Diffraction Structure — MOF matrix isolation: Cooperative conformational mobility enables reliable single crystal transformations

Measurement evidence

Diffraction Structure

MOF matrix isolation: Cooperative conformational mobility enables reliable single crystal transformations · Peralta R.A., Huxley M.T., Young R.J. et al. · Faraday Discussions · 2021 · 84-99

20 measurement groups · 92 results

Reported values remain attached to the sample, method, conditions, extraction quality and source location that produced them.

powder X-ray diffraction (PXRD)

MnMOF-1-ace · Single Crystal

Experimental dried PXRD pattern compared with simulated single-crystal pattern for MnMOF-1-ace.

Geometry
Bruker Advanced D8; Cu Kalpha; capillary stage
Context
pristine/model
Measurement source
p008 / SI page 8 · SI 3.0 Powder X-ray diffractograms of each sample · Figure S3.3
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
PXRD pattern comparisonshows features consistent with structural contraction following desolvation——Caption
Qualitative
p008 / SI page 8 · SI 3.0 Powder X-ray diffractograms of each sample · Figure S3.3

powder X-ray diffraction (PXRD)

MnMOF-1-DCM · Single Crystal

Experimental dried PXRD pattern compared with simulated single-crystal pattern for MnMOF-1-DCM.

Geometry
Bruker Advanced D8; Cu Kalpha; capillary stage
Context
pristine/model
Measurement source
p008 / SI page 8 · SI 3.0 Powder X-ray diffractograms of each sample · Figure S3.4
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
PXRD pattern comparisonshows features consistent with structural contraction following desolvation——Caption
Qualitative
p008 / SI page 8 · SI 3.0 Powder X-ray diffractograms of each sample · Figure S3.4

powder X-ray diffraction (PXRD)

MnMOF-1-DEE · Single Crystal

Experimental dried PXRD pattern compared with simulated single-crystal pattern for MnMOF-1-DEE.

Geometry
Bruker Advanced D8; Cu Kalpha; capillary stage
Context
pristine/model
Measurement source
p009 / SI page 9 · SI 3.0 Powder X-ray diffractograms of each sample · Figure S3.5
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
PXRD pattern comparisonshows features consistent with structural contraction following desolvation——Caption
Qualitative
p009 / SI page 9 · SI 3.0 Powder X-ray diffractograms of each sample · Figure S3.5

powder X-ray diffraction (PXRD)

MnMOF-1-EtOH · Single Crystal

Experimental dried PXRD pattern compared with simulated single-crystal pattern for MnMOF-1-EtOH.

Geometry
Bruker Advanced D8; Cu Kalpha; capillary stage
Context
pristine/model
Measurement source
p007 / SI page 7 · SI 3.0 Powder X-ray diffractograms of each sample · Figure S3.2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
PXRD pattern comparisonshows features consistent with structural contraction following desolvation——Caption
Qualitative
p007 / SI page 7 · SI 3.0 Powder X-ray diffractograms of each sample · Figure S3.2

powder X-ray diffraction (PXRD)

MnMOF-1-MeOH · Single Crystal

Experimental dried PXRD pattern compared with simulated single-crystal pattern for MnMOF-1-MeOH.

Geometry
Bruker Advanced D8; Cu Kalpha; capillary stage
Context
pristine/model
Measurement source
p007 / SI page 7 · SI 3.0 Powder X-ray diffractograms of each sample · Figure S3.1
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
PXRD pattern comparisonshows features consistent with structural contraction following desolvation——Caption
Qualitative
p007 / SI page 7 · SI 3.0 Powder X-ray diffractograms of each sample · Figure S3.1

powder X-ray diffraction (PXRD)

MnMOF-1-p-xylene · Single Crystal

Experimental dried PXRD pattern compared with simulated single-crystal pattern for MnMOF-1-p-xylene.

Geometry
Bruker Advanced D8; Cu Kalpha; capillary stage
Context
pristine/model
Measurement source
p010 / SI page 10 · SI 3.0 Powder X-ray diffractograms of each sample · Figure S3.7
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
PXRD pattern comparisonPXRD pattern obtained for MnMOF-1-p-xylene (exp, dried) and simulated PXRD pattern——Caption
Qualitative
p010 / SI page 10 · SI 3.0 Powder X-ray diffractograms of each sample · Figure S3.7

powder X-ray diffraction (PXRD)

Rh-metalated MnMOF-1 from DCM · Single Crystal

Experimental dried PXRD pattern compared with simulated single-crystal pattern for MnMOF-1.[Rh(CO)2][RhCl2(CO)2] prepared in DCM and acetone.

