Diffraction Structure — Multifunctional coordination polymers based on copper(i) and mercaptonicotinic ligands: Synthesis, and structural, optical and electrical characterization

9 measurement groups · 27 results

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

powder X-ray diffraction

X-ray diffraction and scattering

CP1 orange solid from method A · Powder

PXRD from 2theta = 5-40 deg, step size 0.02 deg, 20 s per step, CuKalpha radiation; experimental and calculated patterns compared

Temperature: 298
Geometry: powder diffractogram
Context: pristine bulk CP1
Measurement source: 2 · PXRD · Figure S1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
phase purity by PXRD	purity confirmed by X-ray powder diffraction	—	—	Text Qualitative	7 · Experimental - Synthesis · Figure S1

single-crystal X-ray diffraction

X-ray diffraction and scattering

CP1 orange/red single crystals · Single Crystal

Bruker Kappa Apex II diffractometer, MoKalpha radiation; room-temperature structure

Temperature: 296
Geometry: single crystal
Context: pristine framework
Measurement source: 5 · Crystallographic data · Table S1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Cu-Cu distances	3.081(1) A and 3.907(1) A	—	(1)	Table Exact Reported	4 · Results and discussion · Table 1
Cu-S bond distances	2.197(2) A and 2.295(2) A (Table 1); SI Table S3 gives 2.197(1) A / 2.295(1) A	—	(2) or (1)	Table Exact Reported	4, 6 · Table 1; Electrical characterization · Table 1; Table S3
S-Cu-S angle	120.83(7) deg	120.83 deg	(7)	Table Exact Reported	4, 6 · Table 1; Electrical characterization · Table 1
space group	P 21/c	—	—	SI Table Exact Reported	5 · Crystallographic data · Table S1
structural dimensionality	2D coordination polymer sheet	—	—	Text Qualitative	2 · Results and discussion · Fig. 2
unit cell volume	646.19(4) A3	646.19 A^3	(4)	SI Table Exact Reported	5 · Crystallographic data · Table S1

variable-temperature X-ray powder diffraction

X-ray diffraction and scattering

CP1 orange solid from method A · Powder

VT-XRPD using Anton Paar TTK450 stage; CP1 heated to 150 C / 375 K according to text

Temperature: up to 423 K (150 C); separate text mentions heated up to 375 K
Geometry: powder diffractogram during heating
Context: pristine CP1
Measurement source: 2, 5 · Results and discussion; Electrical characterization · Figure S12

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
VT-XRPD phase stability	no modification upon heating up to 150 C	423.15 K	—	Text Exact Reported	2 · Results and discussion · Figure S12

powder X-ray diffraction

X-ray diffraction and scattering

CP2 orange/red crystals · Single Crystal

PXRD from 2theta = 5-40 deg, step size 0.02 deg, 20 s per step, CuKalpha radiation; experimental and calculated patterns compared

Temperature: 298
Geometry: powder diffractogram
Context: pristine CP2
Measurement source: 2 · PXRD · Figure S2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
phase purity by PXRD	purity confirmed by X-ray powder diffraction	—	—	Text Qualitative	7 · Experimental - Synthesis · Figure S2

single-crystal X-ray diffraction

X-ray diffraction and scattering

CP2 orange/red crystals · Single Crystal

Oxford Xcalibur S diffractometer, MoKalpha radiation; CP2 data collected at 293 K and 100 K

Temperature: 293 and 100
Geometry: single crystal
Context: pristine framework
Measurement source: 6, 10 · Crystallographic data; Structure refinement details for CP2 · Table S2; Fig. S10-S11

