shelx

Table 1 Crystal data and structure refinement for shelx.
Identification code	shelx
Empirical formula	C₂₀H₃₆Cl₂CoN₈O₂
Formula weight	550.40
Temperature/K	100.00
Crystal system	monoclinic
Space group	C2/c
a/Å	10.4681(7)
b/Å	14.1306(10)
c/Å	18.4697(13)
α/°	90
β/°	92.765(3)
γ/°	90
Volume/Å³	2728.9(3)
Z	4
ρ_calcg/cm³	1.340
μ/mm^‑1	6.991
F(000)	1156.0
Crystal size/mm³	0.21 × 0.18 × 0.07
Radiation	CuKα (λ = 1.54178)
2Θ range for data collection/°	10.524 to 136.818
Index ranges	-12 ≤ h ≤ 12, -16 ≤ k ≤ 16, -22 ≤ l ≤ 22
Reflections collected	36237
Independent reflections	2504 [R_int = 0.0518, R_sigma = 0.0227]
Data/restraints/parameters	2504/0/170
Goodness-of-fit on F²	1.153
Final R indexes [I>=2σ (I)]	R₁ = 0.0758, wR₂ = 0.1799
Final R indexes [all data]	R₁ = 0.0772, wR₂ = 0.1806
Largest diff. peak/hole / e Å^-3	1.33/-1.44

Table 2 Fractional Atomic Coordinates (×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for shelx. U_eq is defined as 1/3 of the trace of the orthogonalised U_IJ tensor.
Atom	x	y	z	U(eq)
Co1	5000	5856.2(9)	7500	18.1(4)
O1W	5000	4387(4)	7500	19.3(12)
O2W	5000	7315(4)	7500	30.3(14)
N1	3460(4)	5883(3)	6720(3)	19.5(10)
N2	2500(4)	5240(3)	6790(3)	22.3(11)
N6	6345(4)	5845(3)	6689(3)	19.7(10)
N7	7214(5)	6561(3)	6683(3)	25.5(11)
C3	1632(6)	5272(5)	6231(4)	30.4(14)
C4	2025(6)	5969(4)	5775(3)	29.2(14)
C5	3169(6)	6338(4)	6094(3)	21.9(12)
C8	7833(6)	6596(5)	6064(3)	29.9(14)
C9	7368(6)	5854(5)	5646(4)	32.7(15)
C10	6438(6)	5400(4)	6051(3)	22.9(12)
C31	500(7)	4617(5)	6187(4)	46(2)
C51	3963(6)	7117(4)	5815(3)	25.9(13)
C81	8828(8)	7339(5)	5939(5)	49(2)
C101	5664(6)	4553(4)	5839(3)	27.1(13)
Cl1	2489.0(13)	8358.5(10)	7246.2(8)	28.3(4)

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

Atom

U(eq)

Co1

5000

5856.2(9)

7500

18.1(4)

O1W

5000

4387(4)

7500

19.3(12)

O2W

5000

7315(4)

7500

30.3(14)

3460(4)

5883(3)

6720(3)

19.5(10)

2500(4)

5240(3)

6790(3)

22.3(11)

6345(4)

5845(3)

6689(3)

19.7(10)

7214(5)

6561(3)

6683(3)

25.5(11)

1632(6)

5272(5)

6231(4)

30.4(14)

2025(6)

5969(4)

5775(3)

29.2(14)

3169(6)

6338(4)

6094(3)

21.9(12)

7833(6)

6596(5)

6064(3)

29.9(14)

7368(6)

5854(5)

5646(4)

32.7(15)

C10

6438(6)

5400(4)

6051(3)

22.9(12)

C31

500(7)

4617(5)

6187(4)

46(2)

C51

3963(6)

7117(4)

5815(3)

25.9(13)

C81

8828(8)

7339(5)

5939(5)

49(2)

C101

5664(6)

4553(4)

5839(3)

27.1(13)

Cl1

2489.0(13)

8358.5(10)

7246.2(8)

28.3(4)

