Identification code | jb141220_1_1 |
Empirical formula | C10H7BF3NO |
Formula weight | 224.98 |
Temperature/K | 100.0(1) |
Crystal system | monoclinic |
Space group | P21/c |
a/Å | 8.8884(2) |
b/Å | 5.65110(10) |
c/Å | 18.6358(4) |
α/° | 90 |
β/° | 101.702(2) |
γ/° | 90 |
Volume/Å3 | 916.61(3) |
Z | 4 |
ρcalcg/cm3 | 1.630 |
μ/mm‑1 | 1.273 |
F(000) | 456.0 |
Crystal size/mm3 | 0.147 × 0.089 × 0.024 |
Radiation | Cu Kα (λ = 1.54184) |
2Θ range for data collection/° | 9.694 to 159.614 |
Index ranges | -11 ≤ h ≤ 10, -6 ≤ k ≤ 5, -22 ≤ l ≤ 23 |
Reflections collected | 7772 |
Independent reflections | 1929 [Rint = 0.0327, Rsigma = 0.0280] |
Data/restraints/parameters | 1929/1/148 |
Goodness-of-fit on F2 | 1.072 |
Final R indexes [I>=2σ (I)] | R1 = 0.0338, wR2 = 0.0895 |
Final R indexes [all data] | R1 = 0.0397, wR2 = 0.0931 |
Largest diff. peak/hole / e Å-3 | 0.26/-0.19 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
F1 | 7044.5(9) | 2034.8(15) | 6061.4(5) | 30.0(2) |
F2 | 8112.6(9) | 5073.8(15) | 6801.6(4) | 28.1(2) |
F3 | 8332.5(9) | 4959.1(15) | 5599.1(5) | 29.9(2) |
O1 | 5680.0(10) | 7561.7(17) | 5356.6(5) | 21.9(2) |
N1 | 3100.0(12) | 9247(2) | 5633.4(6) | 19.7(2) |
C1 | 5786.3(14) | 6079(2) | 5851.6(7) | 19.2(3) |
C2 | 4479.5(14) | 5851(2) | 6249.9(7) | 19.3(3) |
C3 | 4495.2(15) | 4094(2) | 6765.2(7) | 22.6(3) |
C4 | 3297.8(16) | 3818(3) | 7154.1(8) | 25.8(3) |
C5 | 2075.6(16) | 5344(3) | 7034.8(8) | 25.2(3) |
C6 | 1999.5(14) | 7199(2) | 6522.3(7) | 21.3(3) |
C7 | 770.8(15) | 8840(3) | 6382.2(8) | 23.8(3) |
C8 | 755.5(15) | 10631(3) | 5889.9(8) | 24.3(3) |
C9 | 1961.0(15) | 10800(2) | 5511.4(8) | 22.8(3) |
C10 | 3200.2(14) | 7435(2) | 6128.6(7) | 19.2(3) |
B1 | 7362.4(17) | 4461(3) | 6088.6(9) | 22.4(3) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
F1 | 33.1(5) | 18.2(4) | 39.0(5) | 1.2(3) | 8.3(4) | 5.4(3) |
F2 | 20.9(4) | 32.7(5) | 29.6(4) | -1.3(3) | 2.8(3) | 4.2(3) |
F3 | 26.7(4) | 30.7(5) | 36.2(5) | 9.1(4) | 15.4(4) | 11.7(3) |
O1 | 20.1(4) | 20.1(5) | 26.6(5) | 2.8(4) | 7.2(4) | 1.5(4) |
N1 | 16.8(5) | 19.6(6) | 23.8(6) | 1.0(4) | 6.7(4) | 1.3(4) |
C1 | 18.5(6) | 16.8(6) | 22.4(6) | -3.1(5) | 4.0(5) | -0.9(5) |
C2 | 17.8(6) | 18.3(6) | 21.3(6) | -1.4(5) | 2.5(5) | -0.8(5) |
C3 | 20.1(6) | 22.0(7) | 24.7(7) | 1.4(5) | 2.1(5) | -0.4(5) |
C4 | 24.2(7) | 26.6(7) | 25.9(7) | 5.7(5) | 3.7(5) | -3.5(5) |
C5 | 22.4(6) | 30.2(8) | 24.2(7) | 0.8(6) | 7.7(5) | -4.6(5) |
C6 | 18.1(6) | 23.9(7) | 22.4(6) | -2.1(5) | 5.0(5) | -2.6(5) |
C7 | 17.4(6) | 29.1(8) | 26.0(7) | -4.7(5) | 7.1(5) | -0.3(5) |
C8 | 19.7(6) | 25.1(7) | 28.8(7) | -2.9(6) | 6.4(5) | 4.6(5) |
C9 | 20.9(6) | 20.9(7) | 26.9(7) | 0.4(5) | 5.2(5) | 2.7(5) |
C10 | 18.0(6) | 18.8(6) | 20.7(6) | -1.1(5) | 4.1(5) | -1.3(5) |
B1 | 21.0(7) | 21.3(8) | 25.5(7) | 1.0(6) | 6.4(6) | 5.2(5) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
F1 | B1 | 1.3987(19) | C2 | C10 | 1.4286(17) | |
F2 | B1 | 1.4038(18) | C3 | C4 | 1.4125(18) | |
F3 | B1 | 1.4050(17) | C4 | C5 | 1.370(2) | |
O1 | C1 | 1.2355(16) | C5 | C6 | 1.410(2) | |
N1 | C9 | 1.3240(17) | C6 | C7 | 1.4160(19) | |
N1 | C10 | 1.3694(17) | C6 | C10 | 1.4187(17) | |
C1 | C2 | 1.5056(17) | C7 | C8 | 1.364(2) | |
C1 | B1 | 1.6562(19) | C8 | C9 | 1.4005(18) | |
C2 | C3 | 1.3793(19) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
