sp387_s2

Table 1 Crystal data and structure refinement for sp387_s2_150K.
Identification code	sp387_s2_150K
Empirical formula	I₅OSe₈V₄
Formula weight	1485.94
Temperature/K	150(2)
Crystal system	monoclinic
Space group	C2/c
a/Å	21.1319(13)
b/Å	5.8841(3)
c/Å	18.0933(9)
α/°	90
β/°	123.649(2)
γ/°	90
Volume/Å³	1872.81(18)
Z	4
ρ_calcg/cm³	5.270
μ/mm^‑1	25.707
F(000)	2548.0
Crystal size/mm³	0.062 × 0.005 × 0.004
Radiation	MoKα (λ = 0.71073)
2Θ range for data collection/°	4.632 to 61.006
Index ranges	-24 ≤ h ≤ 30, -7 ≤ k ≤ 8, -25 ≤ l ≤ 25
Reflections collected	11066
Independent reflections	2859 [R_int = 0.0444, R_sigma = 0.0469]
Data/restraints/parameters	2859/0/83
Goodness-of-fit on F²	1.059
Final R indexes [I>=2σ (I)]	R₁ = 0.0394, wR₂ = 0.0971
Final R indexes [all data]	R₁ = 0.0542, wR₂ = 0.1032
Largest diff. peak/hole / e Å^-3	1.37/-4.27

Table 2 Fractional Atomic Coordinates (×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for sp387_s2_150K. U_eq is defined as 1/3 of of the trace of the orthogonalised U_IJ tensor.
Atom	x	y	z	U(eq)
I1	3484.5(3)	3196.5(10)	4879.4(3)	18.78(14)
I2	3320.8(3)	10920.7(10)	7899.9(4)	19.21(14)
I3	5000	2046.3(14)	7500	20.60(18)
Se11	5291.9(5)	8652.7(17)	9359.3(5)	20.4(2)
Se12	4542.0(5)	5418.2(17)	8827.6(5)	20.03(19)
Se21	3322.1(5)	8693.4(17)	5976.0(5)	20.1(2)
Se22	3272.1(5)	5445.3(17)	6664.4(5)	20.2(2)
V1	4312.5(8)	5796(3)	6327.6(9)	19.3(3)
V2	4243.5(8)	8312(3)	7679.4(9)	19.0(3)
O1	5000	7027(14)	7500	13.4(15)

Table 2 Fractional Atomic Coordinates (×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for sp387_s2_150K. U_eq is defined as 1/3 of of the trace of the orthogonalised U_IJ tensor.

Atom

U(eq)

3484.5(3)

3196.5(10)

4879.4(3)

18.78(14)

3320.8(3)

10920.7(10)

7899.9(4)

19.21(14)

5000

2046.3(14)

7500

20.60(18)

Se11

5291.9(5)

8652.7(17)

9359.3(5)

20.4(2)

Se12

4542.0(5)

5418.2(17)

8827.6(5)

20.03(19)

Se21

3322.1(5)

8693.4(17)

5976.0(5)

20.1(2)

Se22

3272.1(5)

5445.3(17)

6664.4(5)

20.2(2)

4312.5(8)

5796(3)

6327.6(9)

19.3(3)

4243.5(8)

8312(3)

7679.4(9)

19.0(3)

5000

7027(14)

7500

13.4(15)

Table 3 Anisotropic Displacement Parameters (Å²×10³) for sp387_s2_150K. The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+2hka*b*U₁₂+…].
Atom	U₁₁	U₂₂	U₃₃	U₂₃	U₁₃	U₁₂
I1	14.6(2)	25.7(3)	15.5(2)	-2.2(2)	7.96(19)	-1.2(2)
I2	15.2(2)	24.2(3)	21.4(3)	0.4(2)	12.1(2)	1.3(2)
I3	17.7(4)	24.2(4)	20.7(4)	0	11.1(3)	0
Se11	13.0(4)	35.2(5)	13.9(4)	-1.2(3)	8.0(3)	0.0(3)
Se12	13.2(4)	34.4(5)	14.0(4)	0.8(4)	8.5(3)	-0.5(3)
Se21	10.8(4)	34.4(5)	14.1(4)	1.2(3)	6.3(3)	1.3(3)
Se22	11.3(4)	34.6(5)	15.3(4)	-0.7(4)	7.7(3)	-1.0(3)
V1	10.8(6)	34.8(9)	13.1(6)	-4.4(6)	7.2(5)	-2.9(6)
V2	10.4(6)	34.6(9)	12.4(6)	0.3(6)	6.6(5)	3.3(6)
O1	13(4)	16(4)	8(3)	0	4(3)	0

Table 3 Anisotropic Displacement Parameters (Å²×10³) for sp387_s2_150K. The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+2hka*b*U₁₂+…].

