exp_311

Table 1 Crystal data and structure refinement for exp_311.
Identification code	exp_311
Empirical formula	C₆H₃₀Cl_3.5CoN₆Na_0.5O₃
Formula weight	428.86
Temperature/K	293(2)
Crystal system	trigonal
Space group	P-3c1
a/Å	11.4290(2)
b/Å	11.4290(2)
c/Å	15.5815(2)
α/°	90
β/°	90
γ/°	120
Volume/Å³	1762.61(7)
Z	4
ρ_calcg/cm³	1.616
μ/mm^‑1	1.530
F(000)	896.0
Crystal size/mm³	0.385 × 0.289 × 0.217
Radiation	Mo Kα (λ = 0.71073)
2Θ range for data collection/°	5.228 to 61.77
Index ranges	-16 ≤ h ≤ 16, -16 ≤ k ≤ 16, -22 ≤ l ≤ 22
Reflections collected	65362
Independent reflections	1860 [R_int = 0.0274, R_sigma = 0.0086]
Data/restraints/parameters	1860/0/99
Goodness-of-fit on F²	1.057
Final R indexes [I>=2σ (I)]	R₁ = 0.0267, wR₂ = 0.0716
Final R indexes [all data]	R₁ = 0.0312, wR₂ = 0.0736
Largest diff. peak/hole / e Å^-3	0.48/-0.78

Table 2 Fractional Atomic Coordinates (×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for exp_311. U_eq is defined as 1/3 of of the trace of the orthogonalised U_IJ tensor.
Atom	x	y	z	U(eq)
Co1	3333.33	6666.67	8815.0(2)	17.57(9)
Cl1	-1024.3(4)	5102.3(4)	8748.3(2)	34.23(11)
Cl2	0	0	10000	54.6(3)
Na1	0	0	7500	54.2(5)
N1	2998.1(13)	5111.7(12)	9531.8(8)	24.4(2)
N2	1859.4(13)	5338.1(13)	8095.5(8)	27.3(2)
O1	1992.9(18)	1108.1(17)	8437.6(12)	59.4(4)
C1	1722.2(16)	3907.9(15)	9257.3(10)	30.2(3)
C2	1642.0(17)	3974.4(16)	8296.6(10)	31.6(3)

Table 2 Fractional Atomic Coordinates (×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for exp_311. U_eq is defined as 1/3 of of the trace of the orthogonalised U_IJ tensor.

Atom

U(eq)

Co1

3333.33

6666.67

8815.0(2)

17.57(9)

Cl1

-1024.3(4)

5102.3(4)

8748.3(2)

34.23(11)

Cl2

10000

54.6(3)

Na1

7500

54.2(5)

2998.1(13)

5111.7(12)

9531.8(8)

24.4(2)

1859.4(13)

5338.1(13)

8095.5(8)

27.3(2)

1992.9(18)

1108.1(17)

8437.6(12)

59.4(4)

1722.2(16)

3907.9(15)

9257.3(10)

30.2(3)

1642.0(17)

3974.4(16)

8296.6(10)

31.6(3)

Table 3 Anisotropic Displacement Parameters (Å²×10³) for exp_311. The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+2hka*b*U₁₂+…].
Atom	U₁₁	U₂₂	U₃₃	U₂₃	U₁₃	U₁₂
Co1	19.28(11)	19.28(11)	14.13(14)	0	0	9.64(5)
Cl1	32.16(19)	38.3(2)	27.58(18)	-2.44(13)	2.03(13)	14.08(15)
Cl2	56.8(5)	56.8(5)	50.2(7)	0	0	28.4(2)
Na1	51.5(7)	51.5(7)	59.6(13)	0	0	25.8(4)
N1	28.8(6)	24.8(5)	20.6(5)	1.1(4)	-1.4(4)	14.1(5)
N2	27.7(6)	29.6(6)	22.2(5)	-2.6(4)	-5.3(4)	12.6(5)
O1	52.9(9)	48.3(9)	68.0(10)	-7.3(8)	6.9(8)	18.6(8)
C1	31.7(7)	22.5(6)	30.0(7)	1.8(5)	2.5(5)	8.9(5)
C2	34.2(7)	24.6(6)	28.8(7)	-6.7(5)	-4.5(6)	9.3(6)

Table 3 Anisotropic Displacement Parameters (Å²×10³) for exp_311. The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+2hka*b*U₁₂+…].

