1-methyl-hexylammonium lead iodide

Chemical Formula: C14H36N2PbI4
IUPAC: 1-methyl-hexanaminium lead (II) iodide
Alternate Names: 1-methyl-hexanaminium tetraiodoplumbate(II), [C14H36N2]PbI4, (1-Me-ha)2PbI4
Organic: C7H18N
Inorganic: PbI4, Lead iodide
Dimensionality: 2D n: 1
Formal Stoichiometry: C : 14 , H : 36 , N : 2 , Pb : 1 , I : 4
Atomic structure Verified
Origin: experimental (T = 296.0 K)
Space group: P 2₁/c
Lattice parameters

Crystal system: monoclinic

a:17.4586 Å
b:9.2513 Å
c:8.586403313 Å
α:90°
β:103.2228064°
γ:90°
Fixed parameters:
  • temperature = 296.0 K
T. Li, W. A. Dunlap-Shohl, E. W. Reinheimer, P. Le Magueres, and D. B. Mitzi, Melting temperature suppression of layered hybrid lead halide perovskites via organic ammonium cation branching, Chemical Science 10, 1168‑1175 (2019). doi: 10.1039/C8SC03863E.
System description
Dimensionality: 2D n: 1
Sample type: single crystal

Starting materials: 2-Aminoheptane (1-Me-ha, 99%), hydriodic acid (HI) solution (57 wt%, stabilized, 99.95%), PbI2

Product: Clear light orange plate-like crystals

Description: 1Me-ha∙HI salt was synthesized by adding a stoichiometric volume of HI into 2-Aminoheptane in a cold water bath, evaporating water at 150 ˚C on a hot plate and vacuum drying at 150 ˚C at 40 mtorr for a week. Thin plate-like (1-Me-ha)2PbI4 crystals were grown by adding stoichiometric amounts of PbI2 (0.25 mmol) and 1-Me-ha∙HI (0.5 mmol) to a solution of 0.5 mL HI solution and 0.5 mL methanol followed by slow evaporation of the solution over a week. The crystals were filtered and washed with ethyl ether.

Method: Single crystal X-ray Diffraction

Description: Data were collected using Bruker D8 ADVANCE Series II diffractometer using Mo Kα radiation (= 0.71073 Å).

T. Li, W. A. Dunlap-Shohl, E. W. Reinheimer, P. Le Magueres, and D. B. Mitzi, Melting temperature suppression of layered hybrid lead halide perovskites via organic ammonium cation branching, Chemical Science 10, 1168‑1175 (2019). doi: 10.1039/C8SC03863E.

Entry added on: Aug. 19, 2019, 4:01 p.m.
Entry added by: Manoj Kumar Jana Duke University
Last updated on: June 22, 2022, 9:42 p.m.
Last updated by: Rayan C Duke University
Data correctness verified by:
  • Rayan C Duke University

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Data set ID: 557 Did you find any mistakes or inconsistencies about this data? Send us a note and we'll have a look at it and send you a reply. Thanks!

 

Atomic coordinates


Band gap (fundamental)

See all entries for this property (2 total)

Method: Electroabsorption
Origin: experimental (T = 15.0 K)
Band gap (fundamental)

Crystal system: unknown

Band gap (fundamental), eV
Fixed parameters:
  • temperature = 15.0 K
K. Hansen, C. Wong, C. E. McClure, B. Romrell, L. Flannery, D. Powell, K. Garden, A. Berzansky, M. Eggleston, D. King, C. Shirley, M. Beard, W. Nie, A. Schleife, J. Colton, and L. Whittaker-Brooks, Uncovering Unique Screening Effects in 2D Perovskites: Implications for Exciton and Band Gap Engineering, ResearchSquare Preprint, 1‑22 (2023). doi: https://doi.org/10.21203/rs.3.rs-2667143/v1.
System description
Dimensionality: 2D n: 1
Sample type: film

Starting materials: PbO, HI, H3PO2, heptylamine

Product: spin-coated thin film

Description: First step: (C7)2PbI4 single crystal flakes synthesized as follows: Slow-cooling in HI method: 2.232g (10 mmol) of PbO dissolved in glass vial containing 10 mL of HI and 1.7 mL of H3PO2. Brought to near-boiling temperature. 10 mmol of the organic amine mixed with 5 mL HI, cooled in an ice bath. Solutions were mixed and heated, then cooled to room temperature, upon which single crystal flakes form. Crystals were then washed thrice with diethyl ether and dried under a vacuum. Second step (thin film formation): Flakes were dissolved in 4:1 DMF:DMSO solvent mixture, stirred for 30 minutes. Substrate: quartz substrate with 120 nm gold layer of interdigitated fingers. Precursor solution (0.1-0.3 molar) pipetted onto substrate and then spun at 4000 rpm for 30 seconds, targeting film thickness of 80-300nm. Film was solvent-annealed, then enclosed with 2mL dH2O. When the crystallites were cooled to low temperature, a portion remained in phase I structure, allowing for simultaneous measurements in phase I and II structures.

