exp_123 (2)

Table 1 Crystal data and structure refinement for exp_123 (2).
Identification code	exp_123 (2)
Empirical formula	C₁₀H₃₈ClCoN₆O₁₁
Formula weight	512.84
Temperature/K	293(2)
Crystal system	triclinic
Space group	P1
a/Å	8.1448(2)
b/Å	8.2664(3)
c/Å	8.4973(3)
α/°	102.314(3)
β/°	101.136(2)
γ/°	95.278(2)
Volume/Å³	543.10(3)
Z	1
ρ_calcg/cm³	1.568
μ/mm^‑1	0.976
F(000)	272.0
Crystal size/mm³	? × ? × ?
Radiation	MoKα (λ = 0.71073)
2Θ range for data collection/°	5.148 to 52.74
Index ranges	-11 ≤ h ≤ 11, -11 ≤ k ≤ 11, -12 ≤ l ≤ 12
Reflections collected	28324
Independent reflections	4391 [R_int = 0.0236, R_sigma = 0.0136]
Data/restraints/parameters	4391/3/280
Goodness-of-fit on F²	1.049
Final R indexes [I>=2σ (I)]	R₁ = 0.0178, wR₂ = 0.0464
Final R indexes [all data]	R₁ = 0.0179, wR₂ = 0.0464
Largest diff. peak/hole / e Å^-3	0.33/-0.20
Flack parameter	-0.012(3)

Table 2 Fractional Atomic Coordinates (×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for exp_123 (2). U_eq is defined as 1/3 of of the trace of the orthogonalised U_IJ tensor.
Atom	x	y	z	U(eq)
Co1	7314.4(2)	4745.2(2)	1675.8(2)	17.33(9)
N6	7235(3)	7166(3)	1979(3)	25.5(4)
N3	7218(3)	2340(3)	1550(3)	26.4(5)
N4	4853(3)	4354(3)	1404(3)	25.1(4)
N1	7103(3)	4418(3)	-714(3)	26.2(5)
N5	7712(3)	5193(3)	4089(3)	25.1(4)
N2	9764(3)	4994(3)	1821(3)	28.0(5)
C1	8793(3)	4851(4)	-1065(3)	34.0(5)
C6	7268(4)	7948(3)	3726(3)	33.4(5)
C5	8295(4)	7011(3)	4794(3)	32.4(5)
C2	10095(3)	4323(4)	164(3)	35.0(6)
C3	5594(3)	1718(3)	1888(3)	32.8(5)
C4	4257(3)	2519(3)	974(4)	38.4(6)
O2	3798(3)	5907(3)	4353(3)	49.5(6)
O4	5668(2)	7404(2)	8539(2)	30.6(4)
O3	3138(2)	4553(2)	7918(2)	29.3(4)
O5	3668(3)	7726(2)	10749(2)	36.0(4)
O1	5016(2)	4096(2)	5593(3)	37.5(4)
O6	1578(3)	8335(3)	8956(2)	42.0(5)
C8	3112(3)	5693(3)	6883(3)	22.5(4)
C7	4049(3)	5171(3)	5502(3)	27.3(5)
C10	2988(3)	7875(3)	9352(3)	24.8(4)
C9	3914(3)	7422(3)	7941(3)	22.5(4)
O9	4229(4)	931(3)	5964(4)	68.7(8)
O8	2154(3)	8279(3)	3422(3)	47.7(5)
O7	-429(3)	9540(3)	11055(3)	45.2(5)
O11	10109(3)	673(3)	7467(3)	54.4(6)
O10	6924(3)	441(3)	8043(2)	37.9(4)
Cl1	10394.5(9)	2431.7(8)	4534.8(9)	43.95(18)

Table 2 Fractional Atomic Coordinates (×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for exp_123 (2). U_eq is defined as 1/3 of of the trace of the orthogonalised U_IJ tensor.

