jb250221_1_1

Table 1 Crystal data and structure refinement for jb250221_1_1.
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

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for jb250221_1_1. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
K1829.6(5)1223.9(13)1515.5(11)14.2(2)
F3583.8(12)4924(3)2741(3)15.7(5)
F21063.5(12)4667(3)56(3)16.5(5)
F1482.9(12)7464(4)780(3)18.7(6)
O11970.4(15)8481(4)2289(4)16.8(6)
O24318.6(16)5591(5)6088(4)23.1(7)
N12193.9(18)3602(5)3545(4)14.2(7)
C43618(2)5027(7)5206(5)16.7(9)
C11795(2)6774(6)2396(5)12.6(9)
C22392(2)5455(6)3422(5)12.2(8)
C33092(2)6226(7)4196(5)16.2(8)
C53425(2)3102(7)5349(5)19.6(10)
C62720(2)2452(7)4498(5)18.4(9)
C74530(2)7573(8)5862(6)25.5(11)
B1959(3)5949(7)1476(6)14.1(10)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for jb250221_1_1. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
K122.6(5)10.6(4)9.4(4)0.7(4)1.8(3)-0.7(4)
F323.8(13)15.0(14)9.3(11)0.5(9)6.0(9)-2.0(10)
F225.9(13)15.1(14)9.1(12)-1.1(10)4.4(10)-1.5(10)
F125.9(14)12.5(13)16.1(12)1.6(10)-2.4(10)0.0(11)
O123.1(15)9.7(16)17.5(14)1.8(12)2.4(12)-0.4(12)
O221.7(16)28(2)18.3(16)1.9(13)-3.2(12)-1.9(13)
N120.3(17)14.5(18)7.5(15)-0.2(14)1.3(13)1.7(14)
C419(2)22(3)9.4(19)1.3(17)3.7(16)1.4(18)
C119(2)14(2)6.4(18)0.4(15)6.4(16)0.9(16)
C218(2)16(2)3.0(17)1.4(15)5.0(14)1.2(16)
C324(2)15(2)11.5(18)0.3(18)6.9(15)-0.2(18)
C523(2)22(3)13(2)5.9(18)0.9(18)6.4(18)
C629(2)16(2)11(2)3.5(17)5.5(17)6.0(19)
C727(3)34(3)15(2)1(2)1.2(18)-6(2)
B122(3)13(3)8(2)-0.7(18)5.7(19)1.7(19)

 

Table 4 Bond Lengths for jb250221_1_1.
AtomAtomLength/Å AtomAtomLength/Å
K1K113.823(2) F2B11.413(5)
K1F32.773(3) F1B11.395(5)
K1F322.762(3) O1C11.227(5)
K1F332.900(3) O2C41.367(5)
K1F22.676(3) O2C71.437(6)
K1F242.687(3) N1C21.336(5)
K1F152.820(3) N1C61.344(5)
K1F123.373(3) C4C31.384(6)
K1F162.712(3) C4C51.383(6)
K1O162.759(3) C1C21.514(5)
K1N13.117(4) C1B11.631(6)
K1C163.532(5) C2C31.387(5)
F3B11.413(5) C5C61.383(6)

1-X,-Y,-Z; 2-X,-1/2+Y,1/2-Z; 3+X,1/2-Y,-1/2+Z; 4+X,1/2-Y,1/2+Z; 5-X,1-Y,-Z; 6+X,-1+Y,+Z

 