Atom

U₁₁

U₂₂

U₃₃

U₂₃

U₁₃

U₁₂

Co1

19.28(11)

14.13(14)

9.64(5)

Cl1

32.16(19)

38.3(2)

27.58(18)

-2.44(13)

2.03(13)

14.08(15)

Cl2

56.8(5)

50.2(7)

28.4(2)

Na1

51.5(7)

59.6(13)

25.8(4)

28.8(6)

24.8(5)

20.6(5)

1.1(4)

-1.4(4)

14.1(5)

27.7(6)

29.6(6)

22.2(5)

-2.6(4)

-5.3(4)

12.6(5)

52.9(9)

48.3(9)

68.0(10)

-7.3(8)

6.9(8)

18.6(8)

31.7(7)

22.5(6)

30.0(7)

1.8(5)

2.5(5)

8.9(5)

34.2(7)

24.6(6)

28.8(7)

-6.7(5)

-4.5(6)

9.3(6)

Table 4 Bond Lengths for exp_311.
Atom	Atom	Length/Å	Atom	Atom	Length/Å
Co1	N1¹	1.9677(12)	Na1	O1⁴	2.4579(19)
Co1	N1²	1.9677(12)	Na1	O1⁵	2.4579(19)
Co1	N1	1.9677(12)	Na1	O1⁶	2.4579(19)
Co1	N2¹	1.9601(12)	Na1	O1⁷	2.4579(19)
Co1	N2²	1.9601(12)	N1	C1	1.4819(19)
Co1	N2	1.9602(12)	N2	C2	1.484(2)
Na1	O1³	2.4579(19)	C1	C2	1.504(2)
Na1	O1	2.4579(19)

Table 4 Bond Lengths for exp_311.

Atom

Length/Å

Atom

Length/Å

Co1

N1¹

1.9677(12)

Na1

O1⁴

2.4579(19)

Co1

N1²

1.9677(12)

Na1

O1⁵

2.4579(19)

Co1

1.9677(12)

Na1

O1⁶

2.4579(19)

Co1

N2¹

1.9601(12)

Na1

O1⁷

2.4579(19)

Co1

N2²

1.9601(12)

1.4819(19)

Co1

1.9602(12)

1.484(2)

Na1

O1³

2.4579(19)

1.504(2)

Na1

2.4579(19)

¹+Y-X,1-X,+Z; ²1-Y,1+X-Y,+Z; ³+Y,+X,3/2-Z; ⁴-X,-X+Y,3/2-Z; ⁵-Y+X,-Y,3/2-Z; ⁶+Y-X,-X,+Z; ⁷-Y,+X-Y,+Z

Table 5 Bond Angles for exp_311.
Atom	Atom	Atom	Angle/˚	Atom	Atom	Atom	Angle/˚
N1¹	Co1	N1²	90.95(5)	O1⁴	Na1	O1⁵	88.29(6)
N1¹	Co1	N1	90.95(5)	O1⁵	Na1	O1⁶	88.29(6)
N1²	Co1	N1	90.95(5)	O1⁵	Na1	O1³	174.04(8)
N2¹	Co1	N1	174.50(5)	O1⁶	Na1	O1	87.73(9)
N2²	Co1	N1¹	174.50(6)	O1³	Na1	O1⁷	88.29(6)
N2²	Co1	N1²	85.48(5)	O1⁶	Na1	O1⁷	174.04(8)
N2	Co1	N1	85.48(5)	O1⁵	Na1	O1	96.02(8)
N2¹	Co1	N1¹	85.48(5)	O1³	Na1	O1⁶	96.02(8)
N2²	Co1	N1	93.29(6)	O1⁷	Na1	O1	88.29(6)
N2	Co1	N1¹	93.29(6)	O1⁴	Na1	O1⁷	96.02(8)
N2	Co1	N1²	174.50(5)	O1⁵	Na1	O1⁷	87.73(9)
N2¹	Co1	N1²	93.29(6)	O1⁴	Na1	O1³	87.73(9)
N2¹	Co1	N2²	90.53(6)	O1⁴	Na1	O1⁶	88.29(6)
N2¹	Co1	N2	90.54(6)	C1	N1	Co1	109.36(9)
N2	Co1	N2²	90.54(6)	C2	N2	Co1	108.70(9)
O1³	Na1	O1	88.29(6)	N1	C1	C2	107.27(12)
O1⁴	Na1	O1	174.05(8)	N2	C2	C1	106.31(12)

Table 5 Bond Angles for exp_311.

