Structures, host-guest chemistry and mechanism of stepwise self-assembly of M 4 L 6 tetrahedral cage complexes
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1 Structures, host-guest chemistry and mechanism of stepwise self-assembly of M 4 L 6 tetrahedral cage complexes Benjamin R. Hall, Lauren E. Manck, Ian S. Tidmarsh, Andrew Stephenson, Brian F. Taylor, Emma J. Blaikie, Douglas A. Vander Griend * and Michael D. Ward * Supporting information Part1:Crystalstructuresof[Ni 4 (L bip ) 6 ](BF 4 ) 8 6MeNO 2 and[zn 4 (L bip ) 6 ](BF 4 ) 8 5MeNO 2 Part2:DetailsoftheUV/Visspectroscopictitrationsandsubsequentdataanalysis 1
8 6MeNO2 and [Zn4(Lbip)6](BF4)8 5MeNO2 Fig.](/docs-images/79/79927443/images/2-1.jpg "S1: Structure of one of the independent cage cations of [Ni4(Lbip)6](BF4)8 6MeNO2 with two of the ligands removed for clarity, showing the encapsulated anion. Ni N distances lie in the range 2.04 2.")
2 Electronic Supplementary Material (ESI) for Dalton Transactions Part 1: Crystal structures of [Ni4(Lbip)6](BF4)8 6MeNO2 and [Zn4(Lbip)6](BF4)8 5MeNO2 Fig. S1: Structure of one of the independent cage cations of [Ni4(Lbip)6](BF4)8 6MeNO2 with two of the ligands removed for clarity, showing the encapsulated anion. Ni N distances lie in the range Å; Ni Ni distances along the cage edges lie in the range Å. Fig. S2: Space filling view of the above complex cation with its encapsulated anion (visible in pale green). 2
3 Electronic Supplementary Material (ESI) for Dalton Transactions Fig. S3: Structure of cage cations of [Zn4(Lbip)6](BF4)8 5MeNO2 looking on to the fac tris chelate metal centre Zn(1), i.e. down the (non crystallographic) C3 axis. Zn N distances lie in the range Å; Zn Zn distances along the cage edges lie in the range Å. 3
4 Part2:DetailsoftheUV/Visspectroscopictitrationsandsubsequentdataanalysis (a)titrationof0.0100mco(bf 4 ) 2 with0to2.9equivalentsofl bip at295k. OptimizationSummary: Dataat295K Non negativitywasenforcedwithtruncation(notoptimization). ActivityCoefficientsModel:None. SpecieswithFixedMolarAbsorptivityCurves:None. Solutionsignored:None. OptimizedValues(kJ/mol):ΔG 1 = 154.6(1);ΔG 2 = 148.6(1);ΔG 3 = 136.2(2); ΔG 4 = 49.8(1);ΔG 5 = 49.6(1);ΔG 6 = 31.3(2); EquilibriumRestrictedRMSResidual(7chemicalfactors): UnrestrictedRMSResidual(7mathematicalfactors): RestrictedDataReconstruction(7chemicalfactors): % UnrestrictedDataReconstruction(7mathematicalfactors): % RemainingErrorImbeddedinAbsorbanceValues: R²: % EstimatingmodelsensitivitytoDGvalues... EachDGvalueischangedby1kJ/molinbothdirections. TheresultingaveragechangeinRMSResidualcorrespondstohow sensitivethemodelistothatparticulardgvalue. WhenDG1isshifted,theRMSresidualincreasesby: % WhenDG2isshifted,theRMSresidualincreasesby: % WhenDG3isshifted,theRMSresidualincreasesby: % WhenDG4isshifted,theRMSresidualincreasesby: % WhenDG5isshifted,theRMSresidualincreasesby: % 4
5 WhenDG6isshifted,theRMSresidualincreasesby: % Then,eachDGvalueischangedagain,butnowtheothersareallowed toreoptimize.theresultingchangeinrmsresidualcorrespondstohow independentthatparticulardgvalueis.vanishinglysmallornegativevalues indicatethatonlythedifferencebetweendgvaluesisknownaccurately. WhenDG1isshifted,theRMSresidualincreasesby:3.9515e 012% WhenDG2isshifted,theRMSresidualincreasesby:7.1351e 011% WhenDG3isshifted,theRMSresidualincreasesby:2.4244e 010% WhenDG4isshifted,theRMSresidualincreasesby: e 010% WhenDG5isshifted,theRMSresidualincreasesby: e 010% WhenDG6isshifted,theRMSresidualincreasesby: e 012% 5