Atom

U₁₁

U₂₂

U₃₃

U₂₃

U₁₃

U₁₂

14.6(2)

25.7(3)

15.5(2)

-2.2(2)

7.96(19)

-1.2(2)

15.2(2)

24.2(3)

21.4(3)

0.4(2)

12.1(2)

1.3(2)

17.7(4)

24.2(4)

20.7(4)

11.1(3)

Se11

13.0(4)

35.2(5)

13.9(4)

-1.2(3)

8.0(3)

0.0(3)

Se12

13.2(4)

34.4(5)

14.0(4)

0.8(4)

8.5(3)

-0.5(3)

Se21

10.8(4)

34.4(5)

14.1(4)

1.2(3)

6.3(3)

1.3(3)

Se22

11.3(4)

34.6(5)

15.3(4)

-0.7(4)

7.7(3)

-1.0(3)

10.8(6)

34.8(9)

13.1(6)

-4.4(6)

7.2(5)

-2.9(6)

10.4(6)

34.6(9)

12.4(6)

0.3(6)

6.6(5)

3.3(6)

13(4)

16(4)

8(3)

4(3)

Table 4 Bond Lengths for sp387_s2_150K.
Atom	Atom	Length/Å	Atom	Atom	Length/Å
I1	V1	2.6808(16)	Se21	V2	2.5866(16)
I2	V2	2.6793(16)	Se22	V1	2.5946(16)
I3	V1	2.8395(18)	Se22	V2	2.5009(18)
I3	V1¹	2.8395(18)	V1	Se11¹	2.4940(18)
I3	V2²	2.8396(18)	V1	Se12¹	2.5963(16)
I3	V2³	2.8396(17)	V1	V2¹	2.942(2)
Se11	Se12	2.3172(14)	V1	V2	2.931(2)
Se11	V1¹	2.4940(18)	V1	O1	1.929(3)
Se11	V2	2.5931(16)	V2	I3⁴	2.8396(17)
Se12	V1¹	2.5963(16)	V2	V1¹	2.942(2)
Se12	V2	2.4822(18)	V2	O1	1.951(3)
Se21	Se22	2.3154(14)	O1	V1¹	1.929(3)
Se21	V1	2.4933(18)	O1	V2¹	1.951(3)

Table 4 Bond Lengths for sp387_s2_150K.

Atom

Length/Å

Atom

Length/Å

2.6808(16)

Se21

2.5866(16)

2.6793(16)

Se22

2.5946(16)

2.8395(18)

Se22

2.5009(18)

V1¹

2.8395(18)

Se11¹

2.4940(18)

V2²

2.8396(18)

Se12¹

2.5963(16)

V2³

2.8396(17)

V2¹

2.942(2)

Se11

Se12

2.3172(14)

2.931(2)

Se11

V1¹

2.4940(18)

1.929(3)

Se11

2.5931(16)

I3⁴

2.8396(17)

Se12

V1¹

2.5963(16)

V1¹

2.942(2)

Se12

2.4822(18)

1.951(3)

Se21

Se22

2.3154(14)

V1¹

1.929(3)

Se21

2.4933(18)

V2¹

1.951(3)

