 eV) and [V(DMSO) 5 (H 2 O)]Ag 6 I 8 ( E g = 2.61 eV) [ 27 ], and Ln(III)-containing iodoargentate hybrids [La(DMSO) 8 ] 4 Ag 22 I 34 ·2H 2 O ( E g = 3.30 eV), [Ln(DMSO) 8 ]Ag 7 I 10 [ E g = 2.91 eV (Eu), 3.05 eV (Tb), 2.84 eV (Dy)], and [Yb(DMSO) 7 ]Ag 5 I 8 ( E g = 3.32 eV) [ 28 ], and [Ln(DMSO) 8 ] 2 [Ag 2 I 5 ][Ag 5 I 8 ] [ E g = 3.33 eV (Eu), 3.34 eV (Tb)] [ 24 ]. The band gap of compound 1 is also lower than those of the iodoargentate hybrids containing TM(II) complex with conjugated organic ligands, such as [TM(2,2'-bipy) 3 ]Ag 5 I 7 (2,2'-bipy = 2,2'-bipyridine) [ E g = 1.94 eV (Co), 2.10 eV (Ni), 2.58 eV(Zn)] [ 33 ]. Photocurrent response and photocatalytic properties The photocurrent response of compound 1 under visible light irradiation was investigated on a CHI760E electrochemical workstation with a standard three-electrode system at room temperature. Compound 1 was photosensitive to visible light, and showed rapid photoelectric response under visible light irradiation at room temperature. As shown in Fig. 5 a, its photocurrent densities increased sharply when light was turned on, and immediately dropped to approximately zero once the light was turned off. Under light illumination of a Xe lamp with a power of 180 W, the photocurrent densities of compound 1 was 5.75 µA·cm − 2 in the first on/off switch, and stabilized at 4.83 µA·cm − 2 after eight on/off switch cycles, which exhibited good reproduciblity in photocurrent responses. Compound 1 exhibit higher photocurrent densities than do the Ln(III)-containing iodoargentate hybrids {[Ln 2 (dpdo)(DMF) 14 ](Ag 12 I 18 )} n (bpdo = 4,4'-bipyridine N,N'-dioxide, Ln = La, Nd, Sm), whose current intensities are 0.2 µA, 0.125 µA and 0.25 µA [ 34 ], respectively. The catalytic activity of compound 1 was evaluated by the photocatalytic degradation of methylene blue (MB), which is an organic dye commonly used in industry, in an aqueous solution at room temperature under visible-light irradiation of a Xe lamp in the presence of air. The concentration of MB was monitored by the changes in the absorption intensity at the maximum absorption wavelength of 665 nm in the UV–Vis spectrum (Fig. 5 b). The degradation activity of MB over compound 1 was expressed as C / C 0 , where C 0 and C are the initial and instantaneous concentrations of MB, respectively. As shown in Fig. 5 b, the absorption peak of MB solution decreased rapidly with the increase of irradiation time. After 60 min of light irradiation, the MB solution became colorless in the presence of compound 1 , and the degradation conversion of MB reached 98.8% (Fig. 5 c). Comparatively, approximately 11% of MB was degraded in the blank experiment after 60 min of light irradiation. The plot of Ln( C 0 / C ) against the irradiation time t fits the formula Ln( C 0 / C ) = k t, indicating that the photodegradation reaction catalyzed by 1 conforms to first-order kinetics (Fig. 5 d). The kinetic rate constant k of the degradation reaction is 0.0712 min − 1 . The photocatalytic activity of 1 for MB photodegradation is higher than those of the haloargentate hybrids {([syn/anti-did](Ag 2 I 4 )} (did 2+ = (1 2 z,5 2 z)-1 1 H,5 1 H-1,5(1,3)-diimidazol-3-iuma-3,7(1,2)-dibenzenacyclooctaphane-1 3 ,5 3 -diium) (20.2% of MB in 150 min) [ 35 ], and {(bmpp)[Ag 4 I 6 ]} n (bmpp = 1,3-bis(4-methylpyridine)alkane cation) (37% of MB in 150 min) [ 36 ]. Conclusions In conclusion, an effective organic-inorganic photocatlyst 1 based on iodoargentate was prepared using a solvated Fe(III) complex cation [Fe(DMSO) 6 ] 3+ formed in-situ as the template under solvothermal condition. The 2-D [Ag 10 I 13 ] n 3n‒ layered anion with Ag/I molar ratio of 0.769 is a new member of binary iodoargentate aggregates. Compound 1 exhibit effectively photocatalytic activity in the degradation of the organic dye MB in aqueous solution at room temperature. The results showed that it was possible to design and prepare photocatalyst based iodoargentate hybrid using TM complex cation as the template. Further studies on constructing new halometallate hybrid materials are ongoing. Declarations Author s contributions HZ and DJ wrote the main text of the manuscript, DJ prepared Figures 1 to 3, ZJ prepared the Figures 4 and 5, and performed x-ray diffraction studies and physical measurements. All authors reviewed the manuscript. Funding This work was supported by the National Natural Science Foundation of China (No. 21171123, 20771077). Data availability No datasets were generated or analysed during the current study. Competing interests The authors declare no competing interests. Supplementary Information. The online version contains supplementary materials available at https://doi.org/10.1007 CCDC-2528821 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via [email protected] or http://www.ccdc.cam. ac.uk/data_request/cif. References Sharma VK, Ma XM, Zboril R (2023) Single atom catalyst-mediated generation of reactive species in water treatment. Chem Soc Rev 52:7673–7686 Sánchez BJ, Wang J (2018) Micromotors for environmental applications: a review. Environ Sci Nano 5:1530–1544 Kou JH, Lu CH, Wang J, Chen YK, Xu ZZ, Varma RS (2017) Selectivity enhancement in heterogeneous photocatalytic transformations. 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J Phys Chem B 68:441–451 Singh K, Long JR, Stavropoulos P (1997) Ligand-unsupported metal-metal (M = Cu, Ag) interactions between closed-shell d 10 trinuclear systems. J Am Chem Soc 119:2942–2943 Mu Y, Wang D, Meng XD, Pan J, Han SD, Xue ZZ (2020) Construction of iodoargentates with diverse architecture: template syntheses, structures, and photocatalytic properties. Cryst Growth Des 20:1130–1138 Shen YL, Zhang LM, Sun PP, Liu SZ, Jiang WQ, Jia DX (2018) Iodoargentates from clusters to 1D chains and 2D layers induced by solvated lanthanide complex cations: syntheses, crystal structures, and photoluminescence properties. CrystEngComm 20:520–528 Mishra S, Jeanneau E, Ledoux G, Daniele S (2009) Lanthanide complexes in hybrid halometallate materials: interconversion between a novel 2D microporous framework and a 1D zigzag chain structure of iodoargentates templated by octakis-solvated terbium(III) cation. Dalton Trans 25:4954–4961 Pedersen DB, Wang SL (2007) Iodination of gas-phase-generated Ag nanoparticles: behavior of the two spin orbit components of the AgI exciton in Ag@AgI core-shell nanoparticles. J Phys Chem C 111:1261–1267 Chen QY, Cheng X, Wang T, Yu ZH, Zhang C, Lin SK, Li HH, Chen ZR (2014) A low-dimensional viologen/iodoargentate hybrid [(BV) 2 (Ag 5 I 9 )] n : structure, properties, and theoretical study. Z Anorg Allg Chem 640:439–443 Liu GN, Liu LL, Chu YN, Sun YQ, Zhang ZW, Li CC (2015) Different contributions of aliphatic and conjugated organic cations to both the crystal and electronic structures: three hybrid iodoargentates showing two isomers of the (AgI 2 ) – Chain. Eur J Inorg Chem 3:478–487 Lei XW, Yue CY, Wu F, Jiang XY, Chen LN (2017) Syntheses, crystal structures and photocatalytic properties of transition metal complex directed iodoargentates: [TM(2,2-bipy) 3 ]Ag 5 I 7 . Inorg Chem Commun 77:64–67 Wang DH, Zhao LM, Lin XY, Wang YK, Zhang WT, Song KY, Li HH, Chen ZR (2018) Iodoargentate/iodobismuthate-based materials hybridized with lanthanide-containing metalloviologens: thermochromic behaviors and photocurrent responses. Inorg Chem Front 5:1162–1173 Li YY, Xiao M, Wei DH, Niu YY (2019) Hybrid supramolecules for azolium-linked cyclophane immobilization and conformation study: synthesis, characterization, and photocatalytic degradation. ACS Omega 4:5137–5146 Liu M, Liang Y, Wang CH, Ma CJ, Niu YY (2015) Synthesis, structures and photocatalytic properties of two novel Ag(I) polymers directed by 1,3-Bis(4-methylpyridine)alkane cation. J Cluster Sci 26:1723–1733 Additional Declarations No competing interests reported. Supplementary Files SupplementaryInformation.docx Cite Share Download PDF Status: Under Review Version 1 posted Editorial decision: Revision requested 17 Feb, 2026 Editor assigned by journal 17 Feb, 2026 Submission checks completed at journal 17 Feb, 2026 First submitted to journal 15 Feb, 2026 You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. We do this by developing innovative software and high quality services for the global research community. Our growing team is made up of researchers and industry professionals working together to solve the most critical problems facing scientific publishing. Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-8885980","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":592659300,"identity":"26b29dff-803c-423a-ba93-06ac2134c9c4","order_by":0,"name":"Hongjin Zhu","email":"","orcid":"","institution":"Soochow University","correspondingAuthor":false,"prefix":"","firstName":"Hongjin","middleName":"","lastName":"Zhu","suffix":""},{"id":592659301,"identity":"322a2b3e-df0d-4737-b387-37bc1acf7c04","order_by":1,"name":"Dingxian Jia","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA+klEQVRIiWNgGAWjYBACxmYGBokEIIMNyH7AwMAMEjQgWguzAVFaQEACSrNJEKWFuZ354Y2HO2oT+9jPHqv82WYtz8DevE2CoeYOHoexGVsknjluzMaTl3abty3dsIHnWJkEw7Fn+PxiJpHYdkyOjSHH7DZj22HGBokcMwnGhsN4tLB/A2nhYeN/Y1b4s+2wfYP8G0JaeEC21MixAQ1n4G07nNggwUNQS7FFYtsBYzaJN8bSPOfSk9t40ootEo7h1mLYf3zjzZ9tdYnz+3MMP/4os7btZz+88caHGjxaGsAUkgI2EJGAUwMDgzyEqsOjZBSMglEwCkY8AAA3Jk4+Wz5ZoAAAAABJRU5ErkJggg==","orcid":"","institution":"Soochow University","correspondingAuthor":true,"prefix":"","firstName":"Dingxian","middleName":"","lastName":"Jia","suffix":""}],"badges":[],"createdAt":"2026-02-15 12:38:37","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-8885980/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-8885980/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":103504264,"identity":"6fb7f01e-05c7-4339-9ab8-52adf39dec86","added_by":"auto","created_at":"2026-02-26 13:18:48","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":81866,"visible":true,"origin":"","legend":"\u003cp\u003eCrystal structure of the complex cation [Fe(DMSO)\u003csub\u003e6\u003c/sub\u003e]\u003csup\u003e3+\u003c/sup\u003e of \u003cstrong\u003e1\u003c/strong\u003e with labeling scheme\u003c/p\u003e","description":"","filename":"image1.png","url":"https://assets-eu.researchsquare.com/files/rs-8885980/v1/7abc3d617ad828628fbe0cc3.png"},{"id":103503838,"identity":"ecaad72b-a8c3-42a5-8ee2-1233e99c6e88","added_by":"auto","created_at":"2026-02-26 13:02:59","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":458939,"visible":true,"origin":"","legend":"\u003cp\u003eStructural diagrams of \u003cstrong\u003e1\u003c/strong\u003e: asymmetric structural unit of the polymeric anion [Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e]\u003csub\u003en\u003c/sub\u003e\u003csup\u003e3n– \u003c/sup\u003ewith labeling scheme, showing the coordination environment of each Ag(I) ion (a), and the [Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e]\u003csub\u003en\u003c/sub\u003e\u003csup\u003e3n–\u003c/sup\u003e layer (b)\u003c/p\u003e","description":"","filename":"image2.png","url":"https://assets-eu.researchsquare.com/files/rs-8885980/v1/9e0728c19ac2ccb78c838113.png"},{"id":103508177,"identity":"064ef6d3-6699-4f70-ba1e-0b4ea5bb8430","added_by":"auto","created_at":"2026-02-26 13:47:23","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":921847,"visible":true,"origin":"","legend":"\u003cp\u003ePacking diagrams of \u003cstrong\u003e1\u003c/strong\u003e viewed along the \u003cem\u003ea\u003c/em\u003e (a) and \u003cem\u003eb\u003c/em\u003e (b) axes. The S, C and H atoms of DMSO are omitted for clarity. Cyan octahedron: FeO\u003csub\u003e6.\u003c/sub\u003e Yellow tetrahedron: AgI\u003csub\u003e4\u003c/sub\u003e\u003c/p\u003e","description":"","filename":"image3.png","url":"https://assets-eu.researchsquare.com/files/rs-8885980/v1/131daa8d2ff4baff25fbe8b0.png"},{"id":103064993,"identity":"5b0c2845-6e6b-401d-8fad-7aaa9d6198d6","added_by":"auto","created_at":"2026-02-20 11:07:41","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":80620,"visible":true,"origin":"","legend":"\u003cp\u003eSolid-state UV-Vis-NIR diffuse reflectance (a) and absorption (b) spectra of \u003cstrong\u003e1\u003c/strong\u003e\u003c/p\u003e","description":"","filename":"image4.png","url":"https://assets-eu.researchsquare.com/files/rs-8885980/v1/a0c744f63b71c3f210c3dc60.png"},{"id":103064997,"identity":"38cfa2a3-b772-4e20-ba2e-1c214b97a03f","added_by":"auto","created_at":"2026-02-20 11:07:41","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":197633,"visible":true,"origin":"","legend":"\u003cp\u003e(a)\u003cstrong\u003e \u003c/strong\u003ePhotocurrent response of compound \u003cstrong\u003e1\u003c/strong\u003e under visible light irradiation. (b) Time dependent absorption spectra of MB solutions with photodegradation catalyzed by compound \u003cstrong\u003e1\u003c/strong\u003e. (c) Photocatalytic activities over compound \u003cstrong\u003e1\u003c/strong\u003e and AgI in the degradation of MB. (d) Linear relationship of Ln(\u003cem\u003eC\u003c/em\u003e\u003csub\u003e0\u003c/sub\u003e/\u003cem\u003eC\u003c/em\u003e) versus reaction time over compound \u003cstrong\u003e1 \u003c/strong\u003ein the photodegradation of MB\u003c/p\u003e","description":"","filename":"image5.png","url":"https://assets-eu.researchsquare.com/files/rs-8885980/v1/2eae7ef9787b7b88e4f54329.png"},{"id":103510109,"identity":"a29e34b9-2014-43fc-a19d-43168b8be2e6","added_by":"auto","created_at":"2026-02-26 14:04:22","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":2489858,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-8885980/v1/6e859dbd-1e47-4d50-9e1d-b5d453fed4c7.pdf"},{"id":103064996,"identity":"68565fd9-dae0-404c-8322-ea222d443efb","added_by":"auto","created_at":"2026-02-20 11:07:41","extension":"docx","order_by":0,"title":"","display":"","copyAsset":false,"role":"supplement","size":452845,"visible":true,"origin":"","legend":"","description":"","filename":"SupplementaryInformation.docx","url":"https://assets-eu.researchsquare.com/files/rs-8885980/v1/83a1ee4079df927c569f0e70.docx"}],"financialInterests":"No competing interests reported.","formattedTitle":"Solvothermal synthesis and efficient visible light-driven photocatalytic property of 2-D iodoargentate hybrid directed by solvated Fe(III) cation","fulltext":[{"header":"Introduction","content":"\u003cp\u003eNowadays, the problem of water pollution caused by organic pollutants has drawn growing global attention with the development of economy, industry and agriculture [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e, \u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e]. The solar-driven photocatalytic technology is an environmentally friendly method in which sunlight energy is used to convert pollutants into small molecules or nontoxic substances. This method is considered an effective and economical solution for the degradation of organic pollutants in wastewater [\u003cspan additionalcitationids=\"CR4\" citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e]. The design and synthesis of new efficient photocatalysts with greater charge separation under light irradiation has become a key breakthrough to improve the efficiency for the degradation of pollutants [\u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e]. In recent years, the iodoargentate hybrids, which is an important branch of metal-based inorganic-organic hybrid materials, has attracted increasing attention because of their potential applications in photodegradation