jb120221_1_1

Table 1 Crystal data and structure refinement for jb120221_1_1.
Identification code jb120221_1_1
Empirical formula C6H3BClF3KNO
Formula weight 247.45
Temperature/K 100.0(1)
Crystal system monoclinic
Space group C2/c
a/Å 34.02(3)
b/Å 7.073(7)
c/Å 7.323(7)
α/° 90
β/° 90.209(15)
γ/° 90
Volume/Å3 1762(3)
Z 8
ρcalcg/cm3 1.866
μ/mm‑1 0.913
F(000) 976.0
Crystal size/mm3 0.32 × 0.04 × 0.03
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.79 to 55.108
Index ranges -44 ≤ h ≤ 44, -9 ≤ k ≤ 6, -9 ≤ l ≤ 9
Reflections collected 7115
Independent reflections 2029 [Rint = 0.0999, Rsigma = 0.0931]
Data/restraints/parameters 2029/0/127
Goodness-of-fit on F2 1.000
Final R indexes [I>=2σ (I)] R1 = 0.0545, wR2 = 0.1099
Final R indexes [all data] R1 = 0.1028, wR2 = 0.1268
Largest diff. peak/hole / e Å-3 0.63/-0.60

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for jb120221_1_1. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
K17070.3(3)1340.9(12)1207.5(11)15.4(2)
Cl15215.6(4)2827(2)9976(2)53.6(5)
F17203.8(6)2381(3)7611(3)17.0(5)
F26964.0(6)2128(3)4694(3)16.3(5)
F37239.2(7)4904(3)5678(3)20.4(5)
O16473.7(9)5771(4)6721(4)21.6(7)
N16380.6(10)898(5)7689(4)17.1(7)
C15656.6(13)2095(7)9018(6)26.1(10)
C25751.8(12)183(6)9051(6)22.2(10)
C36116.0(13)-318(6)8376(5)20.0(9)
C46272.6(12)2737(6)7635(5)16.7(8)
C55912.5(12)3378(6)8277(6)23.7(10)
C66573.5(12)4099(6)6849(5)16.3(9)
B17003.9(13)3360(6)6188(6)14.9(9)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for jb120221_1_1. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
K128.5(5)8.1(4)9.7(3)-0.8(4)2.8(3)-0.9(4)
Cl137.9(7)29.0(7)94.1(13)1.9(8)35.0(8)6.0(6)
F127.6(12)14.0(13)9.4(11)0.8(9)-1.5(9)3.5(10)
F229.2(13)11.4(12)8.4(11)-3.6(9)0.6(9)0.0(10)
F331.5(13)9.9(12)19.9(12)1.7(10)5.1(10)-1.7(10)
O133.9(17)9.3(15)21.7(15)1.1(12)1.6(12)2.9(13)
N129.2(19)9.5(18)12.7(16)2.3(14)2.7(13)2.0(15)
C128(2)23(3)28(2)-2(2)6.4(18)3(2)
C227(2)16(2)23(2)-1.2(19)3.8(17)-4.8(19)
C333(2)11(2)16(2)2.1(17)1.4(17)-0.6(19)
C426(2)12(2)12.4(19)1.5(16)-3.4(15)1.0(17)
C531(2)13(2)28(2)-1.8(18)2.2(18)3.1(19)
C629(2)11(2)9.4(17)-2.8(16)-0.5(15)0.8(17)
B127(2)10(2)8.1(18)-0.4(18)-0.9(17)-0.3(19)

 

Table 4 Bond Lengths for jb120221_1_1.
AtomAtomLength/Å AtomAtomLength/Å
K1K113.795(3) F1B11.422(5)
K1K124.123(3) F2B11.405(5)
K1F122.862(4) F3B11.406(5)
K1F132.773(3) O1C61.234(5)
K1F142.766(3) N1C31.344(5)
K1F222.716(3) N1C41.352(5)
K1F352.912(3) C1C21.391(6)
K1F362.745(4) C1C51.371(6)
K1F343.384(3) C2C31.382(6)
K1O162.905(4) C4C51.390(6)
K1N123.034(4) C4C61.520(6)
K1B123.333(6) C6B11.630(6)
Cl1C11.738(5)    

13/2-X,1/2-Y,-Z; 2+X,-Y,-1/2+Z; 3+X,+Y,-1+Z; 43/2-X,1/2-Y,1-Z; 53/2-X,-1/2+Y,1/2-Z; 6+X,1-Y,-1/2+Z

 

