exp_299

Table 1 Crystal data and structure refinement for exp_299.
Identification code	exp_299
Empirical formula	C₁₅H₂₁FeO₆
Formula weight	353.17
Temperature/K	293(2)
Crystal system	orthorhombic
Space group	Pbca
a/Å	15.4883(9)
b/Å	13.6013(7)
c/Å	16.6081(10)
α/°	90
β/°	90
γ/°	90
Volume/Å³	3498.7(3)
Z	8
ρ_calcg/cm³	1.341
μ/mm^‑1	0.885
F(000)	1480.0
Crystal size/mm³	0.223 × 0.16 × 0.128
Radiation	Mo Kα (λ = 0.71073)
2Θ range for data collection/°	4.68 to 54.206
Index ranges	-19 ≤ h ≤ 19, -17 ≤ k ≤ 17, -21 ≤ l ≤ 21
Reflections collected	51732
Independent reflections	3851 [R_int = 0.1365, R_sigma = 0.0579]
Data/restraints/parameters	3851/0/205
Goodness-of-fit on F²	1.010
Final R indexes [I>=2σ (I)]	R₁ = 0.0519, wR₂ = 0.1053
Final R indexes [all data]	R₁ = 0.1162, wR₂ = 0.1251
Largest diff. peak/hole / e Å^-3	0.18/-0.18

Table 2 Fractional Atomic Coordinates (×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for exp_299. U_eq is defined as 1/3 of of the trace of the orthogonalised U_IJ tensor.
Atom	x	y	z	U(eq)
Fe1	3571.8(3)	2689.5(3)	2540.1(2)	48.61(17)
O1	4554.9(14)	1740.1(15)	2501.7(13)	63.7(6)
O2	4236.8(16)	3526.0(15)	1785.2(12)	63.6(6)
O3	2976.3(15)	1952.9(14)	1669.9(12)	62.6(6)
O4	2623.4(15)	3670.5(14)	2486.8(14)	62.0(6)
O5	2977.0(14)	1801.2(14)	3324.1(13)	61.7(6)
O6	4057.7(15)	3390.1(15)	3495.1(13)	65.1(6)
C1	5852(2)	910(3)	2206(3)	89.5(13)
C2	5260(2)	1784(2)	2114(2)	57.6(9)
C3	5480(2)	2570(3)	1622(2)	72.4(11)
C4	4977(3)	3384(2)	1480.7(19)	65.3(10)
C5	5277(3)	4191(3)	914(2)	107.9(15)
C6	1937(3)	1345(3)	772(3)	121.5(17)
C7	2248(3)	2124(3)	1356(2)	70.2(10)
C8	1755(3)	2939(3)	1508(2)	82.3(11)
C9	1967(2)	3691(2)	2043(2)	62.3(9)
C10	1388(2)	4570(3)	2114(3)	96.2(13)
C11	2614(3)	881(2)	4481(2)	102.3(14)
C12	3096(2)	1708(2)	4075(2)	62.1(9)
C13	3602(3)	2332(3)	4530(2)	80.1(11)
C14	4037(2)	3148(3)	4233(2)	64.5(9)
C15	4507(3)	3839(3)	4798(2)	106.4(16)

Table 2 Fractional Atomic Coordinates (×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for exp_299. U_eq is defined as 1/3 of of the trace of the orthogonalised U_IJ tensor.

Atom

U(eq)

Fe1

3571.8(3)

2689.5(3)

2540.1(2)

48.61(17)

4554.9(14)

1740.1(15)

2501.7(13)

63.7(6)

4236.8(16)

3526.0(15)

1785.2(12)

63.6(6)

2976.3(15)

1952.9(14)

1669.9(12)

62.6(6)

2623.4(15)

3670.5(14)

2486.8(14)

62.0(6)

2977.0(14)

1801.2(14)

3324.1(13)

61.7(6)

4057.7(15)

3390.1(15)

3495.1(13)

65.1(6)

5852(2)

910(3)

2206(3)

89.5(13)

