exp_288

Table 1 Crystal data and structure refinement for exp_288.
Identification code	exp_288
Empirical formula	C₁₅H₂₁CoO₆
Formula weight	356.25
Temperature/K	293(2)
Crystal system	monoclinic
Space group	P2₁/c
a/Å	13.9224(14)
b/Å	7.4694(7)
c/Å	16.2302(14)
α/°	90
β/°	98.394(9)
γ/°	90
Volume/Å³	1669.7(3)
Z	4
ρ_calcg/cm³	1.417
μ/mm^‑1	1.052
F(000)	744.0
Crystal size/mm³	0.535 × 0.153 × 0.067
Radiation	Mo Kα (λ = 0.71073)
2Θ range for data collection/°	5.074 to 58.256
Index ranges	-12 ≤ h ≤ 19, -10 ≤ k ≤ 9, -22 ≤ l ≤ 10
Reflections collected	8932
Independent reflections	4101 [R_int = 0.0340, R_sigma = 0.0522]
Data/restraints/parameters	4101/0/205
Goodness-of-fit on F²	0.996
Final R indexes [I>=2σ (I)]	R₁ = 0.0495, wR₂ = 0.1177
Final R indexes [all data]	R₁ = 0.0801, wR₂ = 0.1301
Largest diff. peak/hole / e Å^-3	0.32/-0.30

Table 2 Fractional Atomic Coordinates (×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for exp_288. U_eq is defined as 1/3 of of the trace of the orthogonalised U_IJ tensor.
Atom	x	y	z	U(eq)
Co1	2581.0(3)	7312.3(5)	5313.0(2)	43.96(15)
O1	2472.1(14)	4982(3)	4850.3(11)	50.8(5)
O2	1346.4(15)	8120(3)	4810.9(12)	50.3(5)
O3	1984.7(15)	6444(2)	6207.0(11)	52.0(5)
O4	2822.5(14)	9647(2)	5734.6(11)	52.3(5)
O5	3766.6(17)	6588(3)	5923.9(12)	59.8(5)
O6	3086.8(16)	8085(3)	4358.2(11)	52.9(5)
C1	1800(3)	2500(4)	4107(2)	71.9(10)
C2	1713(2)	4395(4)	4419.0(16)	48.8(7)
C3	850(2)	5334(4)	4216.2(19)	58.9(8)
C4	706(2)	7112(4)	4408.5(18)	51.6(7)
C5	-250(3)	7998(5)	4116(2)	73.4(10)
C6	1441(3)	6402(5)	7505.0(19)	71.2(10)
C7	1919(2)	7355(4)	6856.1(17)	49.5(7)
C8	2231(2)	9109(4)	6999.3(18)	56.3(8)
C9	2642(2)	10160(4)	6441.6(16)	47.1(6)
C10	2913(3)	12071(4)	6650(2)	63.8(9)
C11	5441(3)	6243(6)	6303(2)	96.9(13)
C12	4582(3)	6838(5)	5684(2)	66.2(9)
C13	4730(3)	7586(5)	4931(3)	82.6(12)
C14	3990(3)	8134(5)	4311(2)	64.5(9)
C15	4212(3)	8840(6)	3487(2)	95.2(13)

Table 2 Fractional Atomic Coordinates (×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for exp_288. U_eq is defined as 1/3 of of the trace of the orthogonalised U_IJ tensor.

Atom

U(eq)

Co1

2581.0(3)

7312.3(5)

5313.0(2)

43.96(15)

2472.1(14)

4982(3)

4850.3(11)

50.8(5)

1346.4(15)

8120(3)

4810.9(12)

50.3(5)

1984.7(15)

6444(2)

6207.0(11)

52.0(5)

2822.5(14)

9647(2)

5734.6(11)

52.3(5)

3766.6(17)

6588(3)

5923.9(12)

59.8(5)

3086.8(16)

8085(3)

4358.2(11)

52.9(5)

1800(3)

2500(4)

4107(2)

71.9(10)

1713(2)

4395(4)

4419.0(16)

48.8(7)

850(2)

5334(4)

4216.2(19)

58.9(8)

706(2)

7112(4)

4408.5(18)

51.6(7)

-250(3)

7998(5)

4116(2)

73.4(10)

1441(3)

6402(5)

7505.0(19)

71.2(10)

1919(2)

7355(4)

6856.1(17)

49.5(7)

2231(2)

9109(4)

6999.3(18)

56.3(8)

2642(2)

10160(4)

6441.6(16)

47.1(6)

C10

2913(3)