Atom

U(eq)

Co1

7314.4(2)

4745.2(2)

1675.8(2)

17.33(9)

7235(3)

7166(3)

1979(3)

25.5(4)

7218(3)

2340(3)

1550(3)

26.4(5)

4853(3)

4354(3)

1404(3)

25.1(4)

7103(3)

4418(3)

-714(3)

26.2(5)

7712(3)

5193(3)

4089(3)

25.1(4)

9764(3)

4994(3)

1821(3)

28.0(5)

8793(3)

4851(4)

-1065(3)

34.0(5)

7268(4)

7948(3)

3726(3)

33.4(5)

8295(4)

7011(3)

4794(3)

32.4(5)

10095(3)

4323(4)

164(3)

35.0(6)

5594(3)

1718(3)

1888(3)

32.8(5)

4257(3)

2519(3)

974(4)

38.4(6)

3798(3)

5907(3)

4353(3)

49.5(6)

5668(2)

7404(2)

8539(2)

30.6(4)

3138(2)

4553(2)

7918(2)

29.3(4)

3668(3)

7726(2)

10749(2)

36.0(4)

5016(2)

4096(2)

5593(3)

37.5(4)

1578(3)

8335(3)

8956(2)

42.0(5)

3112(3)

5693(3)

6883(3)

22.5(4)

4049(3)

5171(3)

5502(3)

27.3(5)

C10

2988(3)

7875(3)

9352(3)

24.8(4)

3914(3)

7422(3)

7941(3)

22.5(4)

4229(4)

931(3)

5964(4)

68.7(8)

2154(3)

8279(3)

3422(3)

47.7(5)

-429(3)

9540(3)

11055(3)

45.2(5)

O11

10109(3)

673(3)

7467(3)

54.4(6)

O10

6924(3)

441(3)

8043(2)

37.9(4)

Cl1

10394.5(9)

2431.7(8)

4534.8(9)

43.95(18)

Table 3 Anisotropic Displacement Parameters (Å²×10³) for exp_123 (2). The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+2hka*b*U₁₂+…].
Atom	U₁₁	U₂₂	U₃₃	U₂₃	U₁₃	U₁₂
Co1	16.45(13)	17.76(13)	17.37(13)	3.47(8)	3.16(8)	3.11(8)
N6	26.2(11)	24.3(10)	25.7(10)	6.7(8)	3.9(8)	3.3(8)
N3	29.1(12)	22.7(10)	25.5(10)	2.4(8)	4.2(9)	6.3(8)
N4	22.0(11)	30.1(11)	24.7(10)	7.5(9)	6.8(8)	5.9(9)
N1	25.8(11)	29.2(11)	23.4(10)	6.0(8)	4.4(8)	5.9(8)
N5	25.6(11)	28.3(11)	21.8(10)	5.0(8)	6.0(8)	5.6(8)
N2	22.0(12)	32.7(12)	28.3(12)	5.4(9)	4.4(9)	4.5(9)
C1	34.0(13)	43.6(14)	28.5(12)	10.0(10)	14.8(10)	5.3(11)
C6	41.7(14)	24.0(11)	33.6(13)	0.3(10)	11.5(11)	8.8(10)
C5	38.4(14)	29.7(12)	22.5(11)	-2.4(9)	1.9(10)	1.7(10)
C2	24.7(12)	48.3(15)	34.0(13)	6.8(11)	13.0(10)	8.1(11)
C3	35.2(13)	23.4(11)	39.6(13)	8.1(10)	9.6(11)	-1.5(9)
C4	26.4(13)	33.5(13)	51.6(16)	9.1(12)	3.9(11)	-3.1(10)
O2	81.3(16)	52.9(12)	35.1(10)	25.3(9)	34.8(11)	33.8(12)
O4	21.3(8)	30.4(9)	41.5(9)	15.0(7)	3.9(7)	1.4(6)
O3	40.0(10)	25.1(8)	21.2(8)	5.1(6)	8.0(7)	-5.8(7)
O5	43.2(11)	41.5(10)	22.9(8)	6.6(7)	7.3(7)	5.8(8)
O1	38.4(10)	37.6(10)	46.5(11)	15.9(8)	21.3(8)	16.3(8)
O6	40.1(11)	55.6(12)	39.6(10)	15.1(9)	18.3(8)	24.9(9)
C8	21.4(10)	29.2(11)	18.3(9)	6.9(8)	5.8(8)	5.1(8)
C7	33.6(13)	28.4(12)	24.5(11)	8.2(9)	13.5(10)	8.7(10)
C10	28.7(12)	20.5(10)	25.1(11)	3.5(8)	8.2(9)	2.9(8)
C9	20.7(10)	25.9(11)	23.5(10)	10.9(9)	4.6(8)	5.3(8)
O9	69.5(16)	45.8(13)	81.6(18)	31.1(13)	-22.0(14)	4.7(12)
O8	53.2(13)	52.7(13)	46.5(12)	18.4(10)	18.3(10)	23.8(10)
O7	35.9(10)	61.3(14)	39.0(11)	5.6(10)	13.5(9)	13.0(10)
O11	59.9(14)	59.5(14)	54.7(14)	23.5(11)	21.3(11)	22.0(11)
O10	36.7(10)	39.7(10)	33.3(10)	7.0(8)	2.2(8)	1.2(8)
Cl1	43.8(4)	33.7(3)	45.2(4)	8.2(3)	-11.8(3)	6.9(3)