Table 5 Bond Angles for jb120221_1_1.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
K11K1K1277.44(5) O16K1K12116.14(7)
F13K1K1243.81(7) O16K1K11107.24(9)
F14K1K12115.17(5) O16K1F35150.68(8)
F13K1K1146.67(5) O16K1F34125.40(8)
F12K1K1283.98(8) O16K1N1277.23(11)
F14K1K1146.84(7) O16K1B12130.89(11)
F12K1K11116.31(7) N12K1K1294.58(8)
F14K1F1393.51(8) N12K1K11171.92(7)
F13K1F12123.97(7) N12K1F3499.15(10)
F14K1F1292.75(7) N12K1B1255.14(10)
F13K1F34126.38(8) B12K1K1262.44(9)
F13K1F3560.47(7) B12K1K11118.78(9)
F12K1F3453.83(6) B12K1F3477.89(9)
F14K1F3562.72(9) K14F1K1786.49(7)
F14K1F3442.05(7) K14F1K18123.60(8)
F12K1F3573.85(8) K17F1K1894.05(8)
F13K1O1693.05(8) B1F1K1896.3(2)
F14K1O16110.69(10) B1F1K14119.6(2)
F12K1O16135.27(9) B1F1K17138.2(2)
F12K1N1260.89(9) B1F2K18103.3(2)
F14K1N12138.55(9) K19F3K14107.56(8)
F13K1N12127.40(8) K110F3K1481.44(9)
F14K1B12112.83(10) K19F3K11084.20(8)
F13K1B12105.78(9) B1F3K19126.5(2)
F12K1B1225.10(9) B1F3K1490.8(2)
F22K1K1238.97(5) B1F3K110149.1(2)
F22K1K11107.57(7) C6O1K19119.4(3)
F22K1F1382.77(9) C3N1K18108.7(3)
F22K1F1248.41(8) C3N1C4116.3(4)
F22K1F14122.71(7) C4N1K18134.6(3)
F22K1F3566.27(8) C2C1Cl1119.0(3)
F22K1F3497.53(8) C5C1Cl1120.9(4)
F22K1F36147.57(8) C5C1C2120.1(4)
F22K1O16126.58(9) C3C2C1116.9(4)
F22K1N1264.69(9) N1C3C2125.0(4)
F22K1B1224.22(9) N1C4C5122.9(4)
F36K1K1149.77(5) N1C4C6115.9(3)
F34K1K1183.82(8) C5C4C6121.1(4)
F34K1K12118.45(7) C1C5C4118.7(4)
F36K1K12108.60(7) O1C6C4116.8(4)
F35K1K1146.03(7) O1C6B1122.2(4)
F35K1K1254.26(6) C4C6B1121.1(3)
F36K1F1462.66(7) F1B1K1858.60(18)
F36K1F1364.80(7) F1B1C6111.5(3)
F36K1F12155.19(8) F2B1K1852.48(18)
F36K1F3595.80(8) F2B1F1108.3(3)
F35K1F3470.71(8) F2B1F3109.2(3)
F36K1F34101.64(6) F2B1C6110.3(3)
F36K1O1658.99(9) F3B1K18137.5(3)
F35K1N12127.84(10) F3B1F1107.5(3)
F36K1N12135.88(9) F3B1C6110.0(3)
F36K1B12168.20(10) C6B1K18112.3(2)
F35K1B1272.81(10)     

13/2-X,1/2-Y,-Z; 2+X,-Y,-1/2+Z; 3+X,+Y,-1+Z; 43/2-X,1/2-Y,1-Z; 53/2-X,-1/2+Y,1/2-Z; 6+X,1-Y,-1/2+Z; 7+X,+Y,1+Z; 8+X,-Y,1/2+Z; 9+X,1-Y,1/2+Z; 103/2-X,1/2+Y,1/2-Z

 

Table 6 Torsion Angles for jb120221_1_1.
ABCDAngle/˚ ABCDAngle/˚
K11F1B1K12134.69(19) K14O1C6B1-17.5(5)
K13F1B1K12-103.3(3) K12N1C3C2-175.2(3)
K12F1B1F2-17.7(3) K12N1C4C5172.9(3)
K13F1B1F2-121.0(3) K12N1C4C6-8.0(5)
K11F1B1F2117.0(3) Cl1C1C2C3-176.1(3)
K11F1B1F3-0.8(4) Cl1C1C5C4175.8(3)
K13F1B1F3121.2(3) O1C6B1K12-170.8(3)
K12F1B1F3-135.5(3) O1C6B1F1125.6(4)
K11F1B1C6-121.5(3) O1C6B1F2-114.1(4)
K12F1B1C6103.8(3) O1C6B1F36.4(5)
K13F1B1C60.5(5) N1C4C5C10.8(6)
K12F2B1F119.1(3) N1C4C6O1177.1(4)
K12F2B1F3135.9(3) N1C4C6B1-2.1(5)
K12F2B1C6-103.1(3) C1C2C3N1-0.4(6)
K14F3B1K12-174.42(18) C2C1C5C4-2.6(7)
K15F3B1K1212.8(7) C3N1C4C51.1(6)
K11F3B1K12-61.8(3) C3N1C4C6-179.8(3)
K14F3B1F1-112.1(3) C4N1C3C2-1.4(6)
K11F3B1F10.6(3) C4C6B1K128.3(4)
K15F3B1F175.1(5) C4C6B1F1-55.3(5)
K14F3B1F2130.7(2) C4C6B1F265.0(4)
K15F3B1F2-42.2(6) C4C6B1F3-174.5(3)
K11F3B1F2-116.7(3) C5C1C2C32.4(7)
K15F3B1C6-163.3(3) C5C4C6O1-3.8(6)
K14F3B1C69.5(4) C5C4C6B1177.0(4)
K11F3B1C6122.2(3) C6C4C5C1-178.2(4)
K14O1C6C4163.3(2)      

13/2-X,1/2-Y,1-Z; 2+X,-Y,1/2+Z; 3+X,+Y,1+Z; 4+X,1-Y,1/2+Z; 53/2-X,1/2+Y,1/2-Z

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for jb120221_1_1.
AtomxyzU(eq)
H25574.69-735.539515.4627
H36184.44-1619.398399.5124
H55844.954678.818203.0628

Experimental

Single crystals of C6H3BClF3KNO [jb120221_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 [jb120221_1_1]

Crystal Data for C6H3BClF3KNO (=247.45 g/mol): monoclinic, space group C2/c (no. 15), a = 34.02(3) Å, b = 7.073(7) Å, c = 7.323(7) Å, β = 90.209(15)°, = 1762(3) Å3, Z = 8, T = 100.0(1) K, μ(MoKα) = 0.913 mm-1, Dcalc = 1.866 g/cm3, 7115 reflections measured (4.79° ≤ 2Θ ≤ 55.108°), 2029 unique (Rint = 0.0999, Rsigma = 0.0931) which were used in all calculations. The final R1 was 0.0545 (I > 2σ(I)) and wR2 was 0.1268 (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
2.a Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C5(H5)

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