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
2022年腾讯云新春采购季代金券提前领 领取满减优惠券和域名优惠
2022年春节假期陆续结束，根据惯例在春节之后各大云服务商会继续开始一年的促销活动。今年二月中旬会开启新春采购季的活动，我们已经看到腾讯云商家在春节期间已经有预告活动。当时已经看到有抢先优惠促销活动，目前我们企业和个人可以领取腾讯云代金券满减活动，以及企业用户可以领取域名优惠低至.COM域名1元。 直达链接 - 腾讯云新春采购活动抢先看活动时间：2022年1月20日至2022年2月15日我们可以在...
华纳云CN2高防1810M带宽独享，三网直cn218元/月,2M带宽;独服/高防6折购
华纳云怎么样?华纳云是香港老牌的IDC服务商，成立于2015年，主要提供中国香港/美国节点的服务器及网络安全产品、比如，香港服务器、香港云服务器、香港高防服务器、香港高防IP、美国云服务器、机柜出租以及云虚拟主机等。以极速 BGP 冗余网络、CN2 GIA 回国专线以及多年技能经验，帮助全球数十万家企业实现业务转型攀升。华纳云针对618返场活动，华纳云推出一系列热销产品活动，香港云服务器低至3折，...
欧路云：美国200G高防云-10元/月，香港云-15元/月，加拿大480G高防云-23元/月
欧路云 主要运行弹性云服务器，可自由定制配置，可选加拿大的480G超高防系列，也可以选择美国（200G高防）系列，也有速度直逼内地的香港CN2系列。所有配置都可以在下单的时候自行根据项目 需求来定制自由升级降级 （降级按天数配置费用 退款回预存款）。由专业人员提供一系列的技术支持！官方网站：https://www.oulucloud.com/云服务器（主机测评专属优惠）全场8折 优惠码：zhuji...
solved为你推荐
-
租服务器我想租服务器，请问会提供哪些服务？美国服务器托管美国服务器托管好还是租用好网站空间商域名空间商怎么做免费网站空间申请哪里有永久免费的域名空间可以申请免备案虚拟主机请问哪里好一点的免备案的虚拟主机?山东虚拟主机能否在虚拟机与主机之间建立局域网，让主机与虚拟机同时上网？下载虚拟主机虚拟机软件到那里下载。怎么安装天津虚拟主机天津哪个是新网互联代理呢，我打算购买邮局？虚拟主机测评我们可以用哪些命令来测试一个虚拟主机的好坏？沈阳虚拟主机有没有不限空间、不限流量的网站？