JR272

Table 1 Crystal data and structure refinement for JR272.

Identification code	JR272
Empirical formula	C42.17H32CrF17.48N8O0.52P2.83S0.17
Formula weight	1136.37
Temperature/K	149.99(10)
Crystal system	orthorhombic
Space group	Pbca
a/Å	17.10349(6)
b/Å	17.98863(8)
c/Å	28.79512(12)
α/°	90
β/°	90
γ/°	90
Volume/Å3	8859.35(6)
Z	8
ρcalcg/cm3	1.704
μ/mm‑1	4.261
F(000)	4574.0
Crystal size/mm3	0.319 × 0.243 × 0.189
Radiation	Cu Kα (λ = 1.54184)
2Θ range for data collection/°	6.138 to 148.854
Index ranges	-21 ≤ h ≤ 18, -22 ≤ k ≤ 20, -35 ≤ l ≤ 35
Reflections collected	95378
Independent reflections	8997 [Rint = 0.0245, Rsigma = 0.0096]
Data/restraints/parameters	8997/137/712
Goodness-of-fit on F2	1.040
Final R indexes [I>=2σ (I)]	R1 = 0.0452, wR2 = 0.1200
Final R indexes [all data]	R1 = 0.0459, wR2 = 0.1206
Largest diff. peak/hole / e Å-3	1.59/-0.75

Experimental

Single crystals of C_42.17H₃₂CrF_17.48N₈O_0.52P_2.83S_0.17 [JR272] were []. A suitable crystal was selected and [] on a XtaLAB Synergy, Dualflex, HyPix-Arc diffractometer. The crystal was kept at 149.99(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 [JR272]

Crystal Data for C_42.17375H₃₂CrF_17.4775N₈O_0.5225P_2.82625S_0.17375 (M =1136.37 g/mol): orthorhombic, space group Pbca (no. 61), a = 17.10349(6) Å, b = 17.98863(8) Å, c = 28.79512(12) Å, V = 8859.35(6) Å³, Z = 8, T = 149.99(10) K, μ(Cu Kα) = 4.261 mm^-1, Dcalc = 1.704 g/cm³, 95378 reflections measured (6.138° ≤ 2Θ ≤ 148.854°), 8997 unique (R_int = 0.0245, R_sigma = 0.0096) which were used in all calculations. The final R₁ was 0.0452 (I > 2σ(I)) and wR₂ was 0.1206 (all data).

Refinement model description

Number of restraints - 137, 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. Restrained distances
 S1-O1 ≈ S1-O2 ≈ S1-O3
 with sigma of 0.02
 F19-C41 ≈ F20-C41 ≈ F21-C41
 with sigma of 0.02
 P3-F16 ≈ P3-F14 ≈ P3-F15 ≈ P3-F18 ≈ P3-F17 ≈ P3-F13
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F14) = Uanis(O2)
Uanis(F13) = Uanis(O1)
4. Rigid body (RIGU) restrains
 F17, P3, F13, F15, F18, F14, F16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, O2, S1, C41, O1, F19, F20, F21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O2)=Sof(F19)=Sof(S1)=Sof(C41)=Sof(F20)=Sof(F21)=Sof(O3)=Sof(O1)=1-FVAR(1)
 Sof(P3)=Sof(F13)=Sof(F15)=Sof(F18)=Sof(F17)=Sof(F14)=Sof(F16)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8), C24(H24), C6(H6), C2(H2), C12(H12), C11(H11), C37(H37),
 C38(H38), C7(H7), C13(H13), C3(H3), C16(H16), C17(H17), C23(H23), C35(H35),
 C36(H36), C18(H18), C25(H25), C32(H32), C30(H30), C27(H27), C31(H31), C26(H26),
  C22(H22), C21(H21)
6.b Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C39(H39A,H39B,H39C)

This report has been created with Olex2, compiled on 2020.02.04 svn.rd84adfe8 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.