UM4123

Table 1 Crystal data and structure refinement for UM4123.

Identification code	UM4123
Empirical formula	C44H49N8O12F3
Formula weight	938.91
Temperature/K	170(2)
Crystal system	monoclinic
Space group	P21/c
a/Å	10.0768(9)
b/Å	13.4198(11)
c/Å	32.411(3)
α/°	90
β/°	98.135(3)
γ/°	90
Volume/Å3	4338.8(6)
Z	4
ρcalcg/cm3	1.437
μ/mm‑1	0.114
F(000)	1968.0
Crystal size/mm3	0.29 × 0.16 × 0.13
Radiation	MoKα (λ = 0.71073)
2Θ range for data collection/°	4.87 to 59.998
Index ranges	-14 ≤ h ≤ 14, -18 ≤ k ≤ 18, -45 ≤ l ≤ 45
Reflections collected	120231
Independent reflections	12628 [Rint = 0.0329, Rsigma = 0.0178]
Data/restraints/parameters	12628/360/703
Goodness-of-fit on F2	1.263
Final R indexes [I>=2σ (I)]	R1 = 0.0480, wR2 = 0.0953
Final R indexes [all data]	R1 = 0.0541, wR2 = 0.0975
Largest diff. peak/hole / e Å-3	0.41/-0.49

Experimental:

A suitable single crystals of C₄₄H₄₉N₈O₁₂F₃ (UM4123) was selected and measured on a Bruker D8Venture w/ PhotonIII diffractometer [1]. The crystal was kept at 170(2) K during data collection. The integral intensity were correct for absorption using SADABS software [2] using multi-scan method. Resulting minimum and maximum transmission are 0.945 and 0.985 respectively. The structure was solved with the ShelXT (Sheldrick, 2015a) [3] program and refined with the ShelXL (Sheldrick, 2015c) program using least-square minimisation [4]. Number of restraints used = 360.

Crystal structure determination:

Crystal Data for C₄₄H₄₉N₈O₁₂F₃ (M =938.91 g/mol): monoclinic, space group P2₁/c (no. 14), a = 10.0768(9) Å, b = 13.4198(11) Å, c = 32.411(3) Å, β = 98.135(3)°, V = 4338.8(6) Å³, Z = 4, T = 170(2) K, μ(MoKα) = 0.114 mm^-1, Dcalc = 1.437 g/cm³, 120231 reflections measured (4.87° ≤ 2Θ ≤ 59.998°), 12628 unique (R_int = 0.0329, R_sig = 0.0178) which were used in all calculations. The final R₁ was 0.0480 (I > 2σ(I)) and wR₂ was 0.0975 (all data).

Refinement details: The structure contains CF₃SO₃^- ion disordered in 2 alternative orientations that are superimposed onto each other. The disordered species were refined with geometry restrained to be similar and atomic displacement parameters to correspond to rigid body motions and to be reasonably anisotropic. H atoms were positioned from geometric considerations and refined as riding on the attached atom with Uiso constrained to be 20% larger (50% for methyl group) than Ueqv of the attached atom. However H atoms at water molecules were located from difference Fourier maps and refined with O-H distances and H-O-H angles restrained to be similar.In addition, H atoms at C16 and C30 CH2 groups were freely refined which improved their distance to each other. Otherwise, when refined with constrained geometry of the CH2 group, they were too close to each other.

References:

1. Bruker (2021). Apex4. Bruker AXS Inc., Madison, Wisconsin, USA.
2. Krause, L., Herbst-Irmer, R., Sheldrick, G.M., Stalke, D. (2015). J. Appl. Cryst. 48, 3-10.
3. Sheldrick, G. M. (2015a). Acta Cryst. A17, 3-8.
4. Sheldrick, G. M. (2015c). Acta Cryst. C17, 3-8.
5. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.

Refinement model description

Number of restraints - 360, number of constraints - unknown.

This report has been created with Olex2 [5], compiled on 2023.03.06 svn.rbb2c1857 for OlexSys.