Method: Electroabsorption

Description: Films were spin-coated onto interdigitated Au electrode array - 45 micron distance between opposing fingers. Samples mounted in cryostat with Cu wires soldered to opposing electrode stripes. Xe lamp light spectrally filtered, focused on sample and subsequently on UV-enhanced Si photodiode detector. Sample transmission, substrate transmission, and sample electrotransmission were collected in independent scans.Absorbance and electroabsorbance were then calculated from the respective transmissions. The fundamental gap is determined by the crossover point of absorption curves measured under different electric fields in the fundamental band gap region.

Comment: Significantly more detail in paper.

K. Hansen, C. Wong, C. E. McClure, B. Romrell, L. Flannery, D. Powell, K. Garden, A. Berzansky, M. Eggleston, D. King, C. Shirley, M. Beard, W. Nie, A. Schleife, J. Colton, and L. Whittaker-Brooks, Uncovering Unique Screening Effects in 2D Perovskites: Implications for Exciton and Band Gap Engineering, ResearchSquare Preprint, 1‑22 (2023). doi: https://doi.org/10.21203/rs.3.rs-2667143/v1.

Extraction method: Manual from article (Table S1)
Entry added on: Aug. 16, 2023, 6:46 p.m.
Entry added by: Kelly Ma
Last updated on: Aug. 16, 2023, 6:51 p.m.
Last updated by: Kelly Ma

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Data set ID: 2375 Did you find any mistakes or inconsistencies about this data? Send us a note and we'll have a look at it and send you a reply. Thanks!

Exciton binding energy

See all entries for this property (2 total)

Method: Electroabsorption
Origin: experimental (T = 15.0 K)
Exciton binding energy

Crystal system: unknown

Exciton binding energy, eV
Fixed parameters:
  • temperature = 15.0 K
K. Hansen, C. Wong, C. E. McClure, B. Romrell, L. Flannery, D. Powell, K. Garden, A. Berzansky, M. Eggleston, D. King, C. Shirley, M. Beard, W. Nie, A. Schleife, J. Colton, and L. Whittaker-Brooks, Uncovering Unique Screening Effects in 2D Perovskites: Implications for Exciton and Band Gap Engineering, ResearchSquare Preprint, 1‑22 (2023). doi: https://doi.org/10.21203/rs.3.rs-2667143/v1.
System description
Dimensionality: 2D n: 1
Sample type: film

Starting materials: PbO, HI, H3PO2, heptylamine

Product: spin-coated thin film

Description: First step: (C7)2PbI4 single crystal flakes synthesized as follows: Slow-cooling in HI method: 2.232g (10 mmol) of PbO dissolved in glass vial containing 10 mL of HI and 1.7 mL of H3PO2. Brought to near-boiling temperature. 10 mmol of the organic amine mixed with 5 mL HI, cooled in an ice bath. Solutions were mixed and heated, then cooled to room temperature, upon which single crystal flakes form. Crystals were then washed thrice with diethyl ether and dried under a vacuum. Second step (thin film formation): Flakes were dissolved in 4:1 DMF:DMSO solvent mixture, stirred for 30 minutes. Substrate: quartz substrate with 120 nm gold layer of interdigitated fingers. Precursor solution (0.1-0.3 molar) pipetted onto substrate and then spun at 4000 rpm for 30 seconds, targeting film thickness of 80-300nm. Film was solvent-annealed, then enclosed with 2mL dH2O. When the crystallites were cooled to low temperature, a portion remained in phase I structure, allowing for simultaneous measurements in phase I and II structures.

Method: Electroabsorption

Description: Films were spin-coated onto interdigitated Au electrode array - 45 micron distance between opposing fingers. Samples mounted in cryostat with Cu wires soldered to opposing electrode stripes. Xe lamp light spectrally filtered, focused on sample and subsequently on UV-enhanced Si photodiode detector. Sample transmission, substrate transmission, and sample electrotransmission were collected in independent scans. Absorbance and electroabsorbance were then calculated from the respective transmissions. The exciton binding energy arises as the difference of the 1s exciton peak energy observed in conventional absorption and the fundamental gap as determined by the crossover point of absorption curves measured under different electric fields in the fundamental band gap region.