of organic pollutants in wastewater treatment. The iodoargentate hybrid with organic counter cation, [Me\u003csub\u003e3\u003c/sub\u003eTPA][Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e8\u003c/sub\u003e] (TPA\u0026thinsp;=\u0026thinsp;tri(pyridin-4-yl)amine), exhibited effectively photocatalytic property in the degradation of organic dye methyl violet (MV) with degradation rate of 89% after visible light irradiation of 40 min [\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e]. The iodoargentates hybrids containing metal complex cations, [TM(phen)\u003csub\u003e3\u003c/sub\u003e]Ag\u003csub\u003e2\u003c/sub\u003eI\u003csub\u003e4\u003c/sub\u003e\u0026middot;DMF, [TM(phen)\u003csub\u003e3\u003c/sub\u003e]\u003csub\u003e2\u003c/sub\u003eAg\u003csub\u003e8\u003c/sub\u003eI\u003csub\u003e12\u003c/sub\u003e\u0026middot;7DMF (TM\u0026thinsp;=\u0026thinsp;Co, Ni, Zn, phen\u0026thinsp;=\u0026thinsp;1,10-phenanthroline, DMF\u0026thinsp;=\u0026thinsp;N,N-dimethylformamide), [Mn(2,2'-bipy)\u003csub\u003e2\u003c/sub\u003e(DMF)\u003csub\u003e2\u003c/sub\u003e]Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e7\u003c/sub\u003e, and [{Zn(DMF)\u003csub\u003e2\u003c/sub\u003e(H\u003csub\u003e2\u003c/sub\u003eO)\u003csub\u003e2\u003c/sub\u003e}(4,4'-bipy)\u003csub\u003e1.5\u003c/sub\u003e]Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e7\u003c/sub\u003e\u0026middot;2DMF (4,4'-bipy\u0026thinsp;=\u0026thinsp;4,4'-bipyridine) showed catalytic activities in the photodegradation of crystal violet (CV) with approximately degradation rates of 85%-95%, 76\u0026ndash;93% and 90\u0026ndash;93%, after visible light irradiation of 180 and 360 min, respectively [\u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e, \u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e]. The iodoargentates hybrids containing lanthanide(III) complex cations, [{Nd(DMSO)\u003csub\u003e8\u003c/sub\u003e}(Ag\u003csub\u003e7\u003c/sub\u003eI\u003csub\u003e10\u003c/sub\u003e)]\u003csub\u003en\u003c/sub\u003e (DMSO\u0026thinsp;=\u0026thinsp;dimethylsulfoxide) and [Ln(DMA)\u003csub\u003e7\u003c/sub\u003e]\u003csub\u003e2\u003c/sub\u003eAg\u003csub\u003e16\u003c/sub\u003eI\u003csub\u003e22\u003c/sub\u003e (Ln\u0026thinsp;=\u0026thinsp;Pr, Sm, DMA\u0026thinsp;=\u0026thinsp;N, N-dimethylacetamide) were catalytically active in the photodegradation of methylene blue (MB) and CV with MB degradation rate of 95.8% after 80 min light irradiation, and CV degradation rates of 80.3% and 86.9% after 210 min light irradiation, respectively [\u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e, \u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e]. The compositions, structures and photocatalytic properties of organic-inorganic halometallate hybridsare influenced by various factors during preparation, such as the structure-directing agents (SDAs), the features and charge distributions of counter cations, and synthetic solvents [\u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e]. A large number of iodoargentate aggregates with different compositions and structures had been prepared by using organic cations, transition metal (TM) or lanthanide (Ln) metal complex cations as counter cations or SDAs by solvothermal, extracting or diffusing methods in organic solvent. The recent examples include [AgI\u003csub\u003e2\u003c/sub\u003e]\u003csup\u003e\u0026minus;\u003c/sup\u003e [\u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e], [Ag\u003csub\u003e2\u003c/sub\u003eI\u003csub\u003e3\u003c/sub\u003e]\u003csup\u003e\u0026minus;\u003c/sup\u003e [\u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e, \u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e14\u003c/span\u003e], [Ag\u003csub\u003e2\u003c/sub\u003eI\u003csub\u003e4\u003c/sub\u003e]\u003csup\u003e2\u0026minus;\u003c/sup\u003e [\u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e14\u003c/span\u003e, \u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e], [Ag\u003csub\u003e3\u003c/sub\u003eI\u003csub\u003e6\u003c/sub\u003e]\u003csup\u003e3\u0026minus;\u003c/sup\u003e [\u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e], [Ag\u003csub\u003e4\u003c/sub\u003eI\u003csub\u003e7\u003c/sub\u003e]\u003csup\u003e3\u0026minus;\u003c/sup\u003e [\u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e], [Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e6\u003c/sub\u003e]\u003csup\u003e\u0026minus;\u003c/sup\u003e [\u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e18\u003c/span\u003e], [Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e7\u003c/sub\u003e]\u003csup\u003e2\u0026minus;\u003c/sup\u003e [\u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e] and [Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e8\u003c/sub\u003e]\u003csup\u003e3\u0026minus;\u003c/sup\u003e [\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e]. Considering that the iodoargentates are subtly affected by the organic ligand of and solvent, the reaction of AgI, KI and Fe\u003csub\u003e2\u003c/sub\u003e(SO\u003csub\u003e4\u003c/sub\u003e)\u003csub\u003e3\u003c/sub\u003e was investigated in a mixed solvent of C\u003csub\u003e2\u003c/sub\u003eH\u003csub\u003e5\u003c/sub\u003eOH/DMSO under solvothermal conditions, and a Fe(III)-iodoargentate hybrid [Fe(DMSO)\u003csub\u003e6\u003c/sub\u003e]Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e (\u003cb\u003e1\u003c/b\u003e) was prepared. The [Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e]\u003csup\u003e3\u0026minus;\u003c/sup\u003e represent a new binary iodoargentate aggregate. Herein, the synthesis, crystal structure, and photoelectric and photocatalytic properties of compound \u003cb\u003e1\u003c/b\u003e were reported.\u003c/p\u003e"},{"header":"Experimental Section","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003eMaterials and physical measurements\u003c/h2\u003e \u003cp\u003eChemicals AgI, KI, Fe\u003csub\u003e2\u003c/sub\u003e(SO\u003csub\u003e4\u003c/sub\u003e)\u003csub\u003e3\u003c/sub\u003e, methylene blue (MB), dimethyl sulfoxide (DMSO), and anhydrous ethanol were purchased from McLean Chemical Reagents Co., Ltd. (Shanghai, China). All of the chemicals in the experimental process were of analytical grade and were used without any further purification. Elemental analyses for C, H and N were carried out on a Perkin-Elmer 2400 analyzer. Fourier transform infrared (FT-IR) spectra were recorded with a Nicolet Magna-IR 550 spectrometer in dry KBr discs over the 4000\u0026thinsp;\u0026minus;\u0026thinsp;400 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e range. Powder X-ray diffraction (PXRD) data of the as-prepared samples were collected on a D/MAX-3 C-type X-ray diffractometer using Cu-Kα radiation (\u003cem\u003eλ\u003c/em\u003e\u0026thinsp;=\u0026thinsp;1.5406 \u0026Aring;). Optical diffuse reflectance spectra of powder samples were obtained at room temperature using a Shimadzu UV-3150 spectrometer. Absorption (\u003cem\u003eα\u003c/em\u003e/\u003cem\u003eS\u003c/em\u003e) data were calculated from the reflectance using the Kubelka\u0026minus;Munk function \u003cem\u003eα\u003c/em\u003e/\u003cem\u003eS\u003c/em\u003e = (1\u0026thinsp;\u0026minus;\u0026thinsp;\u003cem\u003eR\u003c/em\u003e)\u003csup\u003e2\u003c/sup\u003e/2\u003cem\u003eR\u003c/em\u003e [\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e].