5260(2)

1784(2)

2114(2)

57.6(9)

5480(2)

2570(3)

1622(2)

72.4(11)

4977(3)

3384(2)

1480.7(19)

65.3(10)

5277(3)

4191(3)

914(2)

107.9(15)

1937(3)

1345(3)

772(3)

121.5(17)

2248(3)

2124(3)

1356(2)

70.2(10)

1755(3)

2939(3)

1508(2)

82.3(11)

1967(2)

3691(2)

2043(2)

62.3(9)

C10

1388(2)

4570(3)

2114(3)

96.2(13)

C11

2614(3)

881(2)

4481(2)

102.3(14)

C12

3096(2)

1708(2)

4075(2)

62.1(9)

C13

3602(3)

2332(3)

4530(2)

80.1(11)

C14

4037(2)

3148(3)

4233(2)

64.5(9)

C15

4507(3)

3839(3)

4798(2)

106.4(16)

Table 3 Anisotropic Displacement Parameters (Å²×10³) for exp_299. The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+2hka*b*U₁₂+…].
Atom	U₁₁	U₂₂	U₃₃	U₂₃	U₁₃	U₁₂
Fe1	51.9(3)	46.5(3)	47.5(3)	0.8(2)	-1.2(2)	-5.7(2)
O1	52.1(15)	53.1(14)	85.9(16)	14.7(12)	3.4(13)	-2.7(11)
O2	70.2(16)	58.2(14)	62.4(14)	14.2(11)	10.7(13)	0.4(12)
O3	70.4(16)	53.9(13)	63.4(15)	-14.7(11)	-10.7(13)	4.5(12)
O4	59.6(14)	50.0(13)	76.5(15)	-12.4(11)	-3.9(13)	1.8(11)
O5	64.1(16)	61.0(14)	60.0(15)	6.3(11)	6.5(12)	-18.2(12)
O6	80.5(17)	59.2(14)	55.5(13)	2.6(11)	-14.5(12)	-22.1(12)
C1	59(2)	66(2)	143(4)	-6(2)	6(2)	-2(2)
C2	50(2)	48(2)	75(2)	-11.6(18)	-2.0(19)	-5.6(17)
C3	65(3)	65(2)	87(3)	2(2)	31(2)	-6.4(19)
C4	86(3)	60(2)	50(2)	1.3(17)	15(2)	-15(2)
C5	135(4)	97(3)	92(3)	32(2)	46(3)	-22(3)
C6	123(4)	128(4)	114(4)	-63(3)	-40(3)	-14(3)
C7	80(3)	68(3)	62(2)	-9.5(19)	-16(2)	-11(2)
C8	70(3)	83(3)	94(3)	-6(2)	-30(2)	9(2)
C9	64(3)	48(2)	75(2)	10.1(18)	8(2)	1.2(18)
C10	82(3)	63(2)	143(4)	16(3)	-6(3)	21(2)
C11	115(4)	81(3)	111(3)	43(2)	27(3)	-10(3)
C12	66(3)	60(2)	61(2)	14.6(18)	9(2)	5.6(19)
C13	100(3)	91(3)	49(2)	15(2)	-5(2)	-2(3)
C14	65(3)	73(2)	56(2)	-8.8(19)	-13.7(19)	0.6(19)
C15	126(4)	116(4)	77(3)	-22(2)	-36(3)	-19(3)

Table 3 Anisotropic Displacement Parameters (Å²×10³) for exp_299. The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+2hka*b*U₁₂+…].

