Apex 2 system

The colorless plate crystal (0.100 × 0.070 × 0.020 mm³), obtained from methanol/dichloromethane, was immersed in Paraton-N oil and placed in the N₂ cold stream at 100 K. The diffraction experiment was performed in a Bruker APEX II system (Bruker, Kanagawa, Japan) (APEX II CCD detector, MoKα: λ = 0.71073 Å). Absorption correction was performed by an empirical method implemented in SADABS [37 ]. Structure solution and refinement were performed by using SHELXS-2014/7 and SHELXL-2014/7 [38 ].
C₂₆H₁₇Sb, Mr = 451.14; orthorhombic, space group P2₁2₁2₁, Z = 4, D_calc = 1.617 g·cm⁻³, a = 5.1377(17), b = 12.092(4), c = 29.834(10) Å, V = 1853.5(11) ų, 16,845 measured and 3415 independent [I > 2σ(I)] reflections, 144 parameters, final R₁ = 0.0383, wR₂ = 0.0744, S = 1.081 [I > 2σ(I)]. CCDC 2041167.
All non-hydrogen atoms were refined anisotropically. The hydrogen atoms were refined isotropically on the calculated positions using a riding model (AFIX 43) with Uiso values constrained to 1.2/1.5 Ueq of their parent atoms.

Single crystal experiments were carried out on a BRUKER D8 QUEST system with graphite-monochromated Mo Kα radiation (λ = 0.71073 Å). The crystal samples were placed in inert oil, mounted on a glass fiber attached to a brass mounting pin, and transferred to the cold dinitrogen gas steam (100 K). Crystal data were collected and integrated using a Bruker Apex II system. The structures were solved by direct method (SHELXS-2014) and refined against F² using SHELXL-2014^{52 (link)}.

The colorless prismatic crystal (0.300 × 0.300 × 0.150 mm³), obtained from ether/hexane, was immersed in Paraton-N oil and placed in the N₂ cold stream at 100 K. The diffraction experiment was performed in a Bruker APEX II system (Bruker, Kanagawa, Japan) (APEX II CCD detector, MoKα: λ = 0.71073 Å). Absorption correction was performed by an empirical method implemented in SADABS [37 ]. Structure solution and refinement were performed by using SHELXS-2014/7 and SHELXL-2014/7 [38 ].
C₂₆H₁₇Sb, Mr = 451.14; orthorhombic, space group P2₁2₁2₁, Z = 4, D_calc = 1.563 g·cm⁻³, a = 8.5914(15), b = 9.9720(17), c = 22.374(4) Å, V = 1916.9(6) ų, 17,554 measured and 3498 independent [I > 2σ(I)] reflections, 244 parameters, final R₁ = 0.0114, wR₂ = 0.0311, S = 0.985 [I > 2σ(I)]. CCDC 2041187.
All non-hydrogen atoms were refined anisotropically. The hydrogen atoms were refined isotropically on the calculated positions using a riding model (AFIX 43) with Uiso values onstrained to 1.2/1.5 Ueq of their parent atoms.