jr286_2

Table 1 Crystal data and structure refinement for jr286_2.

Identification code	jr286_2
Empirical formula	C44H38CrF18N10P3
Formula weight	1193.75
Temperature/K	149.99(10)
Crystal system	monoclinic
Space group	P21/c
a/Å	21.14124(15)
b/Å	22.83951(17)
c/Å	20.55852(15)
α/°	90
β/°	90.3997(7)
γ/°	90
Volume/Å3	9926.55(12)
Z	8
ρcalcg/cm3	1.598
μ/mm‑1	3.837
F(000)	4824.0
Crystal size/mm3	0.637 × 0.394 × 0.037
Radiation	Cu Kα (λ = 1.54184)
2Θ range for data collection/°	4.18 to 147.57
Index ranges	-25 ≤ h ≤ 25, -27 ≤ k ≤ 25, -24 ≤ l ≤ 24
Reflections collected	87579
Independent reflections	18950 [Rint = 0.0541, Rsigma = 0.0346]
Data/restraints/parameters	18950/0/1377
Goodness-of-fit on F2	1.065
Final R indexes [I>=2σ (I)]	R1 = 0.0542, wR2 = 0.1505
Final R indexes [all data]	R1 = 0.0659, wR2 = 0.1579
Largest diff. peak/hole / e Å-3	0.81/-0.55

Experimental

Single crystals of C₄₄H₃₈CrF₁₈N₁₀P₃ [jr286_2] 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 [jr286_2]

Crystal Data for C₄₄H₃₈CrF₁₈N₁₀P₃ (M =1193.75 g/mol): monoclinic, space group P2₁/c (no. 14), a = 21.14124(15) Å, b = 22.83951(17) Å, c = 20.55852(15) Å, β = 90.3997(7)°, V = 9926.55(12) Å³, Z = 8, T = 149.99(10) K, μ(Cu Kα) = 3.837 mm^-1, Dcalc = 1.598 g/cm³, 87579 reflections measured (4.18° ≤ 2Θ ≤ 147.57°), 18950 unique (R_int = 0.0541, R_sigma = 0.0346) which were used in all calculations. The final R₁ was 0.0542 (I > 2σ(I)) and wR₂ was 0.1579 (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, {H7SA,H7SB,H7SC} of C7S
 At 1.5 times of:
  {H29A,H29B,H29C} of C29, {H35A,H35B,H35C} of C35, {H35D,H35E,H35F} of C35B,
  {H29D,H29E,H29F} of C29B, {H6SA,H6SB,H6SC} of C6S, {H12A,H12C,H12D} of C12S,
  {H1SA,H1SB,H1SC} of C1S
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C27(H27), C31(H31), C32(H32), C33(H33), C37(H37), C38(H38),
 C39(H39), C40(H40), C23B(H23B), C22B(H22B), C21B(H21B), C18B(H18B), C17B(H17B),
  C16B(H16B), C13B(H13B), C12B(H12B), C11B(H11B), C8B(H8B), C7B(H7B), C6B(H6B),
 C3B(H3B), C2B(H2B), C1B(H1B), C24B(H24B), C25B(H25B), C26B(H26B), C27B(H27B),
 C31B(H31B), C32B(H32B), C33B(H33B), C37B(H37B), C38B(H38B), C39B(H39B),
 C40B(H40B)
2.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C29B(H29D,H29E,H29F), C35B(H35D,
 H35E,H35F), C1S(H1SA,H1SB,H1SC), C6S(H6SA,H6SB,H6SC), C7S(H7SA,H7SB,H7SC),
 C12S(H12A,H12C,H12D)

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.