Atom

U₁₁

U₂₂

U₃₃

U₂₃

U₁₃

U₁₂

Fe1

51.9(3)

46.5(3)

47.5(3)

0.8(2)

-1.2(2)

-5.7(2)

52.1(15)

53.1(14)

85.9(16)

14.7(12)

3.4(13)

-2.7(11)

70.2(16)

58.2(14)

62.4(14)

14.2(11)

10.7(13)

0.4(12)

70.4(16)

53.9(13)

63.4(15)

-14.7(11)

-10.7(13)

4.5(12)

59.6(14)

50.0(13)

76.5(15)

-12.4(11)

-3.9(13)

1.8(11)

64.1(16)

61.0(14)

60.0(15)

6.3(11)

6.5(12)

-18.2(12)

80.5(17)

59.2(14)

55.5(13)

2.6(11)

-14.5(12)

-22.1(12)

59(2)

66(2)

143(4)

-6(2)

6(2)

-2(2)

50(2)

48(2)

75(2)

-11.6(18)

-2.0(19)

-5.6(17)

65(3)

65(2)

87(3)

2(2)

31(2)

-6.4(19)

86(3)

60(2)

50(2)

1.3(17)

15(2)

-15(2)

135(4)

97(3)

92(3)

32(2)

46(3)

-22(3)

123(4)

128(4)

114(4)

-63(3)

-40(3)

-14(3)

80(3)

68(3)

62(2)

-9.5(19)

-16(2)

-11(2)

70(3)

83(3)

94(3)

-6(2)

-30(2)

9(2)

64(3)

48(2)

75(2)

10.1(18)

8(2)

1.2(18)

C10

82(3)

63(2)

143(4)

16(3)

-6(3)

21(2)

C11

115(4)

81(3)

111(3)

43(2)

27(3)

-10(3)

C12

66(3)

60(2)

61(2)

14.6(18)

9(2)

5.6(19)

C13

100(3)

91(3)

49(2)

15(2)

-5(2)

-2(3)

C14

65(3)

73(2)

56(2)

-8.8(19)

-13.7(19)

0.6(19)

C15

126(4)

116(4)

77(3)

-22(2)

-36(3)

-19(3)

Table 4 Bond Lengths for exp_299.
Atom	Atom	Length/Å	Atom	Atom	Length/Å
Fe1	O1	1.997(2)	C1	C2	1.510(4)
Fe1	O2	1.982(2)	C2	C3	1.388(4)
Fe1	O3	1.986(2)	C3	C4	1.374(4)
Fe1	O4	1.986(2)	C4	C5	1.520(4)
Fe1	O5	2.0009(19)	C6	C7	1.515(4)
Fe1	O6	1.998(2)	C7	C8	1.370(5)
O1	C2	1.269(4)	C8	C9	1.393(4)
O2	C4	1.268(4)	C9	C10	1.500(4)
O3	C7	1.264(4)	C11	C12	1.508(4)
O4	C9	1.255(4)	C12	C13	1.380(4)
O5	C12	1.267(4)	C13	C14	1.388(4)
O6	C14	1.269(4)	C14	C15	1.515(4)

Table 4 Bond Lengths for exp_299.

Atom

Length/Å

Atom

Length/Å

Fe1

1.997(2)

1.510(4)

Fe1

1.982(2)

1.388(4)

Fe1

1.986(2)

1.374(4)

Fe1

1.986(2)

1.520(4)

Fe1

2.0009(19)

1.515(4)

Fe1

1.998(2)

1.370(5)

1.269(4)

1.393(4)

1.268(4)

C10

1.500(4)

1.264(4)

C11

C12

1.508(4)

1.255(4)

C12

C13

1.380(4)

C12

1.267(4)

C13

C14

1.388(4)

C14

1.269(4)

C14

C15

1.515(4)

