N butyllithium solution

THF and Et₂O were dried over sodium/benzophenone and distilled prior to use. Dichloromethane, chloroform and pentane were dried over CaH₂ and distilled prior to use. Acetonitrile solvent was dried using a MBraun Solvent Purification System (model MB-SPS 800) equipped with alumina drying columns. Benzaldehyde (Alfa Aesar, 98%) was dried over CaH₂, distilled and stored under argon. n-Butyllithium solution 11 M in hexanes, Lithium bis(trimethylsilyl)amide, Phosphazene (P₄-tBu) 0.8 M in hexane and terephthalaldehyde were purchased from Sigma-Aldrich and used without further purification. Diisopropylformamide (Alfa Aesar) and piperidinoformamide (Sigma Aldrich) were stored under argon over activated molecular sieves 4 Å. Trifluoromethanesulfonic acid (TCI), Trifluoromethanesulfonic anhydride (ABCR), and Benzaldehyde (Alfa Aesar) were distilled prior to use. Phenyllithium 1.9 M in di-n-butyl ether was purchased from Alfa Aesar and used without purification.

1,2-Dichlorocyclopentane, n-butyl lithium solution, and tris(dibenzylideneacetone) dipalladium(0)-chloroform adduct were purchased from Sigma-Aldrich Co., Ltd. Cesium fluoride and tetrakis(triphenylphosphine)palladium were purchased from Tokyo Chemical Industry. 3-Bromo-2-methylthiophene, acetonitrile, and 4-pyridylboronic acid were purchased from Wako Pure Chemical Industries, Ltd. Triisopropyl borate, N-bromosuccinimide, acetic acid, ethyl acetate, hexane, methanol (MeOH), Na₂CO₃, NaOH and MgSO₄ were purchased from Nacalai Tesque. Tetrahydrofuran (THF) and DMF were purified by utilizing a Glass Contour solvent dispending system. Other reagents were reagent grade and used without further purification. 2-Methyl-3-thienylboronic acid and non-substituted DTE (compound 1) was synthesized according to the procedures of Shinokubo et al.^{49 (link)} 1,2-Bis(2′-methyl-5′-bromothien-3′-yl)perfluorocyclopentene (compound 2) was prepared from compound 1 by reacting with N-bromosuccinimide according to the method reported by Park et al.^{50 (link)}

Toluene (99.7%, VWR, Darmstadt, Germany), tetrahydrofurane (99.5%, VWR), sulfuryl chloride (SO₂Cl₂, 98%, Aldrich, Munich, Germany), n-pentane (98%, Baker, Gross-Gerau, Germany), phosphorous trichloride (PCl₃, 99%, Merck KGaA, Darmstadt, Germany), and 2-(2-Methoxyethoxy) ethanol (C₅H₁₂O₃ 99%, Aldrich) were freshly distilled beforehand. Sodium hydride (60% dispersion in mineral oil, Aldrich), sodium hydroxide (98%, Aldrich), n-butyl lithium solution (1.6 M in hexane, Aldrich), lithium bis(trimethylsilyl)amide (LiN(Si(CH₃)₃)₂, 97%, Aldrich), boron trifluoride diethyl etherate (BF₃·O(C₂H₅)₂, Aldrich), and phosphorous pentachloride (PCl₅, Aldrich) were kept in an argon filled glove box. The dialysis tubes (1.2–1.4 × 10⁻⁴ g mol⁻¹, Reichelt Chemietechnik, Heidelberg, Germany), Celite545^® (Merck KGaA), and the molecular sieve 4 Å (VWR) used for polymer purification were cleaned and dried prior to use (140 °C for 48 h). All synthesis steps were carried out using standard vacuum line Schlenk techniques (under inert gas).

Tellurium (200 mesh, 99.85%), selenium, sulfur, sodium borohydride (powder, 98%), bromine, iodine, n-butyl lithium solution, and 1-bromobutane (BuBr, 99%) were purchased from Aldrich. Sodium sulfite was purchased from EMScience. Tetrabutylammonium bromide (TBAB, 98%) was obtained from Alfa Aesar, and hydrogen tetrachloroaurate hydrate (49 wt% Au) was obtained from Strem Chemicals. The organic solvents dimethyl formamide, hexane, toluene, methanol, dichloromethane, ethanol, and tetrahydrofuran were of analytical grade. They were all used as received. Milli-Q water (18.2 MΩ) was used. All glassware was cleaned in sulfuric acid with Nochromix and rinsed with a large amount of water before use.
Di-butyl disulfide was prepared by addition of n-butyl lithium (1 eq.) to a THF suspension of elemental sulfur followed by water and iodine. A similar procedure was adopted to prepare dibutyl ditelluride, omitting the treatment of the reaction media with iodine and exposing the intermediate tellurol to an oxygen atmosphere for the oxidation step. Di-butyl diselenide was prepared by reacting elemental selenium in aqueous basic media with hydrazine hydrate followed by addition of butyl bromide and Tetrabutylammonium bromide. The synthetic reaction is summarized in Fig. 6. A detailed experimental procedure is presented in the ESI.†

Initially, the crystalline LiMoS₂ was prepared by treating purified natural molybdenum disulfide (DM-1, Scopin Factory, Scopin, Russia) with a particle size (95%) smaller than 7 μm with an excess of 1.6 M n-butyllithium solution in hexane (Aldrich) for 1 week, washing in hexane and drying in vacuum. The obtained compound was immersed in bi-distilled water, sonicated for 15 min, and stirred on a magnetic stirrer for 30 min to prepare the 1 mg·mL⁻¹ dispersion of LiMoS₂. The powdered MR-MoS₂ layered compounds have been obtained by mixing aqueous dispersions of MoS₂ with water solutions of benzyldimethyl{3-[(1-oxotetradecyl)amino]propyl}ammonium chloride (Infamed, Vidnoye, Russia) containing 0.14 (LC1) or 0.5 (LC2) mole of the salt per 1 mole of MoS₂. After stirring of the reaction mixture on a magnetic stirrer for 2 h, the precipitate formed during the stirring, was collected by centrifugation, washed by water, and dried in vacuum. The composition of the products was determined from elemental analysis data (C, H, N, Mo). Found (calculated) for (MR)_0.14MoS₂ (LC1): C 20.48 (20.17), N 1.87 (1.81), H 2.81 (3.04), Mo 43.85 (44.3); for (MR)_0.27MoS₂ (LC2): C 31.33 (31,31), N 2.70 (2.81), H 4.14 (4.72), Mo 36.1 (35.7).