Identification code | jb250221_1_1 |
Empirical formula | C7H6BF3KNO2 |
Formula weight | 243.04 |
Temperature/K | 100.0(1) |
Crystal system | monoclinic |
Space group | P21/c |
a/Å | 17.517(13) |
b/Å | 6.924(5) |
c/Å | 7.458(6) |
α/° | 90 |
β/° | 97.957(16) |
γ/° | 90 |
Volume/Å3 | 895.9(11) |
Z | 4 |
ρcalcg/cm3 | 1.802 |
μ/mm‑1 | 0.616 |
F(000) | 488.0 |
Crystal size/mm3 | 0.23 × 0.08 × 0.02 |
Radiation | MoKα (λ = 0.71073) |
2Θ range for data collection/° | 4.696 to 55.078 |
Index ranges | -22 ≤ h ≤ 22, -9 ≤ k ≤ 8, -9 ≤ l ≤ 9 |
Reflections collected | 7041 |
Independent reflections | 2053 [Rint = 0.0969, Rsigma = 0.1060] |
Data/restraints/parameters | 2053/30/137 |
Goodness-of-fit on F2 | 1.007 |
Final R indexes [I>=2σ (I)] | R1 = 0.0565, wR2 = 0.1091 |
Final R indexes [all data] | R1 = 0.1161, wR2 = 0.1284 |
Largest diff. peak/hole / e Å-3 | 1.00/-0.47 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
K1 | 829.6(5) | 1223.9(13) | 1515.5(11) | 14.2(2) |
F3 | 583.8(12) | 4924(3) | 2741(3) | 15.7(5) |
F2 | 1063.5(12) | 4667(3) | 56(3) | 16.5(5) |
F1 | 482.9(12) | 7464(4) | 780(3) | 18.7(6) |
O1 | 1970.4(15) | 8481(4) | 2289(4) | 16.8(6) |
O2 | 4318.6(16) | 5591(5) | 6088(4) | 23.1(7) |
N1 | 2193.9(18) | 3602(5) | 3545(4) | 14.2(7) |
C4 | 3618(2) | 5027(7) | 5206(5) | 16.7(9) |
C1 | 1795(2) | 6774(6) | 2396(5) | 12.6(9) |
C2 | 2392(2) | 5455(6) | 3422(5) | 12.2(8) |
C3 | 3092(2) | 6226(7) | 4196(5) | 16.2(8) |
C5 | 3425(2) | 3102(7) | 5349(5) | 19.6(10) |
C6 | 2720(2) | 2452(7) | 4498(5) | 18.4(9) |
C7 | 4530(2) | 7573(8) | 5862(6) | 25.5(11) |
B1 | 959(3) | 5949(7) | 1476(6) | 14.1(10) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
K1 | 22.6(5) | 10.6(4) | 9.4(4) | 0.7(4) | 1.8(3) | -0.7(4) |
F3 | 23.8(13) | 15.0(14) | 9.3(11) | 0.5(9) | 6.0(9) | -2.0(10) |
F2 | 25.9(13) | 15.1(14) | 9.1(12) | -1.1(10) | 4.4(10) | -1.5(10) |
F1 | 25.9(14) | 12.5(13) | 16.1(12) | 1.6(10) | -2.4(10) | 0.0(11) |
O1 | 23.1(15) | 9.7(16) | 17.5(14) | 1.8(12) | 2.4(12) | -0.4(12) |
O2 | 21.7(16) | 28(2) | 18.3(16) | 1.9(13) | -3.2(12) | -1.9(13) |
N1 | 20.3(17) | 14.5(18) | 7.5(15) | -0.2(14) | 1.3(13) | 1.7(14) |
C4 | 19(2) | 22(3) | 9.4(19) | 1.3(17) | 3.7(16) | 1.4(18) |
C1 | 19(2) | 14(2) | 6.4(18) | 0.4(15) | 6.4(16) | 0.9(16) |
C2 | 18(2) | 16(2) | 3.0(17) | 1.4(15) | 5.0(14) | 1.2(16) |
C3 | 24(2) | 15(2) | 11.5(18) | 0.3(18) | 6.9(15) | -0.2(18) |
