synthesis and crystal structure of the bioinorganic ...€¦ · 2...

Research ArticleSynthesis and Crystal Structure of the BioinorganicComplex [Sb(Hedta)]middot2H2O

Di Li and Guo-Qing Zhong

State Key Laboratory Cultivation Base for Nonmetal Composite and Functional Materials School of Material Science and EngineeringSouthwest University of Science and Technology Mianyang 621010 China

Correspondence should be addressed to Guo-Qing Zhong zgq316163com

Received 31 October 2013 Revised 12 December 2013 Accepted 15 December 2013 Published 13 February 2014

Academic Editor Concepcion Lopez

Copyright copy 2014 D Li and G-Q Zhong This is an open access article distributed under the Creative Commons AttributionLicense which permits unrestricted use distribution and reproduction in any medium provided the original work is properlycited

The antimony(III) complex [Sb(Hedta)]sdot2H2O was synthesized with ethylenediaminetetraacetic acid (H

4edta) and antimonous

oxide as main raw materials in aqueous solution The composition and structure of the complex were characterized by elementalanalysis infrared spectra single crystal X-ray diffraction X-ray powder diffraction thermogravimetry and differential scanningcalorimetry The crystal structure of the antimony(III) complex belongs to orthorhombic system space group Pna2(1) with cellparameters of 119886 = 184823(18) A 119887 = 109408(12) A 119888 = 73671(5) A 119881 = 14897(2) A3 119885 = 4 and 119863

119888= 1993 g cmminus3 The

Sb(III) ion is five-coordinated by two amido N atoms and three carboxyl O atoms from a single Hedta3minus ligand forming a distortedtrigonal bipyramid geometry The thermal decomposition processes of the complex include dehydration oxidation and pyrolysisof the ligand and the last residue is Sb

2O3at the temperature of 570∘C

1 Introduction

Many of the antimony(III) compounds have been mainlyused in the clinic medicine because of their medicinal utilityand biological activity The aminopolycarboxylate complexesof antimony(III) with effective antimicrobial and anticanceractivity are widely applied to the treatment of a variety ofmicrobial infections including leishmaniasis diarrhea pepticulcers and helicobacter pylori and so forth [1 2] Theethylenediaminetetraacetic acid as one of the multicarboxy-late ligands possesses diverse functional groups such as N-donor and O-donor When a metal ion is in the centerposition the ligand is always allowed to bend and to rotateand one can easily imagine the structural diversity of newsynthesizable materials [3] In fact the design and synthesisof metal-organic frameworks (MOFs) is not only because oftheir fascinating structures and topological novelty but alsobecause of their existing potential applications as functionalmaterials in gas storage heterogeneous catalysis chemicalseparations and microelectronics [4ndash11] So the ethylene-diaminetetraacetic acid (H

4edta) as ligand is a good choice

for building a diversified structure it is not only a plurality

of coordination sites but also an inexpensive and relativesafe substance which can remove toxic heavy metals reduceoxidative stress and increase waste excretion [12 13] Inclinical practice the chelation therapy with H

4edta can

prevent cancer and catalytic reactive oxygen species such ascardiovascular and arteriosclerotic heart disease [14ndash16] Soit is widely used in the pharmaceutical and biological aspects

As we know the main group elements do not easily formcomplexes with organic ligands because of the special prop-erties But owing to the presence of a lone pair of electronsshowing stereochemical behavior the antimony complexeswith aminopolycarboxylate ligands have attracted peoplersquosinterests [17] Because the inorganic salts of antimony(III)have considerable toxicity so the new biological activity andmedicinal function complexes of the main group elementantimony are received more attention [18 19] Besides someantimony(III) compounds have been used as antiparasiticagents and exhibit significant functions as biocides fungi-cides antioxidants and potential therapeutic agents Forexample some antimony compounds are used for treatmentof leishmaniasis various species of the protozoan leishmaniavirus and cancer [20ndash25]

Hindawi Publishing CorporationBioinorganic Chemistry and ApplicationsVolume 2014 Article ID 461605 7 pageshttpdxdoiorg1011552014461605

2 Bioinorganic Chemistry and Applications

Table 1 Crystal data and structure refinement for the title complex

Empirical formula SbC10H17N2O10 119865(000) 888Formula weight 44701 Crystal size 046mm times 040mm times 035mmWavelength 071073 A Theta range for data collection 289ndash2502∘

Temperature 298(2) K Limiting indices minus21 le ℎ le 16 minus13 le 119896 le 13 minus7 le 119897 le 8Crystal system Orthorhombic Reflections collectedunique 71022529 [R(int) = 00461]Space group Pna2(1) Completeness to theta = 2502 999Unit cell dimensions Absorption correction Semiempirical from equivalents119886 184823(18) A Max and min transmission 05547 and 04738119887 109408(12) A Refinement method Full-matrix least-squares on 1198652

119888 73671(5) A Daterestraintsparameters 25291208120573 9000∘ Goodness-of-fit on 1198652 1040119881 14897(2) A3 Final 119877 indices [119868 gt 2120590(119868)] R1 = 00332 119908119877

2= 00811

119885 4 119877 indices (all data) R1 = 00359 1199081198772= 00832

Calculated density 1993 g cmminus3 Absolute structure parameter minus027(4)Absorption coefficient 1909mmminus1 Largest diff peak and hole 0786 and minus0805 e Aminus3

In recent years owing to the development of aminopoly-carboxylic acid complexes of antimony(III) in medicinethe complex of antimony with multicarboxylate ligands hasreceived more and more attention Herein we report thesyntheses of the title complex [Sb(Hedta)]sdot2H

2OThe compo-

sition and crystal structure of the complex have been charac-terized by elemental analysis single crystal X-ray diffractionXRD FTIR and TG-DSC

2 Experimental

21 Materials and General Methods All the chemicals usedin the experiments were analytical reagent as received fromcommercial sources and without further purification Theethylenediaminetetraacetic acid and antimonous oxide werepurchased from Shanghai Reagent Industry

The antimony was determined by a Thermo X-II induc-tively coupled plasma mass spectrometer The content of car-bon hydrogen and nitrogen in the complex wasmeasured bya Vario EL CUBE elemental analyzer The IR spectra wereobtained with a Perkin-Elmer Spectrum One-spectrometerin the range of 225ndash4000 cmminus1 using KBr pellets The ther-mogravimetric analysis of the metal complex was performedby an SDT Q600 thermogravimetric analyzer and the mea-surement was recorded from 30 to 800∘C at the heating rateof 10∘C minminus1 under air flow of 100mLminminus1 The X-raypowder diffraction was performed using a Dmax-II X-raydiffractometer CuK

