Diffraction Structure — Electrocatalytic Hydrogen Evolution from a Cobaloxime-Based Metal-Organic Framework Thin Film

3 measurement groups · 22 results

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

cRED / MicroED and PXRD Pawley fitting

X-ray diffraction and scattering Electron diffraction

Bulk UU-100(Co) powder · Powder

cRED under cryogenic conditions; PXRD Cu K-alpha; structural model refined with DFT.

Temperature: 95 K for cRED; 298 K in Table S3
Context: pristine framework powder
Measurement source: 15943 · Synthesis and Characterization · Figure 2A; Figures S10-S11; Table S3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Co-Co channel distance, long axis	20.9 A	—	—	Text Exact Reported	15943 · Synthesis and Characterization · Figure 1
Co-Co channel distance, short axis	16.3 A	—	—	Text Exact Reported	15943 · Synthesis and Characterization · Figure 1
cRED approximate a=b	a = b = 27.3 A	—	—	Text Rounded Reported	15943 · Synthesis and Characterization · Figure S10
cRED approximate c	c = 19.6 A	—	—	Text Rounded Reported	15943 · Synthesis and Characterization · Figure S10
Structural-model formula	[Zr6(mu3-O)8(OH)8(cobaloxime)2]	—	—	Text Qualitative	15943 · Synthesis and Characterization · Figure 1
HRTEM lattice spacing d001	d001 = 19.1 A	—	—	Caption Exact Reported	15944 · Figure caption · Figure 2C
Pawley-refined a=b from main textMarked as a best value within this paper	a = b = 28.05(5) A	—	(5) A	Text Exact Reported	15943 · Synthesis and Characterization · Figure 2A; Table S3
Pawley-refined c from main textMarked as a best value within this paper	c = 19.07(3) A	—	(3) A	Text Exact Reported	15943 · Synthesis and Characterization · Figure 2A; Table S3
Accessible pore length from model	13.1 A	—	—	Text Exact Reported	15943 · Synthesis and Characterization · Figure 1
Accessible pore width from model	9.0 A	—	—	Text Exact Reported	15943 · Synthesis and Characterization · Figure 1
PXRD Pawley unweighted-profile R factor	Rp = 0.0585	—	—	Caption Exact Reported	15944 · Figure caption · Figure 2A
PXRD Pawley weighted-profile R factor	Rwp = 0.0770	—	—	Caption Exact Reported	15944 · Figure caption · Figure 2A
Assigned space group	P4/mbm	—	—	Text Exact Reported	15943 · Synthesis and Characterization · Figure S10
Pawley a from SI Table S3	a = 26.363 A	—	—	SI Table Exact Reported	S14 · Table S3 · Table S3
Pawley c from SI Table S3	c = 19.919 A	—	—	SI Table Exact Reported	S14 · Table S3 · Table S3

PXRD, SEM, SEM-EDX, ICP-OES, cross-sectional SEM, XPS

X-ray photoelectron spectroscopy X-ray diffraction and scattering Scanning electron microscopy Elemental microanalysis and mapping Bulk elemental and compositional analysis

UU-100(Co)|FTO thin-film electrode · Electrode

As-prepared UU-100(Co)|FTO thin film and films after electrochemical cycling.

Geometry: Thin-film electrode on FTO
Context: pristine framework thin film on conductive substrate
Measurement source: 15944-15945 · Electrochemical Characterization of UU-100(Co)|FTO · Figure 3; Figures S17-S23; Table S4

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
FTO film SEM-EDX Zr:Co ratio	2.7 +/- 0.1	—	+/- 0.1	Text Exact Reported	15944 · Electrochemical Characterization of UU-100(Co)\|FTO · Figure S20
FTO film ICP-OES Zr:Co ratioMarked as a best value within this paper	3.1 +/- 0.2	—	+/- 0.2	Text Exact Reported	15944 · Electrochemical Characterization of UU-100(Co)\|FTO · Table S4
FTO film thicknessMarked as a best value within this paper	~1 um	—	approximately	Text Approximate	15945 · Electrochemical Characterization of UU-100(Co)\|FTO · Figure S18
XPS Co 2p3/2 binding energy	~781 eV	—	approximately	Text Approximate	15945 · Electrochemical Characterization of UU-100(Co)\|FTO · Figure S22
XPS Zr 3d5/2 binding energy	181.5 eV	—	—	Text Exact Reported	15945 · Electrochemical Characterization of UU-100(Co)\|FTO · Figures S21-S22

Post-electrolysis PXRD, SEM, and SEM-EDX

X-ray diffraction and scattering Scanning electron microscopy Elemental microanalysis and mapping

UU-100(Co)|GC thin-film electrode · Electrode

UU-100(Co)|GC after 3 h, 5 h, 6 h, and 18 h electrolysis at -0.45 V vs RHE in acetate buffer pH 4.

Geometry: Post-catalysis electrode
Context: pristine framework on glassy carbon after HER
Measurement source: 15948 · Electrocatalytic HER by UU-100(Co)|GC · Figure 6B-D; Figures S38-S44

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
PXRD reflections retained after 18 h electrolysis	~4.5 deg and ~9 deg	—	approximately	Text Approximate	15948 · Electrocatalytic HER by UU-100(Co)\|GC · Figures 6B and S38
Post-electrolysis Zr:Co ratio	2.4 +/- 0.2	—	+/- 0.2	Text Exact Reported	15948 · Electrocatalytic HER by UU-100(Co)\|GC · Figures 6 and S43