\u003c/p\u003e \u003c/div\u003e\n\u003ch3\u003eSyntheses of [Fe(DMSO)]AgI (1)\u003c/h3\u003e\n\u003cp\u003eAgI (47 mg, 0.2 mmol), KI (66 mg, 0.40 mmol) and Fe\u003csub\u003e2\u003c/sub\u003e(SO\u003csub\u003e4\u003c/sub\u003e)\u003csub\u003e3\u003c/sub\u003e (16 mg, 0.04 mmol) were put in a thick-walled Pyrex glass tube with a length of approximately 15 cm, and then 1.0 mL of C\u003csub\u003e2\u003c/sub\u003eH\u003csub\u003e5\u003c/sub\u003eOH and 0.5 mL of DMSO were added to the glass tube. After the mixture was ultrasonically dispersed for 10 min, the glass tube was sealed, heated at 90\u0026deg;C for 3 days. After naturally cooled to room temperature, red block crystals were obtained in the tube. The crystals were collected by filtration, washed with ethanol, and stored in a vacuum dryer. Yield: 44 mg (68% yield based on AgI). Elemental analysis calcd for C\u003csub\u003e12\u003c/sub\u003eH\u003csub\u003e36\u003c/sub\u003eO\u003csub\u003e6\u003c/sub\u003eS\u003csub\u003e6\u003c/sub\u003eFeAg\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e: C, 4.43; H, 1.12%. Found: C, 4.29; H, 1.08%. IR data (KBr, cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e): 2987 (w), 2907 (w), 1400 (m), 1004 (vs), 948 (s), 938 (s), 710 (w), 403 (m).\u003c/p\u003e\n\u003ch3\u003eX-ray single crystal structure determination\u003c/h3\u003e\n\u003cp\u003eThe intensity data were collected with a Rigaku Saturn CCD diffractometer at 296(2) K using graphite-monochromated Mo-\u003cem\u003eK\u003c/em\u003eα radiation (λ\u0026thinsp;=\u0026thinsp;0.71073 \u0026Aring;) with an \u003cem\u003eω\u003c/em\u003e-scan method to a maximum 2\u003cem\u003eθ\u003c/em\u003e value of 50.70\u0026deg;. An empirical absorption correction was applied for all of the compounds using multi-scan. Structures were solved with direct methods by using the program SHELXS-2015, and refined by a full matrix least-squares technique against \u003cem\u003eF\u003c/em\u003e\u003csup\u003e2\u003c/sup\u003e using SHELXL-2015 [\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e]. The atoms Ag(2) and Ag(9) are slightly disordered, which both were refined as 90% and 10% occupancies. The disordered atom S3 was refined as 50% and 50% occupancies. All the non-hydrogen atoms were refined anisotropically. The hydrogen atoms were positioned with idealized geometry and refined using the riding model. Technical details of data acquisition and selected refinement results are listed in Table \u003cspan refid=\"MOESM1\" class=\"InternalRef\"\u003eS1\u003c/span\u003e, and the selected bond lengths and angles of \u003cb\u003e1\u003c/b\u003e are listed in Table \u003cspan refid=\"MOESM2\" class=\"InternalRef\"\u003eS2\u003c/span\u003e the Supplementary Information.\u003c/p\u003e \u003cp\u003e \u003cb\u003ePhotocurrent response measurement.\u003c/b\u003e \u003c/p\u003e \u003cp\u003eThe photocurrent response behavior of the samples was determined in a standard three-electrode cell using a CHI760E electrochemical workstation, using a platinum wire and a saturated calomel electrode (SCE) as auxiliary and reference electrodes. The sample-coated ITO glass was used as the working electrode. 0.1mol\u0026middot;L\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e Na\u003csub\u003e2\u003c/sub\u003eSO\u003csub\u003e4\u003c/sub\u003e solution is the support solution. The light source was a 180 W high-pressure xenon lamp, about 20 cm from the surface of the ITO electrode. The prepared pure compounds were coated on ITO glass sheets, and one end was covered with conductive glue as the working electrode. 0.1 mol\u0026middot;L\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e Na\u003csub\u003e2\u003c/sub\u003eSO\u003csub\u003e4\u003c/sub\u003e solution was used as the support solution.\u003c/p\u003e \u003cp\u003e \u003cb\u003ePhotocatalytic experiment.\u003c/b\u003e \u003c/p\u003e \u003cp\u003eThe photocatalytic activities of the samples were evaluated by the photodegradation of organic dye methylene blue (MB) in under visible light irradiation of a 180 W Xe lamp with a 400nm cut-off filter. The catalytic reaction was kept at room temperature in a water bath by using circulating water. In the photocatalytic reaction, powder samples (25 mg) were added to 50 mL of aqueous MB solution (1\u0026times;10\u003csup\u003e‒5\u003c/sup\u003e mol\u0026middot;L\u003csup\u003e‒1\u003c/sup\u003e). The mixture was magnetically stirred in the dark for 30 min to establish adsorption equilibrium between the catalyst and solution. Then, the mixture was exposed to visible light irradiation for photodegradation under stirring. Every 10 min, about 5 mL of suspension was taken from the reaction vessel for UV-vis absorption spectra measurement after centrifugation. The UV-Vis-NIR absorption spectra of the resulting solutions were obtained a PE Lambda 35 UV/Vis spectrophotometer.\u003c/p\u003e"},{"header":"Results and discussion","content":"\u003cdiv id=\"Sec7\" class=\"Section2\"\u003e \u003ch2\u003eSyntheses and IR spectra\u003c/h2\u003e \u003cp\u003eCompound \u003cb\u003e1\u003c/b\u003e was prepared by the reaction of AgI, KI and Fe\u003csub\u003e2\u003c/sub\u003e(SO\u003csub\u003e4\u003c/sub\u003e)\u003csub\u003e3\u003c/sub\u003e in a mixed solvent of C\u003csub\u003e2\u003c/sub\u003eH\u003csub\u003e5\u003c/sub\u003eOH/DMSO at 90\u0026deg;C for 3 days. The solvated complex cation [Fe(DMSO)\u003csub\u003e6\u003c/sub\u003e]\u003csup\u003e3+\u003c/sup\u003e acts as the counterion to the iodoargentate anion in the final product. The solvent C\u003csub\u003e2\u003c/sub\u003eH\u003csub\u003e5\u003c/sub\u003eOH played an important role in the crystalization of title compound. In the synthesis of compound \u003cb\u003e1\u003c/b\u003e, when pure DMSO was used as the solvent instead of the C\u003csub\u003e2\u003c/sub\u003eH\u003csub\u003e5\u003c/sub\u003eOH/DMSO mixed solvent, only a clear solution was obtained and no crystals were produced after solvothermal reaction due to the high solubility of compound \u003cb\u003e1\u003c/b\u003e in DMSO. In the FT-IR spectrum of \u003cb\u003e1\u003c/b\u003e, the vibration of the C\u0026ndash;H bond is located in the range of 2987\u0026ndash;2907 cm\u003csup\u003e-1\u003c/sup\u003e. The absorption bands approximately at 1004 cm\u003csup\u003e-1\u003c/sup\u003e and 948 cm\u003csup\u003e-1\u003c/sup\u003e are attributed to the stretching vibrations S\u0026thinsp;=\u0026thinsp;O and C\u0026thinsp;\u0026minus;\u0026thinsp;S bonds of DMSO (Fig. \u003cspan refid=\"MOESM1\" class=\"InternalRef\"\u003eS1\u003c/span\u003e), respectively. The PXRD patterns of the bulk phase of \u003cb\u003e1\u003c/b\u003e were consistent with the simulated PXRD patterns based on the single-crystal XRD data (Fig. \u003cspan refid=\"MOESM2\" class=\"InternalRef\"\u003eS2\u003c/span\u003e), indicating that the bulk phase of the as-prepared compound \u003cb\u003e1\u003c/b\u003e was pure.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec8\" class=\"Section2\"\u003e \u003ch2\u003eCrystal structure\u003c/h2\u003e \u003cp\u003eX-ray single-crystal structure determination showed that compound \u003cb\u003e1\u003c/b\u003e crystallizes in the monoclinic space group \u003cem\u003eP\u003c/em\u003e2\u003csub\u003e1\u003c/sub\u003e/\u003cem\u003ec\u003c/em\u003e with four molecular units in the unit cell (Table \u003cspan refid=\"MOESM1\" class=\"InternalRef\"\u003eS1\u003c/span\u003e). It consists of octahedral complex cation [Fe(DMSO)\u003csub\u003e6\u003c/sub\u003e]\u003csup\u003e3+\u003c/sup\u003e and 2-D polymeric iodoargentate anion [Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e]\u003csub\u003en\u003c/sub\u003e\u003csup\u003e3n\u0026ndash;\u003c/sup\u003e. The Fe\u003csup\u003e3+\u003c/sup\u003e ion was solvated by six DMSO molecules to form a hexakis-DMSO Fe(III) complex cation [Fe(DMSO)\u003csub\u003e6\u003c/sub\u003e]\u003csup\u003e3+\u003c/sup\u003e to act the counter ion of the polymeric anion [Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e]\u003csub\u003en\u003c/sub\u003e\u003csup\u003e3n\u0026ndash;\u003c/sup\u003e in the solvothermal synthesis (Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003ea). The atom