Host-guest co-amorphous structure revealed by the suppression of the first sharp diffraction peak in isotactic poly(4-methyl-1-pentene)

Ayano Chiba; Tomoki Ogihara; Yusuke Hiejima

arxiv: 2604.15892 · v1 · submitted 2026-04-17 · ⚛️ physics.chem-ph · cond-mat.mtrl-sci· cond-mat.soft

Host-guest co-amorphous structure revealed by the suppression of the first sharp diffraction peak in isotactic poly(4-methyl-1-pentene)

Tomoki Ogihara , Yusuke Hiejima , Ayano Chiba This is my paper

Pith reviewed 2026-05-10 07:58 UTC · model grok-4.3

classification ⚛️ physics.chem-ph cond-mat.mtrl-scicond-mat.soft

keywords host-guest co-amorphousfirst sharp diffraction peakpoly(4-methyl-1-pentene)X-ray diffractionamorphous voidsmolecular sievesdecane sorption

0 comments

The pith

Immersion in decane suppresses the first sharp diffraction peak in stretched P4MP1 by filling the polymer's internal voids, forming a host-guest co-amorphous structure at ambient conditions.

A machine-rendered reading of the paper's core claim, the machinery that carries it, and where it could break.

The paper examines how the first sharp diffraction peak in isotactic poly(4-methyl-1-pentene) responds to immersion in decane. It shows that this peak, linked to internal voids in the amorphous matrix, is suppressed when decane molecules enter those voids. The result establishes a host-guest co-amorphous system that operates at room temperature and atmospheric pressure, distinct from conventional mixtures because the guests occupy the host's pre-existing voids. If correct, the structure opens routes to selective sorption and exchange in the liquid phase without needing high pressure or crystallinity.

Core claim

Stretched samples of P4MP1 exhibit clear suppression of the amorphous FSDP when immersed in decane. This suppression occurs because decane molecules occupy the internal voids that produce the FSDP, creating a host-guest co-amorphous arrangement at room temperature and atmospheric pressure. The effect parallels the FSDP behavior seen under pressure with helium and the intensity changes in Bragg peaks of crystalline host-guest systems.

What carries the argument

The first sharp diffraction peak (FSDP), whose intensity drops when guest molecules fill the host polymer's pre-existing internal voids.

If this is right

The co-amorphous structure permits selective sorption and guest exchange, similar to known co-crystals.
Polymers that form such void-based hosts become candidates for liquid-phase molecular sieves.
Changes in FSDP intensity ratios can serve as a diffraction signature comparable to Bragg peak ratio shifts in crystalline host-guest compounds.
The approach works at ambient pressure and temperature, removing the need for high-pressure media to observe void occupation.

Where Pith is reading between the lines

These are editorial extensions of the paper, not claims the author makes directly.

The same void-filling mechanism could be tested in other semicrystalline polymers that display a clear FSDP.
Guest exchange experiments might reveal whether the structure supports reversible molecular sieving in solution.
The parallel with helium-pressurized SiO2 glass suggests that FSDP suppression is a general indicator of void occupation across both polymeric and inorganic amorphous hosts.

Load-bearing premise

That the FSDP suppression is caused specifically by decane molecules occupying internal voids rather than by surface effects, conformational shifts, or unrelated interactions.

What would settle it

Direct measurement of decane density inside the polymer or an experiment in which decane cannot reach the voids but still produces no FSDP change.

Figures

Figures reproduced from arXiv: 2604.15892 by Ayano Chiba, Tomoki Ogihara, Yusuke Hiejima.

**Figure 2.** Figure 2: shows a two-dimensional XRD pattern of the dry stretched sample. The image consists of a superposition of spot-like Bragg reflections and a ringshaped amorphous halo, due to coexistence of crystalline and amorphous regions. In more detail, the XRD image exhibits (i) a ring-shaped amorphous FSDP, (ii) the spot-like Bragg reflections such as the 200 reflection, (iii) a horizontal streak, and (iv) a secondar… view at source ↗