Table 3 Anisotropic Displacement Parameters (Å²×10³) for exp_123 (2). The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+2hka*b*U₁₂+…].

Atom

U₁₁

U₂₂

U₃₃

U₂₃

U₁₃

U₁₂

Co1

16.45(13)

17.76(13)

17.37(13)

3.47(8)

3.16(8)

3.11(8)

26.2(11)

24.3(10)

25.7(10)

6.7(8)

3.9(8)

3.3(8)

29.1(12)

22.7(10)

25.5(10)

2.4(8)

4.2(9)

6.3(8)

22.0(11)

30.1(11)

24.7(10)

7.5(9)

6.8(8)

5.9(9)

25.8(11)

29.2(11)

23.4(10)

6.0(8)

4.4(8)

5.9(8)

25.6(11)

28.3(11)

21.8(10)

5.0(8)

6.0(8)

5.6(8)

22.0(12)

32.7(12)

28.3(12)

5.4(9)

4.4(9)

4.5(9)

34.0(13)

43.6(14)

28.5(12)

10.0(10)

14.8(10)

5.3(11)

41.7(14)

24.0(11)

33.6(13)

0.3(10)

11.5(11)

8.8(10)

38.4(14)

29.7(12)

22.5(11)

-2.4(9)

1.9(10)

1.7(10)

24.7(12)

48.3(15)

34.0(13)

6.8(11)

13.0(10)

8.1(11)

35.2(13)

23.4(11)

39.6(13)

8.1(10)

9.6(11)

-1.5(9)

26.4(13)

33.5(13)

51.6(16)

9.1(12)

3.9(11)

-3.1(10)

81.3(16)

52.9(12)

35.1(10)

25.3(9)

34.8(11)

33.8(12)

21.3(8)

30.4(9)

41.5(9)

15.0(7)

3.9(7)

1.4(6)

40.0(10)

25.1(8)

21.2(8)

5.1(6)

8.0(7)

-5.8(7)

43.2(11)

41.5(10)

22.9(8)

6.6(7)

7.3(7)

5.8(8)

38.4(10)

37.6(10)

46.5(11)

15.9(8)

21.3(8)

16.3(8)

40.1(11)

55.6(12)

39.6(10)

15.1(9)

18.3(8)

24.9(9)

21.4(10)

29.2(11)

18.3(9)

6.9(8)

5.8(8)

5.1(8)

33.6(13)

28.4(12)

24.5(11)

8.2(9)

13.5(10)