S3 is disordered, which was refined as 50% and 50% occupancies. The complex cation [Fe(DMSO)\u003csub\u003e6\u003c/sub\u003e]\u003csup\u003e3+\u003c/sup\u003e is in a distorted octahedral geometry with equatorial and axial O\u0026minus;Fe\u0026minus;O angles in the range of 87.7(2)\u0026minus;91.7(2)\u0026deg; and 176.5(2)\u0026minus;179.0(2)\u0026deg; (Table \u003cspan refid=\"MOESM2\" class=\"InternalRef\"\u003eS2\u003c/span\u003e), respectively. The Fe\u0026ndash;O bond lengths are in the range of 1.981(6)\u0026minus;2.032(6) \u0026Aring;, which are consistent with those of reported Fe(III) complexes of DMSO ligands [\u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e]. The 2-D polymeric anion [Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e]\u003csub\u003en\u003c/sub\u003e\u003csup\u003e3n\u0026ndash;\u003c/sup\u003e is composed of ten crystallographically independent Ag\u003csup\u003e+\u003c/sup\u003e and thirteen I\u003csup\u003e\u0026minus;\u003c/sup\u003e ions (Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003eb). All of the Ag\u003csup\u003e+\u003c/sup\u003e ions are coordinated by four I\u003csup\u003e\u0026minus;\u003c/sup\u003e ions with Ag\u0026ndash;I distances ranging from 2.7424(10) \u0026Aring; to 3.234(11) \u0026Aring;, forming AgI\u003csub\u003e4\u003c/sub\u003e acting as the primarily building units (PBUs). All these AgI\u003csub\u003e4\u003c/sub\u003e PBUs are in approximately tetrahedral geometries with I\u0026ndash;Ag\u0026ndash;I angles in the range of 91.14(3)\u0026ndash;123.80(3)\u0026deg; (Table \u003cspan refid=\"MOESM2\" class=\"InternalRef\"\u003eS2\u003c/span\u003e). The Ag\u0026ndash;I lengths and I\u0026ndash;Ag\u0026ndash;I angles are consistent with the corresponding values observed in 2-D iodoargentate anions [Ag\u003csub\u003e6\u003c/sub\u003eI\u003csub\u003e11\u003c/sub\u003e]\u003csub\u003en\u003c/sub\u003e\u003csup\u003e5n\u0026ndash;\u003c/sup\u003e and [Ag\u003csub\u003e7\u003c/sub\u003eI\u003csub\u003e10\u003c/sub\u003e]\u003csub\u003en\u003c/sub\u003e\u003csup\u003e3n\u0026ndash;\u003c/sup\u003e [\u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e, \u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e]. The ten crystallographically independent AgI\u003csub\u003e4\u003c/sub\u003e PBUs are connected via corner- or edge-sharing, forming the asymmetric structural unit Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e. The Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e units are interconnected via sharing I2, I7, I11 and I13 atoms to form the 2-D layered anion [Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e]\u003csub\u003en\u003c/sub\u003e\u003csup\u003e3n\u0026ndash;\u003c/sup\u003e (Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003eb).\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eIn the [Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e]\u003csub\u003en\u003c/sub\u003e\u003csup\u003e3n\u0026ndash;\u003c/sup\u003e layer, large circles of Ag\u003csub\u003e7\u003c/sub\u003eI\u003csub\u003e7\u003c/sub\u003e with cross sectional dimensions of 7.285 \u0026Aring; \u0026times; 8.592 \u0026Aring; are formed (Fig. \u003cspan refid=\"MOESM3\" class=\"InternalRef\"\u003eS3\u003c/span\u003e). In the [Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e]\u003csub\u003en\u003c/sub\u003e\u003csup\u003e3n\u0026ndash;\u003c/sup\u003e anion, the I atoms adopt \u0026micro;\u003csub\u003e2\u003c/sub\u003e-I (I3, I8, I9, I12), \u0026micro;\u003csub\u003e3\u003c/sub\u003e-I (I2, I5, I7, I13) and \u0026micro;\u003csub\u003e4\u003c/sub\u003e-I (I1, I4, I6, I10, I11) bridging coordination modes. As expected, the Ag\u0026ndash;I bond distances fall in the decreasing order of Ag\u0026ndash;\u0026micro;\u003csub\u003e4\u003c/sub\u003e-I (2.9189 \u0026Aring;)\u0026thinsp;\u0026gt;\u0026thinsp;Ag\u0026ndash;\u0026micro;\u003csub\u003e3\u003c/sub\u003e-I (2.8403 \u0026Aring;)\u0026thinsp;\u0026gt;\u0026thinsp;Ag\u0026ndash;\u0026micro;\u003csub\u003e2\u003c/sub\u003e-I (2.7688 \u0026Aring;). Short Ag⋯Ag distances in the range of 2.912(15)‒3.295(2) \u0026Aring; are observed in the [Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e]\u003csub\u003en\u003c/sub\u003e\u003csup\u003e3n\u0026ndash;\u003c/sup\u003e anion. The Ag⋯Ag distances are less than the sum of the van der Waals radii of Ag\u0026thinsp;\u0026minus;\u0026thinsp;Ag (3.44 \u0026Aring;) [\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e], indicating metal\u0026ndash;metal interactions [\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e]. The [Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e]\u003csub\u003en\u003c/sub\u003e\u003csup\u003e3n\u0026ndash;\u003c/sup\u003e layers are stacked parallel to form channels running along the \u003cem\u003ea\u003c/em\u003e-axis (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ea). The [Fe(DMSO)\u003csub\u003e8\u003c/sub\u003e]\u003csup\u003e3+\u003c/sup\u003e cations are located between the [Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e]\u003csub\u003en\u003c/sub\u003e\u003csup\u003e3n\u0026ndash;\u003c/sup\u003e layers, and are arranged in arrays along the channels (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003eb).\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe characteristic of iodoargentates is that the AgI\u003csub\u003e4\u003c/sub\u003e and/or AgI\u003csub\u003e3\u003c/sub\u003e PBUs can easily copolymerize to form various iodoargentate aggregates in the presence of different kinds of structural directing agents (SDAs) because of the strong affinity of Ag(I) for the iodide ion. The structures of iodoargentate aggregates can be further tuned by the nature of the metal ion and the organic ligands to the metal ion when metal complex cation was used as the SDA. Using the hexakis solvated transition metal(TM) complex cations as the SDAs, a series of binary iodoargentate anions with Ag/I molar ratios in the range of 0.667\u0026ndash;0.750 and different dimensions had been prepared (Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e). The [Ni(DMSO)\u003csub\u003e6\u003c/sub\u003e]\u003csup\u003e2+\u003c/sup\u003e complex cation resulted in the 1-D anion [Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e7\u003c/sub\u003e]\u003csup\u003e2\u0026ndash;\u003c/sup\u003e in DMSO/H\u003csub\u003e2\u003c/sub\u003eO solvent, while the hexakis complex cation [V(DMSO)\u003csub\u003e5\u003c/sub\u003e(H\u003csub\u003e2\u003c/sub\u003eO)]\u003csup\u003e2+\u003c/sup\u003e with mixed solvation ligand led to formation of a 3-D anion [Ag\u003csub\u003e6\u003c/sub\u003eI\u003csub\u003e8\u003c/sub\u003e]\u003csup\u003e2\u0026ndash;\u003c/sup\u003e in the same solvent [\u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e]. The trivalence [Cr(DMSO)\u003csub\u003e6\u003c/sub\u003e]\u003csup\u003e3+\u003c/sup\u003e produced a 1-D polymric anion [Ag\u003csub\u003e6\u003c/sub\u003eI\u003csub\u003e9\u003c/sub\u003e]\u003csub\u003en\u003c/sub\u003e\u003csup\u003e2n\u0026ndash;\u003c/sup\u003e under the same synthetic conditions [\u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e]. The DMSO-solvated lanthanide complex cations, which led to formation of iodoargentate anions with Ag/I molar ratios in the range of 0.400\u0026ndash;0.700 (Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e), exhibited different structural directing effect from the TM complex cations on the formation of iodoargentate aggregates. The trivalence lanthanide complex cations [Ln(DMSO)\u003csub\u003e8\u003c/sub\u003e]\u003csup\u003e3+\u003c/sup\u003e (Ln\u0026thinsp;=\u0026thinsp;La, Ce), [Ln(DMSO)\u003csub\u003e8\u003c/sub\u003e]\u003csup\u003e3+\u003c/sup\u003e (Ln\u0026thinsp;=\u0026thinsp;Eu, Tb, Dy) and [Yb(DMSO)\u003csub\u003e7\u003c/sub\u003e]\u003csup\u003e3+\u003c/sup\u003e led to the iodoargentate anions of 0-D cluster [Ag\u003csub\u003e22\u003c/sub\u003eI\u003csub\u003e34\u003c/sub\u003e]\u003csup\u003e12\u0026minus;\u003c/sup\u003e, 2-D layer [Ag\u003csub\u003e7\u003c/sub\u003eI\u003csub\u003e10\u003c/sub\u003e]\u003csup\u003e3\u0026ndash;\u003c/sup\u003e, and 1-D chain [Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e8\u003c/sub\u003e]\u003csup\u003e3\u0026ndash;\u003c/sup\u003e, respectively [\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e], whileas the [Tb(DMSO)\u003csub\u003e8\u003c/sub\u003e]\u003csup\u003e3+\u003c/sup\u003e gave a iodoargentate that contains both 0-D [Ag\u003csub\u003e2\u003c/sub\u003eI\u003csub\u003e5\u003c/sub\u003e]\u003csup\u003e3\u0026ndash;\u003c/sup\u003e and 2-D [Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e8\u003c/sub\u003e]\u003csup\u003e3\u0026ndash;\u003c/sup\u003e anions [\u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e, \u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e]. In this work, the hexakis Fe(III) complex cation [Fe(DMSO)\u003csub\u003e6\u003c/sub\u003e]\u003csup\u003e3+\u003c/sup\u003e afforded a novel 2-D iodoargentate anion [Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e]\u003csup\u003e3\u0026ndash;\u003c/sup\u003e with a higher Ag/I ratio of 0.769, which is a new member of iodoargentate anion with layered structure. As a result, the compositions and dimensions of the iodoargentates are affected by the ionic radius, valence state, and type of the metal ions when the metal-DMOS complex cations were used as the templates in the syntheses of iodoargentate hybrids.\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab1\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 1\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eA summary of the dimensions and Ag/I molar ratios of the iodoargentate anions templated by DMSO-solvated metal complex cations\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"5\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eCompound\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eIodoargentate\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eDimension\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eAg/I ratio\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c5\"\u003e \u003cp\u003eRef.\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e[Ni(DMSO)\u003csub\u003e6\u003c/sub\u003e]Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e7\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e[Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e7\u003c/sub\u003e]\u003csup\u003e2\u0026ndash;\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e1-D\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e0.714\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\" morerows=\"2\" rowspan=\"3\"\u003e \u003cp\u003e27\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e[Cr(DMSO)\u003csub\u003e6\u003c/sub\u003e]Ag\u003csub\u003e6\u003c/sub\u003eI\u003csub\u003e9\u003c/sub\u003e\u0026middot;H\u003csub\u003e2\u003c/sub\u003eO\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e[Ag\u003csub\u003e6\u003c/sub\u003eI\u003csub\u003e9\u003c/sub\u003e]\u003csup\u003e3\u0026ndash;\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e1-D\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e0.667\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e[V(DMSO)\u003csub\u003e5\u003c/sub\u003e(H\u003csub\u003e2\u003c/sub\u003eO)]Ag\u003csub\u003e6\u003c/sub\u003eI\u003csub\u003e8\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e[Ag\u003csub\u003e6\u003c/sub\u003eI\u003csub\u003e8\u003c/sub\u003e]\u003csup\u003e2\u0026ndash;\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e3-D\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e0.750\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e[Fe(DMSO)\u003csub\u003e6\u003c/sub\u003e]Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e[Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e]\u003csup\u003e3\u0026ndash;\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e2-D\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e0.769\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003ethis work\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e[Yb(DMSO)\u003csub\u003e7\u003c/sub\u003e]Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e8\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e[Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e8\u003c/sub\u003e]\u003csup\u003e3\u0026ndash;\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e1-D\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e0.625\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\" morerows=\"2\" rowspan=\"3\"\u003e \u003cp\u003e28\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e[Ln(DMSO)\u003csub\u003e8\u003c/sub\u003e]Ag\u003csub\u003e7\u003c/sub\u003eI\u003csub\u003e10\u003c/sub\u003e\u003c/p\u003e \u003cp\u003e(Ln\u0026thinsp;=\u0026thinsp;Eu, Tb, Dy)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e[Ag\u003csub\u003e7\u003c/sub\u003eI\u003csub\u003e10\u003c/sub\u003e]\u003csup\u003e3\u0026ndash;\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e1-D\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e0.700\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e[La(DMSO)\u003csub\u003e8\u003c/sub\u003e]\u003csub\u003e4\u003c/sub\u003eAg\u003csub\u003e22\u003c/sub\u003eI\u003csub\u003e34\u003c/sub\u003e\u0026middot;2H\u003csub\u003e2\u003c/sub\u003eO\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e[Ag\u003csub\u003e22\u003c/sub\u003eI\u003csub\u003e34\u003c/sub\u003e]\u003csup\u003e12\u0026ndash;\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e0-D\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e0.647\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\" morerows=\"1\" rowspan=\"2\"\u003e \u003cp\u003e[Ln(DMSO)\u003csub\u003e8\u003c/sub\u003e](Ag\u003csub\u003e2\u003c/sub\u003eI\u003csub\u003e5\u003c/sub\u003e)(Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e8\u003c/sub\u003e)\u003c/p\u003e \u003cp\u003e(Ln\u0026thinsp;=\u0026thinsp;Eu, Tb)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e[Ag\u003csub\u003e2\u003c/sub\u003eI\u003csub\u003e5\u003c/sub\u003e]\u003csup\u003e3\u0026ndash;\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e0-D\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e0.400\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\" morerows=\"1\" rowspan=\"2\"\u003e \u003cp\u003e24, 29\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e[Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e8\u003c/sub\u003e]\u003csup\u003e3\u0026ndash;\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e2-D\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e0.625\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003c/div\u003e\n\u003ch3\u003eSolid-state UV-vis reflectance spectra and optical band gaps\u003c/h3\u003e\n\u003cp\u003eThe solid-state UV-Vis-NIR diffuse reflectance spectrum showed that compound \u003cb\u003e1\u003c/b\u003e exhibited sensitive light reflection properties in the visible light range. It had almost no diffuse reflection signals in near-infrared region (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ea). The reflectance data were converted to absorption spectrum by the Kubelka-Munk function \u003cem\u003eF\u003c/em\u003e(\u003cem\u003eR\u003c/em\u003e) = (1\u0026ndash;\u003cem\u003eR\u003c/em\u003e)\u003csup\u003e2\u003c/sup\u003e/2\u003cem\u003eR\u003c/em\u003e [\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e], which was shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003eb. Compound \u003cb\u003e1\u003c/b\u003e exhibited steep absorption edge. Extrapolating the tangent