**Figure 3.** Figure 3: FIG 3. X [PITH_FULL_IMAGE:figures/full_fig_p004_3.png] view at source ↗

**Figure 4.** Figure 4: FIG 4. SANS patterns of oriented P4MP1 before and after deuterated decane [PITH_FULL_IMAGE:figures/full_fig_p005_4.png] view at source ↗

read the original abstract

While host-guest co-crystals are well established, and co-amorphous solids are recognized in materials science, the concept of a host-guest co-amorphous structure remains largely unexplored. A potential analogue is seen in SiO2 glass under high pressure with helium as a pressure medium; the drop in compressibility in this system is ascribed to helium atoms occupying internal voids. In this study, we investigated a semicrystalline polymer, isotactic poly(4-methyl-pentene-1) (P4MP1), which shares key characteristics with SiO2 glass, particularly regarding the first sharp diffraction peak (FSDP). The FSDP in P4MP1 is attributed to internal voids, as evidenced by its suppression under pressure and recovery upon decompression for molten P4MP1. Notably, the response to helium as a pressure medium is also known to parallel the behavior observed in SiO2 glass. Here, we analyzed two-dimensional X-ray diffraction (2D-XRD) patterns of stretched P4MP1 and found a suppression of FSDP when P4MP1 is immersed in decane. The use of stretched samples enabled the clear isolation of the amorphous FSDP from overlapping crystalline diffractions. Our findings reveal the existence of a host-guest co-amorphous system at room temperature and atmospheric pressure, in which decane molecules occupy the amorphous host matrix of P4MP1. Unlike conventional co-amorphous mixtures, this structure is defined by the specific accommodation of guests within the host's inherent voids. Intriguingly, the signature of this structure in diffraction measurements, manifested as changes in the FSDP intensity ratio, may be regarded to parallel the variations in Bragg peak intensity ratios in host-guest co-crystals. Since selective sorption and guest exchange are well-known in co-crystals, hosts capable of forming co-amorphous structures will be promising materials for molecular sieves, or more generally, liquid-phase molecular sieves.

Editorial analysis

A structured set of objections, weighed in public.

Desk editor's note, referee report, simulated authors' rebuttal, and a circularity audit. Tearing a paper down is the easy half of reading it; the pith above is the substance, this is the friction.

Desk Editor's Note private letter to a colleague

Stretched P4MP1 shows FSDP drop when immersed in decane, but the host-guest void-filling claim needs controls to separate it from ordinary solvent effects.

read the letter

The paper's core observation is that 2D-XRD on stretched isotactic P4MP1 reveals clear suppression of the amorphous first sharp diffraction peak after immersion in decane at room temperature and pressure. The authors link this to decane occupying internal voids, creating a host-guest co-amorphous arrangement distinct from ordinary co-amorphous mixtures or co-crystals. They use the stretching step to separate the amorphous signal from crystalline peaks, which is a practical move that makes the FSDP change easier to track. The analogy to pressure-induced FSDP behavior in molten P4MP1 and in SiO2 glass with helium is drawn directly from existing literature and gives the interpretation a coherent starting point. That experimental isolation of the amorphous component is the part that actually adds something new to the record. The interpretation step is where it gets thinner. The stress-test concern is fair: immersion in a liquid can produce swelling, helix relaxation, or surface-layer changes that alter intermolecular distances without any guest molecule sitting inside pre-existing voids. No reversibility data, no comparison with non-penetrating solvents, and no sorption isotherms are referenced in the abstract or the provided summary, so the specific void-occupation reading is not yet discriminated from these alternatives. The paper does not appear to contain machine-checked proofs or independently falsifiable predictions beyond the diffraction pattern itself. This is the kind of work that belongs in a polymer or soft-matter journal where readers already follow FSDP studies. A materials chemist thinking about amorphous sieves might skim it for the experimental trick, but would wait for stronger controls before treating the host-guest label as settled. It deserves peer review because the raw observation is clean enough to be worth referee time, even if the authors will probably have to add the missing discrimination experiments.

Referee Report

2 major / 1 minor

Summary. The manuscript reports 2D-XRD measurements on stretched isotactic poly(4-methyl-1-pentene) (P4MP1) showing suppression of the amorphous first sharp diffraction peak (FSDP) upon immersion in decane at ambient conditions. By analogy to pressure-induced FSDP changes in molten P4MP1 and SiO2 glass (with helium), the authors interpret the intensity drop as direct evidence that decane molecules occupy the internal voids of the amorphous P4MP1 host matrix, thereby establishing a host-guest co-amorphous structure distinct from conventional co-amorphous mixtures. The stretching protocol is used to isolate the amorphous FSDP from crystalline peaks, and the FSDP intensity ratio change is proposed to parallel Bragg-peak ratio variations in host-guest co-crystals, with suggested applications to liquid-phase molecular sieves.

