Diffraction Structure — Multiple-Hydrogen-Bond Approach to Uncommon Pd(III) Oxidation State: A Pd-Br Chain with High Conductivity and Thermal Stability

Measurement evidence

Diffraction Structure

Multiple-Hydrogen-Bond Approach to Uncommon Pd(III) Oxidation State: A Pd-Br Chain with High Conductivity and Thermal Stability · Mian M.R., Iguchi H., Takaishi S. et al. · Journal of the American Chemical Society · 2017 · 6562-6565

2 measurement groups · 17 results

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

single-crystal X-ray diffraction

Copper-luster rod-like single crystals of compound 3 · Single Crystal

Mo Kalpha radiation, 0.71073 A; Bruker APEX-II diffractometer; structure refined using SHELXL-97 in Yadokari-XG2009.

Temperature
93
Context
pristine target crystal
Measurement source
SI p.S2 · Characterization and Instrumentation · Table S1
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
unit-cell betabeta = 100.940(2) degrees100.94 degree(2)SI Table
Exact Reported
SI p.S4 · Crystallographic parameters of 3 · Table S1
unit-cell volumeV = 829.46(10) A3829.46 Angstrom^3(10)SI Table
Exact Reported
SI p.S4 · Crystallographic parameters of 3 · Table S1
crystal size0.38 x 0.05 x 0.05 mm3SI Table
Exact Reported
SI p.S4 · Crystallographic parameters of 3 · Table S1
crystal systemMonoclinicSI Table
Exact Reported
SI p.S4 · Crystallographic parameters of 3 · Table S1
calculated density2.348 Mg/m32.348 g cm-3SI Table
Exact Reported
SI p.S4 · Crystallographic parameters of 3 · Table S1
interchain distance along c axis7.3296(5) A7.3296 Angstrom(5)Table
Exact Reported
main p.3, article p.6564 · Origin of short Pd-Br-Pd distance · Table 1
mean N...Br(Y) hydrogen-bond distance3.486 A3.486 AngstromTable
Exact Reported
main p.3, article p.6564 · Origin of short Pd-Br-Pd distance · Table 1
N...Br(Y)...N hydrogen-bond angles95.06, 97.00 degreesTable
Exact Reported
main p.3, article p.6564 · Origin of short Pd-Br-Pd distance · Table 1
shortest O...Br(Y) hydrogen-bond distance3.163 A3.163 AngstromText
Exact Reported
main p.2, article p.6563 · Crystal structure · Figure 1
individual Pd-Br distances2.5902(19) A and 2.5916(19) A(19) for both valuesText
Exact Reported
main p.2, article p.6563 · Crystal structure · Figure 1
Pd-Br-Pd distance at 93 KMarked as a best value within this paper5.1818(4) A5.1818 Angstrom(4)Text
Exact Reported
main p.2, article p.6563 · Crystal structure · Figure 1; Table 1
space groupC2SI Table
Exact Reported
SI p.S4 · Crystallographic parameters of 3 · Table S1
unit-cell aa = 22.2432(16) A22.2432 Angstrom(16)SI Table
Exact Reported
SI p.S4 · Crystallographic parameters of 3 · Table S1
unit-cell b / chain repeatb = 5.1818(4) A5.1818 Angstrom(4)SI Table
Exact Reported
SI p.S4 · Crystallographic parameters of 3 · Table S1
unit-cell cc = 7.3296(5) A7.3296 Angstrom(5)SI Table
Exact Reported
SI p.S4 · Crystallographic parameters of 3 · Table S1

temperature-dependent single-crystal X-ray diffraction

Copper-luster rod-like single crystals of compound 3 · Single Crystal

Pd-Br-Pd distance tracked versus temperature and compared with compound 1.

Temperature
93-363
Context
pristine target crystal
Measurement source
main p.2, article p.6563 · Thermal stability of AV state · Figure 2a; Table S2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Pd-Br-Pd distance at 273 K for band-gap correlation5.2044(4) A at 273 K5.2044 Angstrom(4)SI Table
Exact Reported
SI p.S9 · Relationship between d(Pd-Br-Pd) and optical band gap in PdBr chains · Table S2
Pd-Br-Pd distance at 363 K5.2166(4) A5.2166 Angstrom(4)Text
Exact Reported
main p.2, article p.6563 · Thermal stability of AV state · Figure 2a