Thermal vibrations in potassium 3-benzoyl-2-thiophenecarboxylate

The atomic thermal displacement parameters at 293 K for the anion in the title salt have been analyzed in terms of a body having two rigid segments, namely the benzoyl and the 2-thiophenecarboxylate groups. These segments are each nearly planar and have a dihedral angle of 80.1° between them. The internal torsional libration of the anion is physically correlated with its overall external translational and librational motion. Bond distances involving the heavier atoms have an s.u. σ from 0.002 to 0.003 Å while librational corrections in these distances range up to 4σ. A short nonbonded intersegment C...O distance of 2.817 (2) Å becomes 2.831 Å after correction, the correction being 7σ. An intermolecular S...O distance of 3.1891 (14) Å becomes 3.215 Å after correction for independent vibration of the two molecules, the correction being 18σ.

Computing details

Data collection: CAD4(Enraf-Nonius); cell refinement: CAD4(Enraf-Nonius); data reduction: xtal_DIFDAT_ABSORB_SORTRF_ADDREF; program(s) used to solve structure: Xtal; program(s) used to refine structure: xtal_CRYLSQ; molecular graphics: Xtal; software used to prepare material for publication: xtal_BONDLA_CIFIO.

Potassium 3-benzoylthiophene-2-carboxylate

Crystal data

K^+.C12H7O3S^−	F(000) = 1104
Mr = 270.1	Dx = 1.589 Mg m^−3
Orthorhombic, Pbca	Cu Kα radiation, λ = 1.5418 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 22 reflections
a = 10.760 (1) Å	θ = 26.0–30.0°
b = 7.740 (1) Å	µ = 5.79 mm^−1
c = 27.145 (3) Å	T = 293 K
V = 2260.7 (4) Å^3	All faces of forms {001} and {111}, pale yellow
Z = 8	0.37 × 0.37 × 0.31 mm

Data collection

CAD4 diffractometer	2014 reflections with refl_observed_if_F____ > _1.0_σ(F___)
Radiation source: AEG fine focus Cu anode	Rint = 0.027
Ni filter monochromator	θmax = 69.9°, θmin = 3.3°
Peak/background in ω /2θ scan	h = −13→13
Absorption correction: analytical integration Method of Alcock (1974)	k = 0→9
Tmin = 0.274, Tmax = 0.426	l = 0→32
4158 measured reflections	3 standard reflections every 50 min
2141 independent reflections	intensity decay: 1%

Refinement

Refinement on F	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Hydrogen site location: difference Fourier
R[F^2 > 2σ(F^2)] = 0.032	H-atom parameters not defined?
wR(F^2) = 0.037	w = σ^-2(F); σ^-2(I) = σ^-2exp + 0.02I^2
S = 2.49	(Δ/σ)max = 0.0003
2014 reflections	Δρmax = 0.26 e Å^−3
183 parameters	Δρmin = −0.33 e Å^−3
0 restraints	Extinction correction: Becker-Coppens
0 constraints	Extinction coefficient: 22 (4) x 10^4 rad^-1