12071(4)

6650(2)

63.8(9)

C11

5441(3)

6243(6)

6303(2)

96.9(13)

C12

4582(3)

6838(5)

5684(2)

66.2(9)

C13

4730(3)

7586(5)

4931(3)

82.6(12)

C14

3990(3)

8134(5)

4311(2)

64.5(9)

C15

4212(3)

8840(6)

3487(2)

95.2(13)

Table 3 Anisotropic Displacement Parameters (Å²×10³) for exp_288. The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+2hka*b*U₁₂+…].
Atom	U₁₁	U₂₂	U₃₃	U₂₃	U₁₃	U₁₂
Co1	48.8(3)	45.8(2)	37.0(2)	-1.45(15)	5.18(17)	5.55(16)
O1	58.2(14)	48.4(11)	45.4(11)	-4.8(8)	6.0(10)	9.4(9)
O2	45.3(13)	53.6(11)	50.7(11)	-2.7(9)	3.3(10)	9.2(9)
O3	65.9(14)	51.6(11)	39.8(10)	-2.4(8)	11.6(10)	-0.9(10)
O4	61.3(14)	49.0(11)	46.0(11)	-2.4(9)	6.0(10)	-0.5(9)
O5	63.3(16)	62.6(13)	50.9(12)	-0.5(10)	0.2(11)	11.3(11)
O6	54.2(14)	62.6(12)	42.3(11)	2.1(9)	8.2(10)	4.0(10)
C1	100(3)	54.4(19)	62(2)	-7.8(15)	16(2)	-3.4(17)
C2	62(2)	50.3(16)	35.6(14)	0.8(12)	11.9(14)	-5.5(14)
C3	52(2)	60.3(19)	62.3(19)	-4.9(15)	2.4(16)	-7.6(15)
C4	43.9(19)	68.4(19)	44.1(15)	7.0(14)	11.6(14)	5.3(14)
C5	46(2)	96(3)	77(2)	2(2)	2.8(18)	14.7(18)
C6	79(3)	90(3)	47.1(18)	-1.6(17)	16.0(17)	-6.4(19)
C7	47.2(19)	62.5(18)	36.7(14)	0.5(12)	-0.6(14)	7.1(13)
C8	67(2)	60.2(19)	40.6(15)	-10.0(13)	5.5(14)	5.2(15)
C9	38.1(16)	52.5(16)	46.0(15)	-5.6(12)	-9.8(12)	10.8(12)
C10	66(2)	55.7(18)	64(2)	-9.0(15)	-8.5(17)	4.4(15)
C11	69(3)	126(4)	86(3)	-20(3)	-21(2)	22(2)
C12	57(2)	80(2)	57(2)	-18.1(17)	-8.8(18)	10.0(18)
C13	43(2)	136(4)	68(2)	-6(2)	4(2)	-3(2)
C14	63(2)	77(2)	55.0(19)	-9.4(16)	16.7(18)	-12.0(17)
C15	87(3)	133(3)	71(2)	8(2)	29(2)	-20(3)

Table 3 Anisotropic Displacement Parameters (Å²×10³) for exp_288. The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+2hka*b*U₁₂+…].

Atom

U₁₁

U₂₂

U₃₃

U₂₃

U₁₃

U₁₂

Co1

48.8(3)

45.8(2)

37.0(2)

-1.45(15)

5.18(17)

5.55(16)

58.2(14)

48.4(11)

45.4(11)

-4.8(8)

6.0(10)

9.4(9)

45.3(13)

53.6(11)

50.7(11)

-2.7(9)

3.3(10)

9.2(9)

65.9(14)

51.6(11)

39.8(10)

-2.4(8)

11.6(10)

-0.9(10)

61.3(14)

49.0(11)

46.0(11)

-2.4(9)

6.0(10)

-0.5(9)

63.3(16)

62.6(13)

50.9(12)

-0.5(10)

0.2(11)

11.3(11)

54.2(14)

62.6(12)

42.3(11)

2.1(9)

8.2(10)

4.0(10)

100(3)

54.4(19)

62(2)

-7.8(15)

16(2)

-3.4(17)

62(2)

50.3(16)

35.6(14)

0.8(12)

11.9(14)

-5.5(14)

52(2)

60.3(19)

62.3(19)

-4.9(15)

2.4(16)

-7.6(15)

43.9(19)

68.4(19)

44.1(15)

7.0(14)

11.6(14)

5.3(14)

46(2)

96(3)

77(2)

2(2)

2.8(18)

14.7(18)