C5 | 23(2) | 22(3) | 13(2) | 5.9(18) | 0.9(18) | 6.4(18) |
C6 | 29(2) | 16(2) | 11(2) | 3.5(17) | 5.5(17) | 6.0(19) |
C7 | 27(3) | 34(3) | 15(2) | 1(2) | 1.2(18) | -6(2) |
B1 | 22(3) | 13(3) | 8(2) | -0.7(18) | 5.7(19) | 1.7(19) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
K1 | K11 | 3.823(2) | F2 | B1 | 1.413(5) | |
K1 | F3 | 2.773(3) | F1 | B1 | 1.395(5) | |
K1 | F32 | 2.762(3) | O1 | C1 | 1.227(5) | |
K1 | F33 | 2.900(3) | O2 | C4 | 1.367(5) | |
K1 | F2 | 2.676(3) | O2 | C7 | 1.437(6) | |
K1 | F24 | 2.687(3) | N1 | C2 | 1.336(5) | |
K1 | F15 | 2.820(3) | N1 | C6 | 1.344(5) | |
K1 | F12 | 3.373(3) | C4 | C3 | 1.384(6) | |
K1 | F16 | 2.712(3) | C4 | C5 | 1.383(6) | |
K1 | O16 | 2.759(3) | C1 | C2 | 1.514(5) | |
K1 | N1 | 3.117(4) | C1 | B1 | 1.631(6) | |
K1 | C16 | 3.532(5) | C2 | C3 | 1.387(5) | |
F3 | B1 | 1.413(5) | C5 | C6 | 1.383(6) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
F31 | K1 | K12 | 49.07(6) | O15 | K1 | K12 | 106.73(9) | |
F33 | K1 | K12 | 46.03(5) | O15 | K1 | F31 | 112.15(9) | |
F3 | K1 | K12 | 117.67(7) | O15 | K1 | F3 | 135.06(8) | |
F31 | K1 | F33 | 95.10(6) | O15 | K1 | F33 | 91.17(8) | |
F3 | K1 | F33 | 124.34(7) | O15 | K1 | F11 | 125.74(8) | |
F31 | K1 | F3 | 92.90(6) | O15 | K1 | F14 | 148.72(8) | |
F31 | K1 | F14 | 63.18(8) | O15 | K1 | N1 | 77.15(10) | |
F3 | K1 | F14 | 75.63(7) | O15 | K1 | C15 | 17.56(8) | |
F33 | K1 | F11 | 128.94(7) | N1 | K1 | K12 | 172.18(7) | |
F31 | K1 | F11 | 42.15(7) | N1 | K1 | F11 | 96.62(9) | |
F3 | K1 | F11 | 54.41(6) | N1 | K1 | C15 | 93.18(11) | |
F3 | K1 | N1 | 59.70(8) | C15 | K1 | K12 | 91.62(9) | |
F33 | K1 | N1 | 128.12(8) | K17 | F3 | K1 | 123.48(8) | |
F31 | K1 | N1 | 136.31(9) | K17 | F3 | K16 | 84.90(6) | |
F33 | K1 | C15 | 86.81(8) | K1 | F3 | K16 | 93.31(8) | |
F31 | K1 | C15 | 95.60(9) | B1 | F3 | K1 | 97.8(2) | |
F3 | K1 | C15 | 146.79(8) | B1 | F3 | K16 | 139.9(2) | |
F2 | K1 | K12 | 107.52(7) | B1 | F3 | K17 | 118.9(2) | |
F26 | K1 | K12 | 118.64(7) | K1 | F2 | K13 | 100.61(9) | |
F26 | K1 | F33 | 150.82(8) | B1 | F2 | K13 | 149.6(2) | |
F2 | K1 | F31 | 124.34(7) | B1 | F2 | K1 | 102.2(2) | |
F26 | K1 | F31 | 75.33(7) | K14 | F1 | K17 | 83.06(8) | |
F26 | K1 | F3 | 84.13(8) | K18 | F1 | K14 | 87.39(8) | |
F2 | K1 | F3 | 49.50(8) | K18 | F1 | K17 | 105.99(8) | |
F2 | K1 | F33 | 81.93(8) | B1 | F1 | K17 | 90.5(2) | |
F2 | K1 | F26 | 126.39(7) | B1 | F1 | K18 | 122.7(2) | |