Table 5 Bond Angles for exp_299.
Atom	Atom	Atom	Angle/˚	Atom	Atom	Atom	Angle/˚
O1	Fe1	O5	88.94(9)	O1	C2	C1	115.7(3)
O2	Fe1	O1	87.41(9)	O1	C2	C3	123.2(3)
O2	Fe1	O3	94.05(9)	C3	C2	C1	121.1(3)
O2	Fe1	O4	88.31(9)	C4	C3	C2	125.6(3)
O2	Fe1	O5	176.06(9)	O2	C4	C3	124.6(3)
O2	Fe1	O6	91.87(9)	O2	C4	C5	114.5(3)
O3	Fe1	O1	90.27(9)	C3	C4	C5	121.0(4)
O3	Fe1	O4	87.88(9)	O3	C7	C6	114.8(3)
O3	Fe1	O5	87.43(9)	O3	C7	C8	124.7(3)
O3	Fe1	O6	173.50(10)	C8	C7	C6	120.5(4)
O4	Fe1	O1	175.20(9)	C7	C8	C9	125.5(3)
O4	Fe1	O5	95.40(9)	O4	C9	C8	123.3(3)
O4	Fe1	O6	89.63(9)	O4	C9	C10	117.1(3)
O6	Fe1	O1	92.67(10)	C8	C9	C10	119.6(4)
O6	Fe1	O5	86.84(9)	O5	C12	C11	116.3(3)
C2	O1	Fe1	129.9(2)	O5	C12	C13	124.0(3)
C4	O2	Fe1	129.4(2)	C13	C12	C11	119.7(3)
C7	O3	Fe1	128.5(2)	C12	C13	C14	124.9(3)
C9	O4	Fe1	129.7(2)	O6	C14	C13	124.2(3)
C12	O5	Fe1	129.4(2)	O6	C14	C15	115.1(3)
C14	O6	Fe1	129.3(2)	C13	C14	C15	120.6(3)

Table 5 Bond Angles for exp_299.

Atom

Angle/˚

Atom

Angle/˚

Fe1

88.94(9)

115.7(3)

Fe1

87.41(9)

123.2(3)

Fe1

94.05(9)

121.1(3)

Fe1

88.31(9)

125.6(3)

Fe1

176.06(9)

124.6(3)

Fe1

91.87(9)

114.5(3)

Fe1

90.27(9)

121.0(4)

Fe1

87.88(9)

114.8(3)

Fe1

87.43(9)

124.7(3)

Fe1

173.50(10)

120.5(4)

Fe1

175.20(9)

125.5(3)

Fe1

95.40(9)

123.3(3)

Fe1

89.63(9)

C10

117.1(3)

Fe1

92.67(10)

C10

119.6(4)

Fe1

86.84(9)

C12

C11

116.3(3)

Fe1

129.9(2)

C12

C13

124.0(3)

Fe1

129.4(2)

C13

C12

C11

119.7(3)

Fe1

128.5(2)

C12

C13

C14

124.9(3)

Fe1

129.7(2)

C14

C13

124.2(3)

C12

Fe1

129.4(2)

C14

C15

115.1(3)

C14

Fe1

129.3(2)

C13

C14

C15

120.6(3)

Table 6 Torsion Angles for exp_299.
A	B	C	D	Angle/˚	A	B	C	D	Angle/˚
Fe1	O1	C2	C1	-178.1(2)	O1	C2	C3	C4	-0.8(6)
Fe1	O1	C2	C3	0.8(5)	O3	C7	C8	C9	-1.7(6)
Fe1	O2	C4	C3	0.6(5)	O5	C12	C13	C14	1.1(6)
Fe1	O2	C4	C5	179.4(2)	C1	C2	C3	C4	178.0(3)
Fe1	O3	C7	C6	-173.1(2)	C2	C3	C4	O2	0.1(6)
Fe1	O3	C7	C8	7.3(5)	C2	C3	C4	C5	-178.6(3)
Fe1	O4	C9	C8	4.3(5)	C6	C7	C8	C9	178.7(4)
Fe1	O4	C9	C10	-176.6(2)	C7	C8	C9	O4	-4.4(6)
Fe1	O5	C12	C11	-172.8(2)	C7	C8	C9	C10	176.5(4)
Fe1	O5	C12	C13	9.7(5)	C11	C12	C13	C14	-176.3(3)
Fe1	O6	C14	C13	-4.1(5)	C12	C13	C14	O6	-4.0(6)
Fe1	O6	C14	C15	177.6(3)	C12	C13	C14	C15	174.2(3)

Table 6 Torsion Angles for exp_299.

