Diffraction Structure — Temperature effect on the synthesis of two Ni-MOFs with distinct performance in supercapacitor

Measurement evidence

Diffraction Structure

Temperature effect on the synthesis of two Ni-MOFs with distinct performance in supercapacitor · Deng L., Qu H., Zhang Y. et al. · Journal of Solid State Chemistry · 2020 · 121026

4 measurement groups · 24 results

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

Powder X-ray diffraction, Cu-Kalpha radiation, Rigaku D/max 2500 PC

Green block crystals of compound 1 · Single Crystal

As-synthesised sample and sample after electrochemical test compared with simulated single-crystal pattern.

Context
pristine framework before and after electrode test
Measurement source
2,5 · 2.1 Materials and methods; 3.5 Purity and stability · Fig. S3
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
PXRD phase purity and post-test stabilityMeasured PXRD patterns for as-synthesised and after-test samples agree with simulated single-crystal patternText
Qualitative
5 · 3.5 Purity and stability · Fig. S3

Single-crystal X-ray diffraction on Bruker Smart Apex CCD, Mo-Kalpha radiation, lambda = 0.7107 Angstrom

Green block crystals of compound 1 · Single Crystal

Data collection at 293(2) K; structure solved with SHELXT and refined with SHELXL/OLEX2.

Temperature
293(2)
Context
pristine framework
Measurement source
2 · 2.4 X-ray crystallography · Table 1; Fig. 1; Tables S1-S2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Unit cell a7.2599(8)(8)Table
Exact Reported
2 · Table 1 · Table 1
Unit cell b7.5509(9)(9)Table
Exact Reported
2 · Table 1 · Table 1
Unit cell c9.4457(7)(7)Table
Exact Reported
2 · Table 1 · Table 1
Unit cell volume435.50(9)(9)Table
Exact Reported
2 · Table 1 · Table 1
Ni coordination geometrySlightly distorted octahedral geometry; Ni coordinated by two carboxylic O atoms, two water O atoms and two imidazole N atomsText
Exact Reported
3 · 3.1 Crystal structure · Fig. 1a
Crystal system and space grouptriclinic, P-1Table
Exact Reported
2 · Table 1 · Table 1
Hydrogen-bond parametersO4-H4A...O2 d(D-A) 2.874 nm, angle 148.509 deg; O4-H4B...O3 2.831 nm, 161.188 deg; O1-H1A...O4 2.683 nm, 156.021 deg; O1-H1B...O3 2.787 nm, 144.212 degSI Table
Exact Reported
2 · Table S2 · Table S2
Ni-N bond distance range2.1014(18)-2.1015(18)(18)Text
Range
3 · 3.1 Crystal structure
Ni-O bond distance range2.0653(16)-2.0654(18)(16)-(18)Text
Range
3 · 3.1 Crystal structure
Selected Ni-O and Ni-N bond lengthsNi1-O1 2.0654(18) A; Ni1-O2 2.0653(16) A; Ni1-N1 2.1014(18) A; symmetry equivalents Ni1-O1A 2.0654(18) A, Ni1-O2A 2.0653(16) A, Ni1-N1A 2.1015(18) Aas listedSI Table
Exact Reported
2 · Table S1 · Table S1

Powder X-ray diffraction, Cu-Kalpha radiation, Rigaku D/max 2500 PC

Orange block crystals of compound 2 · Single Crystal

As-synthesised sample and sample after electrochemical test compared with simulated single-crystal pattern.

Context
pristine framework before and after electrode test
Measurement source
2,5 · 2.1 Materials and methods; 3.5 Purity and stability · Fig. S4
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
PXRD phase purity and post-test stabilityMeasured PXRD patterns for as-synthesised and after-test samples agree with simulated single-crystal patternText
Qualitative
5 · 3.5 Purity and stability · Fig. S4

Single-crystal X-ray diffraction on Bruker Smart Apex CCD, Mo-Kalpha radiation, lambda = 0.7107 Angstrom

Orange block crystals of compound 2 · Single Crystal

Data collection at 293(2) K; structure solved with SHELXT and refined with SHELXL/OLEX2.

Temperature
293(2)
Context
pristine framework
Measurement source
2 · 2.4 X-ray crystallography · Table 1; Fig. 2; Table S1
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Unit cell a15.011(2)(2)Table
Exact Reported
2 · Table 1 · Table 1
Unit cell b13.820(3)(3)Table
Exact Reported
2 · Table 1 · Table 1
Unit cell c13.3327(18)(18)Table
Exact Reported
2 · Table 1 · Table 1
Unit cell volume2745.9(8)(8)Table
Exact Reported
2 · Table 1 · Table 1
1D channel diameter10.223Text
Exact Reported
3 · 3.2 Crystal structure · Fig. 2d
Ni coordination geometryDistorted [NiO2N2] tetrahedral geometryText
Exact Reported
3 · 3.2 Crystal structure · Fig. 2a
Crystal system and space groupmonoclinic, C2/cTable
Exact Reported
2 · Table 1 · Table 1
Average Ni-N bond distance2.015Text
Exact Reported
3 · 3.2 Crystal structure
Adjacent Ni...Ni distance7.022Text
Exact Reported
3 · 3.2 Crystal structure · Fig. 2c
Average Ni-O bond distance1.964Text
Exact Reported
3 · 3.2 Crystal structure
Selected Ni-O and Ni-N bond lengthsNi1-O1 1.950(3) A; Ni1-O2 1.977(3) A; Ni1-N1 2.008(3) A; Ni1-N2 2.022(3) A(3)SI Table
Exact Reported
2 · Table S1 · Table S1
Topology3D two-fold interpenetrated (4,4)-connected PtS net, point symbol {4^2.8^4}Text
Exact Reported
3 · 3.2 Crystal structure · Fig. 2e; Fig. S1