producedsolved
solved 时间:2021-01-17 阅读:()
1ElectronicSupplementaryInformationIonizedFormofAcetaminophenwithImprovedCompactionPropertiesSathyanarayanaReddyPerumalla,LiminShi,andDepartmentofPharmaceutics,CollegeofPharmacy,UniversityofMinnesota,9-127BWeaver-DensfordHall,ChangquanCalvinSun*308HarvardStreetS.
E.
,Minneapolis,MN55455.
Fax:612-626-2125;Tel:612-624-3722;Email:sunx0053@umn.
eduS1.
Syntheticprocedurefor1.
FigureS1.
X-RaydifferenceFouriermapintheregionoftheatomsO(7)andO(100)inthecrystalstructureof1.
FigureS2.
ORTEPdiagramofasymmetricunitof2.
S2.
MechanicalpropertiesdeterminedbynanoindentationFigureS3.
Nanoindentationload-unloadcurvesofACMFormIand1.
S3.
PowdercompactionS4.
PowderX-raydiffractometryFigureS4.
CalculatedandmeasuredPXRDpatternsof1forbulkpowder.
S5.
X-RaycrystallographicdatacollectionstrategyandrefinementTableS1.
X-Raycrystaldataandstructurerefinementfor1.
TableS2.
X-Raycrystaldataandstructurerefinementfor2.
References2S1.
Synthesisof1:Acetaminophen(ACM,302mg)wasdissolvedinCon.
HCl(1.
6mL)withslightheatingthencooledtoroomtemperature.
Singlecrystalsof1suitableforstructuredeterminationbyX-raydiffractionmethodwereformedwithin30min.
AnX-raydifferenceFouriermaprevealsthatthesiteofprotonationistheamideoxygen,O(7)(FigureS1),whichisconsistentwiththeobservationmadeinliterature(Refs4and7inthepaper).
FigureS1.
X-RaydifferenceFouriermapintheregionoftheatomsO(7)andO(100)inthecrystalstructureof1.
Thesinglemaximumof0.
63e-3neartheatomO7correspondstoprotonatedhydrogen;itsdistancefromO(7)is0.
89,anditsdistancefromO(100)is1.
61.
Wepreparedbulkpowdersof1byeitherlinearlyscalinguptheabove-mentionedreactionorbysuspendingACM(15g)inCon.
HCl(75mL)atroomtemperaturefor12hours.
Ifprolongedheatingisapplied,crystalsof2areproduced(FigureS2).
3FigureS2.
ORTEPdiagramofasymmetricunitof2.
S2.
MechanicalpropertiesdeterminedbynanoindentationCrystalhardness,H,weredeterminedusingananoindenter(TriboIndenterTI-900,HysitronInc.
,MN,USA)withaBerkovichdiamondindentertip.
Beforenanoindentationtesting,thetipareafunctionwasderivedfromaseriesofindentationsonafusedquartzstandard.
Thenanoindentationexperimentswereperformedunderthedisplacementcontrolmode.
Theratesofloadingandunloadingwereboth100nm/sanda10sholdingwasappliedatthemaximumindentationdepthof500nm.
Nanoindentationdatawereanalyzedfollowingthestandardprocedure.
S1RepresentativenanoindentationdataforACMFormIand1areshowninFigureS3.
40100200300400500012341Load(mN)Displacement(nm)FormIFigureS3.
Nanoindentationload-unloadcurvesofACMFormIand1.
Amuchlowerforceisrequiredtomakeanindentofthesamesizeon1thanonACM.
S3.
PowdercompactionAmaterialtestingmachine(model1485,Zwick/Roell,Kennesaw,GA)wasusedtoperformcompactionstudyofbulkpowderof1ataloadingrateof1mm/s.
Powderwasgrindedinamortarusingapestletoreduceparticlesizebeforecompactionstudiesatpressuresrangingfrom25to350MPa,whereadie(round,8mmdiameter)andflat-facedpuncheslubricatedwithmagnesiumstearatewereemployed.
