Apex3 suite

The crystal structure
of the glycine–sulfamic acid 2:1 ionic cocrystal was determined
at −100 °C on a Bruker D8 Quest fixed-χ single-crystal
diffractometer equipped with a sealed-tube X-ray source that delivers
Mo Kα (λ = 0.71073 Å), a TRIUMPH monochromator, a
PHOTON 100 detector, and a nitrogen-flow Oxford Cryosystem attachment.
Unit cell determination, data reduction, and absorption correction
(multiscan method) were conducted using the Bruker APEX3 suite.³¹ Using Olex2,^{32 (link)} the
structure was solved with the ShelXT structure solution program^{33 (link)} using intrinsic phasing and refined with the
ShelXL refinement package^{34 (link)} using least-squares
minimization.

Crystal structures
were determined by single-crystal X-ray diffraction
(SCXRD) with either Cu Kα (λ = 1.5418 Å) radiation
or Mo Kα (λ = 0.71073 Å) radiation and a Bruker D8
Quest fixed-chi diffractometer equipped with a Photon 100 detector
and the nitrogen-flow Oxford Cryosystem attachment. Unit cell determination,
data reduction, and absorption correction (multiscan method) were
conducted using the Bruker APEX3 suite with implemented SADABS software.⁵¹ Structures were solved using SHELXT and refined
using SHELXL contained in Olex2.^{52 (link)} Reflection
data for the nonhydrogen atoms were refined anisotropically. All hydrogen
atoms bonded to carbon (on phenyl rings, methanol, TMA, TEA, TPA,
and TPA cations) were placed geometrically and refined using a riding
model with isotropic thermal parameters: U_iso(H) = 1.5U_eq(−CH₃), U_iso(H) = 1.2U_eq(−CH), U_iso(H) = 1.2U_eq(−CH₂). Hydrogen atoms on water (AFIX 5) and methanol (AFIX 147)
were calculated geometrically and refined using a riding model with
isotropic thermal parameter: U_iso(H) =
1.5U_eq(−OH). The hydrogen atoms
of phenolic hydroxyl groups were located from electron density difference
maps and included in the refinement process using a riding model with U_iso(H) = 1.2U_eq(−OH).
Single-crystal data are presented in Table 1.

The X-ray diffraction data were measured using a Bruker D8 Venture dual-source single crystal X-ray diffractometer, employing Cu Kα radiation (λ = 1.54178 Å). Data were collected using a Photon II CMOS area detector on samples superglued to glass fibers. Reflection data were processed using the Bruker Apex 3 Suite, including an absorption correction through SADABS, and space group determination using XPREP. The structure was determined with SHELX-2019 software. The structure was solved with XT using intrinsic phasing and refined using full-matrix least-squares on F2 through XL. The structure was finalized in Olex 2 (v.1.3.0).