Comment: Significantly more detail in paper.

K. Hansen, C. Wong, C. E. McClure, B. Romrell, L. Flannery, D. Powell, K. Garden, A. Berzansky, M. Eggleston, D. King, C. Shirley, M. Beard, W. Nie, A. Schleife, J. Colton, and L. Whittaker-Brooks, Uncovering Unique Screening Effects in 2D Perovskites: Implications for Exciton and Band Gap Engineering, ResearchSquare Preprint, 1‑22 (2023). doi: https://doi.org/10.21203/rs.3.rs-2667143/v1.

Extraction method: Manual from article (Table S1)
Entry added on: Aug. 16, 2023, 6:47 p.m.
Entry added by: Kelly Ma
Last updated on: Aug. 16, 2023, 6:52 p.m.
Last updated by: Kelly Ma

Download data
Data set ID: 2376 Did you find any mistakes or inconsistencies about this data? Send us a note and we'll have a look at it and send you a reply. Thanks!

Exciton energy

See all entries for this property (2 total)

Method: Electroabsorption
Origin: experimental (T = 15.0 K)
Exciton energy

Crystal system: unknown

Exciton energy, eV
Fixed parameters:
  • temperature = 15.0 K
K. Hansen, C. Wong, C. E. McClure, B. Romrell, L. Flannery, D. Powell, K. Garden, A. Berzansky, M. Eggleston, D. King, C. Shirley, M. Beard, W. Nie, A. Schleife, J. Colton, and L. Whittaker-Brooks, Uncovering Unique Screening Effects in 2D Perovskites: Implications for Exciton and Band Gap Engineering, ResearchSquare Preprint, 1‑22 (2023). doi: https://doi.org/10.21203/rs.3.rs-2667143/v1.
System description
Dimensionality: 2D n: 1
Sample type: film

Starting materials: PbO, HI, H3PO2, heptylamine

Product: spin-coated thin film

Description: First step: (C7)2PbI4 single crystal flakes synthesized as follows: Slow-cooling in HI method: 2.232g (10 mmol) of PbO dissolved in glass vial containing 10 mL of HI and 1.7 mL of H3PO2. Brought to near-boiling temperature. 10 mmol of the organic amine mixed with 5 mL HI, cooled in an ice bath. Solutions were mixed and heated, then cooled to room temperature, upon which single crystal flakes form. Crystals were then washed thrice with diethyl ether and dried under a vacuum. Second step (thin film formation): Flakes were dissolved in 4:1 DMF:DMSO solvent mixture, stirred for 30 minutes. Substrate: quartz substrate with 120 nm gold layer of interdigitated fingers. Precursor solution (0.1-0.3 molar) pipetted onto substrate and then spun at 4000 rpm for 30 seconds, targeting film thickness of 80-300nm. Film was solvent-annealed, then enclosed with 2mL dH2O. When the crystallites were cooled to low temperature, a portion remained in phase I structure, allowing for simultaneous measurements in phase I and II structures.

Method: Electroabsorption

Description: Films were spin-coated onto interdigitated Au electrode array - 45 micron distance between opposing fingers. Samples mounted in cryostat with Cu wires soldered to opposing electrode stripes. Xe lamp light spectrally filtered, focused on sample and subsequently on UV-enhanced Si photodiode detector. Sample transmission, substrate transmission, and sample electrotransmission were collected in independent scans. Absorbance and electroabsorbance were then calculated from the respective transmissions.

Comment: Significantly more detail in paper.

K. Hansen, C. Wong, C. E. McClure, B. Romrell, L. Flannery, D. Powell, K. Garden, A. Berzansky, M. Eggleston, D. King, C. Shirley, M. Beard, W. Nie, A. Schleife, J. Colton, and L. Whittaker-Brooks, Uncovering Unique Screening Effects in 2D Perovskites: Implications for Exciton and Band Gap Engineering, ResearchSquare Preprint, 1‑22 (2023). doi: https://doi.org/10.21203/rs.3.rs-2667143/v1.

Extraction method: Manual from article (Table S1)
Entry added on: Aug. 16, 2023, 6:48 p.m.
Entry added by: Kelly Ma
Last updated on: Aug. 16, 2023, 6:52 p.m.
Last updated by: Kelly Ma

Download data
Data set ID: 2377 Did you find any mistakes or inconsistencies about this data? Send us a note and we'll have a look at it and send you a reply. Thanks!


License

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