Tabletswererelaxedunderambientenvironmentfor24hbeforemeasuringdiametricalbreakingforceusingatextureanalyzer(TA-XT2i,TextureTechnologiesCorp.
,Scarsdale,NY).
Tablettensilestrengthwascalculatedfromthebreakingforceandtabletdimensionsfollowingstandardprocedure.
S25S4.
PowderX-raydiffractometryX-Raypowderdiffractogramwasobtainedonawide-anglediffractometer(D5005,BruckerAXS).
CuKαradiationwasused.
Thevoltageandcurrentappliedwere45kVand40mArespectively.
Themeasurementwasperformedwithastepsizeof0.
02ofrom5oto35o681012141618202224262830323402040608010012014016018020068101214161820222426283032340204060801001201401601802001recordedRelativeintensityDiffractionangle2θ1calculatedtwothetaandadwelltimeof1s.
PXRDdatawereanalyzedusingacommercialsoftware(JADE,MaterialsDataInc.
,Livermore,CA).
Asidefromthedifferentpeakintensities,whichisattributedtothephenomenonofpreferredorientation,experimentalPXRDpatternofthebulkpowderusedforcompactionmatcheswellwiththecalculatedPXRDpattern(FigureS4).
FigureS4.
CalculatedandmeasuredPXRDpatternsof1forbulkpowder.
6S5.
X-RaycrystallographicdatacollectionstrategyandrefinementSuitablesinglecrystalwasplacedontothetipofa0.
1mmdiameterglassfiberandmountedonaBrukerApexIICCDareadetectordiffractometerfordatacollectionat173(2)KusingMoKαradiation(graphitemonochromator).
S3DataprocessingwasaccomplishedwiththeSAINTprocessingprogram.
ThestructurewassolvedusingBrukerSHELXTLandrefinedusingBrukerSHELXTL.
S4Adirect-methodssolutionwascalculated,whichprovidedmostnon-hydrogenatomsfromtheE-map.
Full-matrixleastsquares/differenceFouriercycleswereperformed,whichlocatedtheremainingnon-hydrogenatoms.
Allnon-hydrogenatomswererefinedwithanisotropicdisplacementparameters.
AllhydrogenatomswerelocatedfromthedifferenceFouriermapandallowedtorideontheirparentatomsintherefinementcycles.
KeycrystaldataanddatacollectionparametersaresummarizedinTableS1andS2for1and2respectively.
DatacollectionandstructuresolutionwereconductedattheX-RayCrystallographicLaboratory,S146KolthoffHall,DepartmentofChemistry,UniversityofMinnesota.
7TableS1.
X-Raycrystaldataandstructurerefinementfor1.
EmpiricalformulaC8H12ClNO3Formulaweight205.
64Temperature173(2)KWavelength0.
71073CrystalsystemMonoclinicSpacegroupP2(1)/cUnitcelldimensionsa=6.
2761(6)α=90°.
b=22.
345(2)β=97.
2570(10)°.
c=6.
8833(7)γ=90°.
Volume957.
56(16)3Z4Density(calculated)1.
426Mg/m3Absorptioncoefficient0.
374mm-1F(000)432Crystalsize0.
36x0.
26x0.
16mm3Thetarangefordatacollection1.
82to26.
84°.
Indexranges-72sigma(I)]R1=0.
0272,wR2=0.
0734Rindices(alldata)R1=0.
0306,wR2=0.
0760Largestdiff.
peakandhole0.
193and-0.
243e.
-38TableS2.
Crystaldataandstructurerefinementfor2.
EmpiricalformulaC6H8ClNOFormulaweight145.
58Temperature173(2)KWavelength0.
71073CrystalsystemMonoclinicSpacegroupP2(1)/cUnitcelldimensionsa=6.
4919(6)α=90°.
b=6.
1159(6)β=90.
0320(10)°.
c=16.
8700(16)γ=90°.
Volume669.
80(11)3Z4Density(calculated)1.