drawn from the steep absorption edge to the energy axis yielded the intercept value of 1.80 eV (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003eb), which is corresponding to the band gap (\u003cem\u003eE\u003c/em\u003e\u003csub\u003eg\u003c/sub\u003e) of compound \u003cb\u003e1\u003c/b\u003e. Compound \u003cb\u003e1\u003c/b\u003e exhibited distinct redshift in the absorption edges in comparison with bulk AgI (zinc-blend structure, \u003cem\u003eE\u003c/em\u003e\u003csub\u003eg\u003c/sub\u003e: ~2.40 eV) [\u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e30\u003c/span\u003e]. The band gap of compound \u003cb\u003e1\u003c/b\u003e is comparable to those of the iodoargentate hybrids with organic cations [(BV)\u003csub\u003e2\u003c/sub\u003e(Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e9\u003c/sub\u003e)]\u003csub\u003en\u003c/sub\u003e (BV\u003csup\u003e2+\u003c/sup\u003e = benzyl viologen) (\u003cem\u003eE\u003c/em\u003e\u003csub\u003eg\u003c/sub\u003e = 1.76 eV) [\u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e31\u003c/span\u003e], (H\u003csub\u003e2\u003c/sub\u003edpe)\u003csub\u003e0.5\u003c/sub\u003e(β-AgI\u003csub\u003e2\u003c/sub\u003e) (dpe\u0026thinsp;=\u0026thinsp;1,2-di(4-pyridyl)ethylene) (\u003cem\u003eE\u003c/em\u003e\u003csub\u003eg\u003c/sub\u003e = 1.99 eV) [\u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e32\u003c/span\u003e]. It is smaller than those of the TM(II)-containing iodoargentate hybrids [Cr(DMSO)\u003csub\u003e6\u003c/sub\u003e]Ag\u003csub\u003e6\u003c/sub\u003eI\u003csub\u003e9\u003c/sub\u003e\u0026middot;H\u003csub\u003e2\u003c/sub\u003eO (\u003cem\u003eE\u003c/em\u003e\u003csub\u003eg\u003c/sub\u003e = 3.33 eV), [Ni(DMSO)\u003csub\u003e6\u003c/sub\u003e]Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e7\u003c/sub\u003e (\u003cem\u003eE\u003c/em\u003e\u003csub\u003eg\u003c/sub\u003e = 2.73 eV) and [V(DMSO)\u003csub\u003e5\u003c/sub\u003e(H\u003csub\u003e2\u003c/sub\u003eO)]Ag\u003csub\u003e6\u003c/sub\u003eI\u003csub\u003e8\u003c/sub\u003e (\u003cem\u003eE\u003c/em\u003e\u003csub\u003eg\u003c/sub\u003e = 2.61 eV) [\u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e], and Ln(III)-containing iodoargentate hybrids [La(DMSO)\u003csub\u003e8\u003c/sub\u003e]\u003csub\u003e4\u003c/sub\u003eAg\u003csub\u003e22\u003c/sub\u003eI\u003csub\u003e34\u003c/sub\u003e\u0026middot;2H\u003csub\u003e2\u003c/sub\u003eO (\u003cem\u003eE\u003c/em\u003e\u003csub\u003eg\u003c/sub\u003e = 3.30 eV), [Ln(DMSO)\u003csub\u003e8\u003c/sub\u003e]Ag\u003csub\u003e7\u003c/sub\u003eI\u003csub\u003e10\u003c/sub\u003e [\u003cem\u003eE\u003c/em\u003e\u003csub\u003eg\u003c/sub\u003e = 2.91 eV (Eu), 3.05 eV (Tb), 2.84 eV (Dy)], and [Yb(DMSO)\u003csub\u003e7\u003c/sub\u003e]Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e8\u003c/sub\u003e (\u003cem\u003eE\u003c/em\u003e\u003csub\u003eg\u003c/sub\u003e = 3.32 eV) [\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e], and [Ln(DMSO)\u003csub\u003e8\u003c/sub\u003e]\u003csub\u003e2\u003c/sub\u003e[Ag\u003csub\u003e2\u003c/sub\u003eI\u003csub\u003e5\u003c/sub\u003e][Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e8\u003c/sub\u003e] [\u003cem\u003eE\u003c/em\u003e\u003csub\u003eg\u003c/sub\u003e = 3.33 eV (Eu), 3.34 eV (Tb)] [\u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e]. The band gap of compound \u003cb\u003e1\u003c/b\u003e is also lower than those of the iodoargentate hybrids containing TM(II) complex with conjugated organic ligands, such as [TM(2,2'-bipy)\u003csub\u003e3\u003c/sub\u003e]Ag\u003csub\u003e5\u003c/sub\u003eI\u003csub\u003e7\u003c/sub\u003e (2,2'-bipy\u0026thinsp;=\u0026thinsp;2,2'-bipyridine) [\u003cem\u003eE\u003c/em\u003e\u003csub\u003eg\u003c/sub\u003e = 1.94 eV (Co), 2.10 eV (Ni), 2.58 eV(Zn)] [\u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e33\u003c/span\u003e].\u003c/p\u003e \u003cp\u003e \u003c/p\u003e\n\u003ch3\u003ePhotocurrent response and photocatalytic properties\u003c/h3\u003e\n\u003cp\u003eThe photocurrent response of compound \u003cb\u003e1\u003c/b\u003e under visible light irradiation was investigated on a CHI760E electrochemical workstation with a standard three-electrode system at room temperature. Compound \u003cb\u003e1\u003c/b\u003ewas photosensitive to visible light, and showed rapid photoelectric response under visible light irradiation at room temperature. As shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ea, its photocurrent densities increased sharply when light was turned on, and immediately dropped to approximately zero once the light was turned off. Under light illumination of a Xe lamp with a power of 180 W, the photocurrent densities of compound \u003cb\u003e1\u003c/b\u003e was 5.75 \u0026micro;A\u0026middot;cm\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e in the first on/off switch, and stabilized at 4.83 \u0026micro;A\u0026middot;cm\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e after eight on/off switch cycles, which exhibited good reproduciblity in photocurrent responses. Compound \u003cb\u003e1\u003c/b\u003e exhibit higher photocurrent densities than do the Ln(III)-containing iodoargentate hybrids {[Ln\u003csub\u003e2\u003c/sub\u003e(dpdo)(DMF)\u003csub\u003e14\u003c/sub\u003e](Ag\u003csub\u003e12\u003c/sub\u003eI\u003csub\u003e18\u003c/sub\u003e)}\u003csub\u003en\u003c/sub\u003e (bpdo\u0026thinsp;=\u0026thinsp;4,4'-bipyridine N,N'-dioxide, Ln\u0026thinsp;=\u0026thinsp;La, Nd, Sm), whose current intensities are 0.2 \u0026micro;A, 0.125 \u0026micro;A and 0.25 \u0026micro;A [\u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e34\u003c/span\u003e], respectively.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe catalytic activity of compound \u003cb\u003e1\u003c/b\u003e was evaluated by the photocatalytic degradation of methylene blue (MB), which is an organic dye commonly used in industry, in an aqueous solution at room temperature under visible-light irradiation of a Xe lamp in the presence of air. The concentration of MB was monitored by the changes in the absorption intensity at the maximum absorption wavelength of 665 nm in the UV\u0026ndash;Vis spectrum (Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003eb). The degradation activity of MB over compound \u003cb\u003e1\u003c/b\u003e was expressed as \u003cem\u003eC\u003c/em\u003e/\u003cem\u003eC\u003c/em\u003e\u003csub\u003e0\u003c/sub\u003e, where \u003cem\u003eC\u003c/em\u003e\u003csub\u003e0\u003c/sub\u003e and \u003cem\u003eC\u003c/em\u003e are the initial and instantaneous concentrations of MB, respectively. As shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003eb, the absorption peak of MB solution decreased rapidly with the increase of irradiation time. After 60 min of light irradiation, the MB solution became colorless in the presence of compound \u003cb\u003e1\u003c/b\u003e, and the degradation conversion of MB reached 98.8% (Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ec). Comparatively, approximately 11% of MB was degraded in the blank experiment after 60 min of light irradiation. The plot of Ln(\u003cem\u003eC\u003c/em\u003e\u003csub\u003e0\u003c/sub\u003e/\u003cem\u003eC\u003c/em\u003e) against the irradiation time \u003cem\u003et\u003c/em\u003e fits the formula Ln(\u003cem\u003eC\u003c/em\u003e\u003csub\u003e0\u003c/sub\u003e/\u003cem\u003eC\u003c/em\u003e)\u0026thinsp;=\u0026thinsp;\u003cem\u003ek\u003c/em\u003et, indicating that the photodegradation reaction catalyzed by \u003cb\u003e1\u003c/b\u003e conforms to first-order kinetics (Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ed). The kinetic rate constant \u003cem\u003ek\u003c/em\u003e of the degradation reaction is 0.0712 min\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e. The photocatalytic activity of \u003cb\u003e1\u003c/b\u003e for MB photodegradation is higher than those of the haloargentate hybrids {([syn/anti-did](Ag\u003csub\u003e2\u003c/sub\u003eI\u003csub\u003e4\u003c/sub\u003e)} (did\u003csup\u003e2+\u003c/sup\u003e = (1\u003csup\u003e2\u003c/sup\u003ez,5\u003csup\u003e2\u003c/sup\u003ez)-1\u003csup\u003e1\u003c/sup\u003eH,5\u003csup\u003e1\u003c/sup\u003eH-1,5(1,3)-diimidazol-3-iuma-3,7(1,2)-dibenzenacyclooctaphane-1\u003csup\u003e3\u003c/sup\u003e,5\u003csup\u003e3\u003c/sup\u003e-diium) (20.2% of MB in 150 min) [\u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e35\u003c/span\u003e], and {(bmpp)[Ag\u003csub\u003e4\u003c/sub\u003eI\u003csub\u003e6\u003c/sub\u003e]}\u003csub\u003en\u003c/sub\u003e (bmpp\u0026thinsp;=\u0026thinsp;1,3-bis(4-methylpyridine)alkane cation) (37% of MB in 150 min) [\u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e36\u003c/span\u003e].