F2 | K1 | F11 | 99.90(8) | B1 | F1 | K14 | 149.7(2) | |
F2 | K1 | F14 | 67.90(7) | C1 | O1 | K18 | 119.7(3) | |
F2 | K1 | F15 | 144.64(8) | C4 | O2 | C7 | 116.4(3) | |
F26 | K1 | F11 | 59.64(7) | C2 | N1 | K1 | 131.5(2) | |
F26 | K1 | F15 | 88.73(8) | C2 | N1 | C6 | 116.1(4) | |
F26 | K1 | F14 | 132.15(7) | C6 | N1 | K1 | 111.6(3) | |
F2 | K1 | O15 | 123.44(9) | O2 | C4 | C3 | 125.2(4) | |
F26 | K1 | O15 | 68.22(8) | O2 | C4 | C5 | 116.8(4) | |
F2 | K1 | N1 | 64.95(9) | C5 | C4 | C3 | 118.0(4) | |
F26 | K1 | N1 | 69.00(8) | O1 | C1 | K18 | 42.7(2) | |
F26 | K1 | C15 | 67.24(8) | O1 | C1 | C2 | 116.9(4) | |
F2 | K1 | C15 | 139.17(9) | O1 | C1 | B1 | 121.9(4) | |
F14 | K1 | K12 | 45.13(7) | C2 | C1 | K18 | 154.1(3) | |
F11 | K1 | K12 | 86.63(7) | C2 | C1 | B1 | 121.2(4) | |
F15 | K1 | K12 | 47.48(5) | B1 | C1 | K18 | 81.3(2) | |
F14 | K1 | F33 | 59.99(7) | N1 | C2 | C1 | 116.5(3) | |
F15 | K1 | F3 | 155.88(7) | N1 | C2 | C3 | 124.3(4) | |
F15 | K1 | F31 | 62.99(7) | C3 | C2 | C1 | 119.1(4) | |
F15 | K1 | F33 | 62.71(7) | C4 | C3 | C2 | 118.6(4) | |
F14 | K1 | F11 | 73.45(7) | C6 | C5 | C4 | 119.3(4) | |
F15 | K1 | F11 | 102.31(6) | N1 | C6 | C5 | 123.6(4) | |
F15 | K1 | F14 | 92.61(8) | F3 | B1 | C1 | 111.6(3) | |
F15 | K1 | O15 | 61.12(9) | F2 | B1 | F3 | 107.8(3) | |
F15 | K1 | N1 | 137.79(8) | F2 | B1 | C1 | 109.5(3) | |
F14 | K1 | N1 | 129.09(10) | F1 | B1 | F3 | 108.4(3) | |
F14 | K1 | C15 | 136.29(9) | F1 | B1 | F2 | 109.0(3) | |
F11 | K1 | C15 | 117.34(8) | F1 | B1 | C1 | 110.4(4) | |
F15 | K1 | C15 | 44.62(9) |
A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
---|---|---|---|---|---|---|---|---|---|---|
K11 | F3 | B1 | F2 | 119.8(3) | K1 | N1 | C6 | C5 | 172.1(3) | |
K1 | F3 | B1 | F2 | 15.1(3) | K14 | C1 | C2 | N1 | 146.8(4) | |
K12 | F3 | B1 | F2 | -120.3(3) | K14 | C1 | C2 | C3 | -31.8(7) | |
K12 | F3 | B1 | F1 | -2.4(4) | K14 | C1 | B1 | F3 | -113.3(3) | |
K11 | F3 | B1 | F1 | -122.3(3) | K14 | C1 | B1 | F2 | 127.5(3) | |
K1 | F3 | B1 | F1 | 133.0(3) | K14 | C1 | B1 | F1 | 7.4(3) | |
K12 | F3 | B1 | C1 | 119.4(3) | O1 | C1 | C2 | N1 | 179.5(4) | |
K11 | F3 | B1 | C1 | -0.4(6) | O1 | C1 | C2 | C3 | 0.8(5) | |
K1 | F3 | B1 | C1 | -105.2(3) | O1 | C1 | B1 | F3 | -127.2(4) | |
K1 | F2 | B1 | F3 | -15.9(3) | O1 | C1 | B1 | F2 | 113.6(4) | |
K13 | F2 | B1 | F3 | 122.0(4) | O1 | C1 | B1 | F1 | -6.5(5) | |
