xray072

Table 1 Crystal data and structure refinement for xray072.
Identification code	xray072
Empirical formula	C₉H₁₁I
Formula weight	246.08
Temperature/K	200.0
Crystal system	monoclinic
Space group	P2₁/m
a/Å	8.0879(6)
b/Å	7.0547(5)
c/Å	8.2312(6)
α/°	90
β/°	103.020(2)
γ/°	90
Volume/Å³	457.58(6)
Z	2
ρ_calcg/cm³	1.786
μ/mm^‑1	26.888
F(000)	236.0
Crystal size/mm³	0.241 × 0.186 × 0.103
Radiation	CuKα (λ = 1.54178)
2Θ range for data collection/°	11.032 to 144.13
Index ranges	-9 ≤ h ≤ 9, -8 ≤ k ≤ 8, -8 ≤ l ≤ 10
Reflections collected	4956
Independent reflections	953 [R_int = 0.0599, R_sigma = 0.0502]
Data/restraints/parameters	953/0/61
Goodness-of-fit on F²	1.123
Final R indexes [I>=2σ (I)]	R₁ = 0.0544, wR₂ = 0.1481
Final R indexes [all data]	R₁ = 0.0544, wR₂ = 0.1481
Largest diff. peak/hole / e Å^-3	2.22/-1.75

Table 2 Fractional Atomic Coordinates (×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for xray072. U_eq is defined as 1/3 of of the trace of the orthogonalised U_IJ tensor.
Atom	x	y	z	U(eq)
I1	3535.3(6)	2500	1438.9(5)	50.5(3)
C1	5294(8)	2500	5123(9)	27.3(13)
C2	6688(7)	2500	6460(7)	26.7(11)
C3	8354(7)	2500	6232(8)	26.8(13)
C4	8591(7)	2500	4618(7)	27.6(12)
C5	7259(9)	2500	3241(9)	30.7(14)
C6	5600(8)	2500	3492(8)	28.1(13)
C7	3546(8)	2500	5448(11)	40.7(16)
C8	9802(9)	2500	7719(10)	49.9(19)
C9	7615(13)	2500	1517(11)	50(2)

Table 2 Fractional Atomic Coordinates (×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for xray072. U_eq is defined as 1/3 of of the trace of the orthogonalised U_IJ tensor.

Atom

U(eq)

3535.3(6)

2500

1438.9(5)

50.5(3)

5294(8)

2500

5123(9)

27.3(13)

6688(7)

2500

6460(7)

26.7(11)

8354(7)

2500

6232(8)

26.8(13)

8591(7)

2500

4618(7)

27.6(12)

7259(9)

2500

3241(9)

30.7(14)

5600(8)

2500

3492(8)

28.1(13)

3546(8)

2500

5448(11)

40.7(16)

9802(9)

2500

7719(10)

49.9(19)

7615(13)

2500

1517(11)

50(2)

Table 3 Anisotropic Displacement Parameters (Å²×10³) for xray072. The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+2hka*b*U₁₂+…].
Atom	U₁₁	U₂₂	U₃₃	U₁₃
I1	50.5(5)	39.6(4)	45.0(5)	-23.4(3)
C1	24(3)	23(3)	35(3)	7(2)
C2	28(3)	27(3)	27(3)	9(2)
C3	14(2)	37(4)	23(3)	-9(2)
C4	21(3)	30(3)	33(3)	8(2)
C5	40(4)	26(3)	28(3)	12(3)
C6	29(3)	25(3)	27(3)	-3(2)
C7	27(3)	36(3)	61(4)	15(3)
C8	27(3)	72(6)	42(4)	-10(3)
C9	68(5)	52(5)	36(4)	25(4)

Table 3 Anisotropic Displacement Parameters (Å²×10³) for xray072. The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+2hka*b*U₁₂+…].

Atom

U₁₁

U₂₂

U₃₃

U₂₃

U₁₃

U₁₂

50.5(5)

39.6(4)

45.0(5)

-23.4(3)

24(3)

23(3)

35(3)

7(2)

28(3)

27(3)

9(2)

14(2)

37(4)

23(3)

-9(2)

21(3)

30(3)

33(3)

8(2)

40(4)

26(3)

28(3)

12(3)

29(3)

25(3)

27(3)

-3(2)

27(3)

36(3)

61(4)

15(3)

27(3)

72(6)

42(4)

-10(3)

68(5)

52(5)

36(4)

25(4)

Table 4 Bond Lengths for xray072.
Atom	Atom	Length/Å	Atom	Atom	Length/Å
I1	C6	2.092(7)	C3	C4	1.384(8)
C1	C2	1.387(10)	C3	C8	1.492(10)
C1	C6	1.419(9)	C4	C5	1.377(10)
C1	C7	1.497(7)	C5	C6	1.403(10)
C2	C3	1.402(7)	C5	C9	1.510(8)

Table 4 Bond Lengths for xray072.

