Diffraction Structure — Control of crystalline proton-conducting pathways by water-induced transformations of hydrogen-bonding networks in a metal-organic framework

5 measurement groups · 20 results

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

hydrogen-bond distance analysis from SCXRD-derived structures

X-ray diffraction and scattering

as-synthesised 1·3H2O crystals · Single Crystal

hydrogen-bond distances tabulated for 1·3H2O, 1·2H2O and 1 in SI Tables S4-S6

Temperature: 113
Geometry: single-crystal-derived structures
Context: pristine MOF hydration phases
Measurement source: S5-S6 · Supporting Information · Tables S4-S6

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
N(1)···O(9) hydrogen bond in 1·2H2O	N(1)···O(9) = 3.088(5) Å	—	(5)	SI Table Exact Reported	S5 · Supporting Information · Table S5
short O(9)···O(10) hydrogen bond in 1·3H2O	O(9)···O(10) = 2.638(12) Å	—	(12)	SI Table Exact Reported	S5 · Supporting Information · Table S4
N(1)···O(8) hydrogen bond in anhydrate 1	N(1)···O(8): adp = 3.170(5) Å	—	(5)	SI Table Exact Reported	S6 · Supporting Information · Table S6
all tabulated 2-D-layer hydrogen-bond distances for 1·2H2O	N(1)···O(9) 3.088(5) Å; N(1)'···O(9) 3.041(5) Å; N(1)···O(8): adp 3.219(5) Å; N(1)···O(8)': adp 2.899(5) Å; O(9)···O(7): adp 2.977(5) Å; O(1): ox2-···O(7): adp 2.695(4) Å	—	reported in parentheses for each distance	SI Table Exact Reported	S5 · Supporting Information · Table S5
all tabulated 2-D-layer hydrogen-bond distances for 1·3H2O	N(1)···O(9) 2.850(7) Å; N(1)···O(10) 2.789(7) Å; N(1)···O(8): adp 2.953(6) Å; N(1)···O(8)': adp 2.845(4) Å; O(9)···O(10) 2.638(12) Å; O(9)···O(7): adp 3.037(5) Å; O(10)···O(7): adp 2.993(8) Å; O(1): ox2-···O(7): adp 2.688(4) Å	—	reported in parentheses for each distance	SI Table Exact Reported	S5 · Supporting Information · Table S4
all tabulated 2-D-layer hydrogen-bond distances for anhydrate 1	N(1)···O(8): adp 3.170(5) Å; N(1)···O(8)': adp 2.830(5) Å; O(1): ox2-···O(7): adp 2.702(4) Å	—	reported in parentheses for each distance	SI Table Exact Reported	S6 · Supporting Information · Table S6

single-crystal X-ray diffraction on Rigaku AFC-7R using Mo Kα radiation

X-ray diffraction and scattering

single crystal of 1·2H2O · Single Crystal

single crystal picked from air-drying samples of 1·3H2O and measured at 113 K

Temperature: 113
Atmosphere: low-temperature N2 flow implied
Geometry: single crystal
Context: pristine hydrated MOF phase
Measurement source: 7702 · Crystal Structure Determination · Table 1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
unit-cell parameters and volume for 1·2H2O	a = 7.606(7) Å, b = 16.812(2) Å, c = 8.963(7) Å, β = 104.019(4)°, V = 1112.0(2) Å3	—	(2)	Table Exact Reported	7704 · Structural Analysis · Table 1
calculated density of 1·2H2O	1.831 g/cm3	—	—	Table Exact Reported	7704 · Structural Analysis · Table 1
SCXRD formula for 1·2H2O	C12H22N2O18Zn2	—	—	Table Exact Reported	7704 · Structural Analysis · Table 1
space group for 1·2H2O	P21/c (No. 14), monoclinic	—	—	Table Exact Reported	7704 · Structural Analysis · Table 1

single-crystal X-ray diffraction on Rigaku AFC-7R using graphite-monochromatic Mo Kα radiation

X-ray diffraction and scattering

as-synthesised 1·3H2O crystals · Single Crystal

as-synthesised crystal immediately cooled to 113 K under N2 flow after mounting from mother liquid; structure solved by SIR2004 and refined on F2 with SHELXL-97

Temperature: 113
Atmosphere: N2 flow
Geometry: single crystal on glass fibre
Context: pristine hydrated MOF phase
Measurement source: 7702 · Crystal Structure Determination · Table 1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
unit-cell parameters and volume for 1·3H2O	a = 7.9858(1) Å, b = 9.1574(4) Å, c = 9.4523 Å, α = 62.025(6)°, β = 82.335(7)°, γ = 72.873(7)°, V = 583.39(4) Å3	—	(4)	Table Exact Reported	7704 · Structural Analysis · Table 1
calculated density of 1·3H2O	1.796 g/cm3	—	—	Table Exact Reported	7704 · Structural Analysis · Table 1
SCXRD formula for 1·3H2O	C12H24N2O19Zn2	—	—	Table Exact Reported	7704 · Structural Analysis · Table 1
O(10) water molecule occupancy	50% occupancy	0.5 fraction	—	Text Rounded Reported	7703 · Structural Analysis · Figure 5
space group for 1·3H2O	P-1 (No. 2), triclinic	—	—	Table Exact Reported	7704 · Structural Analysis · Table 1

single-crystal X-ray diffraction on Rigaku AFC-7R using Mo Kα radiation

X-ray diffraction and scattering

dehydrated anhydrate 1 single crystal · Single Crystal

1·2H2O single crystal dried at 50 °C overnight under N2 flow, then cooled to 113 K for diffraction

Temperature: 113
Atmosphere: N2 flow
Geometry: single crystal
Context: pristine dehydrated MOF phase
Measurement source: 7702 · Crystal Structure Determination · Table 1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
unit-cell parameters and volume for anhydrate 1	a = 7.7002(7) Å, b = 16.493(1) Å, c = 9.1611(8) Å, β = 108.314(1)°, V = 1104.5(2) Å3	—	(2)	Table Exact Reported	7704 · Structural Analysis · Table 1
calculated density of anhydrate 1	1.735 g/cm3	—	—	Table Exact Reported	7704 · Structural Analysis · Table 1
SCXRD formula for anhydrate 1	C12H18N2O16Zn2	—	—	Table Exact Reported	7704 · Structural Analysis · Table 1
space group for anhydrate 1	P21/c (No. 14), monoclinic	—	—	Table Exact Reported	7704 · Structural Analysis · Table 1

XRPD using Bruker D8 ADVANCE, Cu Kα radiation

X-ray diffraction and scattering

air-dried 1·2H2O sample · Powder

powdered samples made from ground single crystals compared with pattern simulated from SCXRD structure

Geometry: powder sample
Context: pristine hydrated MOF phase
Measurement source: 7705 · Structural Analysis · Figure 6

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
XRPD phase-purity comparison	no significant difference between measured air-dried 1·2H2O and simulated SCXRD pattern	—	—	Text Qualitative	7705 · Structural Analysis · Figure 6