2870_twin1_hklf4

Table 1 Crystal data and structure refinement for 2870_twin1_hklf4.

Identification code	2870_twin1_hklf4
Empirical formula	C50H55Cl4Fe2N2O2Si2Zn
Formula weight	1091.01
Temperature/K	173
Crystal system	triclinic
Space group	P-1
a/Å	14.1820(10)
b/Å	16.7847(11)
c/Å	21.5947(15)
α/°	77.232(6)
β/°	83.623(6)
γ/°	89.793(6)
Volume/Å3	4981.1(6)
Z	4
ρcalcg/cm3	1.452
μ/mm‑1	1.353
F(000)	2252.0
Crystal size/mm3	0.2 × 0.2 × 0.2
Radiation	MoKα (λ = 0.71073)
2Θ range for data collection/°	4.58 to 52
Index ranges	-17 ≤ h ≤ 17, -20 ≤ k ≤ 20, -26 ≤ l ≤ 26
Reflections collected	22949
Independent reflections	22949 [Rint = ?, Rsigma = 0.1270]
Data/restraints/parameters	22949/48/1165
Goodness-of-fit on F2	0.898
Final R indexes [I>=2σ (I)]	R1 = 0.0520, wR2 = 0.0853
Final R indexes [all data]	R1 = 0.0971, wR2 = 0.0945
Largest diff. peak/hole / e Å-3	0.82/-0.95

Experimental

Single crystals of C₅₀H₅₅Cl₄Fe₂N₂O₂Si₂Zn [2870_twin1_hklf4] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173 K during data collection. Using Olex2 [1], the structure was solved with the XT [2] structure solution program using Direct Methods and refined with the XL [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. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [2870_twin1_hklf4]

Crystal Data for C₅₀H₅₅Cl₄Fe₂N₂O₂Si₂Zn (M =1091.01 g/mol): triclinic, space group P-1 (no. 2), a = 14.1820(10) Å, b = 16.7847(11) Å, c = 21.5947(15) Å, α = 77.232(6)°, β = 83.623(6)°, γ = 89.793(6)°, V = 4981.1(6) Å³, Z = 4, T = 173 K, μ(MoKα) = 1.353 mm^-1, Dcalc = 1.452 g/cm³, 22949 reflections measured (4.58° ≤ 2Θ ≤ 52°), 22949 unique (R_int = ?, R_sigma = 0.1270) which were used in all calculations. The final R₁ was 0.0520 (I > 2σ(I)) and wR₂ was 0.0945 (all data).

Refinement model description

Number of restraints - 48, number of constraints - unknown.

Details:

1. Twinned data refinement
 Scales: 0.4046(5) 0.5954(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Rigid bond restraints
 C9, C6, C10, C8, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C54, C52, C55, C53, C51
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C56, C59, C58, C60, C57
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C59) ≈ Ueq, Uanis(C51) ≈ Ueq, Uanis(C9) ≈ Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.0001
5. Others
 Sof(H2B)=Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38A)=Sof(H38A)=
 Sof(H38B)=Sof(H38C)=1-FVAR(1)
 Sof(H2A)=Sof(C37B)=Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C38B)=Sof(H38D)=
 Sof(H38E)=Sof(H38F)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 N1(H1A), N2(H2A), N2(H2B), N3(H3B), N4(H4B)
6.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C61(H61A,H61B), C86(H86A,H86B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C46(H46),
  C47(H47), C48(H48), C49(H49), C50(H50), C53(H53), C54(H54), C55(H55),
 C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C65(H65), C66(H66), C67(H67),
  C68(H68), C69(H69), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75),
 C78(H78), C79(H79), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C85(H85),
  C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C96(H96), C97(H97),
 C98(H98), C99(H99), C100(H100)
6.d Tetrahedral OH refined with riding coordinates:
 O1(H1), O2(H2), O3(H3A), O4(H4A)
6.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C37A(H37A,H37B,H37C), C37B(H37D,
 H37E,H37F), C38A(H38A,H38B,H38C), C38B(H38D,H38E,H38F), C62(H62A,H62B,H62C),
 C63(H63A,H63B,H63C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C)

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