exp_118 (2)

Table 1 Crystal data and structure refinement for exp_118 (2).
Identification code	exp_118 (2)
Empirical formula	C₁₀H₁₄CuO₄
Formula weight	261.75
Temperature/K	293(2)
Crystal system	monoclinic
Space group	P2₁/n
a/Å	10.2283(12)
b/Å	4.6767(6)
c/Å	11.2851(19)
α/°	90
β/°	91.994(13)
γ/°	90
Volume/Å³	539.49(13)
Z	2
ρ_calcg/cm³	1.611
μ/mm^‑1	2.014
F(000)	270.0
Crystal size/mm³	0.651 × 0.161 × 0.13
Radiation	MoKα (λ = 0.71073)
2Θ range for data collection/°	5.284 to 54.97
Index ranges	-13 ≤ h ≤ 11, -6 ≤ k ≤ 6, -14 ≤ l ≤ 14
Reflections collected	4171
Independent reflections	1229 [R_int = 0.0403, R_sigma = 0.0437]
Data/restraints/parameters	1229/0/72
Goodness-of-fit on F²	1.065
Final R indexes [I>=2σ (I)]	R₁ = 0.0516, wR₂ = 0.1390
Final R indexes [all data]	R₁ = 0.0631, wR₂ = 0.1477
Largest diff. peak/hole / e Å^-3	0.79/-1.21

Table 2 Fractional Atomic Coordinates (×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for exp_118 (2). U_eq is defined as 1/3 of of the trace of the orthogonalised U_IJ tensor.
Atom	x	y	z	U(eq)
Cu1	5000	0	5000	37.3(3)
O1	3386(2)	2024(4)	4942.1(18)	42.1(5)
O2	5654(2)	1961(5)	3658.7(18)	42.6(6)
C2	3114(3)	4119(8)	4267(3)	37.1(7)
C4	5115(3)	4075(8)	3143(3)	37.1(7)
C3	3911(4)	5189(6)	3415(3)	41.2(8)
C1	1841(4)	5536(8)	4478(4)	48.5(9)
C5	5874(4)	5392(8)	2178(3)	51.8(10)

Table 3 Anisotropic Displacement Parameters (Å²×10³) for exp_118 (2). The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+2hka*b*U₁₂+…].
Atom	U₁₁	U₂₂	U₃₃	U₂₃	U₁₃	U₁₂
Cu1	36.6(4)	37.8(4)	38.6(4)	6.1(2)	16.2(2)	4.0(2)
O1	39.9(11)	43.5(12)	43.9(12)	8.4(10)	17.3(9)	3.6(10)
O2	42.5(11)	43.0(12)	43.6(12)	6.4(10)	19.1(9)	3.9(10)
C2	34.3(15)	37.7(15)	39.5(17)	-5.9(15)	3.2(13)	1.3(14)
C4	43.3(17)	39.4(15)	29.1(15)	-0.3(14)	9.5(13)	-2.0(15)
C3	43.6(18)	47(2)	33.6(17)	8.2(13)	5.9(14)	5.7(14)
C1	38.5(18)	59(2)	48(2)	5.0(17)	9.1(15)	9.2(16)
C5	53(2)	60(3)	44(2)	13.4(16)	19.9(18)	4.4(16)

Table 4 Bond Lengths for exp_118 (2).
Atom	Atom	Length/Å	Atom	Atom	Length/Å
Cu1	O1¹	1.902(2)	O2	C4	1.264(4)
Cu1	O1	1.902(2)	C2	C3	1.376(5)
Cu1	O2	1.911(2)	C2	C1	1.488(5)
Cu1	O2¹	1.911(2)	C4	C3	1.382(5)
O1	C2	1.266(4)	C4	C5	1.492(4)

Table 5 Bond Angles for exp_118 (2).
Atom	Atom	Atom	Angle/˚	Atom	Atom	Atom	Angle/˚
O1¹	Cu1	O1	180.0	O1	C2	C3	125.4(3)
O1¹	Cu1	O2¹	93.52(9)	O1	C2	C1	115.1(3)
O1	Cu1	O2¹	86.48(9)	C3	C2	C1	119.5(3)
O1¹	Cu1	O2	86.48(9)	O2	C4	C3	124.8(3)
O1	Cu1	O2	93.52(9)	O2	C4	C5	115.5(3)
O2	Cu1	O2¹	180.0	C3	C4	C5	119.8(3)
C2	O1	Cu1	125.3(2)	C2	C3	C4	124.9(3)
C4	O2	Cu1	125.5(2)

Table 6 Torsion Angles for exp_118 (2).
A	B	C	D	Angle/˚	A	B	C	D	Angle/˚
Cu1	O1	C2	C3	3.8(5)	O1	C2	C3	C4	2.2(6)
Cu1	O1	C2	C1	-173.7(2)	O2	C4	C3	C2	-1.6(6)
Cu1	O2	C4	C3	-4.9(5)	C1	C2	C3	C4	179.6(4)
Cu1	O2	C4	C5	175.0(2)	C5	C4	C3	C2	178.6(4)

Table 7 Hydrogen Atom Coordinates (Å×10⁴) and Isotropic Displacement Parameters (Å²×10³) for exp_118 (2).
Atom	x	y	z	U(eq)
H3	3617	6782	2990	49
H1A	1224	4139	4734	73
H1B	1515	6412	3757	73
H1C	1962	6973	5080	73
H5A	6312	7076	2473	78
H5B	5288	5901	1528	78
H5C	6509	4048	1911	78

Experimental

Single crystals of C₁₀H₁₄CuO₄ [exp_118 (2)] 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 SHELXT [2] structure solution program using Intrinsic Phasing and refined with the SHELXL [3] refinement package using CGLS minimisation.

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 [exp_118 (2)]

Crystal Data for C₁₀H₁₄CuO₄ (M =261.75 g/mol): monoclinic, space group P2₁/n (no. 14), a = 10.2283(12) Å, b = 4.6767(6) Å, c = 11.2851(19) Å, β = 91.994(13)°, V = 539.49(13) Å³, Z = 2, T = 293(2) K, μ(MoKα) = 2.014 mm^-1, Dcalc = 1.611 g/cm³, 4171 reflections measured (5.284° ≤ 2Θ ≤ 54.97°), 1229 unique (R_int = 0.0403, R_sigma = 0.0437) which were used in all calculations. The final R₁ was 0.0516 (I > 2σ(I)) and wR₂ was 0.1477 (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:
 C3(H3)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C)

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