Diffraction Structure

Powder X-ray diffraction in reflection mode; Inel Equinox 1000; monochromated Cu-Kalpha radiation, lambda = 1.5406 A

powder sample of compound 1 · Powder

Room temperature; X-ray tube operated at 30 kV and 30 mA. Patterns compared for calculated single-crystal structure, as-made bulk powder, and sample after boiling water treatment for 24 h.

Temperature: room temperature
Context: pristine target sample
Measurement source: p005 / SI p.S5 · PXRD · Figure S3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
PXRD phase-purity check	as-made bulk powder pattern compared with calculated pattern from single-crystal structure	—	—	Caption Qualitative	p002 / article p.6088 · Phase purity · Figure S3
boiling-water PXRD treatment duration	24 h	24 h	—	Caption Exact Reported	p005 / SI p.S5 · Figure S3 caption · Figure S3

Single-crystal X-ray diffraction; Bruker Smart Apex CCD; Mo Kalpha radiation, lambda = 0.71073 A; SMART/SAINT/SADABS; SHELXL 6.14 refinement

X-ray diffraction and scattering

black needle-like single crystals of compound 1 · Single Crystal

Data collected at 100 K; crystal size 0.30 x 0.18 x 0.11 mm3.

Temperature: 100
Context: pristine target sample
Measurement source: p002 / SI p.S2 · General Procedure · Table S1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
long Cu-I distance in compound 1	3.089(9)	3.089 A	(9)	Text Exact Reported	p002 / article p.6088 · Structure discussion · Figure 1
short Cu-I distance in compound 1	2.690(1)	2.69 A	(1)	Text Exact Reported	p002 / article p.6088 · Structure discussion · Figure 1
long I-I distance in triiodide linker	3.039	3.039 A	—	Text Exact Reported	p002 / article p.6088 · Structure discussion · Figure 1
short I-I distance in triiodide linker	2.839	2.839 A	—	Text Exact Reported	p002 / article p.6088 · Structure discussion · Figure 1
I1-I2-I3 triiodide angle	176.4	176.4 degree	—	Text Exact Reported	p002 / article p.6088 · Structure discussion · Figure 1
unit-cell a parameter	9.3242(14)	9.3242 A	(14)	SI Table Exact Reported	p009 / SI p.S9 · Table S1 · Table S1
unit-cell b parameter	16.887(3)	16.887 A	(3)	SI Table Exact Reported	p009 / SI p.S9 · Table S1 · Table S1
unit-cell c parameter	20.587(3)	20.587 A	(3)	SI Table Exact Reported	p009 / SI p.S9 · Table S1 · Table S1
calculated crystal density	2.600	2.6 g/cm3	—	SI Table Exact Reported	p009 / SI p.S9 · Table S1 · Table S1
crystallographic chemical formula	C10H14N4CuI3	—	—	SI Table Exact Reported	p009 / SI p.S9 · Table S1 · Table S1
R1 refinement residual for I > 2sigma(I)	0.0514	0.0514	—	SI Table Exact Reported	p010 / SI p.S10 · Table S1 · Table S1
space group	Pbca	—	—	SI Table Exact Reported	p009 / SI p.S9 · Table S1 · Table S1
unit-cell volume	3241.6(9)	3241.6 A^3	(9)	SI Table Exact Reported	p009 / SI p.S9 · Table S1 · Table S1

2 measurement groups · 15 results