A monoclinic polymorph of isoxsuprine hydrochloride

Abstract

A monoclinic polymorph of the title compound [systematic name: 2‐hydroxy‐2‐(4‐methoxy­phenyl)‐1‐methyl‐N‐(1‐phen­oxy‐2‐propyl)­ethanaminium chloride], C18H24N2O3+·Cl−, has been found in addition to the already known triclinic polymorph. The molecular conformation in both polymorphs is very similar.

35Cl dynamic nuclear polarization solid-state NMR of active pharmaceutical ingredients

“…S13, ESI †). [81][82][83][84] 2.3 NMR 13 C and 35 Cl SSNMR DNP experiments were conducted on a 9.4 T (400 MHz)/263 GHz Bruker Avance III solid-state DNP NMR spectrometer 50 using a 3.2 mm HXY probe configured for 1 H-13 C- 35 Cl experiments located at the DOE Ames Laboratory.…”

Generation of crystal structures using known crystal structures as analogues

“…Some successes also occur in systems with chemically different molecules in the asymmetric unit (Z r > 1). For example, CSD entry BAHFAR01 (Yathirajan et al, 2004), is matched by the analogue in CSD entry PEZCUT (Dastychová et al, 2007). Both structures are ionic systems with a positively charged organic component and a chloride counterion.…”

35Cl solid-state NMR of HCl salts of active pharmaceutical ingredients: structural prediction, spectral fingerprinting and polymorph recognition

“…78 Euler angles were calculated using the EFGShield software program. 79 All calculations were performed on coordinates derived from reported crystal structures [80][81][82][83][84][85][86][87][88][89][90][91][92] using the CASTEP [66][67][68][69] code in the Materials Studio 5.0 software suite which utilizes the gauge-including projector augmented wave algorithm (GIPAW) 66 for NMR calculations. Calculations utilized the generalized gradient approximation (GGA), revised Perdew, Burke and Ernzerhof (rPBE) functional with on-the-fly pseudopotentials, a k-point spacing of 0.08 Å, and a plane wave basis set cut-off energy of 500 eV.…”

“…In all cases, initial molecular coordinates of the heavy (non-hydrogen) atoms were obtained from singlecrystal X-ray structures. 80,[82][83][84][85][86]88,[90][91][92] As mentioned in the Table 2 Experimental and theoretical 35 Cl EFG and CS tensor parameters for HCl pharmaceuticals with three and four or more close H⋯Cl contacts a Definitions of EFG and CS tensor parameters are given in Table 1.…”