444Mg/m3Absorptioncoefficient0.
480mm-1F(000)304Crystalsize0.
19x0.
16x0.
15mm3Thetarangefordatacollection2.
41to27.
56°.
Indexranges-82sigma(I)]R1=0.
0226,wR2=0.
0658Rindices(alldata)R1=0.
0228,wR2=0.
0660Extinctioncoefficient0.
017(3)Largestdiff.
peakandhole0.
271and-0.
207e.
-39References:(S1)W.
C.
Oliver,G.
M.
Pharr,J.
Mater.
Res.
1992,7,1564-1583(S2)J.
T.
Fell,J.
M.
Newton,J.
Pharm.
Sci.
1970,59,688-691.
(S3)Bruker(2007).
APEX2,SADABSandSAINT.
BrukerAXSInc.
,Madison,Wisconsin,USA.
(S4)G.
M.
Sheldrick,ActaCrystallogr.
2008,A64,112–122.
E.
,Minneapolis,MN55455.
Fax:612-626-2125;Tel:612-624-3722;Email:sunx0053@umn.
eduS1.
Syntheticprocedurefor1.
FigureS1.
X-RaydifferenceFouriermapintheregionoftheatomsO(7)andO(100)inthecrystalstructureof1.
FigureS2.
ORTEPdiagramofasymmetricunitof2.
S2.
MechanicalpropertiesdeterminedbynanoindentationFigureS3.
Nanoindentationload-unloadcurvesofACMFormIand1.
S3.
PowdercompactionS4.
PowderX-raydiffractometryFigureS4.
CalculatedandmeasuredPXRDpatternsof1forbulkpowder.
S5.
X-RaycrystallographicdatacollectionstrategyandrefinementTableS1.
X-Raycrystaldataandstructurerefinementfor1.
TableS2.
X-Raycrystaldataandstructurerefinementfor2.
References2S1.
Synthesisof1:Acetaminophen(ACM,302mg)wasdissolvedinCon.
HCl(1.
6mL)withslightheatingthencooledtoroomtemperature.
Singlecrystalsof1suitableforstructuredeterminationbyX-raydiffractionmethodwereformedwithin30min.
AnX-raydifferenceFouriermaprevealsthatthesiteofprotonationistheamideoxygen,O(7)(FigureS1),whichisconsistentwiththeobservationmadeinliterature(Refs4and7inthepaper).
FigureS1.
X-RaydifferenceFouriermapintheregionoftheatomsO(7)andO(100)inthecrystalstructureof1.
Thesinglemaximumof0.
63e-3neartheatomO7correspondstoprotonatedhydrogen;itsdistancefromO(7)is0.
89,anditsdistancefromO(100)is1.
61.
Wepreparedbulkpowdersof1byeitherlinearlyscalinguptheabove-mentionedreactionorbysuspendingACM(15g)inCon.
HCl(75mL)atroomtemperaturefor12hours.
Ifprolongedheatingisapplied,crystalsof2areproduced(FigureS2).
3FigureS2.
ORTEPdiagramofasymmetricunitof2.
S2.
MechanicalpropertiesdeterminedbynanoindentationCrystalhardness,H,weredeterminedusingananoindenter(TriboIndenterTI-900,HysitronInc.
,MN,USA)withaBerkovichdiamondindentertip.
Beforenanoindentationtesting,thetipareafunctionwasderivedfromaseriesofindentationsonafusedquartzstandard.
Thenanoindentationexperimentswereperformedunderthedisplacementcontrolmode.
Theratesofloadingandunloadingwereboth100nm/sanda10sholdingwasappliedatthemaximumindentationdepthof500nm.
Nanoindentationdatawereanalyzedfollowingthestandardprocedure.
S1RepresentativenanoindentationdataforACMFormIand1areshowninFigureS3.
40100200300400500012341Load(mN)Displacement(nm)FormIFigureS3.
Nanoindentationload-unloadcurvesofACMFormIand1.