120572radiation (120582= 0154056 nm stepwidth

2120579 = 02∘ scan speed 8∘min)

22 Synthesis of the Complex [Sb(Hedta)]sdot2H2O The title

complex was obtained by aqueous solution synthesis First146 g (5mmol) ethylenediaminetetraacetic acid was solubi-lized in 200mLboiling distilledwaterThen 0875 g (3mmol)antimonous oxide was gradually added to the above solutionstirring and maintaining the temperature at 90∘C After fourhours when the pH was about 2-3 the reaction was stoppedThe unreacted antimonous oxide was filtered The colorless

filtrate was slowly concentrated to 100mL The concentratedsolution was placed at room temperature for about one weekand the colorless flaky crystals of the antimony(III) complexwas obtained The yield was about 82 Anal Calcd for thetitle complex SbC

10H17N2O10() Sb 2724 C 2687 N 627

H 383 Found () Sb 2711 C 2668 N 619 H 374

23 X-Ray Diffraction Crystallography The appropriate crys-tals were cut from larger crystals and mounted on a BrukerSmart Apex II CCD diffractometer with graphite monochro-mated Mo K

120572radiation (120582 = 071073 A) The data were

collected at 298(2) K A colorless and transparent crystal withdimensions 046mm times 040mm times 035mm was mountedon a glass fiber Diffraction data were collected in 120596 modein the range of 289∘ndash2502∘ The structure was solved bydirect methods SHELXS-97 and refined by full-matrix least-squares using SHELXL-97 [26 27] All nonhydrogen atomswere obtained from the difference Fourier map and full-matrix least-squares refinements on 1198652 were carried out withanisotropic thermal parameters Hydrogen atoms of the lig-and were generated geometrically The structure refinementparameters for the title complex are given in Table 1 and thecrystallographic data are depositedwith theCambridgeCrys-tallographic Data Centre under deposition number CCDC953660

3 Results and Discussion

31 X-Ray Crystal Structure Analysis The single crystal X-ray diffraction analysis reveals that the complex [Sb(Hedta)]sdot2H2O crystallises in the orthorhombic system with space

group Pna2(1) Crystallographic data and structure refine-ment parameters for the title complex are given inTable 1 andthe selected bond distances and angles are shown in Table 2The key fragments of the structures and the atom numberingare shown in Figure 1 and the crystal packing diagram ofthe complex is shown in Figure 2 The asymmetric unit ofthe complex consists of one Hedta3minus one trivalent antimony

Bioinorganic Chemistry and Applications 3

Table 2 Selected bond lengths (A) and angles (∘) for the title complex

Sb(1)ndashO(1) 2182(4) O(7)ndashC(9) 1218(7) N(1)ndashSb(1)ndashN(2) 759(2)Sb(1)ndashO(5) 2199(4) O(8)ndashC(9) 1299(7) C(4)ndashN(1)ndashSb(1) 1075(3)Sb(1)ndashO(3) 2243(4) O(1)ndashSb(1)ndashO(5) 1428(2) C(6)ndashN(1)ndashSb(1) 1086(4)Sb(1)ndashN(1) 2336(5) O(1)ndashSb(1)ndashO(3) 10436(16) C(1)ndashN(1)ndashSb(1) 1097(3)Sb(1)ndashN(2) 2402(5) O(5)ndashSb(1)ndashO(3) 8538(15) C(8)ndashN(2)ndashSb(1) 1048(3)O(1)ndashC(3) 1307(8) O(1)ndashSb(1)ndashN(1) 7409(16) C(2)ndashN(2)ndashSb(1) 1085(3)O(2)ndashC(3) 1222(7) O(5)ndashSb(1)ndashN(1) 7560(18) C(10)ndashN(2)ndashSb(1) 1149(4)O(3)ndashC(5) 1273(7) O(3)ndashSb(1)ndashN(1) 7103(17) C(3)ndashO(1)ndashSb(1) 1200(4)O(4)ndashC(5) 1229(7) O(1)ndashSb(1)ndashN(2) 7888(16) C(7)ndashO(5)ndashSb(1) 1189(4)O(5)ndashC(7) 1286(7) O(5)ndashSb(1)ndashN(2) 7326(17) C(5)ndashO(3)ndashSb(1) 1201(4)O(6)ndashC(7) 1238(7) O(3)ndashSb(1)ndashN(2) 14417(16)

Table 3 Hydrogen bond lengths (A) and bond angles (∘) for the title complex

DndashH 119889(DndashH) 119889(Hsdot sdot sdotA) 119889(Dsdot sdot sdotA) angDHA A symmetry operationO8ndashH8 0820 1742 2556 17190 O9O9ndashH9C 0850 1854 2702 17529 O4 [minus119909 + 1

2

119910 +

1

2

119911 +

1

2

]

O9ndashH9D 0850 1935 2783 17528 O6 [minus119909 + 1 minus119910 + 1 119911 + 12

]

O10ndashH10E 0850 2110 2950 16924 O9O10ndashH10F 0850 2091 2930 16918 O2 [minus119909 + 1

2

119910 minus

1

2

119911 +

1

2

]

O10

O9

O6 O4

O7

C9

C8

O5 O3 C5

Sb1

C6

N1

C10 O1C3

O2

C4N2 C1

O8

C2

C7

Figure 1 The molecular structure of the title complex

ion and two crystalline water molecules Sb(III) ion for planeforms a distorted trigonal bipyramidal configuration TheSb(III) ion is five-coordinated by three carboxyl oxygenatoms (O1 O3 and O5) and two nitrogen atoms (N1 and N2)from the same Hedta3minus ligand Therefore a carboxyl group(O7 and O8) and all water molecules in the title complex arenot coordinated The bond lengths of Sb1ndashO1 Sb1ndashO3 andSb1ndashO5 are in the range of 2182ndash2243 A and it belongs tothe typical distance of the aminopolycarboxylate complexesof antimony(III) [28] But with respect to the bond lengths ofCndashO there are two types of carboxyl groups in the complexThe C5(7)ndashO3(5) is longer than C5(7)ndashO4(6) about 004 Alike the usual ionized carboxyl group But the C3(9)ndashO1(8) is

longer than C3(9)ndashO2(7) about 008 A which is comparablewith the value of a free carboxylic acid and this type ofcoordination seems to cause the especially strong acidityof Sb-(Hedta) The bond angles of N1ndashSb1ndashO3 N1ndashSb1ndashO5N1ndashSb1ndashN2 and N1ndashSb1ndashO1 are almost similar if the Sb1ndashN1 is perpendicular to the equator plane they look like aninverted umbrella and the SbndashN bond lengths are 2336(5) Aand 2402(5) A and the SbndashO band lengths are Sb1ndashO1 =2182(4) A Sb1ndashO3 = 2243(4) A and Sb1ndashO5 = 2199(4) Arespectively