Table 3 Anisotropic Displacement Parameters (Å²×10³) for shelx. The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+2hka*b*U₁₂+…].
Atom	U₁₁	U₂₂	U₃₃	U₂₃	U₁₃	U₁₂
Co1	14.5(6)	14.1(7)	25.6(7)	0	-0.6(5)	0
O1W	16(3)	6(2)	37(3)	0	0(2)	0
O2W	26(3)	20(3)	45(4)	0	-1(3)	0
N1	20(2)	13(2)	26(2)	0.0(18)	0.9(19)	0.5(19)
N2	17(2)	18(2)	31(3)	5(2)	-3.8(19)	-3.3(19)
N6	17(2)	14(2)	28(3)	0.1(19)	-0.9(19)	-3.1(18)
N7	26(3)	21(2)	30(3)	-3(2)	3(2)	-3(2)
C3	25(3)	29(3)	36(3)	4(3)	-10(3)	-6(3)
C4	31(3)	25(3)	30(3)	5(3)	-10(3)	-6(3)
C5	25(3)	15(3)	25(3)	0(2)	-2(2)	4(2)
C8	28(3)	26(3)	36(3)	3(3)	9(3)	-4(3)
C9	39(4)	29(3)	30(3)	1(3)	10(3)	4(3)
C10	24(3)	18(3)	26(3)	2(2)	1(2)	6(2)
C31	35(4)	45(4)	56(5)	14(4)	-18(3)	-19(3)
C51	32(3)	20(3)	26(3)	3(2)	2(2)	-2(3)
C81	55(5)	40(4)	55(5)	-1(4)	30(4)	-12(4)
C101	33(3)	22(3)	26(3)	-3(2)	-4(3)	3(3)
Cl1	25.9(7)	23.6(7)	35.0(8)	-1.6(6)	-1.7(6)	10.1(6)

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

Atom

U₁₁

U₂₂

U₃₃

U₂₃

U₁₃

U₁₂

Co1

14.5(6)

14.1(7)

25.6(7)

-0.6(5)

O1W

16(3)

6(2)

37(3)

0(2)

O2W

26(3)

20(3)

45(4)

-1(3)

20(2)

13(2)

26(2)

0.0(18)

0.9(19)

0.5(19)

17(2)

18(2)

31(3)

5(2)

-3.8(19)

-3.3(19)

17(2)

14(2)

28(3)

0.1(19)

-0.9(19)

-3.1(18)

26(3)

21(2)

30(3)

-3(2)

3(2)

-3(2)

25(3)

29(3)

36(3)

4(3)

-10(3)

-6(3)

31(3)

25(3)

30(3)

5(3)

-10(3)

-6(3)

25(3)

15(3)

25(3)

0(2)

-2(2)

4(2)

28(3)

26(3)

36(3)

3(3)

9(3)

-4(3)

39(4)

29(3)

30(3)

1(3)

10(3)

4(3)

C10

24(3)

18(3)

26(3)

2(2)

1(2)

6(2)

C31

35(4)

45(4)

56(5)

14(4)

-18(3)

-19(3)

C51

32(3)

20(3)

26(3)

3(2)

2(2)

-2(3)

C81

55(5)

40(4)

55(5)

-1(4)

30(4)

-12(4)

C101

33(3)

22(3)

26(3)

-3(2)

-4(3)

3(3)

Cl1

25.9(7)

23.6(7)

35.0(8)

-1.6(6)

-1.7(6)

10.1(6)

Table 4 Bond Lengths for shelx.
Atom	Atom	Length/Å	Atom	Atom	Length/Å
Co1	O1W	2.076(5)	N6	C10	1.342(7)
Co1	O2W	2.062(6)	N7	C8	1.343(8)
Co1	N1¹	2.110(5)	C3	C4	1.372(9)
Co1	N1	2.110(5)	C3	C31	1.502(9)
Co1	N6	2.105(5)	C4	C5	1.410(8)
Co1	N6¹	2.105(5)	C5	C51	1.486(8)
N1	N2	1.366(6)	C8	C9	1.377(9)
N1	C5	1.345(7)	C8	C81	1.504(9)
N2	C3	1.342(7)	C9	C10	1.410(9)
N6	N7	1.361(6)	C10	C101	1.488(8)

Table 4 Bond Lengths for shelx.