Significance. If the void-occupation interpretation is substantiated, the work would introduce a new conceptual category of host-guest co-amorphous solids at room temperature and atmospheric pressure, extending crystalline host-guest chemistry into the amorphous regime with potential for selective sorption. The experimental isolation of the amorphous FSDP via stretching is a useful technical step, and the explicit parallel to co-crystal diffraction signatures is a clear framing device. The result would be strengthened by quantitative metrics and controls that directly test the proposed mechanism against generic solvent-polymer interactions.

major comments (2)

[Abstract and results section] Abstract and results section: The central claim that FSDP suppression demonstrates decane occupation of the host's native internal voids (rather than surface adsorption, swelling-induced conformational relaxation of isotactic helices, or non-specific packing changes) is not supported by any referenced control experiments such as reversibility after solvent removal, comparison with non-penetrating solvents of similar size, or sorption isotherms. The pressure/helium analogies cited for molten P4MP1 do not automatically transfer to ambient liquid immersion, leaving the mechanistic link load-bearing but untested.
[Results section on 2D-XRD patterns] Results section on 2D-XRD patterns: The reported FSDP suppression is described qualitatively without accompanying quantitative intensity ratios (pre- vs. post-immersion), error bars, or statistical measures of reproducibility across samples. This makes it difficult to evaluate the magnitude of the effect or to compare it rigorously with the pressure-response data invoked for the SiO2-glass analogy.

minor comments (1)

[Introduction or discussion] The manuscript would benefit from a brief explicit statement of the void-size scale reported for P4MP1 and the molecular dimensions of decane to allow readers to assess steric compatibility.

Simulated Author's Rebuttal

2 responses · 1 unresolved

We thank the referee for the constructive and detailed comments, which help clarify the interpretive limits of our observations. We respond point by point below, indicating where revisions will be made to the manuscript.

read point-by-point responses

Referee: [Abstract and results section] Abstract and results section: The central claim that FSDP suppression demonstrates decane occupation of the host's native internal voids (rather than surface adsorption, swelling-induced conformational relaxation of isotactic helices, or non-specific packing changes) is not supported by any referenced control experiments such as reversibility after solvent removal, comparison with non-penetrating solvents of similar size, or sorption isotherms. The pressure/helium analogies cited for molten P4MP1 do not automatically transfer to ambient liquid immersion, leaving the mechanistic link load-bearing but untested.

Authors: We agree that the mechanistic interpretation would be strengthened by direct controls. Our claim rests on the documented analogy between FSDP suppression in molten P4MP1 under pressure (and in SiO2 glass with helium) and the observed intensity drop upon decane immersion, together with the use of stretched samples to isolate the amorphous signal. We acknowledge that this analogy does not automatically extend to room-temperature liquid immersion and that alternatives such as swelling or surface effects cannot be ruled out without additional data. In the revised manuscript we will expand the discussion to explicitly address these alternatives, state the interpretive nature of the analogy, and note that the suggested controls (reversibility, non-penetrating solvent comparisons, sorption isotherms) lie outside the present experimental scope. revision: partial
Referee: [Results section on 2D-XRD patterns] Results section on 2D-XRD patterns: The reported FSDP suppression is described qualitatively without accompanying quantitative intensity ratios (pre- vs. post-immersion), error bars, or statistical measures of reproducibility across samples. This makes it difficult to evaluate the magnitude of the effect or to compare it rigorously with the pressure-response data invoked for the SiO2-glass analogy.

Authors: We accept this criticism. The original text emphasized the qualitative observation to establish the phenomenon. In the revised version we will report the quantitative FSDP intensity ratios before and after immersion, together with error bars and reproducibility statistics obtained from multiple independent samples. These numbers will be placed in the results section and used to enable a direct numerical comparison with the pressure-response data cited for molten P4MP1 and SiO2 glass. revision: yes

standing simulated objections not resolved

Direct experimental controls (reversibility after solvent removal, comparison with non-penetrating solvents of similar size, and sorption isotherms) were not performed and cannot be added without new measurements outside the scope of the current study.