In Tables 2 and 3 there are three types of hydrogenbonds in the crystal of the Sb(III) complex and theyinclude the weak hydrogen bonds between the crystallinewater molecules (O10ndashH10E sdot sdot sdotO9 2950 A) the crystallinewater and the oxygen atoms of the carbonyl groups (O9ndashH9C sdot sdot sdotO4 2702 A O9ndashH9D sdot sdot sdotO6 2783 A and O10ndashH10F sdot sdot sdotO2 2930 A) and the strong hydrogen bondsbetween the crystalline water and the oxygen atoms ofthe hydroxyl groups (O8ndashH8 sdot sdot sdotO9 2556 A) In Figure 3because there are a lot of crystal water molecules in the com-plex the interstitial water molecules and the carboxyl oxygenatoms will form hydrogen bonds which make the structuremore stable

32 X-Ray Powder Diffraction TheX-ray powder diffractiondata of [Sb(Hedta)]sdot2H

2O was collected in the diffraction

angle range of 3∘ndash80∘ The XRD pattern of the complex isshown in Figure 4(a) The main diffraction peaks appear at2120579 = 956∘ 1530∘ and 1685∘ for the title complex The indexcalculation of the XRD data bases on the computer programof least squares method [29] and the calculated results are


b

0

c

a

c

Figure 2 Crystal packing diagram of the title complex

c

a

Figure 3 Packing diagram of the title complex showing H bondingalong the b axis

shown in Table 4 Table 4 shows that the calculated spacing119889

ℎ119896119897is consistent with the experimental ones and the largest

relative deviation between the experimental and calculatedspacing 119889

ℎ119896119897is less than 03This indicates that the resultant

is a single phase compound [17] The crystal structure ofthe complex belongs to an orthorhombic system with thelattice parameters 119886 = 18479 A 119887 = 10957 A and 119888 =7343 A respectively The results of indexes to the XRD datafor the complex are consistent with the results of singlecrystal The experimental pattern exhibiting some peaks isslightly broadened in comparison with the simulated patternin Figure 4(b) which may be due to the preferred orientationof the powder samplesThe experimental XRD pattern agreeswell with the simulated pattern generated on the basis of thesingle crystal analyses for the title complex

33 FT-IR Spectra The FT-IR spectra of the title complex areshown in Figure 5 The infrared spectra of the complex showthat wide absorption bands in the region 3400ndash3600 cmminus1can be assigned to the OndashH stretching vibration of the watermolecules The peaks observed from 3017 to 2927 cmminus1 arein good agreement with the CndashH vibrations If the band at1700ndash1750 cmminus1 shows the existence of a free carboxyl groupwhile at about 1650 cmminus1 suggests that carboxyl groups are

10 20 30 40 50 60 70 800

5000

10000

15000

20000

25000

10 20 30 40 50 60 70 80

Inte

nsity

(au

)

(a)

(b)

2120579 (∘)

Figure 4 XRD patterns for title complex generated from theexperimental data (a) and simulated from the single crystal X-raydata (b)

4000 3500 3000 2500 2000 1500 1000 500

0

20

40

60

80

100T

() 35

6834

65 2968

1654

1416

1364

1308

1092

918 86

073

7 663

458

378

125130

17

2927

1038

317

Wavenumber (cmminus1)

Figure 5 FT-IR spectra of the title complex

coordinated In which the ]as(COO) band of the complex[Sb(Hedta)]sdot2H

2O appears at 1654 cmminus1 both 1364 cmminus1 and

1308 cmminus1 are the ]s(COO) bands The difference value of290 cmminus1 and 346 cmminus1 between the asymmetric and sym-metric stretching vibration of the carboxylate group is in linewith a monodentate type of coordination [29] In addition1092 cmminus1 is the specific absorption peak about the CndashNvibrations Compared with the Na

2H2edta ligand the CndashN

at 1137 cmminus1 shifts towards lower frequencies and it confirmsthat the nitrogen atoms of the ligand are coordinated to theSb(III) ion In the far-infrared region the absorption peakfound in the 378 cmminus1 region is assigned to the ](SbndashN)vibration and in the 317 cmminus1 region is assigned to the ](SbndashO) stretching vibration

34Thermal Analysis The thermal decomposition process ofcomplexes can help us understand the coordination structure


Table 4 Experimental data and calculated results for powder X-raydiffraction pattern of the complex [Sb(Hedta)]sdot2H2O (orthorhom-bic system 119886 = 18479 A 119887 = 10957 A and 119888 = 7343 A)

No 2120579 (∘) ℎ 119896 119897 119889exp (A) 119889cal (A) 119868119868

0

1 956 2 0 0 9242 9240 10002 1252 2 1 0 7064 7063 153 1296 1 0 1 6827 6824 124 1451 0 1 1 6100 6100 955 1530 1 1 1 5788 5792 4266 1617 0 2 0 5477 5478 167 1685 1 2 0 5256 5253 1728 1741 2 1 1 5090 5091 529 1811 2 2 0 4713 4712 2110 1919 4 0 0 4621 4620 8511 2048 3 1 1 4332 4334 5512 2085 4 1 0 4257 4257 9713 2169 3 2 0 4094 4094 3014 2240 2 2 1 3966 3966 4515 2415 4 1 1 3682 3683 2716 2486 1 3 0 3579 3583 0917 2610 2 0 2 3411 3412 2818 2737 2 1 2 3256 3258 1819 2821 3 0 2 3160 3154 5920 2895 6 0 0 3081 3080 9421 2969 1 2 2 3007 3009 11822 3112 4 0 2 2871 2874 10623 3161 5 2 1 2828 2828 1324 3273 3 2 2 2733 2733 5025 3300 1 4 0 2712 2710 3626 3354 4 3 1 2670 2669 1127 3410 2 4 0 2627 2626 3428 3524 1 4 1 2544 2542 1129 3584 3 4 0 2503 2503 3530 3707 1 0 3 2423 2426 10231 3780 7 2 0 2378 2378 3032 3811 2 0 3 2360 2366 6733 3895 2 1 3 2311 2313 3434 3981 4 3 2 2262 2259 0835 4018 4 4 1 2242 2244 2536 4050 1 2 3 2225 2219 1237 4095 0 4 2 2202 2196 0938 4139 2 2 3 2178 2172 1739 4177 4 0 3 2161 2163 1240 4228 7 0 2 2137 2143 1141 4331 1 5 1 2087 2086 1942 4519 4 2 3 2006 2012 1343 4569 2 3 3 1984 1986 4144 4662 8 3 0 1947 1952 1345 4718 3 3 3 1926 1931 1246 4817 5 4 2 1888 1888 1847 4893 4 3 3 1860 1861 18