Amuchlowerforceisrequiredtomakeanindentofthesamesizeon1thanonACM.
S3.
PowdercompactionAmaterialtestingmachine(model1485,Zwick/Roell,Kennesaw,GA)wasusedtoperformcompactionstudyofbulkpowderof1ataloadingrateof1mm/s.
Powderwasgrindedinamortarusingapestletoreduceparticlesizebeforecompactionstudiesatpressuresrangingfrom25to350MPa,whereadie(round,8mmdiameter)andflat-facedpuncheslubricatedwithmagnesiumstearatewereemployed.
Tabletswererelaxedunderambientenvironmentfor24hbeforemeasuringdiametricalbreakingforceusingatextureanalyzer(TA-XT2i,TextureTechnologiesCorp.
,Scarsdale,NY).
Tablettensilestrengthwascalculatedfromthebreakingforceandtabletdimensionsfollowingstandardprocedure.
S25S4.
PowderX-raydiffractometryX-Raypowderdiffractogramwasobtainedonawide-anglediffractometer(D5005,BruckerAXS).
CuKαradiationwasused.
Thevoltageandcurrentappliedwere45kVand40mArespectively.
Themeasurementwasperformedwithastepsizeof0.
02ofrom5oto35o681012141618202224262830323402040608010012014016018020068101214161820222426283032340204060801001201401601802001recordedRelativeintensityDiffractionangle2θ1calculatedtwothetaandadwelltimeof1s.
PXRDdatawereanalyzedusingacommercialsoftware(JADE,MaterialsDataInc.
,Livermore,CA).
Asidefromthedifferentpeakintensities,whichisattributedtothephenomenonofpreferredorientation,experimentalPXRDpatternofthebulkpowderusedforcompactionmatcheswellwiththecalculatedPXRDpattern(FigureS4).
FigureS4.
CalculatedandmeasuredPXRDpatternsof1forbulkpowder.
6S5.
X-RaycrystallographicdatacollectionstrategyandrefinementSuitablesinglecrystalwasplacedontothetipofa0.
1mmdiameterglassfiberandmountedonaBrukerApexIICCDareadetectordiffractometerfordatacollectionat173(2)KusingMoKαradiation(graphitemonochromator).
S3DataprocessingwasaccomplishedwiththeSAINTprocessingprogram.
ThestructurewassolvedusingBrukerSHELXTLandrefinedusingBrukerSHELXTL.
S4Adirect-methodssolutionwascalculated,whichprovidedmostnon-hydrogenatomsfromtheE-map.
Full-matrixleastsquares/differenceFouriercycleswereperformed,whichlocatedtheremainingnon-hydrogenatoms.
Allnon-hydrogenatomswererefinedwithanisotropicdisplacementparameters.
AllhydrogenatomswerelocatedfromthedifferenceFouriermapandallowedtorideontheirparentatomsintherefinementcycles.
KeycrystaldataanddatacollectionparametersaresummarizedinTableS1andS2for1and2respectively.
DatacollectionandstructuresolutionwereconductedattheX-RayCrystallographicLaboratory,S146KolthoffHall,DepartmentofChemistry,UniversityofMinnesota.
7TableS1.
X-Raycrystaldataandstructurerefinementfor1.
EmpiricalformulaC8H12ClNO3Formulaweight205.
64Temperature173(2)KWavelength0.
71073CrystalsystemMonoclinicSpacegroupP2(1)/cUnitcelldimensionsa=6.
2761(6)α=90°.
b=22.
345(2)β=97.
2570(10)°.
c=6.
8833(7)γ=90°.
Volume957.
56(16)3Z4Density(calculated)1.
426Mg/m3Absorptioncoefficient0.
374mm-1F(000)432Crystalsize0.
36x0.
26x0.
16mm3Thetarangefordatacollection1.
82to26.
84°.
Indexranges-72sigma(I)]R1=0.
0272,wR2=0.
0734Rindices(alldata)R1=0.
0306,wR2=0.
0760Largestdiff.
peakandhole0.
