This file FILENAME was updated on 2017-12-21 by Grant W. Fahnhorst ------------------- GENERAL INFORMATION ------------------- Title of Dataset: Supporting Data for Poly(isoprenecarboxylates) from glucose via anhydromevalonolactone. ACS Macro Lett. 2016, 5, 1128-1131. Author Information: Principal Investigator Contact Information Name: Thomas R. Hoye Institution: University of Minnesota Address: Department of Chemistry, 207 Pleasant Street, SE, Minneapolis, Minnesota 55455 Email: hoyex001@umn.edu Associate or Co-investigator Contact information Name: Nicolas R. Ball-Jones Institution: University of Minnesota Address: Department of Chemistry, 207 Pleasant Street, SE, Minneapolis, Minnesota 55455 Email: nballjon@gmail.com Associate or Co-investigator Contact Information Name: Grant W. Fahnhorst Institution: University of Minnesota Address: Department of Chemistry, 207 Pleasant Street, SE, Minneapolis, Minnesota 55455 Email: fahn0018@umn.edu Date of data collection: ca. May 2015 ~ August 2016 Geographic location of data collection: University of Minnesota Information about funding sources that supported the collection of the data: This research was supported by a grant from the National Science Foundation through the Center for Sustainable Polymers (grant CHE-1413862). -------------------------- SHARING/ACCESS INFORMATION -------------------------- 1. Licenses/restrictions placed on the data: None The figures and some files contained here are the property of ACS Macro Letters 2. Links to publications that cite or use the data: Link to article page on ACS Macro Letters http://pubs.acs.org/doi/abs/10.1021/acsmacrolett.6b00560 3. Links to other publicly accessible locations of the data: Link to Center for Sustainable Polymers publications page https://csp.umn.edu/publications/ 4. Links/relationships to ancillary data sets: N/A 5. Was data derived from another source? No 6. Recommended citation for the data: LEAVE BLANK --------------------- DATA & FILE OVERVIEW --------------------- Purpose Statement: This document describes... General Notes: Raw data files are named according to the number of the compound in the manuscript. Folders are organized by the desired analytical technique used. Files Contained: Copy directory structure. Under each top-level file or folder, add description of the data, file formats, software required to open, and any other information (e.g., conditions, filenaming, weirdness) to help understand and explain the files. The Folder is organized into two main folders 1) Manuscript Chemdraw Figures -contains raw chemdraw files based and are identified by the scheme, figure, or table followed by the number as identified in the main text of the document. 2) Raw Data Files - DSC Excel Files, contains 5 files - IR Spectra, contains 10 files total - NMR Spectra, contains 11 subfolders and 935 files total The NMR files housed within the NMR spectra folder both the 1H and 13 C NMR spectra for the monomers and polymers,labeled as the number given within the actual document. These files contain all the parameters, as given and developed, via the Bruker software. - Rheology- TA instruments TTS Files, contains 8 files total - SEC- Excel File, contains 2 files total - TGA txt files, contains 5 files total Each of these folders labeled in (2) are organized by the number of labeling of each compound listed in the text of the main document. The terms PEIC, PMIC, etc. stand for the acronyms that the polymers are given within the text of the actual document [Poly(Methyl IsopreneCarboxylate) is for PMIC]. DSC: Thermal analyzer instrument. -IR: Infrared (IR) spectroscopy DMSO: Dimethyl sulfoxide TTS: time-temperature superposition NMP: Nitroxide-mediated radical polymerization TGA: Thermogravimetric analysis SEC: Size-exclusion chromatography Additional related data collected that was not included in the current data package: None Are there multiple versions of the dataset? No -------------------------- METHODOLOGICAL INFORMATION -------------------------- Description of methods used for collection, generation, and processing of data: "General Experimental Protocols Anhydrous THF, DCM, and diethyl ether were taken immediately prior to use from a column of activated alumina. Reported reaction temperatures are the temperature of the external heating or cooling bath. Instrumental methods: NMR: 1H and 13C NMR spectra were recorded on a Bruker Avance 500 (500 MHz) or a Varian Inova 500 (500 MHz) spectrometers. 1H NMR chemical shifts in CDCl3 are referenced to TMS (d 0.00 ppm). Non-first-order multiplets in 1H NMR spectra have been identified as ‘nfom.’ The following format is used to report resonances: chemical shift in ppm [multiplicity, coupling constant(s) in Hz, integral, and assignment]. 1H NMR assignments are indicated by the substructural environment (e.g., CHaHb). Coupling constant analysis was led by methods we have described elsewhere.1 13C NMR chemical shifts for spectra recorded in CDCl3 are referenced to the carbon resonance in CDCl3 (d 77.16). ATR-FTIR: Fourier transform infrared (FTIR) spectra were recorded with a Bruker Alpha Platinum ATR-FTIR instrument (diamond single-bounce crystal). Typically 16 scans were acquired and a 4 s acquisition time was used. Mass spectrometry of non-polymeric samples: MS measurements were made using electron impact ionization on an Agilent 5975 MSD at 70 eV GC-MS. The column stationary phase was an Agilent HP-5 with a 0.25 µm film thickness, 30 m long, × 0.32 mm i.d. Size Exclusion Chromatography (SEC): SEC was conducted on a liquid chromatograph (Agilent 1100 series) fitted with a refractive index detector (HP1047A). Polymer samples were dissolved in CHCl3 (1-2 mg•mL-1) and eluted through three successive Varian PLgel Mixed C columns (7.5 mm id; 25 cm l) at 35 °C at a flow rate of 1 mL•min-1. Dispersity and mass-average molar mass of the samples were referenced to polystyrene standards. Thermogravimetric Analysis (TGA): TGA was performed (TA Instruments Q500) at a heating rate of 10 °C•min-1 under an atmosphere of nitrogen. The sample size was 5–15 mg. Differential Scanning Calorimetry (DSC): Differential scanning calorimetry (TA Instruments Q1000 DSC) was performed on samples hermetically sealed in aluminum pans. Each sample was heated to 250 °C, cooled to -60 °C, and reheated to 250 °C. Glass transition temperatures were taken as the inflection point and are reported as measured on the second (or third) heating cycle. Linear Viscosity (Rheology) Measurements: A 0.50 g sample of solid polymer was placed onto the bottom rheometer plate (2.5 cm d) held at the desired reference temperature (70 °C above the Tg). The top plate was manually lowered under a steady rate sweep at a frequency of 0.1/s for approximately 2 full rotations to prepare the sample for the measurements. A dynamic strain sweep was taken at this temperature to ensure linearity within the sample. The dynamic linear viscoelastic measurements were carried out within the linear viscoelastic regime at temperatures in the range from 10 to 125 °C. The dynamic measurements were conducted in the range of 0.1-100 rad/s at a strain of 1%. A gap of approximately 1.0 mm was used to minimize edge effects. The rheological measurements were carried out under an atmosphere of nitrogen to minimize oxidative events of the polymer samples during testing. Entanglement molecular weights were approximated using the equation. The plateau moduli were calculated using the minimum of tan delta vs G’." This description was taken directly from the supporting information on ACS Macro Letters publication. People involved with sample collection, processing, analysis and/or submission: NA