exp_324

Table 1 Crystal data and structure refinement for exp_324.
Identification code	exp_324
Empirical formula	C₆H₂₆CoI₃N₆O
Formula weight	637.96
Temperature/K	293(2)
Crystal system	orthorhombic
Space group	Pbca
a/Å	11.49946(14)
b/Å	13.43359(17)
c/Å	23.3392(3)
α/°	90
β/°	90
γ/°	90
Volume/Å³	3605.42(7)
Z	8
ρ_calcg/cm³	2.351
μ/mm^‑1	6.088
F(000)	2384.0
Crystal size/mm³	0.648 × 0.452 × 0.361
Radiation	Mo Kα (λ = 0.71073)
2Θ range for data collection/°	4.974 to 61.52
Index ranges	-16 ≤ h ≤ 16, -19 ≤ k ≤ 19, -33 ≤ l ≤ 33
Reflections collected	201048
Independent reflections	5578 [R_int = 0.0988, R_sigma = 0.0177]
Data/restraints/parameters	5578/0/171
Goodness-of-fit on F²	1.170
Final R indexes [I>=2σ (I)]	R₁ = 0.0283, wR₂ = 0.0583
Final R indexes [all data]	R₁ = 0.0330, wR₂ = 0.0595
Largest diff. peak/hole / e Å^-3	1.65/-1.73

Table 2 Fractional Atomic Coordinates (×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for exp_324. U_eq is defined as 1/3 of of the trace of the orthogonalised U_IJ tensor.
Atom	x	y	z	U(eq)
I1	8301.5(2)	8895.4(2)	2790.5(2)	30.88(6)
I2	6123.0(2)	6882.1(2)	1658.1(2)	34.90(6)
I3	7059.5(3)	4532.7(2)	4899.5(2)	46.04(8)
Co1	5278.4(3)	6922.6(3)	3634.0(2)	19.06(8)
N1	6388(3)	7020(2)	4275.6(12)	32.9(6)
N2	6647(2)	6536.5(19)	3180.8(10)	23.1(5)
N3	5480(2)	8333.9(19)	3424.5(13)	30.5(6)
N4	3985(2)	7409(2)	4111.2(12)	32.4(6)
N5	4935(2)	5523.3(18)	3818.9(12)	27.7(5)
N6	4247(2)	6710.9(18)	2976.9(11)	24.4(5)
C1	7598(3)	7023(3)	4058.9(15)	35.6(7)
C2	7654(3)	6320(2)	3562.4(14)	29.2(6)
C3	4858(3)	8980(2)	3839.2(18)	39.5(8)
C4	3732(3)	8477(3)	3976.5(17)	39.0(8)
C5	3949(3)	5149(2)	3464.3(16)	33.0(7)
C6	4035(3)	5632(2)	2888.3(14)	30.0(6)
O1	5112(8)	7277(15)	5310(4)	94(6)
O1A	5290(7)	8228(10)	5208(3)	71(3)

Table 2 Fractional Atomic Coordinates (×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for exp_324. U_eq is defined as 1/3 of of the trace of the orthogonalised U_IJ tensor.

Atom

U(eq)

8301.5(2)

8895.4(2)

2790.5(2)

30.88(6)

6123.0(2)

6882.1(2)

1658.1(2)

34.90(6)

7059.5(3)

4532.7(2)

4899.5(2)

46.04(8)

Co1

5278.4(3)

6922.6(3)

3634.0(2)

19.06(8)

6388(3)

7020(2)

4275.6(12)

32.9(6)

6647(2)

6536.5(19)

3180.8(10)

23.1(5)

5480(2)

8333.9(19)

3424.5(13)

30.5(6)

3985(2)

7409(2)

4111.2(12)

32.4(6)

4935(2)

5523.3(18)

3818.9(12)

27.7(5)

4247(2)

6710.9(18)

2976.9(11)

24.4(5)

7598(3)

7023(3)

4058.9(15)

35.6(7)

7654(3)

6320(2)

3562.4(14)

29.2(6)

4858(3)

8980(2)

3839.2(18)

39.5(8)

3732(3)

8477(3)

3976.5(17)

39.0(8)

3949(3)

5149(2)

3464.3(16)

33.0(7)

4035(3)

5632(2)

2888.3(14)

30.0(6)

