Crystal structure determination of: mfr200009 (C₃₆H₂₈Cu₂F₁₂N₁₀O₈S₈)

Table 1 : Crystal data and structure refinement for mfr200009.

Experimental

Crystal structure data for mfr200009 was collected on a Xcalibur, Atlas, Gemini ultra diffractometer equipped with an fine-focus sealed X-ray tube (λ _{Cu Kα} = 1.54184 Å) and an Oxford Cryosystems CryostreamPlus open-flow N₂ cooling device. Cell refinement, data collection and data reduction were undertaken via software CrysAlisPro 1.171.40.82a (Rigaku OD, 2020). Intensities were corrected for absorption using CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm..

Using Olex2 (Dolomanov, 2009), the structure was solved using SHELXT 2014/5 (Sheldrick, 2014) and refined by XL (Sheldrick, 2008).

Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Crystal structure determination of [mfr200009]

Crystal Data for C₃₆H₂₈Cu₂F₁₂N₁₀O₈S₈ (M =1340.24 g/mol): monoclinic, space group I2/a (no. 15), a = 14.9090(3) Å, b = 20.2337(3) Å, c = 16.0723(4) Å, β = 94.937(2)°, V = 4830.45(17) Å³, Z = 4, T = 150.0(2) K, μ(Cu Kα) = 5.307 mm^-1, Dcalc = 1.843 g/cm³, 20209 reflections measured (7.04° ≤ 2Θ ≤ 133.792°), 4236 unique (R_int = 0.0509, R_sigma = 0.0328) which were used in all calculations. The final R₁ was 0.0473 (I > 2σ(I)) and wR₂ was 0.1333 (all data).

Special details of refinement:

The counterions in the asymetric unit of this structure and part of one of the tetradentate ligands have been modelled as disordered over two positions. The occupancies of the disordered atoms were refined independently of the atomic displacement parameters. In the case of the counterions, as they are disordered across a centre of symmetry, the occupancies were constrained to be 0.5. The displacement parameters of all partially-occupied non- hydrogen atoms were restrained using the SIMU card and the the geometry of the disordered moieties were restrained using the SADI card.

Comments:

N/A

Refinement model description

Number of restraints - 625, number of constraints - unknown.

Details:

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 O4-S4 ≈ O1-S3
 with sigma of 0.02
 C18-F6 ≈ C17-F1
 with sigma of 0.02
 C18-S4 ≈ C17-S3
 with sigma of 0.02
 S4-F4 ≈ S3-F3
 with sigma of 0.04
 C18-F4 ≈ C17-F3
 with sigma of 0.02
 C18-F5 ≈ C17-F2
 with sigma of 0.02
 F6-F4 ≈ F1-F3
 with sigma of 0.04
 S4-N5 ≈ S3-N5
 with sigma of 0.02
 F4-F5 ≈ F3-F2
 with sigma of 0.04
 S4-O3 ≈ S3-O2
 with sigma of 0.02
 F6-S4 ≈ F1-S3
 with sigma of 0.04
 F6-F5 ≈ F1-F2
 with sigma of 0.04
 S4-F5 ≈ S3-F2
 with sigma of 0.04
 O4-C18 ≈ O1-C17
 with sigma of 0.04
 O4-N5 ≈ O1-N5
 with sigma of 0.04
 O4-O3 ≈ O1-O2
 with sigma of 0.04
 N5-O3 ≈ N5-O2
 with sigma of 0.04
 C18-N5 ≈ C17-N5
 with sigma of 0.04
 C18-O3 ≈ C17-O2
 with sigma of 0.04
 O5-O6 ≈ O8-O7
 with sigma of 0.04
 O5-N6 ≈ O8-N6
 with sigma of 0.04
 O5-C19 ≈ O8-C20
 with sigma of 0.04
 S5-O5 ≈ S6-O8
 with sigma of 0.02
 F7-F8 ≈ F10-F12
 with sigma of 0.04
 S5-O6 ≈ S6-O7
 with sigma of 0.02
 S5-N6 ≈ S6-N6
 with sigma of 0.02
 S5-C19 ≈ S6-C20
 with sigma of 0.02
 S5-F8 ≈ S6-F12
 with sigma of 0.04
 F9-F8 ≈ F11-F12
 with sigma of 0.02
 F9-F7 ≈ F11-F10
 with sigma of 0.04
 F9-C19 ≈ F11-C20
 with sigma of 0.02
 O6-N6 ≈ O7-N6
 with sigma of 0.04
 O6-C19 ≈ O7-C20
 with sigma of 0.04
 F7-C19 ≈ F10-C20
 with sigma of 0.02
 F8-C19 ≈ F12-C20
 with sigma of 0.04
 N6-C19 ≈ N6-C20
 with sigma of 0.04
 S5-F9 ≈ S6-F11
 with sigma of 0.04
 S5-F7 ≈ S6-F10
 with sigma of 0.04
 S2-C15A ≈ S2-C15B
 with sigma of 0.02
 C15A-C16 ≈ C16-C15B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S3 ≈ S4 ≈ F1 ≈ F2 ≈ F3 ≈ F4 ≈ F5 ≈ F6 ≈ O1
≈ O2 ≈ O3 ≈ O4 ≈ N5 ≈ C17 ≈ C18: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 2A
S5 ≈ S6 ≈ F7 ≈ F8 ≈ F9 ≈ F10 ≈ F11 ≈ F12 ≈ O5
≈ O6 ≈ O7 ≈ O8 ≈ N6 ≈ C19 ≈ C20: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 2A
C15A ≈ C15B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H16A(0.62814) H16B(0.62814) H16C(0.37186) H16D(0.37186)
 C15A(0.62814) H15A(0.62814) H15B(0.62814) C15B(0.37186) H15C(0.37186)
 H15D(0.37186) S3(0.5) S4(0.5) S5(0.5) S6(0.5) F1(0.5) F2(0.5) F3(0.5) F4(0.5)
 F5(0.5) F6(0.5) F7(0.5) F8(0.5) F9(0.5) F10(0.5) F11(0.5) F12(0.5) O1(0.5)
 O2(0.5) O3(0.5) O4(0.5) O5(0.5) O6(0.5) O7(0.5) O8(0.5) N5(0.5) N6(0.5)
 C17(0.5) C18(0.5) C19(0.5) C20(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C16(H16A,H16B), C16(H16C,H16D), C15A(H15A,H15B),
 C15B(H15C,H15D)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12)

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