K1 | F2 | B1 | F1 | -133.4(3) | O2 | C4 | C3 | C2 | -178.1(3) | |
K13 | F2 | B1 | F1 | 4.5(6) | O2 | C4 | C5 | C6 | 179.5(3) | |
K1 | F2 | B1 | C1 | 105.7(3) | N1 | C2 | C3 | C4 | -1.7(6) | |
K13 | F2 | B1 | C1 | -116.3(4) | C4 | C5 | C6 | N1 | -1.2(6) | |
K14 | F1 | B1 | F3 | 111.1(3) | C1 | C2 | C3 | C4 | 176.8(3) | |
K12 | F1 | B1 | F3 | 1.7(3) | C2 | N1 | C6 | C5 | 1.3(6) | |
K15 | F1 | B1 | F3 | -75.2(5) | C2 | C1 | B1 | F3 | 53.0(5) | |
K14 | F1 | B1 | F2 | -131.8(2) | C2 | C1 | B1 | F2 | -66.2(4) | |
K15 | F1 | B1 | F2 | 41.8(6) | C2 | C1 | B1 | F1 | 173.7(3) | |
K12 | F1 | B1 | F2 | 118.8(3) | C3 | C4 | C5 | C6 | -0.3(6) | |
K14 | F1 | B1 | C1 | -11.4(4) | C5 | C4 | C3 | C2 | 1.7(5) | |
K15 | F1 | B1 | C1 | 162.2(3) | C6 | N1 | C2 | C1 | -178.4(3) | |
K12 | F1 | B1 | C1 | -120.9(3) | C6 | N1 | C2 | C3 | 0.2(5) | |
K14 | O1 | C1 | C2 | -159.7(2) | C7 | O2 | C4 | C3 | -3.1(5) | |
K14 | O1 | C1 | B1 | 20.5(5) | C7 | O2 | C4 | C5 | 177.2(4) | |
K1 | N1 | C2 | C1 | 13.1(5) | B1 | C1 | C2 | N1 | -0.7(5) | |
K1 | N1 | C2 | C3 | -168.3(3) | B1 | C1 | C2 | C3 | -179.4(3) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H3 | 3206.84 | 7550.34 | 4035.62 | 19 |
H5 | 3773.07 | 2233.71 | 6026.01 | 24 |
H6 | 2601.81 | 1120.42 | 4590.49 | 22 |
H7A | 4533.59 | 7842.01 | 4572.83 | 38 |
H7B | 5044.21 | 7809.2 | 6525.56 | 38 |
H7C | 4155.49 | 8420.11 | 6332.04 | 38 |
Experimental
Single crystals of C7H6BF3KNO2 [jb250221_1_1] were []. A suitable crystal was selected and [] on a Bruker APEX-II Duo (Mo) 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 [jb250221_1_1]
Crystal Data for C7H6BF3KNO2 (M =243.04 g/mol): monoclinic, space group P21/c (no. 14), a = 17.517(13) Å, b = 6.924(5) Å, c = 7.458(6) Å, β = 97.957(16)°, V = 895.9(11) Å3, Z = 4, T = 100.0(1) K, μ(MoKα) = 0.616 mm-1, Dcalc = 1.802 g/cm3, 7041 reflections measured (4.696° ≤ 2Θ ≤ 55.078°), 2053 unique (Rint = 0.0969, Rsigma = 0.1060) which were used in all calculations. The final R1 was 0.0565 (I > 2σ(I)) and wR2 was 0.1284 (all data).
Refinement model description
Number of restraints - 30, 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. Rigid body (RIGU) restrains
O1, C1, C2, C6, N1, C3
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
C3(H3), C5(H5), C6(H6)
3.b Idealised Me refined as rotating group:
C7(H7A,H7B,H7C)
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.