Geometry
Bruker Advanced D8; Cu Kalpha; capillary stage
Context
guest-loaded
Measurement source
p011 / SI page 11 · SI 3.0 Powder X-ray diffractograms of each sample · Figure S3.9
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
PXRD pattern comparisonPXRD pattern obtained for MnMOF-1.[Rh(CO)2][RhCl2(CO)2] prepared in DCM (exp) and acetone (exp)——Caption
Qualitative
p011 / SI page 11 · SI 3.0 Powder X-ray diffractograms of each sample · Figure S3.9

powder X-ray diffraction (PXRD)

Rh-metalated MnMOF-1 from p-xylene · Single Crystal

Experimental dried PXRD pattern compared with simulated single-crystal pattern for MnMOF-1.[Rh(CO)2][RhCl2(CO)2] prepared in p-xylene.

Geometry
Bruker Advanced D8; Cu Kalpha; capillary stage
Context
guest-loaded
Measurement source
p010 / SI page 10 · SI 3.0 Powder X-ray diffractograms of each sample · Figure S3.8
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
PXRD pattern comparisonPXRD pattern obtained for MnMOF-1.[Rh(CO)2][RhCl2(CO)2] prepared in p-xylene——Caption
Qualitative
p010 / SI page 10 · SI 3.0 Powder X-ray diffractograms of each sample · Figure S3.8

powder X-ray diffraction (PXRD)

MnMOF-1-THF · Single Crystal

Experimental dried PXRD pattern compared with simulated single-crystal pattern for MnMOF-1-THF.

Geometry
Bruker Advanced D8; Cu Kalpha; capillary stage
Context
pristine/model
Measurement source
p009 / SI page 9 · SI 3.0 Powder X-ray diffractograms of each sample · Figure S3.6
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
PXRD pattern comparisonshows features consistent with structural contraction following desolvation——Caption
Qualitative
p009 / SI page 9 · SI 3.0 Powder X-ray diffractograms of each sample · Figure S3.6

single-crystal X-ray diffraction (SCXRD)

MnMOF-1-ace · Single Crystal

Unit-cell and structural comparison of MnMOF-1 solvatomorphs; new structures collected at 100 K where indicated.

Context
pristine/model
Measurement source
p004-p005 / journal pages 87-88 · Results and discussion · Tables 1-2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
CCDC deposition number1977803——SI Table
Exact Reported
p015 / SI page 15 · SI 4.0 Structure refinement details and tables · Table S4.1
empirical formulaC97.5H111N12O19.5Mn3——SI Table
Exact Reported
p015 / SI page 15 · SI 4.0 Structure refinement details and tables · Table S4.1
pyrazole ring torsion anglenot determined——Table
Qualitative
p005 / journal page 88 · Results and discussion · Table 2
final R1 index [I>=2sigma(I)]0.0726——SI Table
Exact Reported
p015 / SI page 15 · SI 4.0 Structure refinement details and tables · Table S4.1
volume per repeat unit vs desolvated116%——Table
Rounded Reported
p005 / journal page 88 · Results and discussion · Table 2
space groupP21/m——Table
Qualitative
p004 / journal page 87 · Results and discussion · Table 1
unit cell volume5060.6(18)——Table
Exact Reported
p004 / journal page 87 · Results and discussion · Table 1
final wR2 index [I>=2sigma(I)]0.2023——SI Table
Exact Reported
p015 / SI page 15 · SI 4.0 Structure refinement details and tables · Table S4.1

single-crystal X-ray diffraction (SCXRD)

MnMOF-1-CH3CN · Single Crystal

Unit-cell and structural comparison of MnMOF-1 solvatomorphs; new structures collected at 100 K where indicated.