Circularity Check

0 steps flagged

No circularity: claim rests on independent experimental observation plus external prior evidence

full rationale

The paper's derivation proceeds from direct 2D-XRD data on stretched P4MP1 showing FSDP suppression upon decane immersion, interpreted by analogy to previously reported pressure and helium effects on the same polymer and on SiO2 glass. No equations, fitted parameters, or predictions are introduced that reduce to the input data by construction. The void-FSDP attribution is presented as supported by cited external measurements rather than self-definition or a load-bearing self-citation chain. The host-guest conclusion is an interpretive inference, not a renaming or smuggling of an ansatz. The chain is therefore self-contained against external benchmarks.

Axiom & Free-Parameter Ledger

0 free parameters · 1 axioms · 1 invented entities

The central claim depends on interpreting FSDP as a direct reporter of void occupancy and on the analogy to high-pressure helium behavior in glass; no free parameters are fitted in the abstract, but the new structure is an interpretive construct.

axioms (1)

domain assumption The first sharp diffraction peak (FSDP) in P4MP1 arises from internal voids in the amorphous structure.
Invoked to link FSDP suppression directly to guest occupation; supported by cited pressure/decompression behavior but treated as established.

invented entities (1)

host-guest co-amorphous structure no independent evidence
purpose: To classify the observed system in which decane occupies inherent voids of the P4MP1 amorphous matrix.
Introduced as the key discovery; independent evidence is limited to the diffraction signature itself with no additional falsifiable prediction stated.

pith-pipeline@v0.9.0 · 5684 in / 1342 out tokens · 36216 ms · 2026-05-10T07:58:38.593804+00:00 · methodology

discussion (0)

Reference graph

Works this paper leans on

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Host-guest co-amorphous structure revealed by the suppression of the first sharp diffraction peak in isotactic poly(4-methyl-1-pentene)

A. Chiba, A. Oshima, and R. Akiyama, Langmuir 35, 17177 (2019). Supplemental Material for “Host-guest co-amorphous structure revealed by the suppression of the first sharp diffraction peak in isotactic poly(4-methyl-1-pentene)” Tomoki Ogihara,1 Yusuke Hiejima,2 and Ayano Chiba1* 1Department of Physics, Keio University, Yokohama, 223-8522, Japan 2Departmen...

work page 2019

[1] [1]

T. Sato, N. Funamori, and T. Yagi, Nat. Commun. 2, 345 (2011)

work page 2011

[2] [2]

G. Shen, Q. Mei, V. B. Prakapenta, P. Lazor, S. Sinogeikin, Y. Meng, and C. Park, Proc. Natl. Acad. Sci. U.S.A. 2, 345 (2011)

work page 2011

[3] [3]

This phenomenon is seen in hosts with rigid frameworks, such as metal-organic frameworks (MOFs)

The ability of a host structure to maintain its crystalline form upon guest desorption is known as permanent porosity. This phenomenon is seen in hosts with rigid frameworks, such as metal-organic frameworks (MOFs). In the case of polymer hosts, the crystalline structure known as the δ e form in syndiotactic polystyrene (sPS) corresponds to this type of s...

work page 1997

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D. L. Price, S. C. Moss, R. Reijers, M-L. Saboungi, and S. Susman, J. Phys. C: Solid State Phys. 21, L1069 (1988)

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S. R. Elliott, Nature 354, 445 (1991)

work page 1991

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S. R. Elliott, J. Phys.: Condens. Matter. 4, 7661 (1992)

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S. R. Elliott, Phys. Rev. Lett. 67, 711 (1991)

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Although the voids are not mentioned, the concept of density fluctuation may be seen in the figure in W. H. Zachariasen, J. Am. Chem. Soc. 54, 3841 (1932)

work page 1932

[9] [9]

Susman, K

S. Susman, K. J. Volin, D. L. Price, M. Grimsditch, J. P. Rino, R. K. Kalia, P. Vashishta, G. Gwanmesia, Y. Wang, and R. C. Liebermann, Phys. Rev. B 43, 1194 (1991)

work page 1991

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Meade, R

C. Meade, R. J. Hemley, and H. K. Mao, Phys. Rev. Lett. 69, 1387 (1992)

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Hirata, S

A. Hirata, S. Sato, M. Shiga, Y. Onodera, K. Kimoto, and S. Kohara, NPG Asia Mater. 16, 25 (2024)

work page 2024

[12] [12]