Atom

Length/Å

Atom

Length/Å

Co1

O1W

2.076(5)

C10

1.342(7)

Co1

O2W

2.062(6)

1.343(8)

Co1

N1¹

2.110(5)

1.372(9)

Co1

2.110(5)

C31

1.502(9)

Co1

2.105(5)

1.410(8)

Co1

N6¹

2.105(5)

C51

1.486(8)

1.366(6)

1.377(9)

1.345(7)

C81

1.504(9)

1.342(7)

C10

1.410(9)

1.361(6)

C10

C101

1.488(8)

Table 5 Bond Angles for shelx.
Atom	Atom	Atom	Angle/˚	Atom	Atom	Atom	Angle/˚
O1W	Co1	N1	91.03(13)	N7	N6	Co1	118.1(4)
O1W	Co1	N1¹	91.03(12)	C10	N6	Co1	135.0(4)
O1W	Co1	N6	89.57(13)	C10	N6	N7	105.3(5)
O1W	Co1	N6¹	89.57(13)	C8	N7	N6	112.6(5)
O2W	Co1	O1W	180.0	N2	C3	C4	106.5(5)
O2W	Co1	N1¹	88.97(13)	N2	C3	C31	121.6(6)
O2W	Co1	N1	88.97(12)	C4	C3	C31	131.9(6)
O2W	Co1	N6¹	90.43(13)	C3	C4	C5	106.4(5)
O2W	Co1	N6	90.43(13)	N1	C5	C4	109.6(5)
N1¹	Co1	N1	177.9(3)	N1	C5	C51	123.0(5)
N6	Co1	N1	91.70(18)	C4	C5	C51	127.4(5)
N6¹	Co1	N1¹	91.70(18)	N7	C8	C9	106.1(5)
N6¹	Co1	N1	88.32(18)	N7	C8	C81	121.5(6)
N6	Co1	N1¹	88.31(18)	C9	C8	C81	132.4(6)
N6	Co1	N6¹	179.1(3)	C8	C9	C10	106.5(6)
N2	N1	Co1	117.8(3)	N6	C10	C9	109.5(5)
C5	N1	Co1	136.8(4)	N6	C10	C101	123.1(5)
C5	N1	N2	105.2(5)	C9	C10	C101	127.3(6)
C3	N2	N1	112.3(5)

Table 5 Bond Angles for shelx.

Atom

Angle/˚

Atom

Angle/˚

O1W

Co1

91.03(13)

Co1

118.1(4)

O1W

Co1

N1¹

91.03(12)

C10

Co1

135.0(4)

O1W

Co1

89.57(13)

C10

105.3(5)

O1W

Co1

N6¹

89.57(13)

112.6(5)

O2W

Co1

O1W

180.0

106.5(5)

O2W

Co1

N1¹

88.97(13)

C31

121.6(6)

O2W

Co1

88.97(12)

C31

131.9(6)

O2W

Co1

N6¹

90.43(13)

106.4(5)

O2W

Co1

90.43(13)

109.6(5)

N1¹

Co1

177.9(3)

C51

123.0(5)

Co1

91.70(18)

C51

127.4(5)

N6¹

Co1

N1¹

91.70(18)

106.1(5)

N6¹

Co1

88.32(18)

C81

121.5(6)

Co1

N1¹

88.31(18)

C81

132.4(6)

Co1

N6¹

179.1(3)

C10

106.5(6)

Co1

117.8(3)

C10

109.5(5)

Co1

136.8(4)

C10

C101

123.1(5)

105.2(5)

C10

C101

127.3(6)

112.3(5)

Table 6 Torsion Angles for shelx.
A	B	C	D	Angle/˚	A	B	C	D	Angle/˚
Co1	N1	N2	C3	-174.7(4)	N6	N7	C8	C81	179.4(6)
Co1	N1	C5	C4	173.5(4)	N7	N6	C10	C9	-0.5(6)
Co1	N1	C5	C51	-7.3(9)	N7	N6	C10	C101	178.8(5)
Co1	N6	N7	C8	-166.6(4)	N7	C8	C9	C10	0.9(7)
Co1	N6	C10	C9	164.0(4)	C3	C4	C5	N1	-0.1(7)
Co1	N6	C10	C101	-16.6(9)	C3	C4	C5	C51	-179.2(6)
N1	N2	C3	C4	-0.5(7)	C5	N1	N2	C3	0.5(6)
N1	N2	C3	C31	179.1(6)	C8	C9	C10	N6	-0.2(7)
N2	N1	C5	C4	-0.2(6)	C8	C9	C10	C101	-179.5(6)
N2	N1	C5	C51	178.9(5)	C10	N6	N7	C8	1.1(6)
N2	C3	C4	C5	0.4(7)	C31	C3	C4	C5	-179.3(7)
N6	N7	C8	C9	-1.3(7)	C81	C8	C9	C10	-179.9(7)

Table 6 Torsion Angles for shelx.