Angle/˚

Fe1

-178.1(2)

-0.8(6)

Fe1

0.8(5)

-1.7(6)

Fe1

0.6(5)

C12

C13

C14

1.1(6)

Fe1

179.4(2)

178.0(3)

Fe1

-173.1(2)

0.1(6)

Fe1

7.3(5)

-178.6(3)

Fe1

4.3(5)

178.7(4)

Fe1

C10

-176.6(2)

-4.4(6)

Fe1

C12

C11

-172.8(2)

C10

176.5(4)

Fe1

C12

C13

9.7(5)

C11

C12

C13

C14

-176.3(3)

Fe1

C14

C13

-4.1(5)

C12

C13

C14

-4.0(6)

Fe1

C14

C15

177.6(3)

C12

C13

C14

C15

174.2(3)

Table 7 Hydrogen Atom Coordinates (Å×10⁴) and Isotropic Displacement Parameters (Å²×10³) for exp_299.
Atom	x	y	z	U(eq)
H1A	5790.31	640.75	2737.18	134
H1B	6438.45	1113.53	2124.21	134
H1C	5702.16	418.89	1814.57	134
H3	6013.64	2543.79	1366.54	87
H5A	4951.83	4160.01	422.61	162
H5B	5879.66	4104.1	797.04	162
H5C	5190.82	4820.3	1163.49	162
H6A	2335.53	1295.75	330.47	182
H6B	1377.24	1521.75	571.48	182
H6C	1902.85	722.68	1043.15	182
H8	1235.98	2996.18	1231.41	99
H10A	1447.6	4852.87	2640.92	144
H10B	799.25	4372.08	2032.33	144
H10C	1545.38	5047.72	1715.06	144
H11A	2030.7	1082.49	4584.97	153
H11B	2893.21	720.33	4979.98	153
H11C	2612.51	315.04	4136	153
H13	3656.85	2195.63	5075.95	96
H15A	5093.42	3624.91	4860.29	160
H15B	4225.28	3838.42	5313.02	160
H15C	4499.11	4492.3	4578.84	160

Table 7 Hydrogen Atom Coordinates (Å×10⁴) and Isotropic Displacement Parameters (Å²×10³) for exp_299.

Atom

U(eq)

H1A

5790.31

640.75

2737.18

134

H1B

6438.45

1113.53

2124.21

134

H1C

5702.16

418.89

1814.57

134

6013.64

2543.79

1366.54

H5A

4951.83

4160.01

422.61

162

H5B

5879.66

4104.1

797.04

162

H5C

5190.82

4820.3

1163.49

162

H6A

2335.53

1295.75

330.47

182

H6B

1377.24

1521.75

571.48

182

H6C

1902.85

722.68

1043.15

182

1235.98

2996.18

1231.41

H10A

1447.6

4852.87

2640.92

144

H10B

799.25

4372.08

2032.33

144

H10C

1545.38

5047.72

1715.06

144

H11A

2030.7

1082.49

4584.97

153

H11B

2893.21

720.33

4979.98

153

H11C

2612.51

315.04

4136

153

H13

3656.85

2195.63

5075.95

H15A

5093.42

3624.91

4860.29

160

H15B

4225.28

3838.42

5313.02

160

H15C

4499.11

4492.3

4578.84

160

Experimental

Single crystals of C₁₅H₂₁FeO₆ [exp_299] 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_299]

Crystal Data for C₁₅H₂₁FeO₆ (M =353.17 g/mol): orthorhombic, space group Pbca (no. 61), a = 15.4883(9) Å, b = 13.6013(7) Å, c = 16.6081(10) Å, V = 3498.7(3) Å³, Z = 8, T = 293(2) K, μ(Mo Kα) = 0.885 mm^-1, Dcalc = 1.341 g/cm³, 51732 reflections measured (4.68° ≤ 2Θ ≤ 54.206°), 3851 unique (R_int = 0.1365, R_sigma = 0.0579) which were used in all calculations. The final R₁ was 0.0519 (I > 2σ(I)) and wR₂ was 0.1251 (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)

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