6 (b)titrationof0.0100mco(bf 4 ) 2 with0to3.1equivalentsofl bip at308k. OptimizationSummary: Dataat308K Non negativitywasenforcedwithtruncation(notoptimization). ActivityCoefficientsModel:None. SpecieswithFixedMolarAbsorptivityCurves:None. Solutionsignored:None. OptimizedValues(kJ/mol):ΔG 1 = 166(2);ΔG 2 = 162(1);ΔG 3 = 154(1);ΔG 4 = 57.8(8); ΔG 5 = 62.3(8);ΔG 6 = 6.2(3); EquilibriumRestrictedRMSResidual(7chemicalfactors): UnrestrictedRMSResidual(7mathematicalfactors): RestrictedDataReconstruction(7chemicalfactors): % UnrestrictedDataReconstruction(7mathematicalfactors): % RemainingErrorImbeddedinAbsorbanceValues: R²: % 6
7 EstimatingmodelsensitivitytoDGvalues... EachDGvalueischangedby1kJ/molinbothdirections. TheresultingaveragechangeinRMSResidualcorrespondstohow sensitivethemodelistothatparticulardgvalue. WhenDG1isshifted,theRMSresidualincreasesby: % WhenDG2isshifted,theRMSresidualincreasesby: % WhenDG3isshifted,theRMSresidualincreasesby: % WhenDG4isshifted,theRMSresidualincreasesby: % WhenDG5isshifted,theRMSresidualincreasesby: % WhenDG6isshifted,theRMSresidualincreasesby: % Then,eachDGvalueischangedagain,butnowtheothersareallowed toreoptimize.theresultingchangeinrmsresidualcorrespondstohow independentthatparticulardgvalueis.vanishinglysmallornegativevalues indicatethatonlythedifferencebetweendgvaluesisknownaccurately. WhenDG1isshifted,theRMSresidualincreasesby:2.1554e 009% WhenDG2isshifted,theRMSresidualincreasesby: 5.852e 009% WhenDG3isshifted,theRMSresidualincreasesby:9.7575e 009% WhenDG4isshifted,theRMSresidualincreasesby:9.7845e 009% WhenDG5isshifted,theRMSresidualincreasesby:9.7867e 009% WhenDG6isshifted,theRMSresidualincreasesby: % 7
8 Titrationof0.0100MCo(BF 4 ) 2 with0to2.9equivalentsofl bip at283k. OptimizationSummary: Dataat283K Non negativitywasenforcedwithtruncation(notoptimization). ActivityCoefficientsModel:None. SpecieswithFixedMolarAbsorptivityCurves:None. Solutionsignored:None. OptimizedValues(kJ/mol):ΔG 1 = 153(3);ΔG 2 = 106.5(1);ΔG 3 = 101.2(1); ΔG 4 = 52.8(5);ΔG 5 = 43.5(1);ΔG 6 = 41.2(1); EquilibriumRestrictedRMSResidual(7chemicalfactors): UnrestrictedRMSResidual(7mathematicalfactors): RestrictedDataReconstruction(7chemicalfactors): % UnrestrictedDataReconstruction(7mathematicalfactors): % RemainingErrorImbeddedinAbsorbanceValues: R²: % EstimatingmodelsensitivitytoDGvalues... EachDGvalueischangedby1kJ/molinbothdirections. TheresultingaveragechangeinRMSResidualcorrespondstohow sensitivethemodelistothatparticulardgvalue. WhenDG1isshifted,theRMSresidualincreasesby:4.5722e 009% WhenDG2isshifted,theRMSresidualincreasesby: % WhenDG3isshifted,theRMSresidualincreasesby: % WhenDG4isshifted,theRMSresidualincreasesby: % WhenDG5isshifted,theRMSresidualincreasesby:3.9349% WhenDG6isshifted,theRMSresidualincreasesby:3.7672% Then,eachDGvalueischangedagain,butnowtheothersareallowed toreoptimize.theresultingchangeinrmsresidualcorrespondstohow independentthatparticulardgvalueis.vanishinglysmallornegativevalues 8
9 indicatethatonlythedifferencebetweendgvaluesisknownaccurately. WhenDG1isshifted,theRMSresidualincreasesby: e 008% WhenDG2isshifted,theRMSresidualincreasesby: 1.644e 008% WhenDG3isshifted,theRMSresidualincreasesby: e 008% WhenDG4isshifted,theRMSresidualincreasesby: e 008% WhenDG5isshifted,theRMSresidualincreasesby: e 008% WhenDG6isshifted,theRMSresidualincreasesby: e 008% 9
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