C9 | N1 | C10 | 123.67(11) | C8 | C7 | C6 | 120.80(12) | |
O1 | C1 | C2 | 118.46(11) | C7 | C8 | C9 | 119.02(12) | |
O1 | C1 | B1 | 120.40(11) | N1 | C9 | C8 | 120.31(13) | |
C2 | C1 | B1 | 121.11(11) | N1 | C10 | C2 | 121.08(11) | |
C3 | C2 | C1 | 120.34(11) | N1 | C10 | C6 | 117.76(11) | |
C3 | C2 | C10 | 117.17(12) | C6 | C10 | C2 | 121.15(12) | |
C10 | C2 | C1 | 122.48(11) | F1 | B1 | F2 | 109.25(12) | |
C2 | C3 | C4 | 122.30(12) | F1 | B1 | F3 | 108.60(11) | |
C5 | C4 | C3 | 120.17(13) | F1 | B1 | C1 | 112.20(11) | |
C4 | C5 | C6 | 120.36(12) | F2 | B1 | F3 | 109.20(11) | |
C5 | C6 | C7 | 122.73(12) | F2 | B1 | C1 | 109.26(11) | |
C5 | C6 | C10 | 118.84(12) | F3 | B1 | C1 | 108.28(11) | |
C7 | C6 | C10 | 118.43(12) |
A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
---|---|---|---|---|---|---|---|---|---|---|
O1 | C1 | C2 | C3 | 174.79(12) | C4 | C5 | C6 | C10 | 0.7(2) | |
O1 | C1 | C2 | C10 | -6.50(19) | C5 | C6 | C7 | C8 | 178.94(13) | |
O1 | C1 | B1 | F1 | -125.35(13) | C5 | C6 | C10 | N1 | 179.93(12) | |
O1 | C1 | B1 | F2 | 113.32(13) | C5 | C6 | C10 | C2 | -0.72(19) | |
O1 | C1 | B1 | F3 | -5.51(17) | C6 | C7 | C8 | C9 | 1.3(2) | |
C1 | C2 | C3 | C4 | 179.76(12) | C7 | C6 | C10 | N1 | 0.03(18) | |
C1 | C2 | C10 | N1 | 0.47(19) | C7 | C6 | C10 | C2 | 179.37(12) | |
C1 | C2 | C10 | C6 | -178.85(11) | C7 | C8 | C9 | N1 | -0.3(2) | |
C2 | C1 | B1 | F1 | 56.99(16) | C9 | N1 | C10 | C2 | -178.35(12) | |
C2 | C1 | B1 | F2 | -64.34(16) | C9 | N1 | C10 | C6 | 1.00(19) | |
C2 | C1 | B1 | F3 | 176.83(11) | C10 | N1 | C9 | C8 | -0.9(2) | |
C2 | C3 | C4 | C5 | -1.0(2) | C10 | C2 | C3 | C4 | 1.0(2) | |
C3 | C2 | C10 | N1 | 179.22(12) | C10 | C6 | C7 | C8 | -1.2(2) | |
C3 | C2 | C10 | C6 | -0.10(19) | B1 | C1 | C2 | C3 | -7.51(18) | |
C3 | C4 | C5 | C6 | 0.2(2) | B1 | C1 | C2 | C10 | 171.21(12) | |
C4 | C5 | C6 | C7 | -179.41(13) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H1 | 3865(17) | 9370(30) | 5366(9) | 24 |
H3 | 5323.15 | 3054.58 | 6859.87 | 27 |
H4 | 3339.55 | 2596.52 | 7492.04 | 31 |
H5 | 1291.47 | 5156.92 | 7293.17 | 30 |
H7 | -35.41 | 8694.8 | 6628.68 | 29 |
H8 | -43.53 | 11723.24 | 5806.95 | 29 |
H9 | 1961.45 | 12008.63 | 5172.71 | 27 |
Experimental
Single crystals of C10H7BF3NO [jb141220_1_1] were []. A suitable crystal was selected and [] on a XtaLAB Synergy, Dualflex, Pilatus 300K diffractometer. The crystal was kept at 100.0(1) 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.
Crystal structure determination of [jb141220_1_1]
Crystal Data for C10H7BF3NO (M =224.98 g/mol): monoclinic, space group P21/c (no. 14), a = 8.8884(2) Å, b = 5.65110(10) Å, c = 18.6358(4) Å, β = 101.702(2)°, V = 916.61(3) Å3, Z = 4, T = 100.0(1) K, μ(Cu Kα) = 1.273 mm-1, Dcalc = 1.630 g/cm3, 7772 reflections measured (9.694° ≤ 2Θ ≤ 159.614°), 1929 unique (Rint = 0.0327, Rsigma = 0.0280) which were used in all calculations. The final R1 was 0.0338 (I > 2σ(I)) and wR2 was 0.0931 (all data).
Refinement model description
Number of restraints - 1, number of constraints - unknown.
Details:
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H) groups
2. Restrained distances
N1-H1
0.93 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9)
This report has been created with Olex2, compiled on 2020.11.12 svn.r5f609507 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.