8.7(10)

C10

28.7(12)

20.5(10)

25.1(11)

3.5(8)

8.2(9)

2.9(8)

20.7(10)

25.9(11)

23.5(10)

10.9(9)

4.6(8)

5.3(8)

69.5(16)

45.8(13)

81.6(18)

31.1(13)

-22.0(14)

4.7(12)

53.2(13)

52.7(13)

46.5(12)

18.4(10)

18.3(10)

23.8(10)

35.9(10)

61.3(14)

39.0(11)

5.6(10)

13.5(9)

13.0(10)

O11

59.9(14)

59.5(14)

54.7(14)

23.5(11)

21.3(11)

22.0(11)

O10

36.7(10)

39.7(10)

33.3(10)

7.0(8)

2.2(8)

1.2(8)

Cl1

43.8(4)

33.7(3)

45.2(4)

8.2(3)

-11.8(3)

6.9(3)

Table 4 Bond Lengths for exp_123 (2).
Atom	Atom	Length/Å	Atom	Atom	Length/Å
Co1	N6	1.971(2)	C1	C2	1.503(4)
Co1	N3	1.961(2)	C6	C5	1.499(4)
Co1	N4	1.961(2)	C3	C4	1.501(4)
Co1	N1	1.962(2)	O2	C7	1.251(3)
Co1	N5	1.961(2)	O4	C9	1.423(3)
Co1	N2	1.964(2)	O3	C8	1.419(3)
N6	C6	1.482(3)	O5	C10	1.246(3)
N3	C3	1.477(3)	O1	C7	1.245(3)
N4	C4	1.493(4)	O6	C10	1.250(3)
N1	C1	1.492(3)	C8	C7	1.529(3)
N5	C5	1.490(3)	C8	C9	1.526(3)
N2	C2	1.485(3)	C10	C9	1.535(3)

Table 4 Bond Lengths for exp_123 (2).

Atom

Length/Å

Atom

Length/Å

Co1

1.971(2)

1.503(4)

Co1

1.961(2)

1.499(4)

Co1

1.961(2)

1.501(4)

Co1

1.962(2)

1.251(3)

Co1

1.961(2)

1.423(3)

Co1

1.964(2)

1.419(3)

1.482(3)

C10

1.246(3)

1.477(3)

1.245(3)

1.493(4)

C10

1.250(3)

1.492(3)

1.529(3)

1.490(3)

1.526(3)

1.485(3)

C10

1.535(3)

Table 5 Bond Angles for exp_123 (2).
Atom	Atom	Atom	Angle/˚	Atom	Atom	Atom	Angle/˚
N3	Co1	N6	173.42(11)	C2	N2	Co1	109.21(16)
N3	Co1	N1	92.48(10)	N1	C1	C2	107.9(2)
N3	Co1	N2	91.68(10)	N6	C6	C5	108.27(19)
N4	Co1	N6	89.95(9)	N5	C5	C6	107.7(2)
N4	Co1	N3	85.44(10)	N2	C2	C1	107.0(2)
N4	Co1	N1	91.51(9)	N3	C3	C4	106.8(2)
N4	Co1	N2	175.94(11)	N4	C4	C3	107.2(2)
N1	Co1	N6	92.33(9)	O3	C8	C7	112.25(18)
N1	Co1	N2	85.75(10)	O3	C8	C9	108.57(17)
N5	Co1	N6	85.50(9)	C9	C8	C7	109.86(18)
N5	Co1	N3	90.04(9)	O2	C7	C8	115.9(2)
N5	Co1	N4	92.93(9)	O1	C7	O2	124.5(2)
N5	Co1	N1	175.05(11)	O1	C7	C8	119.6(2)
N5	Co1	N2	89.93(10)	O5	C10	O6	126.3(2)
N2	Co1	N6	93.15(10)	O5	C10	C9	118.5(2)
C6	N6	Co1	110.46(16)	O6	C10	C9	115.2(2)
C3	N3	Co1	108.87(16)	O4	C9	C8	109.30(17)
C4	N4	Co1	109.77(17)	O4	C9	C10	112.01(18)
C1	N1	Co1	109.58(17)	C8	C9	C10	108.41(17)
C5	N5	Co1	108.91(16)

Table 5 Bond Angles for exp_123 (2).