Atom

Length/Å

Atom

Length/Å

2.092(7)

1.384(8)

1.387(10)

1.492(10)

1.419(9)

1.377(10)

1.497(7)

1.403(10)

1.402(7)

1.510(8)

Table 5 Bond Angles for xray072.
Atom	Atom	Atom	Angle/˚	Atom	Atom	Atom	Angle/˚
C2	C1	C6	117.8(5)	C5	C4	C3	122.5(5)
C2	C1	C7	119.3(6)	C4	C5	C6	118.4(6)
C6	C1	C7	122.8(6)	C4	C5	C9	119.6(6)
C1	C2	C3	121.8(5)	C6	C5	C9	122.0(7)
C2	C3	C8	119.4(5)	C1	C6	I1	119.1(5)
C4	C3	C2	118.3(5)	C5	C6	I1	119.8(5)
C4	C3	C8	122.3(5)	C5	C6	C1	121.1(7)

Table 5 Bond Angles for xray072.

Atom

Angle/˚

Atom

Angle/˚

117.8(5)

122.5(5)

119.3(6)

118.4(6)

122.8(6)

119.6(6)

121.8(5)

122.0(7)

119.4(5)

119.1(5)

118.3(5)

119.8(5)

122.3(5)

121.1(7)

Table 6 Torsion Angles for xray072.
A	B	C	D	Angle/˚	A	B	C	D	Angle/˚
C1	C2	C3	C4	0.000(2)	C4	C5	C6	C1	0.000(2)
C1	C2	C3	C8	180.000(2)	C6	C1	C2	C3	0.000(2)
C2	C1	C6	I1	180.000(1)	C7	C1	C2	C3	180.000(2)
C2	C1	C6	C5	0.000(2)	C7	C1	C6	I1	0.000(1)
C2	C3	C4	C5	0.000(2)	C7	C1	C6	C5	180.000(1)
C3	C4	C5	C6	0.000(2)	C8	C3	C4	C5	180.000(2)
C3	C4	C5	C9	180.000(1)	C9	C5	C6	I1	0.000(1)
C4	C5	C6	I1	180.000(1)	C9	C5	C6	C1	180.000(1)

Table 6 Torsion Angles for xray072.

Angle/˚

0.000(2)

180.000(2)

0.000(2)

180.000(1)

180.000(2)

0.000(2)

0.000(1)

0.000(2)

180.000(1)

0.000(2)

180.000(2)

180.000(1)

0.000(1)

180.000(1)

Table 7 Hydrogen Atom Coordinates (Å×10⁴) and Isotropic Displacement Parameters (Å²×10³) for xray072.
Atom	x	y	z	U(eq)
H2	6508.43	2500	7561.67	32
H4	9716.63	2500	4453.73	33
H7A	2705.11	2500	4384.17	61
H7C	3393.48	1365.77	6085.99	61
H7B	3393.48	3634.23	6085.99	61
H8A	9364.73	2500	8736.71	75
H8B	10497.11	1365.77	7699.05	75
H8C	10497.11	3634.23	7699.05	75
H9A	6539.61	2500	680.6	75
H9B	8267.8	3634.23	1375.97	75
H9C	8267.8	1365.77	1375.97	75

Table 7 Hydrogen Atom Coordinates (Å×10⁴) and Isotropic Displacement Parameters (Å²×10³) for xray072.

Atom

U(eq)

6508.43

2500

7561.67

9716.63

2500

4453.73

H7A

2705.11

2500

4384.17

H7C

3393.48

1365.77

6085.99

H7B

3393.48

3634.23

6085.99

H8A

9364.73

2500

8736.71

H8B

10497.11

1365.77

7699.05

H8C

10497.11

3634.23

7699.05

H9A

6539.61

2500

680.6

H9B

8267.8

3634.23

1375.97

H9C

8267.8

1365.77

1375.97

Table 8 Atomic Occupancy for xray072.
Atom	Occupancy		Atom	Occupancy		Atom	Occupancy
H7C	0.5		H7B	0.5		H8B	0.5
H8C	0.5		H9B	0.5		H9C	0.5

Table 8 Atomic Occupancy for xray072.

Atom

Occupancy

Atom

Occupancy

Atom

Occupancy

H7C

0.5

H7B

0.5

H8B

0.5

H8C

0.5

H9B

0.5

H9C

0.5

Experimental

Single crystals of C₉H₁₁I [xray072] were []. A suitable crystal was selected and [glycerol] on a Bruker APEX-II CCD diffractometer. The crystal was kept at 200.0 K during data collection. Using Olex2 [1], the structure was solved with the XT [2] structure solution program using Intrinsic Phasing and refined with the SHELXL [3] refinement package using Least Squares minimisation.

Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.

Crystal structure determination of [xray072]

Crystal Data for C₉H₁₁I (M =246.08 g/mol): monoclinic, space group P2₁/m (no. 11), a = 8.0879(6) Å, b = 7.0547(5) Å, c = 8.2312(6) Å, β = 103.020(2)°, V = 457.58(6) Å³, Z = 2, T = 200.0 K, μ(CuKα) = 26.888 mm^-1, Dcalc = 1.786 g/cm³, 4956 reflections measured (11.032° ≤ 2Θ ≤ 144.13°), 953 unique (R_int = 0.0599, R_sigma = 0.0502) which were used in all calculations. The final R₁ was 0.0544 (I > 2σ(I)) and wR₂ was 0.1481 (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. Others
 Fixed Sof: H7C(0.5) H7B(0.5) H8B(0.5) H8C(0.5) H9B(0.5) H9C(0.5)
3.a Me refined with riding coordinates:
 C7(H7A,H7C,H7B), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4)

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