5112(8)

7277(15)

5310(4)

94(6)

O1A

5290(7)

8228(10)

5208(3)

71(3)

Table 3 Anisotropic Displacement Parameters (Å²×10³) for exp_324. The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+2hka*b*U₁₂+…].
Atom	U₁₁	U₂₂	U₃₃	U₂₃	U₁₃	U₁₂
I1	29.75(10)	21.01(9)	41.89(12)	-4.60(8)	3.98(8)	-1.20(7)
I2	24.55(10)	49.05(13)	31.09(11)	1.50(9)	-0.88(8)	1.76(9)
I3	62.40(17)	43.46(14)	32.25(12)	8.78(9)	-0.91(11)	1.49(12)
Co1	20.04(16)	18.40(16)	18.73(16)	0.93(13)	0.24(13)	2.57(13)
N1	40.5(15)	34.9(14)	23.3(12)	-4.5(10)	-7.4(11)	9.1(12)
N2	20.5(11)	25.4(11)	23.4(11)	-1.0(9)	0.1(9)	0.3(9)
N3	28.3(12)	22.8(12)	40.4(15)	4.8(11)	-1.8(11)	-1.3(10)
N4	33.7(14)	33.9(14)	29.6(13)	-1.1(11)	7.7(11)	7.0(11)
N5	27.5(12)	23.9(12)	31.6(13)	6.0(10)	1.0(10)	2.2(10)
N6	22.0(11)	24.4(11)	26.9(12)	2.8(9)	-2.6(9)	1.4(9)
C1	34.1(16)	37.5(17)	35.2(16)	-1.3(13)	-13.7(14)	-6.0(14)
C2	18.2(12)	35.7(16)	33.6(15)	0.8(12)	-3.6(11)	2.8(11)
C3	46(2)	22.9(15)	50(2)	-6.4(14)	-3.5(17)	4.5(14)
C4	36.9(17)	32.6(17)	48(2)	-7.2(15)	4.5(16)	15.3(14)
C5	25.1(14)	23.4(14)	51(2)	2.4(13)	-1.3(14)	-4.7(11)
C6	26.8(14)	27.8(14)	35.3(16)	-6.2(12)	-6.8(12)	-1.3(11)
O1	59(5)	184(18)	39(4)	-41(7)	1(4)	-4(7)
O1A	65(4)	118(9)	32(3)	-12(4)	2(3)	4(5)

Table 3 Anisotropic Displacement Parameters (Å²×10³) for exp_324. The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+2hka*b*U₁₂+…].

Atom

U₁₁

U₂₂

U₃₃

U₂₃

U₁₃

U₁₂

29.75(10)

21.01(9)

41.89(12)

-4.60(8)

3.98(8)

-1.20(7)

24.55(10)

49.05(13)

31.09(11)

1.50(9)

-0.88(8)

1.76(9)

62.40(17)

43.46(14)

32.25(12)

8.78(9)

-0.91(11)

1.49(12)

Co1

20.04(16)

18.40(16)

18.73(16)

0.93(13)

0.24(13)

2.57(13)

40.5(15)

34.9(14)

23.3(12)

-4.5(10)

-7.4(11)

9.1(12)

20.5(11)

25.4(11)

23.4(11)

-1.0(9)

0.1(9)

0.3(9)

28.3(12)

22.8(12)

40.4(15)

4.8(11)

-1.8(11)

-1.3(10)

33.7(14)

33.9(14)

29.6(13)

-1.1(11)

7.7(11)

7.0(11)

27.5(12)

23.9(12)

31.6(13)

6.0(10)

1.0(10)

2.2(10)

22.0(11)

24.4(11)

26.9(12)

2.8(9)

-2.6(9)

1.4(9)

34.1(16)

37.5(17)

35.2(16)

-1.3(13)

-13.7(14)

-6.0(14)

18.2(12)

35.7(16)

33.6(15)

0.8(12)

-3.6(11)

2.8(11)

46(2)

22.9(15)

50(2)

-6.4(14)

-3.5(17)

4.5(14)

36.9(17)

32.6(17)

48(2)

-7.2(15)

4.5(16)

15.3(14)

25.1(14)

23.4(14)

51(2)

2.4(13)

-1.3(14)

-4.7(11)

26.8(14)

27.8(14)

35.3(16)