Table 5 Bond Angles for jb250221_1_1.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
F31K1K1249.07(6) O15K1K12106.73(9)
F33K1K1246.03(5) O15K1F31112.15(9)
F3K1K12117.67(7) O15K1F3135.06(8)
F31K1F3395.10(6) O15K1F3391.17(8)
F3K1F33124.34(7) O15K1F11125.74(8)
F31K1F392.90(6) O15K1F14148.72(8)
F31K1F1463.18(8) O15K1N177.15(10)
F3K1F1475.63(7) O15K1C1517.56(8)
F33K1F11128.94(7) N1K1K12172.18(7)
F31K1F1142.15(7) N1K1F1196.62(9)
F3K1F1154.41(6) N1K1C1593.18(11)
F3K1N159.70(8) C15K1K1291.62(9)
F33K1N1128.12(8) K17F3K1123.48(8)
F31K1N1136.31(9) K17F3K1684.90(6)
F33K1C1586.81(8) K1F3K1693.31(8)
F31K1C1595.60(9) B1F3K197.8(2)
F3K1C15146.79(8) B1F3K16139.9(2)
F2K1K12107.52(7) B1F3K17118.9(2)
F26K1K12118.64(7) K1F2K13100.61(9)
F26K1F33150.82(8) B1F2K13149.6(2)
F2K1F31124.34(7) B1F2K1102.2(2)
F26K1F3175.33(7) K14F1K1783.06(8)
F26K1F384.13(8) K18F1K1487.39(8)
F2K1F349.50(8) K18F1K17105.99(8)
F2K1F3381.93(8) B1F1K1790.5(2)
F2K1F26126.39(7) B1F1K18122.7(2)
F2K1F1199.90(8) B1F1K14149.7(2)
F2K1F1467.90(7) C1O1K18119.7(3)
F2K1F15144.64(8) C4O2C7116.4(3)
F26K1F1159.64(7) C2N1K1131.5(2)
F26K1F1588.73(8) C2N1C6116.1(4)
F26K1F14132.15(7) C6N1K1111.6(3)
F2K1O15123.44(9) O2C4C3125.2(4)
F26K1O1568.22(8) O2C4C5116.8(4)
F2K1N164.95(9) C5C4C3118.0(4)
F26K1N169.00(8) O1C1K1842.7(2)
F26K1C1567.24(8) O1C1C2116.9(4)
F2K1C15139.17(9) O1C1B1121.9(4)
F14K1K1245.13(7) C2C1K18154.1(3)
F11K1K1286.63(7) C2C1B1121.2(4)
F15K1K1247.48(5) B1C1K1881.3(2)
F14K1F3359.99(7) N1C2C1116.5(3)
F15K1F3155.88(7) N1C2C3124.3(4)
F15K1F3162.99(7) C3C2C1119.1(4)
F15K1F3362.71(7) C4C3C2118.6(4)
F14K1F1173.45(7) C6C5C4119.3(4)
F15K1F11102.31(6) N1C6C5123.6(4)
F15K1F1492.61(8) F3B1C1111.6(3)
F15K1O1561.12(9) F2B1F3107.8(3)
F15K1N1137.79(8) F2B1C1109.5(3)
F14K1N1129.09(10) F1B1F3108.4(3)
F14K1C15136.29(9) F1B1F2109.0(3)
F11K1C15117.34(8) F1B1C1110.4(4)
F15K1C1544.62(9)     

1-X,-1/2+Y,1/2-Z; 2-X,-Y,-Z; 3+X,1/2-Y,-1/2+Z; 4-X,1-Y,-Z; 5+X,-1+Y,+Z; 6+X,1/2-Y,1/2+Z; 7-X,1/2+Y,1/2-Z; 8+X,1+Y,+Z

 

Table 6 Torsion Angles for jb250221_1_1.
ABCDAngle/˚ ABCDAngle/˚
K11F3B1F2119.8(3) K1N1C6C5172.1(3)
K1F3B1F215.1(3) K14C1C2N1146.8(4)
K12F3B1F2-120.3(3) K14C1C2C3-31.8(7)
K12F3B1F1-2.4(4) K14C1B1F3-113.3(3)
K11F3B1F1-122.3(3) K14C1B1F2127.5(3)
K1F3B1F1133.0(3) K14C1B1F17.4(3)
K12F3B1C1119.4(3) O1C1C2N1179.5(4)
K11F3B1C1-0.4(6) O1C1C2C30.8(5)
K1F3B1C1-105.2(3) O1C1B1F3-127.2(4)
K1F2B1F3-15.9(3) O1C1B1F2113.6(4)
K13F2B1F3122.0(4) O1C1B1F1-6.5(5)
K1F2B1F1-133.4(3) O2C4C3C2-178.1(3)
K13F2B1F14.5(6) O2C4C5C6179.5(3)
K1F2B1C1105.7(3) N1C2C3C4-1.7(6)
K13F2B1C1-116.3(4) C4C5C6N1-1.2(6)
K14F1B1F3111.1(3) C1C2C3C4176.8(3)
K12F1B1F31.7(3) C2N1C6C51.3(6)
K15F1B1F3-75.2(5) C2C1B1F353.0(5)
K14F1B1F2-131.8(2) C2C1B1F2-66.2(4)
K15F1B1F241.8(6) C2C1B1F1173.7(3)
K12F1B1F2118.8(3) C3C4C5C6-0.3(6)
K14F1B1C1-11.4(4) C5C4C3C21.7(5)
K15F1B1C1162.2(3) C6N1C2C1-178.4(3)
K12F1B1C1-120.9(3) C6N1C2C30.2(5)
K14O1C1C2-159.7(2) C7O2C4C3-3.1(5)
K14O1C1B120.5(5) C7O2C4C5177.2(4)
K1N1C2C113.1(5) B1C1C2N1-0.7(5)
K1N1C2C3-168.3(3) B1C1C2C3-179.4(3)

1+X,1/2-Y,1/2+Z; 2-X,1/2+Y,1/2-Z; 3+X,1/2-Y,-1/2+Z; 4+X,1+Y,+Z; 5-X,1-Y,-Z

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for jb250221_1_1.
AtomxyzU(eq)
H33206.847550.344035.6219
H53773.072233.716026.0124
H62601.811120.424590.4922
H7A4533.597842.014572.8338
H7B5044.217809.26525.5638
H7C4155.498420.116332.0438

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.

  1. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.
  2. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
  3. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.

Crystal structure determination of [jb250221_1_1]

Crystal Data for C7H6BF3KNO2 (=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)°, = 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)

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