Special details

Geometry. See Text for corrected distances

Refinement. Two complete octants merged

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
K	0.33560 (4)	0.02464 (5)	−0.042742 (15)	0.0386 (2)
S1	0.37341 (4)	0.65858 (6)	0.058823 (19)	0.0398 (2)
C1	0.41217 (15)	0.3135 (2)	0.03443 (6)	0.0313 (8)
C2	0.43791 (14)	0.4598 (2)	0.06870 (7)	0.0294 (8)
C3	0.51328 (15)	0.4623 (2)	0.10929 (6)	0.0299 (8)
C4	0.51837 (18)	0.6268 (2)	0.13223 (8)	0.0402 (10)
C5	0.44638 (19)	0.7447 (2)	0.10861 (9)	0.0449 (11)
O1	0.46176 (12)	0.17154 (16)	0.04483 (5)	0.0401 (7)
O2	0.34303 (11)	0.34482 (18)	−0.00136 (5)	0.0398 (7)
C6	0.58073 (16)	0.3088 (2)	0.12859 (7)	0.0334 (9)
O3	0.69051 (13)	0.2868 (2)	0.11966 (7)	0.0580 (10)
C7	0.51255 (16)	0.1899 (2)	0.16245 (6)	0.0312 (8)
C8	0.5787 (2)	0.0727 (3)	0.19097 (8)	0.0418 (10)
C9	0.5170 (2)	−0.0329 (3)	0.22375 (8)	0.0526 (13)
C10	0.3893 (2)	−0.0253 (3)	0.22773 (9)	0.0522 (13)
C11	0.3228 (2)	0.0880 (3)	0.19922 (8)	0.0463 (11)
C12	0.38375 (17)	0.1966 (2)	0.16683 (7)	0.0358 (9)
H4	0.567 (2)	0.650 (3)	0.1617 (10)	0.061 (7)*
H5	0.441 (2)	0.866 (4)	0.1157 (11)	0.072 (8)*
H8	0.665 (2)	0.066 (3)	0.1865 (9)	0.043 (6)*
H9	0.561 (2)	−0.101 (3)	0.2466 (11)	0.064 (7)*
H10	0.346 (2)	−0.095 (4)	0.2506 (12)	0.073 (8)*
H11	0.238 (2)	0.081 (3)	0.2027 (9)	0.057 (7)*
H12	0.340 (2)	0.279 (3)	0.1473 (8)	0.041 (6)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
K	0.0389 (2)	0.0372 (2)	0.0397 (2)	0.00077 (16)	0.00232 (15)	−0.00196 (16)
S1	0.0401 (2)	0.0358 (2)	0.0436 (3)	0.00701 (18)	0.00028 (19)	0.0082 (2)
C1	0.0297 (8)	0.0362 (9)	0.0282 (8)	−0.0011 (7)	0.0022 (6)	0.0003 (7)
C2	0.0295 (8)	0.0298 (8)	0.0288 (9)	0.0009 (6)	0.0028 (6)	0.0025 (6)
C3	0.0302 (8)	0.0306 (8)	0.0289 (8)	−0.0021 (6)	0.0021 (6)	0.0009 (7)
C4	0.0435 (10)	0.0364 (9)	0.0408 (11)	−0.0023 (8)	−0.0019 (8)	−0.0070 (8)
C5	0.0482 (11)	0.0308 (9)	0.0557 (13)	0.0006 (8)	0.0063 (9)	−0.0042 (9)
O1	0.0474 (7)	0.0349 (6)	0.0379 (7)	0.0077 (5)	−0.0034 (5)	−0.0028 (5)
O2	0.0398 (6)	0.0467 (7)	0.0329 (7)	0.0002 (6)	−0.0071 (5)	0.0005 (6)
C6	0.0337 (8)	0.0355 (9)	0.0311 (9)	0.0025 (7)	−0.0030 (7)	−0.0011 (7)
O3	0.0324 (7)	0.0682 (10)	0.0733 (12)	0.0094 (6)	0.0074 (7)	0.0209 (9)
C7	0.0396 (9)	0.0284 (8)	0.0256 (8)	0.0017 (7)	−0.0033 (7)	−0.0043 (6)
C8	0.0499 (11)	0.0379 (9)	0.0375 (11)	0.0052 (8)	−0.0107 (8)	0.0013 (8)
C9	0.0792 (16)	0.0409 (11)	0.0376 (12)	0.0036 (10)	−0.0140 (10)	0.0104 (9)
C10	0.0771 (15)	0.0413 (11)	0.0382 (12)	−0.0100 (10)	0.0062 (10)	0.0056 (9)
C11	0.0528 (12)	0.0433 (11)	0.0427 (12)	−0.0074 (9)	0.0071 (9)	0.0009 (9)
C12	0.0409 (9)	0.0341 (9)	0.0324 (9)	0.0018 (7)	0.0010 (7)	0.0002 (7)

Geometric parameters (Å, º)

K—O1	2.9642 (14)	C6—O3	1.218 (2)
K—O2	2.7220 (15)	C6—C7	1.493 (2)
S1—C2	1.7091 (17)	C7—C8	1.389 (3)
S1—C5	1.699 (2)	C7—C12	1.392 (3)
C1—C2	1.492 (2)	C8—C9	1.379 (3)
C1—O1	1.253 (2)	C8—H8	0.94 (2)
C1—O2	1.247 (2)	C9—C10	1.380 (4)
C2—C3	1.368 (2)	C9—H9	0.94 (3)
C3—C4	1.418 (3)	C10—C11	1.371 (3)
C3—C6	1.488 (2)	C10—H10	0.95 (3)
C4—C5	1.358 (3)	C11—C12	1.382 (3)
C4—H4	0.97 (3)	C11—H11	0.92 (2)
C5—H5	0.96 (3)	C12—H12	0.95 (2)
O1—K—O2	46.0 (1)	O3—C6—C7	120.9 (2)
C2—S1—C5	92.3 (1)	C6—C7—C8	119.6 (2)
C2—C1—O1	116.5 (2)	C6—C7—C12	121.3 (2)
C2—C1—O2	116.7 (2)	C8—C7—C12	119.1 (2)
O1—C1—O2	126.9 (2)	C7—C8—C9	120.0 (2)
S1—C2—C1	120.7 (1)	C7—C8—H8	118 (2)
S1—C2—C3	110.7 (1)	C9—C8—H8	122 (2)
C1—C2—C3	128.5 (2)	C8—C9—C10	120.4 (2)
C2—C3—C4	112.9 (2)	C8—C9—H9	120.8 (2)
C2—C3—C6	124.1 (2)	C10—C9—H9	118 (2)
C4—C3—C6	122.9 (2)	C9—C10—C11	120.2 (2)
C3—C4—C5	112.0 (2)	C9—C10—H10	121 (2)
C3—C4—H4	123.3 (9)	C11—C10—H10	119 (2)
C5—C4—H4	124.7 (9)	C10—C11—C12	120.0 (2)
S1—C5—C4	112.1 (2)	C10—C11—H11	115 (2)
S1—C5—H5	121.0 (9)	C12—C11—H11	125 (2)
C4—C5—H5	126.7 (9)	C7—C12—C11	120.3 (2)
C3—C6—O3	121.0 (2)	C7—C12—H12	118 (2)
C3—C6—C7	118.0 (2)	C11—C12—H12	122 (2)
S1—C2—C1—O2	0.6 (2)	C2—C3—C6—C7	−84.7 (2)