193and-0.
243e.
-38TableS2.
Crystaldataandstructurerefinementfor2.
EmpiricalformulaC6H8ClNOFormulaweight145.
58Temperature173(2)KWavelength0.
71073CrystalsystemMonoclinicSpacegroupP2(1)/cUnitcelldimensionsa=6.
4919(6)α=90°.
b=6.
1159(6)β=90.
0320(10)°.
c=16.
8700(16)γ=90°.
Volume669.
80(11)3Z4Density(calculated)1.
444Mg/m3Absorptioncoefficient0.
480mm-1F(000)304Crystalsize0.
19x0.
16x0.
15mm3Thetarangefordatacollection2.
41to27.
56°.
Indexranges-82sigma(I)]R1=0.
0226,wR2=0.
0658Rindices(alldata)R1=0.
0228,wR2=0.
0660Extinctioncoefficient0.
017(3)Largestdiff.
peakandhole0.
271and-0.
207e.
-39References:(S1)W.
C.
Oliver,G.
M.
Pharr,J.
Mater.
Res.
1992,7,1564-1583(S2)J.
T.
Fell,J.
M.
Newton,J.
Pharm.
Sci.
1970,59,688-691.
(S3)Bruker(2007).
APEX2,SADABSandSAINT.
BrukerAXSInc.
,Madison,Wisconsin,USA.
(S4)G.
M.
Sheldrick,ActaCrystallogr.
2008,A64,112–122.
- producedsolved相关文档
- Spainsolved
- ComPASSsolved
- earlysolved
- denedsolved
- situationsolved
- picksolved
零途云：香港站群云服务器16IP220元/月，云服务器低至39元/月
零途云(Lingtuyun.com)新上了香港站群云服务器 – CN2精品线路，香港多ip站群云服务器16IP/5M带宽,4H4G仅220元/月，还有美国200g高防云服务器低至39元/月起。零途云是一家香港公司，主要产品香港cn2 gia线路、美国Cera线路云主机，美国CERA高防服务器，日本CN2直连服务器;同时提供香港多ip站群云服务器。即日起，购买香港/美国/日本云服务器享受9折优惠，新...
2022年最新PHP短网址生成系统/短链接生成系统/URL缩短器系统源码
全新PHP短网址系统URL缩短器平台，它使您可以轻松地缩短链接，根据受众群体的位置或平台来定位受众，并为缩短的链接提供分析见解。系统使用了Laravel框架编写，前后台双语言使用，可以设置多域名，还可以开设套餐等诸多功能，值得使用。链接: https://pan.baidu.com/s/1ti6XqJ22tp1ULTJw7kYHog?pwd=sarg 提取码: sarg文件解压密码 www.wn7...
RackNerd美国大硬盘服务器促销：120G SSD+192TB HDD,1Gbps大带宽,月付$599，促销美国月付$服务器促销带宽
racknerd怎么样?racknerd最近发布了一些便宜美国服务器促销，包括大硬盘服务器，提供120G SSD+192TB HDD，有AMD和Intel两个选择，默认32G内存，1Gbps带宽，每个月100TB流量，5个IP地址，月付$599。价格非常便宜，需要存储服务器的朋友可以关注一下。RackNerd主要经营美国圣何塞、洛杉矶、达拉斯、芝加哥、亚特兰大、新泽西机房基于KVM虚拟化的VPS、...
solved为你推荐
-
海外服务器租用国外服务器租用已备案域名查询如何查询网站的域名是否已经备案美国vps主机我用的美国VPS主机429元/月，感觉好贵，请问有比较便宜点的吗？国内ip代理谁有最快的国内IP代理HTTP美国服务器托管美国服务器租用有哪些系列？手机网站空间手机网页空间需要多大？韩国虚拟主机香港和韩国的虚拟主机哪个比较好？韩国虚拟主机香港虚拟主机和韩国虚拟主机比较,哪个更好?备案域名哪些域名可以在国内备案？免费二级域名免费注册二级域名的网站