Table 4 Continued

No 2120579 (∘) ℎ 119896 119897 119889exp (A) 119889cal (A) 119868119868

0

48 4989 0 4 3 1826 1825 1949 5090 2 4 3 1792 1791 1050 5392 4 4 3 1698 1697 1351 5845 3 6 2 1578 1580 0852 5877 0 7 0 1569 1565 0853 5994 2 7 0 1542 1543 1254 6066 0 4 4 1525 1525 1155 6179 5 3 4 1500 1499 0956 6446 2 1 5 1442 1438 0957 6757 2 5 4 1388 1391 09

100 200 300 400 500 600 7000

20

40

60

80

100

1285Wei

ght (

)

814

4455

19110

20

40

60

80

100

Temperature (∘C)

minus20

DSC

(Wmiddotm

gminus1)

534∘C

330∘C

294∘C

492∘C

81∘C

Figure 6 TG-DSC curves of the title complex

of the complexes [30] The TG-DSC curves of the titlecomplex are given in Figure 6 and the possible pyrolysisreaction and the experimental and calculated percentagemass losses in the thermal decomposition process of thecomplex are summarized in Table 5The first mass loss of thecomplex [Sb(Hedta)]sdot2H

2O occurs about 81∘C in DSC curve

corresponding to the release of two molecules in crystallinewater This is consistent with the single crystal structureThe experimental percentage mass loss (814) is close tothe calculated one (806) Then a small endothermic peakin DSC curve appears at 294∘C Because there is not anycorresponding mass loss of the sample in the TG curve itcan be attributable to structure rearrangement or phase trans-formation in the solid complex Thereafter the exothermicpeak at 330∘C corresponds to oxidation and decompositionof the ligand and the experimental mass loss (4455) isclose to the calculated one (4457)This step decompositionproduct is Sb

2(CO3)3 Then Sb

2(CO3)3is decomposed into

Sb2O4(Scheme 1) and the experimental and theoretical mass

losses are 1285 and 1298 respectively This is why thereis an appreciable endothermic peak at 492∘C in DSC curveHowever some of the compounds of antimony may bevolatile at high temperature The final step of the exothermicpeak appears at 534∘C in DSC curve The SbndashO single bondis ruptured and then half of the antimony compound may


Table 5 Thermal decomposition data of the title complex

Reaction DSC (∘C) Mass loss ()119882exp 119882theor

[Sb(Hedta)]sdot2H2Odarr minus2H2O 81 (endo) 814 806[Sb(Hedta)]darr structural rearrangement 294 (endo)[Sb(Hedta)]darr minusC85H13N2O35 330 (exo) 4455 4457

12Sb2(CO3)3darr minusC3O5 492 (exo) 1285 1298

12Sb2O4

darr minusSb05O125 534 (endo) 1911 180914Sb2O3 1535a 1630baThe experimental percentage mass of the residue in the sample bthe calculated percentage mass of the residue in the sample

O Sb

O

O Sb O

Scheme 1 Structure of the Sb2O4

be oxidized and volatilized The final residue is antimonousoxide and the experimental result (1535) is in agreementwith the result of theoretical calculation (1630)

4 Conclusion

The complex [Sb(Hedta)]sdot2H2O was synthesized with the

reaction of ethylenediaminetetraacetic acid and antimonousoxide as the reactants The composition and structure ofthe complex were characterized by EA singlerystal X-raydiffraction XRD FTIR and TG-DSC The crystal structureof the complex belongs to orthorhombic system space groupPna2(1) with cell parameters of 119886 = 184823(18) A 119887 =109408(12) A 119888 = 73671(5) A 119885 = 4 and 119863

119888=

1993 g cmminus3 Sb(III) ion is five-coordinated by two amidoN atoms and three carboxyl O atoms from a single Hedta3minusligand forming a distorted trigonal bipyramid geometry

5 Extra Material

Crystallographic data for the title complex [Sb(Hedta)]sdot2H2O

has been deposited with the Cambridge CrystallographicData Centre The deposition number is CCDC-953660 Thedata can be obtained free of charge on application to theDirector CCDC 12 Union Road Cambridge CB2 1EZ UKfax +44 1223 366 033 e-mail depositccdcacuk or on theweb www httpwwwccdccamacuk or from the authorsup on request

Conflict of Interests

The authors declare that there is no conflict of interestsregarding the publication of this paper

Acknowledgments

The authors gratefully acknowledge the financial supportfrom the National Natural Science Foundation of China(no 21201142) and the Scientific Research Funds of SichuanProvincial Education Department of China (no 10ZA016)The authors are very grateful to State Key Laboratory Cultiva-tion Base for Nonmetal Composite and Functional Materialsand Engineering Research Center of Biomass Materials ofEducation Ministry for the testing

References

[1] J A Lessa D C Reis I C Mendes et al ldquoAntimony(III) com-plexes with pyridine-derived thiosemicarbazones structuralstudies and investigation on the antitrypanosomal activityrdquoPolyhedron vol 30 no 2 pp 372ndash380 2011

[2] D C Reis M C X Pinto E M Souza-Fagundes S M S VWardell J L Wardell and H Beraldo ldquoAntimony(III) com-plexes with 2-benzoylpyridine-derived thiosemicarbazonescytotoxicity against human leukemia cell linesrdquo European Jour-nal of Medicinal Chemistry vol 45 no 9 pp 3904ndash3910 2010

[3] A Y Robin and K M Fromm ldquoCoordination polymer net-works with O- and N-donors what they are why and how theyare maderdquo Coordination Chemistry Reviews vol 250 no 15-16pp 2127ndash2157 2006

[4] J Cui Y Li Z Guo and H Zheng ldquoA porous metal-organicframework based on Zn

6O2clusters chemical stability gas

adsorption properties and solvatochromic behaviorrdquo ChemicalCommunications vol 49 no 6 pp 555ndash557 2013

[5] GH Cui CHHe CH Jiao J C Geng andV A Blatov ldquoTwometal-organic frameworks with unique high-connected bin-odal network topologies synthesis structures and catalyticpropertiesrdquo Chemical Engineering Communications vol 14 no12 pp 4210ndash4216 2012