Atom

Angle/˚

Atom

Angle/˚

Co1

173.42(11)

Co1

109.21(16)

Co1

92.48(10)

107.9(2)

Co1

91.68(10)

108.27(19)

Co1

89.95(9)

107.7(2)

Co1

85.44(10)

107.0(2)

Co1

91.51(9)

106.8(2)

Co1

175.94(11)

107.2(2)

Co1

92.33(9)

112.25(18)

Co1

85.75(10)

108.57(17)

Co1

85.50(9)

109.86(18)

Co1

90.04(9)

115.9(2)

Co1

92.93(9)

124.5(2)

Co1

175.05(11)

119.6(2)

Co1

89.93(10)

C10

126.3(2)

Co1

93.15(10)

C10

118.5(2)

Co1

110.46(16)

C10

115.2(2)

Co1

108.87(16)

109.30(17)

Co1

109.77(17)

C10

112.01(18)

Co1

109.58(17)

C10

108.41(17)

Co1

108.91(16)

Table 6 Torsion Angles for exp_123 (2).
A	B	C	D	Angle/˚	A	B	C	D	Angle/˚
Co1	N6	C6	C5	32.1(3)	O3	C8	C9	O4	67.7(2)
Co1	N3	C3	C4	42.5(2)	O3	C8	C9	C10	-54.7(2)
Co1	N4	C4	C3	35.2(3)	O5	C10	C9	O4	-19.1(3)
Co1	N1	C1	C2	35.7(2)	O5	C10	C9	C8	101.6(2)
Co1	N5	C5	C6	40.7(2)	O6	C10	C9	O4	162.3(2)
Co1	N2	C2	C1	40.2(2)	O6	C10	C9	C8	-77.1(2)
N6	C6	C5	N5	-47.3(3)	C7	C8	C9	O4	-55.4(2)
N3	C3	C4	N4	-50.4(3)	C7	C8	C9	C10	-177.80(19)
N1	C1	C2	N2	-49.3(3)	C9	C8	C7	O2	-73.0(3)
O3	C8	C7	O2	166.1(2)	C9	C8	C7	O1	105.5(3)
O3	C8	C7	O1	-15.4(3)

Table 6 Torsion Angles for exp_123 (2).

Angle/˚

Co1

32.1(3)

67.7(2)

Co1

42.5(2)

C10

-54.7(2)

Co1

35.2(3)

C10

-19.1(3)

Co1

35.7(2)

C10

101.6(2)

Co1

40.7(2)

C10

162.3(2)

Co1

40.2(2)

C10

-77.1(2)

-47.3(3)

-55.4(2)

-50.4(3)

C10

-177.80(19)

-49.3(3)

-73.0(3)

166.1(2)

105.5(3)

-15.4(3)

Table 7 Hydrogen Atom Coordinates (Å×10⁴) and Isotropic Displacement Parameters (Å²×10³) for exp_123 (2).
Atom	x	y	z	U(eq)
H6A	8116	7638	1680	31
H6B	6297	7336	1337	31
H3A	7305	1804	549	32
H3B	8072	2155	2287	32
H4A	4570	4834	2337	30
H4B	4360	4809	607	30
H1A	6696	3359	-1216	31
H1B	6387	5065	-1101	31
H5A	6763	4894	4390	30
H5B	8493	4601	4467	30
H2A	10198	6069	2181	34
H2B	10252	4441	2534	34
H1C	9022	6045	-967	41
H1D	8821	4275	-2179	41
H6C	6127	7901	3909	40
H6D	7767	9112	3996	40
H5C	9485	7267	4810	39
H5D	8138	7328	5916	39
H2C	10004	3113	-68	42
H2D	11223	4768	113	42
H3C	5632	2019	3063	39
H3D	5358	511	1508	39
H4C	4088	2072	-206	46
H4D	3195	2303	1299	46
H4	6205	8273	8487	46
H3	2681	3625	7368	44
H8	1934	5747	6386	27
H9	3779	8241	7261	27
H9A	3705	351	5020	103
H9B	4410	1951	5926	103
H8A	2620	8417	2638	72
H8B	2664	7625	3928	72
H7A	111	9976	12039	68
H7B	264	9253	10452	68
H11A	10265	898	6572	82
H11B	10771	-8	7737	82
H10A	7866	371	7761	57
H10B	6211	653	7268	57