Atom

Angle/˚

Atom

Angle/˚

N1¹

Co1

N1²

90.95(5)

O1⁴

Na1

O1⁵

88.29(6)

N1¹

Co1

90.95(5)

O1⁵

Na1

O1⁶

88.29(6)

N1²

Co1

90.95(5)

O1⁵

Na1

O1³

174.04(8)

N2¹

Co1

174.50(5)

O1⁶

Na1

87.73(9)

N2²

Co1

N1¹

174.50(6)

O1³

Na1

O1⁷

88.29(6)

N2²

Co1

N1²

85.48(5)

O1⁶

Na1

O1⁷

174.04(8)

Co1

85.48(5)

O1⁵

Na1

96.02(8)

N2¹

Co1

N1¹

85.48(5)

O1³

Na1

O1⁶

96.02(8)

N2²

Co1

93.29(6)

O1⁷

Na1

88.29(6)

Co1

N1¹

93.29(6)

O1⁴

Na1

O1⁷

96.02(8)

Co1

N1²

174.50(5)

O1⁵

Na1

O1⁷

87.73(9)

N2¹

Co1

N1²

93.29(6)

O1⁴

Na1

O1³

87.73(9)

N2¹

Co1

N2²

90.53(6)

O1⁴

Na1

O1⁶

88.29(6)

N2¹

Co1

90.54(6)

Co1

109.36(9)

Co1

N2²

90.54(6)

Co1

108.70(9)

O1³

Na1

88.29(6)

107.27(12)

O1⁴

Na1

174.05(8)

106.31(12)

¹+Y-X,1-X,+Z; ²1-Y,1+X-Y,+Z; ³-Y,+X-Y,+Z; ⁴-X,-X+Y,3/2-Z; ⁵-Y+X,-Y,3/2-Z; ⁶+Y,+X,3/2-Z; ⁷+Y-X,-X,+Z

Table 6 Hydrogen Atom Coordinates (Å×10⁴) and Isotropic Displacement Parameters (Å²×10³) for exp_311.
Atom	x	y	z	U(eq)
H1E	1740.28	992.2	8961.98	89
H2C	2350(20)	3860(20)	8001(13)	36(5)
H1A	3630(20)	4940(20)	9450(13)	37(5)
H1C	1720(20)	3120(20)	9466(15)	43(6)
H1D	1040(20)	3950(20)	9506(13)	33(5)
H2D	800(20)	3320(20)	8100(13)	40(5)
H2A	1140(20)	5330(20)	8201(13)	37(5)
H1B	2910(20)	5190(20)	10036(15)	40(6)
H2B	1980(20)	5470(20)	7572(14)	41(6)
H1F	2820(40)	1800(40)	8520(20)	92(11)

Table 6 Hydrogen Atom Coordinates (Å×10⁴) and Isotropic Displacement Parameters (Å²×10³) for exp_311.

Atom

U(eq)

H1E

1740.28

992.2

8961.98

H2C

2350(20)

3860(20)

8001(13)

36(5)

H1A

3630(20)

4940(20)

9450(13)

37(5)

H1C

1720(20)

3120(20)

9466(15)

43(6)

H1D

1040(20)

3950(20)

9506(13)

33(5)

H2D

800(20)

3320(20)

8100(13)

40(5)

H2A

1140(20)

5330(20)

8201(13)

37(5)

H1B

2910(20)

5190(20)

10036(15)

40(6)

H2B

1980(20)

5470(20)

7572(14)

41(6)

H1F

2820(40)

1800(40)

8520(20)

92(11)

Experimental

Single crystals of C₆H₃₀Cl_3.5CoN₆Na_0.5O₃ [exp_311] were []. A suitable crystal was selected and [] 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_311]

Crystal Data for C₆H₃₀Cl_3.5CoN₆Na_0.5O₃ (M =428.86 g/mol): trigonal, space group P-3c1 (no. 165), a = 11.4290(2) Å, c = 15.5815(2) Å, V = 1762.61(7) Å³, Z = 4, T = 293(2) K, μ(Mo Kα) = 1.530 mm^-1, Dcalc = 1.616 g/cm³, 65362 reflections measured (5.228° ≤ 2Θ ≤ 61.77°), 1860 unique (R_int = 0.0274, R_sigma = 0.0086) which were used in all calculations. The final R₁ was 0.0267 (I > 2σ(I)) and wR₂ was 0.0736 (all data).

Refinement model description

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

Details:

1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
2.a Rotating group:
 O1(H1E)

This report has been created with Olex2, compiled on 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction. Please let us know if there are any errors or if you would like to have additional features.