[6] X L Zhao D Sun S Yuan et al ldquoComparison of the effectof functional groups on gas-uptake capacities by fixing thevolumes of cages A and B and modifying the inner wall of cageC in rht-type MOFsrdquo Inorganic Chemistry vol 51 no 19 pp10350ndash10355 2012

[7] S R Kim K W Dawson B S Gelfand J M Taylor and G KShimizu ldquoEnhancing proton conduction in a metal-organicframework by isomorphous ligand replacementrdquo Journal of theAmerican Chemical Society vol 135 no 3 pp 963ndash966 2013

[8] X T Zhang D Sun B Li L M Fan B Li and P H WeildquoUnusual high thermal stablility of a 2Drarr 3D polycatenatedFe(II) metal-organic framework showing guest-dependentspin-crossover behavior and high spin-transition temperaturerdquoCrystal Growth amp Design vol 12 no 8 pp 3845ndash3848 2012

[9] J-P Zhang Y-B Zhang J-B Lin and X-M Chen ldquoMetal azo-late frameworks from crystal engineering to functional materi-alsrdquo Chemical Reviews vol 112 no 2 pp 1001ndash1033 2012

[10] D Sun G-G Luo N Zhang R-B Huang and L-S ZhengldquoSimultaneous self-assembly of a cage-like silver(i) complexencapsulating an Ag6 neutral cluster core and carbon dioxidefixationrdquo Chemical Communications vol 47 no 5 pp 1461ndash1463 2011

[11] D Banerjee and J B Parise ldquoRecent advances in s-block metalcarboxylate networksrdquo Crystal Growth and Design vol 11 no10 pp 4704ndash4720 2011

[12] K C Atwood IV E Woockner R S Baratz and W ISampson ldquoWhy the NIH Trial to Assess Chelation Therapy(TACT) should be abandonedrdquoMedGenMedMedscape GeneralMedicine vol 10 no 5 article 115 2008

[13] W Blumer and E M Cranton ldquoNinety percent reduction incancer mortality after chelation therapy with EDTArdquo Journal ofAdvancement in Medicine vol 2 no 1-2 pp 183ndash188 1989

[14] A M van Rij C Solomon S G K Packer and W G HopkinsldquoChelation therapy for intermittent claudication a double-blind randomized controlled trialrdquo Circulation vol 90 no 3pp 1194ndash1199 1994

[15] E Ernst ldquoChelation therapy for coronary heart disease an over-view of all clinical investigationsrdquo American Heart Journal vol140 no 1 pp 139ndash141 2000

[16] M L Knudtson D G Wyse P D Galbraith et al ldquoChelationtherapy for ischemic heart disease a randomized controlledtrialrdquo Journal of the American Medical Association vol 287 no4 pp 481ndash486 2002

[17] G Q Zhong and Y C Guo ldquoStudies on synthesis and indexesof X-ray powder diffraction data of hydrogen ethylenediamineterraacetato-antimony(III) monohydraterdquo Journal of ChangdeTeachers University vol 14 no 3 pp 39ndash42 2002

[18] A-K Leuz H Monch and C A Johnson ldquoSorption of Sb(III)and Sb(V) to goethite influence on Sb(III) oxidation andmobilizationrdquo Environmental Science and Technology vol 40no 23 pp 7277ndash7282 2006

[19] M Filella N Belzile and Y-W Chen ldquoAntimony in theenvironment a review focused on natural waters II Relevantsolution chemistryrdquo Earth-Science Reviews vol 59 no 1ndash4 pp265ndash285 2002

[20] S Rais A Perianin M Lenoir et al ldquoSodium stibogluconate(Pentostam) potentiates oxidant production in murine visceralleishmaniasis and in human bloodrdquo Antimicrobial Agents andChemotherapy vol 44 no 9 pp 2406ndash2410 2000

[21] R C Palenik K A Abboud and G J Palenik ldquoBond valencesums and structural studies of antimony complexes containing

Sb bonded only toO ligandsrdquo Inorganica Chimica Acta vol 358no 4 pp 1034ndash1040 2005

[22] G Cantos C L Barbieri M Iacomini P A J Gorin and L RTravassos ldquoSynthesis of antimony complexes of yeast mannanandmannanderivatives and their effect on Leishmania-infectedmacrophagesrdquo Biochemical Journal vol 289 no 1 pp 155ndash1601993

[23] J Shen B Jin Q Jiang G Zhong Y Hu and J Huo ldquoSynthesischaracterization and magnetic properties of heterometallictrinuclear complex with Sb(III) and Ho(III)rdquo Inorganica Chim-ica Acta vol 385 pp 158ndash163 2012

[24] P Sharma D Perez A Cabrera N Rosas and J L AriasldquoPerspectives of antimony compounds in oncologyrdquo Acta Phar-macologica Sinica vol 29 no 8 pp 881ndash890 2008

[25] S K Hadjikakou C D Antoniadis N Hadjiliadis et al ldquoSyn-thesis and characterization of new water stable antimony(III)complex with pyrimidine-2-thione and in vitro biologicalstudyrdquo Inorganica Chimica Acta vol 358 no 10 pp 2861ndash28662005

[26] G M Sheldrick SHELXS 97 Program for the Solution of CrystalStructure University of Gottingen 1997

[27] G M Sheldrick SHELXS 97 Program for the Refinement ofCrystal Structure University of Gottingen 1997

[28] M Shimoi Y Orita T Uehiro et al ldquoThe Structure of(hydrogen ethylenediaminetetraacetato) antimony(III) dihy-drate Sb(C

10H13N2O8)sdot2H2Ordquo Bulletin of the Chemical Society

of Japan vol 53 no 11 pp 3189ndash3194 1980[29] G-Q Zhong Y-C Guo Y-R Chen X-S Zang and S-R Luan

ldquoSynthesis and crystal structure of the complex of thioglycollicacid and trivalent antimony ionrdquo Acta Chimica Sinica vol 59no 10 pp 1599ndash1603 2001

[30] G Q Zhong J Shen Q Y Jiang Y Q Jia M J Chenand Z P Zhang ldquoSynthesis characterization and thermaldecompositionof SbIII-M-SbIII type trinuclear complexes ofethylenediamine-N N N1015840 N1015840-tetraacetate (MCo(II) La(III)Nd(III) Dy(III))rdquo Journal ofThermal Analysis and Calorimetryvol 92 no 2 pp 607ndash616 2008


Table 1 Crystal data and structure refinement for the title complex

Empirical formula SbC10H17N2O10 119865(000) 888Formula weight 44701 Crystal size 046mm times 040mm times 035mmWavelength 071073 A Theta range for data collection 289ndash2502∘