-6.2(12)

-6.8(12)

-1.3(11)

59(5)

184(18)

39(4)

-41(7)

1(4)

-4(7)

O1A

65(4)

118(9)

32(3)

-12(4)

2(3)

4(5)

Table 4 Bond Lengths for exp_324.
Atom	Atom	Length/Å	Atom	Atom	Length/Å
Co1	N1	1.972(3)	N3	C3	1.484(4)
Co1	N2	1.966(2)	N4	C4	1.496(4)
Co1	N3	1.972(3)	N5	C5	1.491(4)
Co1	N4	1.970(3)	N6	C6	1.484(4)
Co1	N5	1.968(2)	C1	C2	1.496(5)
Co1	N6	1.959(2)	C3	C4	1.496(5)
N1	C1	1.480(5)	C5	C6	1.496(5)
N2	C2	1.489(4)

Table 4 Bond Lengths for exp_324.

Atom

Length/Å

Atom

Length/Å

Co1

1.972(3)

1.484(4)

Co1

1.966(2)

1.496(4)

Co1

1.972(3)

1.491(4)

Co1

1.970(3)

1.484(4)

Co1

1.968(2)

1.496(5)

Co1

1.959(2)

1.496(5)

1.480(5)

1.496(5)

1.489(4)

Table 5 Bond Angles for exp_324.
Atom	Atom	Atom	Angle/˚	Atom	Atom	Atom	Angle/˚
N2	Co1	N1	84.73(11)	N6	Co1	N5	84.94(11)
N2	Co1	N3	91.49(11)	C1	N1	Co1	110.4(2)
N2	Co1	N4	175.05(12)	C2	N2	Co1	110.61(19)
N2	Co1	N5	91.51(11)	C3	N3	Co1	110.1(2)
N3	Co1	N1	92.77(12)	C4	N4	Co1	110.3(2)
N4	Co1	N1	92.14(12)	C5	N5	Co1	110.67(19)
N4	Co1	N3	84.83(12)	C6	N6	Co1	110.52(19)
N5	Co1	N1	91.52(12)	N1	C1	C2	107.7(3)
N5	Co1	N3	174.98(11)	N2	C2	C1	107.8(3)
N5	Co1	N4	92.40(12)	N3	C3	C4	107.0(3)
N6	Co1	N1	174.71(11)	C3	C4	N4	108.0(3)
N6	Co1	N2	91.43(10)	N5	C5	C6	107.6(2)
N6	Co1	N3	90.96(11)	N6	C6	C5	108.0(3)
N6	Co1	N4	91.93(12)

Table 5 Bond Angles for exp_324.

Atom

Angle/˚

Atom

Angle/˚

Co1

84.73(11)

Co1

84.94(11)

Co1

91.49(11)

Co1

110.4(2)

Co1

175.05(12)

Co1

110.61(19)

Co1

91.51(11)

Co1

110.1(2)

Co1

92.77(12)

Co1

110.3(2)

Co1

92.14(12)

Co1

110.67(19)

Co1

84.83(12)

Co1

110.52(19)

Co1

91.52(12)

107.7(3)

Co1

174.98(11)

107.8(3)

Co1

92.40(12)

107.0(3)

Co1

174.71(11)

108.0(3)

Co1

91.43(10)

107.6(2)

Co1

90.96(11)

108.0(3)

Co1

91.93(12)

Table 6 Hydrogen Atom Coordinates (Å×10⁴) and Isotropic Displacement Parameters (Å²×10³) for exp_324.
Atom	x	y	z	U(eq)
H1A	6255.22	7576.77	4471.58	39
H1B	6287.94	6506.66	4511.65	39
H2A	6479.99	5999.14	2973.42	28
H2B	6831.92	7027.01	2941.27	28
H3A	6233.69	8486.2	3424.02	37
H3B	5203.2	8437.25	3073.53	37
H4A	3353.98	7042.9	4046.15	39
H4B	4170.84	7350.28	4479.8	39
H5A	5563.54	5152.95	3754.1	33
H5B	4754.88	5471.45	4188.52	33
H6A	3573.81	7020.09	3037.47	29
H6B	4569.29	6969.08	2663.65	29
H1C	8128.4	6810.42	4357.87	43
H1D	7815.86	7687.63	3938.02	43
H2C	8377.1	6410.16	3355.19	35
H2D	7616.98	5637.3	3696.73	35
H3C	4715.56	9630.42	3672.78	47
H3D	5317.38	9064.91	4184.19	47
H4C	3207.07	8520.68	3651.97	47
H4D	3365.78	8796.26	4302.65	47
H5C	3213.97	5315.37	3643.86	40
H5D	3995.43	4430.72	3426.01	40
H6C	4667.86	5340.35	2671.03	36
H6D	3318.18	5533.89	2676.32	36
H1E	5294.1	7719.53	5554.81	141
H1F	5719.42	6921.04	5277.8	141
H1AA	4734.56	8643.49	5237.83	107
H1AB	5899.67	8573.11	5263.05	107