Table 7 Hydrogen Atom Coordinates (Å×10⁴) and Isotropic Displacement Parameters (Å²×10³) for exp_123 (2).

Atom

U(eq)

H6A

8116

7638

1680

H6B

6297

7336

1337

H3A

7305

1804

549

H3B

8072

2155

2287

H4A

4570

4834

2337

H4B

4360

4809

607

H1A

6696

3359

-1216

H1B

6387

5065

-1101

H5A

6763

4894

4390

H5B

8493

4601

4467

H2A

10198

6069

2181

H2B

10252

4441

2534

H1C

9022

6045

-967

H1D

8821

4275

-2179

H6C

6127

7901

3909

H6D

7767

9112

3996

H5C

9485

7267

4810

H5D

8138

7328

5916

H2C

10004

3113

-68

H2D

11223

4768

113

H3C

5632

2019

3063

H3D

5358

511

1508

H4C

4088

2072

-206

H4D

3195

2303

1299

6205

8273

8487

2681

3625

7368

1934

5747

6386

3779

8241

7261

H9A

3705

351

5020

103

H9B

4410

1951

5926

103

H8A

2620

8417

2638

H8B

2664

7625

3928

H7A

111

9976

12039

H7B

264

9253

10452

H11A

10265

898

6572

H11B

10771

-8

7737

H10A

7866

371

7761

H10B

6211

653

7268

Experimental

Single crystals of C₁₀H₃₈ClCoN₆O₁₁ [exp_123 (2)] were []. A suitable crystal was selected and [] on a 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.

Crystal structure determination of [exp_123 (2)]

Crystal Data for C₁₀H₃₈ClCoN₆O₁₁ (M =512.84 g/mol): triclinic, space group P1 (no. 1), a = 8.1448(2) Å, b = 8.2664(3) Å, c = 8.4973(3) Å, α = 102.314(3)°, β = 101.136(2)°, γ = 95.278(2)°, V = 543.10(3) Å³, Z = 1, T = 293(2) K, μ(MoKα) = 0.976 mm^-1, Dcalc = 1.568 g/cm³, 28324 reflections measured (5.148° ≤ 2Θ ≤ 52.74°), 4391 unique (R_int = 0.0236, R_sigma = 0.0136) which were used in all calculations. The final R₁ was 0.0178 (I > 2σ(I)) and wR₂ was 0.0464 (all data).

Refinement model description

Number of restraints - 3, number of constraints - unknown.

Details:

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O9(H9A,H9B), O8(H8A,H8B), O7(H7A,H7B), O11(H11A,H11B), O10(H10A,H10B)
2.b Ternary CH refined with riding coordinates:
 C8(H8), C9(H9)
2.c Secondary CH2 refined with riding coordinates:
 N6(H6A,H6B), N3(H3A,H3B), N4(H4A,H4B), N1(H1A,H1B), N5(H5A,H5B), N2(H2A,H2B),
 C1(H1C,H1D), C6(H6C,H6D), C5(H5C,H5D), C2(H2C,H2D), C3(H3C,H3D), C4(H4C,H4D)
2.d Idealised tetrahedral OH refined as rotating group:
 O4(H4), O3(H3)

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