Temperature 298(2) K Limiting indices minus21 le ℎ le 16 minus13 le 119896 le 13 minus7 le 119897 le 8Crystal system Orthorhombic Reflections collectedunique 71022529 [R(int) = 00461]Space group Pna2(1) Completeness to theta = 2502 999Unit cell dimensions Absorption correction Semiempirical from equivalents119886 184823(18) A Max and min transmission 05547 and 04738119887 109408(12) A Refinement method Full-matrix least-squares on 1198652

119888 73671(5) A Daterestraintsparameters 25291208120573 9000∘ Goodness-of-fit on 1198652 1040119881 14897(2) A3 Final 119877 indices [119868 gt 2120590(119868)] R1 = 00332 119908119877

2= 00811

119885 4 119877 indices (all data) R1 = 00359 1199081198772= 00832

Calculated density 1993 g cmminus3 Absolute structure parameter minus027(4)Absorption coefficient 1909mmminus1 Largest diff peak and hole 0786 and minus0805 e Aminus3

In recent years owing to the development of aminopoly-carboxylic acid complexes of antimony(III) in medicinethe complex of antimony with multicarboxylate ligands hasreceived more and more attention Herein we report thesyntheses of the title complex [Sb(Hedta)]sdot2H

2OThe compo-

sition and crystal structure of the complex have been charac-terized by elemental analysis single crystal X-ray diffractionXRD FTIR and TG-DSC

2 Experimental

21 Materials and General Methods All the chemicals usedin the experiments were analytical reagent as received fromcommercial sources and without further purification Theethylenediaminetetraacetic acid and antimonous oxide werepurchased from Shanghai Reagent Industry

The antimony was determined by a Thermo X-II induc-tively coupled plasma mass spectrometer The content of car-bon hydrogen and nitrogen in the complex wasmeasured bya Vario EL CUBE elemental analyzer The IR spectra wereobtained with a Perkin-Elmer Spectrum One-spectrometerin the range of 225ndash4000 cmminus1 using KBr pellets The ther-mogravimetric analysis of the metal complex was performedby an SDT Q600 thermogravimetric analyzer and the mea-surement was recorded from 30 to 800∘C at the heating rateof 10∘C minminus1 under air flow of 100mLminminus1 The X-raypowder diffraction was performed using a Dmax-II X-raydiffractometer CuK

120572radiation (120582= 0154056 nm stepwidth

2120579 = 02∘ scan speed 8∘min)

22 Synthesis of the Complex [Sb(Hedta)]sdot2H2O The title

complex was obtained by aqueous solution synthesis First146 g (5mmol) ethylenediaminetetraacetic acid was solubi-lized in 200mLboiling distilledwaterThen 0875 g (3mmol)antimonous oxide was gradually added to the above solutionstirring and maintaining the temperature at 90∘C After fourhours when the pH was about 2-3 the reaction was stoppedThe unreacted antimonous oxide was filtered The colorless

filtrate was slowly concentrated to 100mL The concentratedsolution was placed at room temperature for about one weekand the colorless flaky crystals of the antimony(III) complexwas obtained The yield was about 82 Anal Calcd for thetitle complex SbC

10H17N2O10() Sb 2724 C 2687 N 627

H 383 Found () Sb 2711 C 2668 N 619 H 374

23 X-Ray Diffraction Crystallography The appropriate crys-tals were cut from larger crystals and mounted on a BrukerSmart Apex II CCD diffractometer with graphite monochro-mated Mo K

120572radiation (120582 = 071073 A) The data were

collected at 298(2) K A colorless and transparent crystal withdimensions 046mm times 040mm times 035mm was mountedon a glass fiber Diffraction data were collected in 120596 modein the range of 289∘ndash2502∘ The structure was solved bydirect methods SHELXS-97 and refined by full-matrix least-squares using SHELXL-97 [26 27] All nonhydrogen atomswere obtained from the difference Fourier map and full-matrix least-squares refinements on 1198652 were carried out withanisotropic thermal parameters Hydrogen atoms of the lig-and were generated geometrically The structure refinementparameters for the title complex are given in Table 1 and thecrystallographic data are depositedwith theCambridgeCrys-tallographic Data Centre under deposition number CCDC953660

3 Results and Discussion

31 X-Ray Crystal Structure Analysis The single crystal X-ray diffraction analysis reveals that the complex [Sb(Hedta)]sdot2H2O crystallises in the orthorhombic system with space

group Pna2(1) Crystallographic data and structure refine-ment parameters for the title complex are given inTable 1 andthe selected bond distances and angles are shown in Table 2The key fragments of the structures and the atom numberingare shown in Figure 1 and the crystal packing diagram ofthe complex is shown in Figure 2 The asymmetric unit ofthe complex consists of one Hedta3minus one trivalent antimony






2

119910 +

1

2

119911 +

1

2

]


]


2

119910 minus

1

2

119911 +

1

2

]

O10

O9

O6 O4

O7

C9

C8

O5 O3 C5

Sb1

C6

N1

C10 O1C3

O2

C4N2 C1

O8

C2

C7









b

0

c

a

c


c

a








10 20 30 40 50 60 70 800

5000

10000

15000

20000

25000

10 20 30 40 50 60 70 80

Inte

nsity

(au

)

(a)

(b)

2120579 (∘)


