de Oliveira Adriano Bof, Bresolin Leandro, Gervini Vanessa Carratu, Beck Johannes, Daniels Jörg
Departamento de Química, Universidade Federal de Sergipe, Av. Marcelo Deda Chagas s/n, Campus Universitário, 49107-230 São Cristóvão-SE, Brazil.
Escola de Química e Alimentos, Universidade Federal do Rio Grande, Av. Itália km 08, Campus Carreiros, 96203-900 Rio Grande-RS, Brazil.
IUCrdata. 2023 Nov 30;8(Pt 11):x231018. doi: 10.1107/S2414314623010180. eCollection 2023 Nov.
A second crystalline modification of the title compound, CHNS [common name: -jasmone thio-semicarbazone] was crystallized from tetra-hydro-furane at room temperature. There is one crystallographic independent mol-ecule in the asymmetric unit, showing disorder in the -jasmone chain [site-occupancy ratio = 0.590 (14):0.410 (14)]. The thio-semicarbazone entity is approximately planar, with the maximum deviation from the mean plane through the N/N/C/S/N atoms being 0.0463 (14) Å [r.m.s.d. = 0.0324 Å], while for the five-membered ring of the jasmone fragment, the maximum deviation from the mean plane through the carbon atoms amounts to 0.0465 (15) Å [r.m.s.d. = 0.0338 Å]. The mol-ecule is not planar due to the dihedral angle between these two fragments, which is 8.93 (1)°, and due to the -hybridized carbon atoms in the jasmone fragment chain. In the crystal, the mol-ecules are connected by N-H⋯S and C-H⋯S inter-actions, with graph-set motifs (8) and (7), building mono-periodic hydrogen-bonded ribbons along [010]. A Hirshfeld surface analysis indicates that the major contributions for the crystal cohesion are H⋯H (67.8%), H⋯S/S⋯H (15.0%), H⋯C/C⋯H (8.5%) and H⋯N/N⋯H (5.6%) [only non-disordered atoms and those with the highest s.o.f. were considered]. This work reports the second crystalline modification of the -jasmone thio-semicarbazone structure, the first one being published recently [Orsoni (2020 ▸). , 8681-8697] with the crystals obtained in ethanol at 273 K.
标题化合物CHNS[通用名称:茉莉酮硫代半卡巴腙]的第二种晶体变体在室温下从四氢呋喃中结晶出来。不对称单元中有一个晶体学独立分子,茉莉酮链存在无序[占有率 = 0.590 (14):0.410 (14)]。硫代半卡巴腙实体近似平面,通过N/N/C/S/N原子的平均平面的最大偏差为0.0463 (14) Å[r.m.s.d. = 0.0324 Å],而对于茉莉酮片段的五元环,通过碳原子的平均平面的最大偏差为0.0465 (15) Å[r.m.s.d. = 0.0338 Å]。由于这两个片段之间的二面角为8.93 (1)°,且茉莉酮片段链中存在sp³杂化碳原子,分子不是平面的。在晶体中,分子通过N-H⋯S和C-H⋯S相互作用连接,具有图集 motif (8)和 (7),沿[010]方向形成单周期氢键带。 Hirshfeld表面分析表明,晶体凝聚的主要贡献来自H⋯H(67.8%)、H⋯S/S⋯H(15.0%)、H⋯C/C⋯H(8.5%)和H⋯N/N⋯H(5.6%)[仅考虑非无序原子和占有率最高的原子]。这项工作报道了茉莉酮硫代半卡巴腙结构的第二种晶体变体,第一种最近已发表[Orsoni (2020 ▸). , 8681-8697],晶体是在273 K的乙醇中获得的。