Context
pristine/model
Measurement source
p004-p005 / journal pages 87-88 · Results and discussion · Tables 1-2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
pyrazole ring torsion angle13.6——Table
Rounded Reported
p005 / journal page 88 · Results and discussion · Table 2
volume per repeat unit vs desolvated110%——Table
Rounded Reported
p005 / journal page 88 · Results and discussion · Table 2
space groupP-1——Table
Qualitative
p004 / journal page 87 · Results and discussion · Table 1
unit cell volume4794.5(19)——Table
Exact Reported
p004 / journal page 87 · Results and discussion · Table 1

single-crystal X-ray diffraction (SCXRD)

MnMOF-1-DCM · Single Crystal

Unit-cell and structural comparison of MnMOF-1 solvatomorphs; new structures collected at 100 K where indicated.

Context
pristine/model
Measurement source
p004-p005 / journal pages 87-88 · Results and discussion · Tables 1-2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
CCDC deposition number1977802——SI Table
Exact Reported
p014 / SI page 14 · SI 4.0 Structure refinement details and tables · Table S4.1
empirical formulaC84H84N12O12Mn3Cl18——SI Table
Exact Reported
p014 / SI page 14 · SI 4.0 Structure refinement details and tables · Table S4.1
pyrazole ring torsion anglenot determined——Table
Qualitative
p005 / journal page 88 · Results and discussion · Table 2
final R1 index [I>=2sigma(I)]0.101——SI Table
Exact Reported
p014 / SI page 14 · SI 4.0 Structure refinement details and tables · Table S4.1
volume per repeat unit vs desolvated116%——Table
Rounded Reported
p005 / journal page 88 · Results and discussion · Table 2
space groupP21/m——Table
Qualitative
p004 / journal page 87 · Results and discussion · Table 1
unit cell volume5077.8(18)——Table
Exact Reported
p004 / journal page 87 · Results and discussion · Table 1
final wR2 index [I>=2sigma(I)]0.2925——SI Table
Exact Reported
p014 / SI page 14 · SI 4.0 Structure refinement details and tables · Table S4.1

single-crystal X-ray diffraction (SCXRD)

MnMOF-1-DEE · Single Crystal

Unit-cell and structural comparison of MnMOF-1 solvatomorphs; new structures collected at 100 K where indicated.

Context
pristine/model
Measurement source
p004-p005 / journal pages 87-88 · Results and discussion · Tables 1-2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
CCDC deposition number1977799——SI Table
Exact Reported
p013 / SI page 13 · SI 4.0 Structure refinement details and tables · Table S4.1
empirical formulaC97H126N12O18Mn3——SI Table
Exact Reported
p013 / SI page 13 · SI 4.0 Structure refinement details and tables · Table S4.1
pyrazole ring torsion angle171.5——Table
Rounded Reported
p005 / journal page 88 · Results and discussion · Table 2
final R1 index [I>=2sigma(I)]0.2135——SI Table
Exact Reported
p013 / SI page 13 · SI 4.0 Structure refinement details and tables · Table S4.1
volume per repeat unit vs desolvated109%——Table
Rounded Reported
p005 / journal page 88 · Results and discussion · Table 2
space groupP-1——Table
Qualitative
p004 / journal page 87 · Results and discussion · Table 1
unit cell volume4750.4(17)——Table
Exact Reported
p004 / journal page 87 · Results and discussion · Table 1
final wR2 index [I>=2sigma(I)]0.5779——SI Table
Exact Reported
p013 / SI page 13 · SI 4.0 Structure refinement details and tables · Table S4.1

single-crystal X-ray diffraction (SCXRD)

MnMOF-1-des · Unknown

Unit-cell and structural comparison of MnMOF-1 solvatomorphs; new structures collected at 100 K where indicated.

Context
pristine/model
Measurement source
p004-p005 / journal pages 87-88 · Results and discussion · Tables 1-2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
pyrazole ring torsion angle155.6——Table
Rounded Reported
p005 / journal page 88 · Results and discussion · Table 2
space groupC2/c——Table
Qualitative
p004 / journal page 87 · Results and discussion · Table 1
unit cell volume8711.0(9)——Table
Exact Reported
p004 / journal page 87 · Results and discussion · Table 1

single-crystal X-ray diffraction (SCXRD)

MnMOF-1-DMF/as · Single Crystal

Unit-cell and structural comparison of MnMOF-1 solvatomorphs; new structures collected at 100 K where indicated.