4000 3500 3000 2500 2000 1500 1000 500

0

20

40

60

80

100T

() 35

6834

65 2968

1654

1416

1364

1308

1092

918 86

073

7 663

458

378

125130

17

2927

1038

317











No 2120579 (∘) ℎ 119896 119897 119889exp (A) 119889cal (A) 119868119868

0

1 956 2 0 0 9242 9240 10002 1252 2 1 0 7064 7063 153 1296 1 0 1 6827 6824 124 1451 0 1 1 6100 6100 955 1530 1 1 1 5788 5792 4266 1617 0 2 0 5477 5478 167 1685 1 2 0 5256 5253 1728 1741 2 1 1 5090 5091 529 1811 2 2 0 4713 4712 2110 1919 4 0 0 4621 4620 8511 2048 3 1 1 4332 4334 5512 2085 4 1 0 4257 4257 9713 2169 3 2 0 4094 4094 3014 2240 2 2 1 3966 3966 4515 2415 4 1 1 3682 3683 2716 2486 1 3 0 3579 3583 0917 2610 2 0 2 3411 3412 2818 2737 2 1 2 3256 3258 1819 2821 3 0 2 3160 3154 5920 2895 6 0 0 3081 3080 9421 2969 1 2 2 3007 3009 11822 3112 4 0 2 2871 2874 10623 3161 5 2 1 2828 2828 1324 3273 3 2 2 2733 2733 5025 3300 1 4 0 2712 2710 3626 3354 4 3 1 2670 2669 1127 3410 2 4 0 2627 2626 3428 3524 1 4 1 2544 2542 1129 3584 3 4 0 2503 2503 3530 3707 1 0 3 2423 2426 10231 3780 7 2 0 2378 2378 3032 3811 2 0 3 2360 2366 6733 3895 2 1 3 2311 2313 3434 3981 4 3 2 2262 2259 0835 4018 4 4 1 2242 2244 2536 4050 1 2 3 2225 2219 1237 4095 0 4 2 2202 2196 0938 4139 2 2 3 2178 2172 1739 4177 4 0 3 2161 2163 1240 4228 7 0 2 2137 2143 1141 4331 1 5 1 2087 2086 1942 4519 4 2 3 2006 2012 1343 4569 2 3 3 1984 1986 4144 4662 8 3 0 1947 1952 1345 4718 3 3 3 1926 1931 1246 4817 5 4 2 1888 1888 1847 4893 4 3 3 1860 1861 18

Table 4 Continued

No 2120579 (∘) ℎ 119896 119897 119889exp (A) 119889cal (A) 119868119868

0

48 4989 0 4 3 1826 1825 1949 5090 2 4 3 1792 1791 1050 5392 4 4 3 1698 1697 1351 5845 3 6 2 1578 1580 0852 5877 0 7 0 1569 1565 0853 5994 2 7 0 1542 1543 1254 6066 0 4 4 1525 1525 1155 6179 5 3 4 1500 1499 0956 6446 2 1 5 1442 1438 0957 6757 2 5 4 1388 1391 09

100 200 300 400 500 600 7000

20

40

60

80

100

1285Wei

ght (

)

814

4455

19110

20

40

60

80

100

Temperature (∘C)

minus20

DSC

(Wmiddotm

gminus1)

534∘C

330∘C

294∘C

492∘C

81∘C





2(CO3)3 Then Sb









12Sb2O4


O Sb

O

O Sb O



4 Conclusion



119888=


5 Extra Material





Acknowledgments


References










































2

119910 +

1

2

119911 +

1

2

]


]


2

119910 minus

1

2

119911 +

1

2

]

O10

O9

O6 O4

O7

C9

C8

O5 O3 C5

Sb1

C6

N1

C10 O1C3

O2

C4N2 C1

O8

C2

C7









b

0

c

a

c


c

a








10 20 30 40 50 60 70 800

5000

10000

15000

20000

25000

10 20 30 40 50 60 70 80

Inte

nsity

(au

)

(a)

(b)

2120579 (∘)


4000 3500 3000 2500 2000 1500 1000 500

0

20

40

60

80

100T

() 35

6834

65 2968

1654

1416

1364

1308

1092

918 86

073

7 663

458

378

125130

17

2927

1038

317











No 2120579 (∘) ℎ 119896 119897 119889exp (A) 119889cal (A) 119868119868

0

1 956 2 0 0 9242 9240 10002 1252 2 1 0 7064 7063 153 1296 1 0 1 6827 6824 124 1451 0 1 1 6100 6100 955 1530 1 1 1 5788 5792 4266 1617 0 2 0 5477 5478 167 1685 1 2 0 5256 5253 1728 1741 2 1 1 5090 5091 529 1811 2 2 0 4713 4712 2110 1919 4 0 0 4621 4620 8511 2048 3 1 1 4332 4334 5512 2085 4 1 0 4257 4257 9713 2169 3 2 0 4094 4094 3014 2240 2 2 1 3966 3966 4515 2415 4 1 1 3682 3683 2716 2486 1 3 0 3579 3583 0917 2610 2 0 2 3411 3412 2818 2737 2 1 2 3256 3258 1819 2821 3 0 2 3160 3154 5920 2895 6 0 0 3081 3080 9421 2969 1 2 2 3007 3009 11822 3112 4 0 2 2871 2874 10623 3161 5 2 1 2828 2828 1324 3273 3 2 2 2733 2733 5025 3300 1 4 0 2712 2710 3626 3354 4 3 1 2670 2669 1127 3410 2 4 0 2627 2626 3428 3524 1 4 1 2544 2542 1129 3584 3 4 0 2503 2503 3530 3707 1 0 3 2423 2426 10231 3780 7 2 0 2378 2378 3032 3811 2 0 3 2360 2366 6733 3895 2 1 3 2311 2313 3434 3981 4 3 2 2262 2259 0835 4018 4 4 1 2242 2244 2536 4050 1 2 3 2225 2219 1237 4095 0 4 2 2202 2196 0938 4139 2 2 3 2178 2172 1739 4177 4 0 3 2161 2163 1240 4228 7 0 2 2137 2143 1141 4331 1 5 1 2087 2086 1942 4519 4 2 3 2006 2012 1343 4569 2 3 3 1984 1986 4144 4662 8 3 0 1947 1952 1345 4718 3 3 3 1926 1931 1246 4817 5 4 2 1888 1888 1847 4893 4 3 3 1860 1861 18

Table 4 Continued

No 2120579 (∘) ℎ 119896 119897 119889exp (A) 119889cal (A) 119868119868

0

48 4989 0 4 3 1826 1825 1949 5090 2 4 3 1792 1791 1050 5392 4 4 3 1698 1697 1351 5845 3 6 2 1578 1580 0852 5877 0 7 0 1569 1565 0853 5994 2 7 0 1542 1543 1254 6066 0 4 4 1525 1525 1155 6179 5 3 4 1500 1499 0956 6446 2 1 5 1442 1438 0957 6757 2 5 4 1388 1391 09

100 200 300 400 500 600 7000

20

40

60

80

100

1285Wei

ght (

)

814

4455

19110

20

40

60

80

100

Temperature (∘C)

minus20

DSC

(Wmiddotm

gminus1)

534∘C

330∘C

294∘C

492∘C

81∘C





2(CO3)3 Then Sb









12Sb2O4


O Sb

O

O Sb O



4 Conclusion



119888=


5 Extra Material





Acknowledgments


References






































b

0

c

a

c


c

a








10 20 30 40 50 60 70 800

5000

10000

15000

20000

25000

10 20 30 40 50 60 70 80

Inte

nsity

(au

)

(a)

(b)

2120579 (∘)