Angle/˚

Co1

-174.7(4)

C81

179.4(6)

Co1

173.5(4)

C10

-0.5(6)

Co1

C51

-7.3(9)

C10

C101

178.8(5)

Co1

-166.6(4)

C10

0.9(7)

Co1

C10

164.0(4)

-0.1(7)

Co1

C10

C101

-16.6(9)

C51

-179.2(6)

-0.5(7)

0.5(6)

C31

179.1(6)

C10

-0.2(7)

-0.2(6)

C10

C101

-179.5(6)

C51

178.9(5)

C10

1.1(6)

0.4(7)

C31

-179.3(7)

-1.3(7)

C81

C10

-179.9(7)

Table 7 Hydrogen Atom Coordinates (Å×10⁴) and Isotropic Displacement Parameters (Å²×10³) for shelx.
Atom	x	y	z	U(eq)
H1W	4210(60)	3960(50)	7540(30)	29
H2W	4290(70)	7670(60)	7360(40)	45
H2	2454.71	4849.1	7158.69	70(30)
H7	7354.34	6957.83	7045.31	12(14)
H4	1607.31	6164.41	5331.98	40(20)
H9	7623.43	5681.04	5177.58	40(20)
H31A	754.58	3994.57	6378.94	69
H31B	189.14	4552.57	5680.81	80(30)
H31C	-181.43	4876.66	6473.96	126
H51A	3664.02	7723.68	6001.31	39
H51B	3888.67	7121.88	5284.54	36(19)
H51C	4858.7	7019.71	5976.71	55
H81A	8577.76	7934.86	6163.9	73
H81B	8898.59	7435.32	5416.56	80(30)
H81C	9654.96	7131.97	6153.87	113
H10A	6049.64	3988.73	6066.56	41
H10B	5640.37	4481.6	5310.46	31(18)
H10C	4791.11	4631.78	5998.87	46

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

Atom

U(eq)

H1W

4210(60)

3960(50)

7540(30)

H2W

4290(70)

7670(60)

7360(40)

2454.71

4849.1

7158.69

70(30)

7354.34

6957.83

7045.31

12(14)

1607.31

6164.41

5331.98

40(20)

7623.43

5681.04

5177.58

40(20)

H31A

754.58

3994.57

6378.94

H31B

189.14

4552.57

5680.81

80(30)

H31C

-181.43

4876.66

6473.96

126

H51A

3664.02

7723.68

6001.31

H51B

3888.67

7121.88

5284.54

36(19)

H51C

4858.7

7019.71

5976.71

H81A

8577.76

7934.86

6163.9

H81B

8898.59

7435.32

5416.56

80(30)

H81C

9654.96

7131.97

6153.87

113

H10A

6049.64

3988.73

6066.56

H10B

5640.37

4481.6

5310.46

31(18)

H10C

4791.11

4631.78

5998.87

Experimental

Single crystals of C₂₀H₃₆Cl₂CoN₈O₂ [shelx] were []. A suitable crystal was selected and [] on a D8 Venture diffractometer. The crystal was kept at 100.00 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 XL [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. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [shelx]

Crystal Data for C₂₀H₃₆Cl₂CoN₈O₂ (M =550.40 g/mol): monoclinic, space group C2/c (no. 15), a = 10.4681(7) Å, b = 14.1306(10) Å, c = 18.4697(13) Å, β = 92.765(3)°, V = 2728.9(3) Å³, Z = 4, T = 100.00 K, μ(CuKα) = 6.991 mm^-1, Dcalc = 1.340 g/cm³, 36237 reflections measured (10.524° ≤ 2Θ ≤ 136.818°), 2504 unique (R_int = 0.0518, R_sigma = 0.0227) which were used in all calculations. The final R₁ was 0.0758 (I > 2σ(I)) and wR₂ was 0.1806 (all data).

Refinement model description

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

Details:

1. Fixed Uiso
 At 1.5 times of:
  All H(H) groups, All C(H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N7(H7), C4(H4), C9(H9)
2.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C51(H51A,H51B,H51C), C81(H81A,H81B,H81C), C101(H10A,H10B,
 H10C)

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