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Cu-S bond distances at room temperature	2.480(7), 2.326(7), 2.254(8), 2.498(8), 2.285(5), 2.233(8) A	—	—	SI Table Exact Reported	7 · Bond lengths · Table S3
ligand disorder occupancy at 100 K	53% / 47%	—	—	Text Exact Reported	10 · Structure refinement details for CP2 · Fig. S10-S11
ligand disorder occupancy at room temperature	50% / 50%	—	—	Text Exact Reported	10 · Structure refinement details for CP2 · Fig. S10-S11
unit cell volume at 100 K	1429.45(10) A3	1429.45 A^3	(10)	SI Table Exact Reported	6 · Crystallographic data · Table S2
unit cell volume at 293 K	1444.43(10) A3	1444.43 A^3	(10)	SI Table Exact Reported	6 · Crystallographic data · Table S2
S-Cu-S angle range at room temperature	103.2(4)-111.6(3) deg	—	—	Table Range	4, 6 · Table 1; Electrical characterization · Table 1
space group	P 63	—	—	SI Table Exact Reported	6 · Crystallographic data · Table S2
structural dimensionality	1D coordination polymer channel-like chain	—	—	Text Qualitative	3 · Results and discussion · Fig. 3
water content from TGA/SQUEEZE interpretation	1/3 water molecule in the asymmetric unit	—	—	Text Approximate	10 · Structure refinement details for CP2

variable-temperature X-ray powder diffraction

X-ray diffraction and scattering

CP2 orange/red crystals · Single Crystal

VT-XRPD using Anton Paar TTK450 stage

Geometry: powder diffractogram during heating/cooling
Context: pristine CP2
Measurement source: 3 · Results and discussion · Figure S13

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
VT-XRPD transition temperature	around 190 C	463.15 K	—	Text Approximate	3 · Results and discussion · Figure S13

powder X-ray diffraction

X-ray diffraction and scattering

CP3 yellow crystals from method A · Single Crystal

PXRD from 2theta = 5-40 deg, step size 0.02 deg, 20 s per step, CuKalpha radiation; experimental and calculated patterns compared

Temperature: 298
Geometry: powder diffractogram
Context: pristine CP3
Measurement source: 3 · PXRD · Figure S3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
phase purity by PXRD	purity confirmed by X-ray powder diffraction	—	—	Text Qualitative	8 · Experimental - Synthesis · Figure S3

single-crystal X-ray diffraction

X-ray diffraction and scattering

CP3 yellow crystals from method A · Single Crystal

Oxford Xcalibur S diffractometer, MoKalpha radiation; room-temperature structure

Temperature: 293
Geometry: single crystal
Context: pristine framework
Measurement source: 5, 9 · Crystallographic data · Table S1; Fig. S9

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Cu-Cu distances	Cu1-Cu1 3.218(2) A; Cu2-Cu2 2.822(1) A / 3.420(1) A	—	—	SI Table Exact Reported	7 · Bond lengths · Table S3
Cu-I bond distances	I1-Cu1: 2.724(1), 2.690(1), 2.601(1) A; I2-Cu2: 2.721(1), 2.709(1), 2.631(1) A	—	(1)	SI Table Exact Reported	7 · Bond lengths · Table S3
I-Cu-I angle range	100.57(4)-117.37(4) deg	—	—	Table Range	4 · Results and discussion · Table 1
space group	P 21/c	—	—	SI Table Exact Reported	5 · Crystallographic data · Table S1
structural dimensionality	2D sheets from 1D ladder-like [Cu2I2]n chains interlinked by H2dtdn	—	—	Text Qualitative	3 · Results and discussion · Fig. 4
unit cell volume	2186.47(17) A3	2186.47 A^3	(17)	SI Table Exact Reported	5 · Crystallographic data · Table S1

variable-temperature X-ray powder diffraction

X-ray diffraction and scattering

CP3 yellow crystals from method A · Single Crystal

VT-XRPD using Anton Paar TTK450 stage

Geometry: powder diffractogram during heating/cooling
Context: pristine CP3
Measurement source: 3 · Results and discussion · Figure S14

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
VT-XRPD transition temperature	around 180 C	453.15 K	—	Text Approximate	3 · Results and discussion · Figure S14