Smart apex 2 ccd platform

Green blocks of 2 were obtained by allowing a saturated CH₃CN solution of 2 with ether to cool at −30 °C. A crystal of 2 was placed onto the tips of a thin glass optical fiber and mounted on a Bruker SMART APEX II CCD platform diffractometer for data collection at 100.0(5) K (40 ). The full data collection was carried out using MoKα radiation (graphite monochromator). The intensity data were corrected for absorption (41 ). Final cell constants were calculated from the xyz centroids after integration (42 ). The structures were solved using SIR2011 (43 ) and refined using SHELXL-2014/7 (44 ). A direct-methods solution was calculated and provided most nonhydrogen atoms from the E-map. Full-matrix least squares/difference Fourier cycles were performed which located the remaining nonhydrogen atoms. All nonhydrogen atoms were refined with anisotropic displacement parameters. All other hydrogen atoms were placed in ideal positions and refined as riding atoms with relative isotropic displacement parameters. The asymmetric unit for each compound contains one iron complex and one cocrystallized diethyl ether molecule, both in general positions. Refer to Table 1 for additional crystal and refinement information. Selected bond lengths and angles are listed in Table 2.

Complexes 1–3 were obtained by diffusing diethyl ether into a solution of these complexes in DMF. All complexes formed as colorless needles. The crystals were placed onto the tip of a 0.1 mm diameter glass capillary tube or fiber and mounted on a Bruker SMART APEX II CCD Platform diffractometer for data collection at 100.0(1) K [59 ]. The full data collection was carried out using MoKα radiation (graphite monochromator). The intensity data were corrected for absorption and decay (SADABS) [60 ]. Final cell constants were calculated from the xyz centroids of 4034 reflection after integration (SAINT) [61 ]. The structures were solved using SIR-97 [62 ] and refined using SHELXL-97 [63 ]. Direct-methods provided most non-hydrogen atoms from the E-map. Full-matrix least squares/difference Fourier cycles were performed which located the remaining non-hydrogen atoms. All non-hydrogen atoms were refined with anisotropic displacement parameters. All hydrogen atoms were placed in ideal positions and refined as riding atoms with relative isotropic displacement parameters. Refer to Table 1 for additional crystal and refinement information.

Single crystals were placed onto the tip of a 0.1 mm diameter glass capillary tube or fiber and mounted on a Bruker SMART APEX II CCD Platform diffractometer for a data collection at 100.0(1) K.⁶⁰ A preliminary set of cell constants and an orientation matrix were calculated from reflections harvested from three orthogonal wedges of reciprocal space. The full data collection was carried out using MoKα radiation (graphite monochromator) with appropriate frame times ranging from 45–90 seconds with a detector distance of 4.00 cm. The structure was solved using SIR97⁶¹ and refined using SHELXL-97.⁶² A direct-methods solution was calculated which provided most non-hydrogen atoms from the E-map. Full-matrix least squares/difference Fourier cycles were performed which located the remaining non-hydrogen atoms. All non-hydrogen atoms were refined with anisotropic displacement parameters. All hydrogen atoms were placed in ideal positions and refined as riding atoms with relative isotropic displacement parameters. Tables with relevant parameters are in the Supporting Information.