4000 3500 3000 2500 2000 1500 1000 500

0

20

40

60

80

100T

() 35

6834

65 2968

1654

1416

1364

1308

1092

918 86

073

7 663

458

378

125130

17

2927

1038

317











No 2120579 (∘) ℎ 119896 119897 119889exp (A) 119889cal (A) 119868119868

0

1 956 2 0 0 9242 9240 10002 1252 2 1 0 7064 7063 153 1296 1 0 1 6827 6824 124 1451 0 1 1 6100 6100 955 1530 1 1 1 5788 5792 4266 1617 0 2 0 5477 5478 167 1685 1 2 0 5256 5253 1728 1741 2 1 1 5090 5091 529 1811 2 2 0 4713 4712 2110 1919 4 0 0 4621 4620 8511 2048 3 1 1 4332 4334 5512 2085 4 1 0 4257 4257 9713 2169 3 2 0 4094 4094 3014 2240 2 2 1 3966 3966 4515 2415 4 1 1 3682 3683 2716 2486 1 3 0 3579 3583 0917 2610 2 0 2 3411 3412 2818 2737 2 1 2 3256 3258 1819 2821 3 0 2 3160 3154 5920 2895 6 0 0 3081 3080 9421 2969 1 2 2 3007 3009 11822 3112 4 0 2 2871 2874 10623 3161 5 2 1 2828 2828 1324 3273 3 2 2 2733 2733 5025 3300 1 4 0 2712 2710 3626 3354 4 3 1 2670 2669 1127 3410 2 4 0 2627 2626 3428 3524 1 4 1 2544 2542 1129 3584 3 4 0 2503 2503 3530 3707 1 0 3 2423 2426 10231 3780 7 2 0 2378 2378 3032 3811 2 0 3 2360 2366 6733 3895 2 1 3 2311 2313 3434 3981 4 3 2 2262 2259 0835 4018 4 4 1 2242 2244 2536 4050 1 2 3 2225 2219 1237 4095 0 4 2 2202 2196 0938 4139 2 2 3 2178 2172 1739 4177 4 0 3 2161 2163 1240 4228 7 0 2 2137 2143 1141 4331 1 5 1 2087 2086 1942 4519 4 2 3 2006 2012 1343 4569 2 3 3 1984 1986 4144 4662 8 3 0 1947 1952 1345 4718 3 3 3 1926 1931 1246 4817 5 4 2 1888 1888 1847 4893 4 3 3 1860 1861 18

Table 4 Continued

No 2120579 (∘) ℎ 119896 119897 119889exp (A) 119889cal (A) 119868119868

0

48 4989 0 4 3 1826 1825 1949 5090 2 4 3 1792 1791 1050 5392 4 4 3 1698 1697 1351 5845 3 6 2 1578 1580 0852 5877 0 7 0 1569 1565 0853 5994 2 7 0 1542 1543 1254 6066 0 4 4 1525 1525 1155 6179 5 3 4 1500 1499 0956 6446 2 1 5 1442 1438 0957 6757 2 5 4 1388 1391 09

100 200 300 400 500 600 7000

20

40

60

80

100

1285Wei

ght (

)

814

4455

19110

20

40

60

80

100

Temperature (∘C)

minus20

DSC

(Wmiddotm

gminus1)

534∘C

330∘C

294∘C

492∘C

81∘C





2(CO3)3 Then Sb









12Sb2O4


O Sb

O

O Sb O



4 Conclusion



119888=


5 Extra Material





Acknowledgments


References







































No 2120579 (∘) ℎ 119896 119897 119889exp (A) 119889cal (A) 119868119868

0

1 956 2 0 0 9242 9240 10002 1252 2 1 0 7064 7063 153 1296 1 0 1 6827 6824 124 1451 0 1 1 6100 6100 955 1530 1 1 1 5788 5792 4266 1617 0 2 0 5477 5478 167 1685 1 2 0 5256 5253 1728 1741 2 1 1 5090 5091 529 1811 2 2 0 4713 4712 2110 1919 4 0 0 4621 4620 8511 2048 3 1 1 4332 4334 5512 2085 4 1 0 4257 4257 9713 2169 3 2 0 4094 4094 3014 2240 2 2 1 3966 3966 4515 2415 4 1 1 3682 3683 2716 2486 1 3 0 3579 3583 0917 2610 2 0 2 3411 3412 2818 2737 2 1 2 3256 3258 1819 2821 3 0 2 3160 3154 5920 2895 6 0 0 3081 3080 9421 2969 1 2 2 3007 3009 11822 3112 4 0 2 2871 2874 10623 3161 5 2 1 2828 2828 1324 3273 3 2 2 2733 2733 5025 3300 1 4 0 2712 2710 3626 3354 4 3 1 2670 2669 1127 3410 2 4 0 2627 2626 3428 3524 1 4 1 2544 2542 1129 3584 3 4 0 2503 2503 3530 3707 1 0 3 2423 2426 10231 3780 7 2 0 2378 2378 3032 3811 2 0 3 2360 2366 6733 3895 2 1 3 2311 2313 3434 3981 4 3 2 2262 2259 0835 4018 4 4 1 2242 2244 2536 4050 1 2 3 2225 2219 1237 4095 0 4 2 2202 2196 0938 4139 2 2 3 2178 2172 1739 4177 4 0 3 2161 2163 1240 4228 7 0 2 2137 2143 1141 4331 1 5 1 2087 2086 1942 4519 4 2 3 2006 2012 1343 4569 2 3 3 1984 1986 4144 4662 8 3 0 1947 1952 1345 4718 3 3 3 1926 1931 1246 4817 5 4 2 1888 1888 1847 4893 4 3 3 1860 1861 18

Table 4 Continued

No 2120579 (∘) ℎ 119896 119897 119889exp (A) 119889cal (A) 119868119868

0

48 4989 0 4 3 1826 1825 1949 5090 2 4 3 1792 1791 1050 5392 4 4 3 1698 1697 1351 5845 3 6 2 1578 1580 0852 5877 0 7 0 1569 1565 0853 5994 2 7 0 1542 1543 1254 6066 0 4 4 1525 1525 1155 6179 5 3 4 1500 1499 0956 6446 2 1 5 1442 1438 0957 6757 2 5 4 1388 1391 09

100 200 300 400 500 600 7000

20

40

60

80

100

1285Wei

ght (

)

814

4455

19110

20

40

60

80

100

Temperature (∘C)

minus20

DSC

(Wmiddotm

gminus1)

534∘C

330∘C

294∘C

492∘C

81∘C





2(CO3)3 Then Sb









12Sb2O4


O Sb

O

O Sb O



4 Conclusion



119888=


5 Extra Material





Acknowledgments


References










































12Sb2O4


O Sb

O

O Sb O



4 Conclusion



119888=


5 Extra Material





Acknowledgments


References





































synthesis and crystal structure of the bioinorganic ...€¦ · 2...

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