06Cl

Table 1 Crystal data and structure refinement for 06Cl.

Identification code	06Cl
Empirical formula	C42H39Cl5.6N2O6
Formula weight	866.09
Temperature/K	293(2)
Crystal system	triclinic
Space group	P-1
a/Å	7.464
b/Å	12.493
c/Å	21.027
α/°	83.96
β/°	83.58
γ/°	83.25
Volume/Å3	1926.5
Z	2
ρcalcg/cm3	1.493
μ/mm‑1	0.435
F(000)	896.0
Crystal size/mm3	0.5 × 0.06 × 0.02
Radiation	Synchrotron Monochromator X-ray (λ = 0.68882)
2Θ range for data collection/°	5.184 to 46.636
Index ranges	-8 ≤ h ≤ 8, -14 ≤ k ≤ 14, -24 ≤ l ≤ 24
Reflections collected	15946
Independent reflections	5405 [Rint = 0.0597, Rsigma = 0.0448]
Data/restraints/parameters	5405/46/535
Goodness-of-fit on F2	1.104
Final R indexes [I>=2σ (I)]	R1 = 0.0934, wR2 = 0.2194
Final R indexes [all data]	R1 = 0.0947, wR2 = 0.2203
Largest diff. peak/hole / e Å-3	0.66/-0.43

Experimental

Single crystals of C₄₂H₃₉Cl_5.6N₂O₆ [06Cl] were []. A suitable crystal was selected and [] on a diffractometer. The crystal was kept at 293(2) K during data collection. Using Olex2 [1], the structure was solved with the XS [2] structure solution program using Direct Methods and refined with the ShelXL [3] refinement package using CGLS minimisation.

1. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.

Crystal structure determination of [06Cl]

Crystal Data for C₄₂H₃₉Cl_5.6N₂O₆ (M =866.09 g/mol): triclinic, space group P-1 (no. 2), a = 7.464 Å, b = 12.493 Å, c = 21.027 Å, α = 83.96°, β = 83.58°, γ = 83.25°, V = 1926.5 Å³, Z = 2, T = 293(2) K, μ(Synchrotron Monochromator X-ray) = 0.435 mm^-1, Dcalc = 1.493 g/cm³, 15946 reflections measured (5.184° ≤ 2Θ ≤ 46.636°), 5405 unique (R_int = 0.0597, R_sigma = 0.0448) which were used in all calculations. The final R₁ was 0.0934 (I > 2σ(I)) and wR₂ was 0.2203 (all data).

Refinement model description

Number of restraints - 46, 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
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Shared sites
{C13, C13A}
{C27, C27A}
{C14, C14A}
{C24A, C24}
{C28, C28A}
{C25A, C25}
3. Restrained distances
 C7-C2A
 1.55 with sigma of 0.02
 C6AA-C4AA
 1.55 with sigma of 0.02
 C7_$1-C2A_$1
 1.55 with sigma of 0.02
 C6AA_$1-C4AA_$1
 1.55 with sigma of 0.02
 C8-C4
 1.55 with sigma of 0.02
 C5-C3
 1.55 with sigma of 0.02
 C31-C2A
 1.55 with sigma of 0.02
 H3A-H7BD
 2 with sigma of 0.02
4. Rigid bond restraints
 C7, C2A, C4AA, C6AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5, C3, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C2A ≈ C7 ≈ C4AA ≈ C6AA: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C5 ≈ C3 ≈ C31: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C4) = Uanis(C4A)
Uanis(C8) = Uanis(C8A)
Uanis(C32) = Uanis(C32A)
Uanis(C30) = Uanis(C30A)
Uanis(C13) = Uanis(C13A)
Uanis(C27) = Uanis(C27A)
Uanis(C14) = Uanis(C14A)
Uanis(C2) = Uanis(C2A)
Uanis(C24) = Uanis(C24A)
Uanis(C24A) = Uanis(C24)
Uanis(C28) = Uanis(C28A)
Uanis(C25) = Uanis(C25A)
Uanis(C25A) = Uanis(C25)
6. Others
 Sof(H15A)=Sof(H23A)=Sof(C25)=Sof(C28)=Sof(H31A)=Sof(H7BD)=Sof(H7BC)=Sof(C2A)=
 Sof(H2AA)=Sof(H2AB)=Sof(C13A)=Sof(H13A)=Sof(C27A)=Sof(H27A)=Sof(C14A)=
 Sof(H14A)=Sof(C24A)=1-FVAR(1)
 Sof(C13)=Sof(C14)=Sof(H15)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C27)=Sof(H31)=
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H7AB)=Sof(H7AA)=Sof(C28A)=Sof(H28A)=Sof(C25A)=
 Sof(H25A)=FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=1-FVAR(2)
 Sof(H1AA)=Sof(H1AB)=Sof(C4)=Sof(H4A)=Sof(H4B)=FVAR(2)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=1-FVAR(3)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(3)
 Sof(H6BD)=Sof(H6BE)=Sof(H6BF)=Sof(C32A)=Sof(H32C)=Sof(H32D)=1-FVAR(4)
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=FVAR(4)
 Sof(H19C)=Sof(H19D)=Sof(H33C)=Sof(H33D)=Sof(C30A)=Sof(H30A)=1-FVAR(5)
 Sof(H19A)=Sof(H19B)=Sof(C30)=Sof(H30)=Sof(H33A)=Sof(H33B)=FVAR(5)
7.a Ternary CH refined with riding coordinates:
 C30(H30), C31(H31), C31(H31A), C30A(H30A)
7.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C19(H19C,H19D), C22(H22A,H22B), C32(H32A,H32B), C33(H33A,
 H33B), C33(H33C,H33D), C1(H1AA,H1AB), C1(H1BC,H1BD), C2(H2A,H2B), C3(H3A,H3B),
 C4(H4A,H4B), C7(H7AB,H7AA), C7(H7BD,H7BC), C4AA(H4AC,H4AD), C2A(H2AA,H2AB),
 C4A(H4AA,H4AB), C32A(H32C,H32D)
7.c Me refined with riding coordinates:
 C6(H6AA,H6AB,H6AC), C6(H6BD,H6BE,H6BF)
7.d Aromatic/amide H refined with riding coordinates:
 C15(H15), C15(H15A), C21(H21), C23(H23), C23(H23A), C24(H24), C29(H29),
 C13A(H13A), C27A(H27A), C14A(H14A), C28A(H28A), C25A(H25A)
7.e Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C6AA(H6AD,H6AE,H6AF), C8A(H8AA,H8AB,H8AC)

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