Table 6 Hydrogen Atom Coordinates (Å×10⁴) and Isotropic Displacement Parameters (Å²×10³) for exp_324.

Atom

U(eq)

H1A

6255.22

7576.77

4471.58

H1B

6287.94

6506.66

4511.65

H2A

6479.99

5999.14

2973.42

H2B

6831.92

7027.01

2941.27

H3A

6233.69

8486.2

3424.02

H3B

5203.2

8437.25

3073.53

H4A

3353.98

7042.9

4046.15

H4B

4170.84

7350.28

4479.8

H5A

5563.54

5152.95

3754.1

H5B

4754.88

5471.45

4188.52

H6A

3573.81

7020.09

3037.47

H6B

4569.29

6969.08

2663.65

H1C

8128.4

6810.42

4357.87

H1D

7815.86

7687.63

3938.02

H2C

8377.1

6410.16

3355.19

H2D

7616.98

5637.3

3696.73

H3C

4715.56

9630.42

3672.78

H3D

5317.38

9064.91

4184.19

H4C

3207.07

8520.68

3651.97

H4D

3365.78

8796.26

4302.65

H5C

3213.97

5315.37

3643.86

H5D

3995.43

4430.72

3426.01

H6C

4667.86

5340.35

2671.03

H6D

3318.18

5533.89

2676.32

H1E

5294.1

7719.53

5554.81

141

H1F

5719.42

6921.04

5277.8

141

H1AA

4734.56

8643.49

5237.83

107

H1AB

5899.67

8573.11

5263.05

107

Table 7 Atomic Occupancy for exp_324.
Atom	Occupancy	Atom	Occupancy	Atom	Occupancy
O1	0.463(15)	H1E	0.463(15)	H1F	0.463(15)
O1A	0.537(15)	H1AA	0.537(15)	H1AB	0.537(15)

Table 7 Atomic Occupancy for exp_324.

Atom

Occupancy

Atom

Occupancy

Atom

Occupancy

0.463(15)

H1E

0.463(15)

H1F

0.463(15)

O1A

0.537(15)

H1AA

0.537(15)

H1AB

0.537(15)

Experimental

Single crystals of C₆H₂₆CoI₃N₆O [exp_324] were [slow evaporation from water]. A suitable crystal was selected and [silicone grease] on a XtaLAB Mini II 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 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 [exp_324]

Crystal Data for C₆H₂₆CoI₃N₆O (M =637.96 g/mol): orthorhombic, space group Pbca (no. 61), a = 11.49946(14) Å, b = 13.43359(17) Å, c = 23.3392(3) Å, V = 3605.42(7) Å³, Z = 8, T = 293(2) K, μ(Mo Kα) = 6.088 mm^-1, Dcalc = 2.351 g/cm³, 201048 reflections measured (4.974° ≤ 2Θ ≤ 61.52°), 5578 unique (R_int = 0.0988, R_sigma = 0.0177) which were used in all calculations. The final R₁ was 0.0283 (I > 2σ(I)) and wR₂ was 0.0595 (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,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Sof(O1A)=Sof(H1AA)=Sof(H1AB)=1-FVAR(1)
 Sof(O1)=Sof(H1E)=Sof(H1F)=FVAR(1)
3.a Free rotating group:
 O1(H1E,H1F), O1A(H1AA,H1AB)
3.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), N5(H5A,H5B), N6(H6A,H6B),
 C1(H1C,H1D), C2(H2C,H2D), C3(H3C,H3D), C4(H4C,H4D), C5(H5C,H5D), C6(H6C,H6D)

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