Table 5 Bond Angles for sp387_s2_150K.
Atom	Atom	Atom	Angle/˚	Atom	Atom	Atom	Angle/˚
V1	I3	V1¹	78.02(6)	O1	V1	Se11¹	92.22(18)
V1¹	I3	V2²	126.81(4)	O1	V1	Se12¹	88.39(6)
V1	I3	V2³	126.81(4)	O1	V1	Se21	92.18(18)
V1¹	I3	V2³	127.10(4)	O1	V1	Se22	89.51(6)
V1	I3	V2²	127.10(4)	O1	V1	V2¹	40.98(9)
V2³	I3	V2²	78.62(6)	O1	V1	V2	41.23(9)
Se12	Se11	V1¹	65.20(5)	I2	V2	I3⁴	94.36(5)
Se12	Se11	V2	60.42(5)	I2	V2	V1	142.23(6)
V1¹	Se11	V2	70.63(5)	I2	V2	V1¹	142.32(6)
Se11	Se12	V1¹	60.69(5)	I3⁴	V2	V1	90.23(5)
Se11	Se12	V2	65.30(5)	I3⁴	V2	V1¹	90.01(5)
V2	Se12	V1¹	70.76(5)	Se11	V2	I2	90.05(5)
Se22	Se21	V1	65.19(5)	Se11	V2	I3⁴	84.54(5)
Se22	Se21	V2	61.05(5)	Se11	V2	V1¹	53.11(4)
V1	Se21	V2	70.45(5)	Se11	V2	V1	127.73(6)
Se21	Se22	V1	60.72(5)	Se12	V2	I2	97.86(5)
Se21	Se22	V2	64.83(5)	Se12	V2	I3⁴	136.75(6)
V2	Se22	V1	70.20(5)	Se12	V2	Se11	54.28(4)
I1	V1	I3	94.22(5)	Se12	V2	Se21	136.99(7)
I1	V1	V2	142.80(6)	Se12	V2	Se22	82.90(6)
I1	V1	V2¹	141.12(6)	Se12	V2	V1	104.17(7)
I3	V1	V2	90.61(5)	Se12	V2	V1¹	56.43(5)
I3	V1	V2¹	90.38(5)	Se21	V2	I2	89.90(5)
Se11¹	V1	I1	96.60(5)	Se21	V2	I3⁴	84.06(5)
Se11¹	V1	I3	136.21(6)	Se21	V2	Se11	168.55(8)
Se11¹	V1	Se12¹	54.11(4)	Se21	V2	V1¹	127.77(6)
Se11¹	V1	Se22	137.07(7)	Se21	V2	V1	53.28(4)
Se11¹	V1	V2¹	56.26(5)	Se22	V2	I2	97.29(5)
Se11¹	V1	V2	105.12(7)	Se22	V2	I3⁴	136.30(6)
Se12¹	V1	I1	89.32(5)	Se22	V2	Se11	137.17(7)
Se12¹	V1	I3	83.83(5)	Se22	V2	Se21	54.11(4)
Se12¹	V1	V2	127.88(6)	Se22	V2	V1¹	105.10(7)
Se12¹	V1	V2¹	52.81(4)	Se22	V2	V1	56.40(5)
Se21	V1	I1	98.03(5)	V1	V2	V1¹	74.99(6)
Se21	V1	I3	137.02(6)	O1	V2	I2	167.8(2)
Se21	V1	Se11¹	82.98(6)	O1	V2	I3⁴	73.5(2)
Se21	V1	Se12¹	137.06(7)	O1	V2	Se11	88.76(6)
Se21	V1	Se22	54.10(4)	O1	V2	Se12	91.24(18)
Se21	V1	V2¹	104.58(7)	O1	V2	Se21	88.89(6)
Se21	V1	V2	56.26(5)	O1	V2	Se22	91.79(18)
Se22	V1	I1	90.29(5)	O1	V2	V1¹	40.40(9)
Se22	V1	I3	84.96(5)	O1	V2	V1	40.65(9)
Se22	V1	Se12¹	168.72(8)	V1	O1	V1¹	135.9(5)
Se22	V1	V2¹	128.59(6)	V1¹	O1	V2¹	98.12(6)
Se22	V1	V2	53.40(4)	V1¹	O1	V2	98.62(6)
V2	V1	V2¹	75.55(6)	V1	O1	V2	98.12(6)
O1	V1	I1	167.2(2)	V1	O1	V2¹	98.62(6)
O1	V1	I3	73.1(2)	V2	O1	V2¹	134.4(4)

Table 5 Bond Angles for sp387_s2_150K.