79(3)

90(3)

47.1(18)

-1.6(17)

16.0(17)

-6.4(19)

47.2(19)

62.5(18)

36.7(14)

0.5(12)

-0.6(14)

7.1(13)

67(2)

60.2(19)

40.6(15)

-10.0(13)

5.5(14)

5.2(15)

38.1(16)

52.5(16)

46.0(15)

-5.6(12)

-9.8(12)

10.8(12)

C10

66(2)

55.7(18)

64(2)

-9.0(15)

-8.5(17)

4.4(15)

C11

69(3)

126(4)

86(3)

-20(3)

-21(2)

22(2)

C12

57(2)

80(2)

57(2)

-18.1(17)

-8.8(18)

10.0(18)

C13

43(2)

136(4)

68(2)

-6(2)

4(2)

-3(2)

C14

63(2)

77(2)

55.0(19)

-9.4(16)

16.7(18)

-12.0(17)

C15

87(3)

133(3)

71(2)

8(2)

29(2)

-20(3)

Table 4 Bond Lengths for exp_288.
Atom	Atom	Length/Å	Atom	Atom	Length/Å
Co1	O1	1.893(2)	C1	C2	1.514(4)
Co1	O2	1.890(2)	C2	C3	1.388(4)
Co1	O3	1.8887(17)	C3	C4	1.386(4)
Co1	O4	1.8853(19)	C4	C5	1.501(4)
Co1	O5	1.877(2)	C6	C7	1.504(4)
Co1	O6	1.8838(19)	C7	C8	1.389(4)
O1	C2	1.259(3)	C8	C9	1.384(4)
O2	C4	1.272(4)	C9	C10	1.502(4)
O3	C7	1.269(3)	C11	C12	1.512(5)
O4	C9	1.269(3)	C12	C13	1.385(5)
O5	C12	1.267(4)	C13	C14	1.393(5)
O6	C14	1.272(4)	C14	C15	1.511(4)

Table 4 Bond Lengths for exp_288.

Atom

Length/Å

Atom

Length/Å

Co1

1.893(2)

1.514(4)

Co1

1.890(2)

1.388(4)

Co1

1.8887(17)

1.386(4)

Co1

1.8853(19)

1.501(4)

Co1

1.877(2)

1.504(4)

Co1

1.8838(19)

1.389(4)

1.259(3)

1.384(4)

1.272(4)

C10

1.502(4)

1.269(3)

C11

C12

1.512(5)

1.269(3)

C12

C13

1.385(5)

C12

1.267(4)

C13

C14

1.393(5)

C14

1.272(4)

C14

C15

1.511(4)

Table 5 Bond Angles for exp_288.
Atom	Atom	Atom	Angle/˚	Atom	Atom	Atom	Angle/˚
O2	Co1	O1	96.15(9)	O1	C2	C1	114.2(3)
O3	Co1	O1	88.28(8)	O1	C2	C3	125.7(3)
O3	Co1	O2	88.10(9)	C3	C2	C1	120.2(3)
O4	Co1	O1	173.78(8)	C4	C3	C2	125.4(3)
O4	Co1	O2	87.94(9)	O2	C4	C3	124.7(3)
O4	Co1	O3	96.55(8)	O2	C4	C5	115.1(3)
O5	Co1	O1	87.58(9)	C3	C4	C5	120.2(3)
O5	Co1	O2	173.69(8)	O3	C7	C6	114.9(3)
O5	Co1	O3	86.93(9)	O3	C7	C8	125.9(3)
O5	Co1	O4	88.77(9)	C8	C7	C6	119.3(3)
O5	Co1	O6	96.74(9)	C9	C8	C7	125.1(3)
O6	Co1	O1	88.47(8)	O4	C9	C8	125.1(3)
O6	Co1	O2	88.47(9)	O4	C9	C10	114.5(3)
O6	Co1	O3	175.00(9)	C8	C9	C10	120.4(3)
O6	Co1	O4	86.96(8)	O5	C12	C11	114.2(3)
C2	O1	Co1	123.59(18)	O5	C12	C13	125.8(3)
C4	O2	Co1	123.88(19)	C13	C12	C11	120.0(4)
C7	O3	Co1	123.15(19)	C12	C13	C14	124.5(4)
C9	O4	Co1	124.00(18)	O6	C14	C13	125.5(3)
C12	O5	Co1	123.6(2)	O6	C14	C15	113.3(3)
C14	O6	Co1	123.4(2)	C13	C14	C15	121.2(3)

Table 5 Bond Angles for exp_288.