Context
pristine/model
Measurement source
p004-p005 / journal pages 87-88 · Results and discussion · Tables 1-2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
pyrazole ring torsion angle157.2——Table
Rounded Reported
p005 / journal page 88 · Results and discussion · Table 2
volume per repeat unit vs desolvated118%——Table
Rounded Reported
p005 / journal page 88 · Results and discussion · Table 2
space groupP21/c——Table
Qualitative
p004 / journal page 87 · Results and discussion · Table 1
unit cell volume10291(4)——Table
Exact Reported
p004 / journal page 87 · Results and discussion · Table 1

single-crystal X-ray diffraction (SCXRD)

MnMOF-1-EtOH · Single Crystal

Unit-cell and structural comparison of MnMOF-1 solvatomorphs; new structures collected at 100 K where indicated.

Context
pristine/model
Measurement source
p004-p005 / journal pages 87-88 · Results and discussion · Tables 1-2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
CCDC deposition number1977800——SI Table
Exact Reported
p014 / SI page 14 · SI 4.0 Structure refinement details and tables · Table S4.1
empirical formulaC93H120N12O21Mn3——SI Table
Exact Reported
p014 / SI page 14 · SI 4.0 Structure refinement details and tables · Table S4.1
pyrazole ring torsion anglenot determined——Table
Qualitative
p005 / journal page 88 · Results and discussion · Table 2
final R1 index [I>=2sigma(I)]0.048——SI Table
Exact Reported
p014 / SI page 14 · SI 4.0 Structure refinement details and tables · Table S4.1
volume per repeat unit vs desolvated119%——Table
Rounded Reported
p005 / journal page 88 · Results and discussion · Table 2
space groupP21/m——Table
Qualitative
p004 / journal page 87 · Results and discussion · Table 1
unit cell volume5185.5(18)——Table
Exact Reported
p004 / journal page 87 · Results and discussion · Table 1
final wR2 index [I>=2sigma(I)]0.1433——SI Table
Exact Reported
p014 / SI page 14 · SI 4.0 Structure refinement details and tables · Table S4.1

single-crystal X-ray diffraction (SCXRD)

MnMOF-1-MeOH · Single Crystal

Unit-cell and structural comparison of MnMOF-1 solvatomorphs; new structures collected at 100 K where indicated.

Context
pristine/model
Measurement source
p004-p005 / journal pages 87-88 · Results and discussion · Tables 1-2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
CIF bundle CCDC coverageCCDC 1977797-1977804——Text
Exact Reported
text lines 19-20 and subsequent data blocks · CIF data blocks
CCDC deposition number1977797——SI Table
Exact Reported
p013 / SI page 13 · SI 4.0 Structure refinement details and tables · Table S4.1
empirical formulaC90H126N12O27Mn3——SI Table
Exact Reported
p013 / SI page 13 · SI 4.0 Structure refinement details and tables · Table S4.1
pyrazole ring torsion anglenot determined——Table
Qualitative
p005 / journal page 88 · Results and discussion · Table 2
final R1 index [I>=2sigma(I)]0.0602——SI Table
Exact Reported
p013 / SI page 13 · SI 4.0 Structure refinement details and tables · Table S4.1
volume per repeat unit vs desolvated117%——Table
Rounded Reported
p005 / journal page 88 · Results and discussion · Table 2
space groupP21/m——Table
Qualitative
p004 / journal page 87 · Results and discussion · Table 1
unit cell volume5112.3(18)——Table
Exact Reported
p004 / journal page 87 · Results and discussion · Table 1
final wR2 index [I>=2sigma(I)]0.1927——SI Table
Exact Reported
p013 / SI page 13 · SI 4.0 Structure refinement details and tables · Table S4.1

single-crystal X-ray diffraction (SCXRD)

MnMOF-1-p-xylene · Single Crystal

Unit-cell and structural comparison of MnMOF-1 solvatomorphs; new structures collected at 100 K where indicated.

Context
pristine/model
Measurement source
p004-p005 / journal pages 87-88 · Results and discussion · Tables 1-2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
CCDC deposition number1977798——SI Table
Exact Reported
p013 / SI page 13 · SI 4.0 Structure refinement details and tables · Table S4.1
empirical formulaC105H103.5N12O12Mn3——SI Table
Exact Reported
p013 / SI page 13 · SI 4.0 Structure refinement details and tables · Table S4.1
pyrazole ring torsion angle26.0——Table
Rounded Reported
p005 / journal page 88 · Results and discussion · Table 2
final R1 index [I>=2sigma(I)]0.148——SI Table
Exact Reported
p013 / SI page 13 · SI 4.0 Structure refinement details and tables · Table S4.1
volume per repeat unit vs desolvated113%——Table
Rounded Reported
p005 / journal page 88 · Results and discussion · Table 2
space groupP-1——Table
Qualitative
p004 / journal page 87 · Results and discussion · Table 1
unit cell volume4931.1(18)——Table
Exact Reported
p004 / journal page 87 · Results and discussion · Table 1
final wR2 index [I>=2sigma(I)]0.443——SI Table
Exact Reported
p013 / SI page 13 · SI 4.0 Structure refinement details and tables · Table S4.1