Atom

Angle/˚

Atom

Angle/˚

V1¹

78.02(6)

Se11¹

92.22(18)

V1¹

V2²

126.81(4)

Se12¹

88.39(6)

V2³

126.81(4)

Se21

92.18(18)

V1¹

V2³

127.10(4)

Se22

89.51(6)

V2²

127.10(4)

V2¹

40.98(9)

V2³

V2²

78.62(6)

41.23(9)

Se12

Se11

V1¹

65.20(5)

I3⁴

94.36(5)

Se12

Se11

60.42(5)

142.23(6)

V1¹

Se11

70.63(5)

V1¹

142.32(6)

Se11

Se12

V1¹

60.69(5)

I3⁴

90.23(5)

Se11

Se12

65.30(5)

I3⁴

V1¹

90.01(5)

Se12

V1¹

70.76(5)

Se11

90.05(5)

Se22

Se21

65.19(5)

Se11

I3⁴

84.54(5)

Se22

Se21

61.05(5)

Se11

V1¹

53.11(4)

Se21

70.45(5)

Se11

127.73(6)

Se21

Se22

60.72(5)

Se12

97.86(5)

Se21

Se22

64.83(5)

Se12

I3⁴

136.75(6)

Se22

70.20(5)

Se12

Se11

54.28(4)

94.22(5)

Se12

Se21

136.99(7)

142.80(6)

Se12

Se22

82.90(6)

V2¹

141.12(6)

Se12

104.17(7)

90.61(5)

Se12

V1¹

56.43(5)

V2¹

90.38(5)

Se21

89.90(5)

Se11¹

96.60(5)

Se21

I3⁴

84.06(5)

Se11¹

136.21(6)

Se21

Se11

168.55(8)

Se11¹

Se12¹

54.11(4)

Se21

V1¹

127.77(6)

Se11¹

Se22

137.07(7)

Se21

53.28(4)

Se11¹

V2¹

56.26(5)

Se22

97.29(5)

Se11¹

105.12(7)

Se22

I3⁴

136.30(6)

Se12¹

89.32(5)

Se22

Se11

137.17(7)

Se12¹

83.83(5)

Se22

Se21

54.11(4)

Se12¹

127.88(6)

Se22

V1¹

105.10(7)

Se12¹

V2¹

52.81(4)

Se22

56.40(5)

Se21

98.03(5)

V1¹

74.99(6)

Se21

137.02(6)

167.8(2)

Se21

Se11¹

82.98(6)

I3⁴

73.5(2)

Se21

Se12¹

137.06(7)

Se11

88.76(6)

Se21

Se22

54.10(4)

Se12

91.24(18)

Se21

V2¹

104.58(7)

Se21

88.89(6)

Se21

56.26(5)

Se22

91.79(18)

Se22

90.29(5)

V1¹

40.40(9)

Se22

84.96(5)

40.65(9)

Se22

Se12¹

168.72(8)

V1¹

135.9(5)

Se22

V2¹

128.59(6)

V1¹

V2¹

98.12(6)

Se22

53.40(4)

V1¹

98.62(6)

V2¹

75.55(6)

98.12(6)

167.2(2)

V2¹

98.62(6)

73.1(2)

V2¹

134.4(4)

Experimental

Single crystals of I₅OSe₈V₄ [sp387_s2_150K] were []. A suitable crystal was selected and [] on a Bruker D8 Venture, PHOTON-III CMOS diffractometer. The crystal was kept at 150(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 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 [sp387_s2_150K]

Crystal Data for I₅OSe₈V₄ (M =1485.94 g/mol): monoclinic, space group C2/c (no. 15), a = 21.1319(13) Å, b = 5.8841(3) Å, c = 18.0933(9) Å, β = 123.649(2)°, V = 1872.81(18) Å³, Z = 4, T = 150(2) K, μ(MoKα) = 25.707 mm^-1, Dcalc = 5.270 g/cm³, 11066 reflections measured (4.632° ≤ 2Θ ≤ 61.006°), 2859 unique (R_int = 0.0444, R_sigma = 0.0469) which were used in all calculations. The final R₁ was 0.0394 (I > 2σ(I)) and wR₂ was 0.1032 (all data).

Refinement model description

Number of restraints - 0, number of constraints - unknown.

Details:

N/A

This report has been created with Olex2, compiled on 2020.11.12 svn.r5f609507 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.