JR281

Table 1 Crystal data and structure refinement for JR281.

Identification code	JR281
Empirical formula	C52H35CrF9N7O10S3
Formula weight	1237.05
Temperature/K	150.01(10)
Crystal system	triclinic
Space group	P-1
a/Å	13.1076(5)
b/Å	13.8460(5)
c/Å	14.7792(5)
α/°	100.865(3)
β/°	90.278(3)
γ/°	108.118(3)
Volume/Å3	2497.76(16)
Z	2
ρcalcg/cm3	1.645
μ/mm‑1	3.975
F(000)	1258.0
Crystal size/mm3	0.522 × 0.286 × 0.164
Radiation	Cu Kα (λ = 1.54184)
2Θ range for data collection/°	6.104 to 141.146
Index ranges	-15 ≤ h ≤ 15, -16 ≤ k ≤ 16, -13 ≤ l ≤ 18
Reflections collected	18796
Independent reflections	9338 [Rint = 0.0199, Rsigma = 0.0215]
Data/restraints/parameters	9338/0/742
Goodness-of-fit on F2	1.041
Final R indexes [I>=2σ (I)]	R1 = 0.0500, wR2 = 0.1271
Final R indexes [all data]	R1 = 0.0516, wR2 = 0.1283
Largest diff. peak/hole / e Å-3	1.85/-0.78

Experimental

Single crystals of C₅₂H₃₅CrF₉N₇O₁₀S₃ [JR281] were []. A suitable crystal was selected and [] on a SuperNova, Dual, Cu at home/near, Atlas diffractometer. The crystal was kept at 150.01(10) K during data collection. Using Olex2 [1], the structure was solved with the SHELXT [2] structure solution program using Intrinsic Phasing and refined with the SHELXL [3] refinement package using Least Squares minimisation.

1. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.
2. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
3. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.

Crystal structure determination of [JR281]

Crystal Data for C₅₂H₃₅CrF₉N₇O₁₀S₃ (M =1237.05 g/mol): triclinic, space group P-1 (no. 2), a = 13.1076(5) Å, b = 13.8460(5) Å, c = 14.7792(5) Å, α = 100.865(3)°, β = 90.278(3)°, γ = 108.118(3)°, V = 2497.76(16) Å³, Z = 2, T = 150.01(10) K, μ(Cu Kα) = 3.975 mm^-1, Dcalc = 1.645 g/cm³, 18796 reflections measured (6.104° ≤ 2Θ ≤ 141.146°), 9338 unique (R_int = 0.0199, R_sigma = 0.0215) which were used in all calculations. The final R₁ was 0.0500 (I > 2σ(I)) and wR₂ was 0.1283 (all data).

Refinement model description

Number of restraints - 0, number of constraints - unknown.

Details:

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
  C26(H26), C29(H29), C30(H30), C31(H31), C34(H34), C38(H38), C41(H41),
 C42(H42), C43(H43), C45(H45), C46(H46), C47(H47)
2.b Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C53(H53A,H53B,H53C)

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