single-crystal X-ray diffraction (SCXRD)

Rh-metalated MnMOF-1 from p-xylene · Single Crystal

Structure determination of Rh-metalated MnMOF-1 formed in p-xylene.

Context
guest-loaded
Measurement source
p008-p009 / journal pages 91-92 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2 · Fig. 2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
anion Rh-C bond length 11.753(16)——Text
Exact Reported
p008-p009 / journal pages 91-92 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
anion Rh-C bond length 21.827(16)——Text
Exact Reported
p008-p009 / journal pages 91-92 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
anion Rh-Cl bond length 12.358(3)——Text
Exact Reported
p008-p009 / journal pages 91-92 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
anion Rh-Cl bond length 22.321(3)——Text
Exact Reported
p008-p009 / journal pages 91-92 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
CCDC deposition number1977801——SI Table
Exact Reported
p014 / SI page 14 · SI 4.0 Structure refinement details and tables · Table S4.1
Cl to vacant axial site distance3.73——Text
Exact Reported
p008-p009 / journal pages 91-92 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
empirical formulaC111H106N12O16Mn3Rh2Cl2——SI Table
Exact Reported
p014 / SI page 14 · SI 4.0 Structure refinement details and tables · Table S4.1
metalated N-N separation2.80——Text
Exact Reported
p008-p009 / journal pages 91-92 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
pre-metalation N-N separation2.93——Text
Exact Reported
p008-p009 / journal pages 91-92 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
final R1 index [I>=2sigma(I)]0.1033——SI Table
Exact Reported
p014 / SI page 14 · SI 4.0 Structure refinement details and tables · Table S4.1
Rh-C bond length 11.860(13)——Text
Exact Reported
p008-p009 / journal pages 91-92 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
Rh-C bond length 21.906(12)——Text
Exact Reported
p008-p009 / journal pages 91-92 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
Rh-N bond length 12.060(7)——Text
Exact Reported
p008-p009 / journal pages 91-92 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
Rh-N bond length 22.094(7)——Text
Exact Reported
p008-p009 / journal pages 91-92 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
final wR2 index [I>=2sigma(I)]0.2994——SI Table
Exact Reported
p014 / SI page 14 · SI 4.0 Structure refinement details and tables · Table S4.1

single-crystal X-ray diffraction (SCXRD)

MnMOF-1-THF · Single Crystal

Unit-cell and structural comparison of MnMOF-1 solvatomorphs; new structures collected at 100 K where indicated.

Context
pristine/model
Measurement source
p004-p005 / journal pages 87-88 · Results and discussion · Tables 1-2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
CCDC deposition number1977804——SI Table
Exact Reported
p015 / SI page 15 · SI 4.0 Structure refinement details and tables · Table S4.1
empirical formulaC111H138Mn3N12O21——SI Table
Exact Reported
p015 / SI page 15 · SI 4.0 Structure refinement details and tables · Table S4.1
pyrazole ring torsion angle168.8——Table
Rounded Reported
p005 / journal page 88 · Results and discussion · Table 2
final R1 index [I>=2sigma(I)]0.2041——SI Table
Exact Reported
p015 / SI page 15 · SI 4.0 Structure refinement details and tables · Table S4.1
volume per repeat unit vs desolvated124%——Table
Rounded Reported
p005 / journal page 88 · Results and discussion · Table 2
space groupP-1——Table
Qualitative
p004 / journal page 87 · Results and discussion · Table 1
unit cell volume5411(2)——Table
Exact Reported
p004 / journal page 87 · Results and discussion · Table 1
final wR2 index [I>=2sigma(I)]0.4668——SI Table
Exact Reported
p015 / SI page 15 · SI 4.0 Structure refinement details and tables · Table S4.1