Chiba, N

A. Chiba, N. Funamori, K. Nakayama, Y. Ohishi, S. M. Bennington, S. Rastogi, A. Shukla, K. Tsuji, and M. Takenaka, Phys. Rev. E 85, 021807 (2012)

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J. R. Katz, Trans. Faraday Soc. 32, 77 (1936)

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R. L. Miller, R. F. Boyer, and J. Heijboer, J. Polym . Sci. Pol. Phys. 22, 2021 (1984)

work page 2021

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A. Arbe, A. -C. Fenix, J. Colmenero, D. Richter, and P. Fouquet, Soft Matter 4, 1792 (2008)

work page 2008

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L. C. Lopez, G. L. Wilkes, P. M. Stricklen, and S. A. White, J. Macromol. Sci. Part C Polym. Rev. 32, 301 (1992)

work page 1992

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G. Tu, H. Zheng, J. Yang, H. Zhou, C. Feng, and H. Gao, Int. J. Mol. Sci. 26 , 600 (2025)

work page 2025

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C. E. Wilkes, and M. H. Lehr, J. Macromol. Sci. -Phys. B7, 225 (1973). *Contact author: ayano@phys.keio.ac.jp

work page 1973

[19] [19]

Chiba, M

A. Chiba, M. Inui, Y. Kajihara, K. Fuchizaki, and R. Akiyama, J. Chem. Phys. 146, 194503 (2017)

work page 2017

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J. H. Griffith and B. G. Rånby, J. Polym. Sci. 44, 369 (1960)

work page 1960

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A. C. Puleo, D. R. Paul, and P. K. Wong, Polymer 30, 1357 (1989)

work page 1989

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Rastogi, M

S. Rastogi, M. Newman, and A. Keller, Nature 353, 55 (1991)

work page 1991

[23] [23]

Murashige, Y

H. Murashige, Y. Hiejima, Y. Sanada, and A. Chiba, Macromol. Symp. 408, 2200090 (2023)

work page 2023

[24] [24]

Inoue, T

K. Inoue, T. Oka, K. Miura, and N. Yagi, AIP Conf. Proc. 705, 336 (2004)

work page 2004

[25] [25]

The patterns for the dry sample, as well as those recorded 20 minutes and 7 hours afte r immersion in the solvent, are shown

See Supplemental Material at [URL] for a comparison of the two-dimensional diffraction patterns of oriented P4MP1 in the FSDP region before and after solvent occlusion. The patterns for the dry sample, as well as those recorded 20 minutes and 7 hours afte r immersion in the solvent, are shown

work page

[26] [26]

Takata, J

S. Takata, J. Suzuki, T. Shinohara, T. Oku, T. Tominaga, K. Ohishi, H. Iwase, T. Nakatani, Y. Inamura, T. Ito, K. Suzuya, K. Aizawa, M. Arai, T. Otomo, and M. Sugiyama, JPS Conf. Proc. 8, 036020 (2015)

work page 2015

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Kusanagi, M

H. Kusanagi, M. Takase, Y. Chatani, and H. Tadokoro, J. Polym. Sci. Pol. Phys. 16, 131 (1978)

work page 1978

[28] [28]

K. Mita, H. Okumura, K. Kimura, T. Isaki, M. Takenaka, and T. Kanaya, Polym. J. 45, 79 (2013)

work page 2013

[29] [29]

Host-guest co-amorphous structure revealed by the suppression of the first sharp diffraction peak in isotactic poly(4-methyl-1-pentene)

A. Chiba, A. Oshima, and R. Akiyama, Langmuir 35, 17177 (2019). Supplemental Material for “Host-guest co-amorphous structure revealed by the suppression of the first sharp diffraction peak in isotactic poly(4-methyl-1-pentene)” Tomoki Ogihara,1 Yusuke Hiejima,2 and Ayano Chiba1* 1Department of Physics, Keio University, Yokohama, 223-8522, Japan 2Departmen...

work page 2019