Atom

Angle/˚

Atom

Angle/˚

Co1

96.15(9)

114.2(3)

Co1

88.28(8)

125.7(3)

Co1

88.10(9)

120.2(3)

Co1

173.78(8)

125.4(3)

Co1

87.94(9)

124.7(3)

Co1

96.55(8)

115.1(3)

Co1

87.58(9)

120.2(3)

Co1

173.69(8)

114.9(3)

Co1

86.93(9)

125.9(3)

Co1

88.77(9)

119.3(3)

Co1

96.74(9)

125.1(3)

Co1

88.47(8)

125.1(3)

Co1

88.47(9)

C10

114.5(3)

Co1

175.00(9)

C10

120.4(3)

Co1

86.96(8)

C12

C11

114.2(3)

Co1

123.59(18)

C12

C13

125.8(3)

Co1

123.88(19)

C13

C12

C11

120.0(4)

Co1

123.15(19)

C12

C13

C14

124.5(4)

Co1

124.00(18)

C14

C13

125.5(3)

C12

Co1

123.6(2)

C14

C15

113.3(3)

C14

Co1

123.4(2)

C13

C14

C15

121.2(3)

Table 6 Hydrogen Atom Coordinates (Å×10⁴) and Isotropic Displacement Parameters (Å²×10³) for exp_288.
Atom	x	y	z	U(eq)
H1A	2132.61	2512.75	3628.97	108
H1B	1164.19	1998.84	3956.73	108
H1C	2160.28	1788.37	4538.67	108
H3	325.73	4718.95	3927.09	71
H5A	-381.26	8873.34	4518.51	110
H5B	-755.64	7113.19	4052.29	110
H5C	-225.61	8574.59	3591.11	110
H6A	801.44	6878.08	7507.9	107
H6B	1820.21	6572.85	8042.64	107
H6C	1397.87	5146.35	7378.59	107
H8	2157.92	9615.83	7509.86	68
H10A	3607.01	12186.63	6739.23	96
H10B	2660.57	12415.87	7146.79	96
H10C	2644.05	12832.47	6198.14	96
H11A	5630.98	7194.68	6690.08	145
H11B	5972.77	5946.81	6012.45	145
H11C	5263.76	5210.54	6599.03	145
H13	5367.01	7731.09	4833.71	99
H15A	4083.61	7923.7	3070.33	143
H15B	4883.13	9182.02	3540.93	143
H15C	3810.68	9862.25	3324.91	143

Table 6 Hydrogen Atom Coordinates (Å×10⁴) and Isotropic Displacement Parameters (Å²×10³) for exp_288.

Atom

U(eq)

H1A

2132.61

2512.75

3628.97

108

H1B

1164.19

1998.84

3956.73

108

H1C

2160.28

1788.37

4538.67

108

325.73

4718.95

3927.09

H5A

-381.26

8873.34

4518.51

110

H5B

-755.64

7113.19

4052.29

110

H5C

-225.61

8574.59

3591.11

110

H6A

801.44

6878.08

7507.9

107

H6B

1820.21

6572.85

8042.64

107

H6C

1397.87

5146.35

7378.59

107

2157.92

9615.83

7509.86

H10A

3607.01

12186.63

6739.23

H10B

2660.57

12415.87

7146.79

H10C

2644.05

12832.47

6198.14

H11A

5630.98

7194.68

6690.08

145

H11B

5972.77

5946.81

6012.45

145

H11C

5263.76

5210.54

6599.03

145

H13

5367.01

7731.09

4833.71

H15A

4083.61

7923.7

3070.33

143

H15B

4883.13

9182.02

3540.93

143

H15C

3810.68

9862.25

3324.91

143

Experimental

Single crystals of C₁₅H₂₁CoO₆ [exp_288] 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_288]

Crystal Data for C₁₅H₂₁CoO₆ (M =356.25 g/mol): monoclinic, space group P2₁/c (no. 14), a = 13.9224(14) Å, b = 7.4694(7) Å, c = 16.2302(14) Å, β = 98.394(9)°, V = 1669.7(3) Å³, Z = 4, T = 293(2) K, μ(Mo Kα) = 1.052 mm^-1, Dcalc = 1.417 g/cm³, 8932 reflections measured (5.074° ≤ 2Θ ≤ 58.256°), 4101 unique (R_int = 0.0340, R_sigma = 0.0522) which were used in all calculations. The final R₁ was 0.0495 (I > 2σ(I)) and wR₂ was 0.1301 (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) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C13(H13)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C)

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.