\u003c/p\u003e"},{"header":"Conclusions","content":"\u003cp\u003eIn conclusion, an effective organic-inorganic photocatlyst \u003cb\u003e1\u003c/b\u003e based on iodoargentate was prepared using a solvated Fe(III) complex cation [Fe(DMSO)\u003csub\u003e6\u003c/sub\u003e]\u003csup\u003e3+\u003c/sup\u003e formed in-situ as the template under solvothermal condition. The 2-D [Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e]\u003csub\u003en\u003c/sub\u003e\u003csup\u003e3n‒\u003c/sup\u003e layered anion with Ag/I molar ratio of 0.769 is a new member of binary iodoargentate aggregates. Compound \u003cb\u003e1\u003c/b\u003e exhibit effectively photocatalytic activity in the degradation of the organic dye MB in aqueous solution at room temperature. The results showed that it was possible to design and prepare photocatalyst based iodoargentate hybrid using TM complex cation as the template. Further studies on constructing new halometallate hybrid materials are ongoing.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eAuthor\u003c/strong\u003e\u003cstrong\u003es contributions\u0026nbsp;\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eHZ and DJ wrote the main text of the manuscript, DJ prepared Figures 1 to 3, ZJ prepared the Figures 4 and 5, and performed x-ray diffraction studies and physical\u003cstrong\u003e\u0026nbsp;\u003c/strong\u003emeasurements. All authors reviewed the manuscript.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eFunding\u003c/strong\u003e\u0026nbsp;\u003c/p\u003e\n\u003cp\u003eThis work was supported by the National Natural Science Foundation of China (No. 21171123, 20771077).\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eData availability\u0026nbsp;\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eNo datasets were generated or analysed during the current study.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eCompeting interests\u003c/strong\u003e\u0026nbsp;\u003c/p\u003e\n\u003cp\u003eThe authors declare no competing interests.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eSupplementary\u0026nbsp;\u003c/strong\u003e\u003cstrong\u003eInformation.\u0026nbsp;\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe online version contains supplementary materials available at \u0026nbsp;https://doi.org/10.1007\u003c/p\u003e\n\u003cp\u003eCCDC-2528821 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via [email protected] or http://www.ccdc.cam. ac.uk/data_request/cif.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eSharma VK, Ma XM, Zboril R (2023) Single atom catalyst-mediated generation of reactive species in water treatment. Chem Soc Rev 52:7673\u0026ndash;7686\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eS\u0026aacute;nchez BJ, Wang J (2018) Micromotors for environmental applications: a review. Environ Sci Nano 5:1530\u0026ndash;1544\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eKou JH, Lu CH, Wang J, Chen YK, Xu ZZ, Varma RS (2017) Selectivity enhancement in heterogeneous photocatalytic transformations. 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J Cluster Sci 26:1723\u0026ndash;1733\u003c/span\u003e\u003c/li\u003e\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"transition-metal-chemistry","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"tmch","sideBox":"Learn more about [Transition Metal Chemistry](http://link.springer.com/journal/11243)","snPcode":"11243","submissionUrl":"https://submission.nature.com/new-submission/11243/3","title":"Transition Metal Chemistry","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"","lastPublishedDoi":"10.21203/rs.3.rs-8885980/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-8885980/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eA Fe(III)-iodoargentate hybrid [Fe(DMSO)\u003csub\u003e6\u003c/sub\u003e]Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e (\u003cb\u003e1\u003c/b\u003e) (DMSO\u0026thinsp;=\u0026thinsp;dimethyl sulfoxide) was prepared using a solvated Fe(III) complex cation [Fe(DMSO)\u003csub\u003e6\u003c/sub\u003e]\u003csup\u003e3+\u003c/sup\u003e formed in-situ as the template under solvothermal conditions. It consists of a [Fe(DMSO)\u003csub\u003e8\u003c/sub\u003e]\u003csup\u003e3+\u003c/sup\u003e complex cation and a 2-D [Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e]\u003csub\u003en\u003c/sub\u003e\u003csup\u003e3n‒\u003c/sup\u003e layered anion. The 2-D [Ag\u003csub\u003e10\u003c/sub\u003eI\u003csub\u003e13\u003c/sub\u003e]\u003csub\u003en\u003c/sub\u003e\u003csup\u003e3n‒\u003c/sup\u003e anion is composed of ten crystallographically independent AgI\u003csub\u003e4\u003c/sub\u003e tetrahedral units through corner- and edge-sharing, which contains large circles of Ag\u003csub\u003e7\u003c/sub\u003eI\u003csub\u003e7\u003c/sub\u003e with cross sectional dimensions of 7.285 \u0026Aring; \u0026times; 8.592 \u0026Aring;. Compound \u003cb\u003e1\u003c/b\u003e exhibits rapid photocurrent response with steady current density of 4.83 \u0026micro;A\u0026middot;cm\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e after e under visible light irradiation. It shows high photocatalytic activities in the degradation of MB with degradation ratio of 98.8% after light irradiation of 60 min.\u003c/p\u003e","manuscriptTitle":"Solvothermal synthesis and efficient visible light-driven photocatalytic property of 2-D iodoargentate hybrid directed by solvated Fe(III) cation","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2026-02-20 11:07:36","doi":"10.21203/rs.3.rs-8885980/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2026-02-17T10:15:38+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2026-02-17T10:12:41+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2026-02-17T08:18:52+00:00","index":"","fulltext":""},{"type":"submitted","content":"Transition Metal Chemistry","date":"2026-02-15T12:30:47+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"transition-metal-chemistry","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"tmch","sideBox":"Learn more about [Transition Metal Chemistry](http://link.springer.com/journal/11243)","snPcode":"11243","submissionUrl":"https://submission.nature.com/new-submission/11243/3","title":"Transition Metal Chemistry","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"ebe8bba3-02a7-4dc0-bf15-fe6ff6012e64","owner":[],"postedDate":"February 20th, 2026","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"under-review","subjectAreas":[],"tags":[],"updatedAt":"2026-05-11T09:11:07+00:00","versionOfRecord":[],"versionCreatedAt":"2026-02-20 11:07:36","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-8885980","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-8885980","identity":"rs-8885980","version":["v1"]},"buildId":"XKTyCvWXoU3ODBz1xrDgd","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}