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The title compound, {[K
2(C
22H
12O
6)(H
2O)
6]·2H
2O}
n, was prepared by slow evaporation of an aqueous solution of potassium dibenzoylterephthalate. The molecular complex contains two potassium cations, one 2,5-dibenzoylterephthalate anion, six coordinated water molecules and two uncoordinated water molecules. The 2,5-dibenzoylterephthalate anion lies on a center of symmetry. Each potassium cation is coordinated by seven O atoms, two from 2,5-dibenzoylterephthalate anions and the remainder from four bridging and one terminal water molecules. The uncoordinated water molecules are linked to the carboxylate O atoms and the coordinated water molecules by a network of intermolecular O—H
O hydrogen bonds, forming a layer structure.
Supporting information
CCDC reference: 298543
Key indicators
- Single-crystal X-ray study
- T = 180 K
- Mean (C-C) = 0.002 Å
Some non-H atoms missing
- R factor = 0.045
- wR factor = 0.119
- Data-to-parameter ratio = 18.0
checkCIF/PLATON results
No syntax errors found
Alert level A
ABSMU01_ALERT_1_A The ratio of given/expected absorption coefficient lies
outside the range 0.90 <> 1.10
Calculated value of mu = 0.857
Value of mu given = 0.428
CHEMW01_ALERT_1_A The ratio of given/expected molecular weight as calculated
from the _chemical_formula_sum lies outside
the range 0.90 <> 1.10
Calculated formula weight = 594.6508
Formula weight given = 297.3200
Alert level B
PLAT420_ALERT_2_B D-H Without Acceptor O6 - H6B1 ... ?
Alert level C
CHEMW01_ALERT_1_C The difference between the given and expected weight for
compound is greater 1 mass unit. Check that all hydrogen
atoms have been taken into account.
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT155_ALERT_4_C The Triclinic Unitcell is NOT Reduced .......... ?
PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.46 Ratio
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 8
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.48 Ratio
Alert level G
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: C22 H28 K2 O14
Atom count from _chemical_formula_moiety:C24 H26 O14
FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and the formula from the _atom_site* data.
Atom count from _chemical_formula_sum:C22 H28 K2 O14
Atom count from the _atom_site data: C11 H14 K1 O7
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G ALERT: Large difference may be due to a
symmetry error - see SYMMG tests
From the CIF: _cell_formula_units_Z 2
From the CIF: _chemical_formula_sum C22 H28 K2 O14
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
C 44.00 22.00 22.00
H 56.00 28.00 28.00
K 4.00 2.00 2.00
O 28.00 14.00 14.00
2 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
7 ALERT level C = Check and explain
4 ALERT level G = General alerts; check
8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2001); software used to prepare material for publication: SHELXTL.
Poly[[tetra-µ
2-aqua-diaqua-µ
2-2,5-dibenzoylterephthalato dipotassium(I)]
dihydrate]
top
Crystal data top
[K2(C22H12O6)(H2O)6]·2H2O | Z = 1 |
Mr = 297.32 | F(000) = 310.0 |
Triclinic, P1 | Dx = 1.492 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 6.153 (2) Å | Cell parameters from 3510 reflections |
b = 8.455 (3) Å | θ = 2.5–28.1° |
c = 13.769 (4) Å | µ = 0.43 mm−1 |
α = 69.441 (11)° | T = 180 K |
β = 79.673 (13)° | Plate, colorless |
γ = 87.265 (14)° | 0.46 × 0.40 × 0.18 mm |
V = 659.7 (4) Å3 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 3699 independent reflections |
Radiation source: fine-focus sealed tube | 3553 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
φ and ω scans | θmax = 31.1°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | h = −8→8 |
Tmin = 0.827, Tmax = 0.927 | k = −11→11 |
9790 measured reflections | l = −19→19 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.119 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0578P)2 + 0.4465P] where P = (Fo2 + 2Fc2)/3 |
3699 reflections | (Δ/σ)max < 0.001 |
205 parameters | Δρmax = 0.37 e Å−3 |
0 restraints | Δρmin = −0.47 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | −0.20943 (6) | −0.35876 (5) | −0.09249 (3) | 0.03384 (12) | |
O1 | 0.54096 (19) | 0.03835 (14) | −0.24719 (8) | 0.0263 (2) | |
O2 | 0.44209 (19) | −0.22953 (14) | −0.21387 (8) | 0.0273 (2) | |
O3 | 0.00604 (18) | −0.14597 (14) | −0.29777 (9) | 0.0266 (2) | |
O7 | 0.2059 (2) | 0.14606 (16) | −0.12166 (10) | 0.0327 (3) | |
O4 | 0.1771 (2) | −0.52350 (17) | −0.11663 (10) | 0.0324 (3) | |
H4B2 | 0.201 (4) | −0.615 (4) | −0.131 (2) | 0.050 (7)* | |
H4B1 | 0.274 (4) | −0.451 (3) | −0.160 (2) | 0.047 (7)* | |
C1 | 0.4886 (2) | −0.08000 (18) | −0.27434 (10) | 0.0209 (2) | |
C3 | 0.3440 (2) | −0.06656 (17) | −0.53632 (10) | 0.0201 (2) | |
H3A | 0.2370 | −0.1133 | −0.5609 | 0.024* | |
O5 | −0.2190 (2) | 0.0123 (2) | −0.09086 (10) | 0.0404 (3) | |
H5B2 | −0.287 (5) | 0.023 (4) | −0.144 (3) | 0.064 (8)* | |
H5B1 | −0.104 (5) | 0.054 (4) | −0.113 (2) | 0.061 (9)* | |
C4 | 0.3293 (2) | −0.10359 (16) | −0.42838 (10) | 0.0191 (2) | |
C5 | 0.1303 (2) | −0.20430 (17) | −0.35595 (10) | 0.0194 (2) | |
C6 | 0.0899 (2) | −0.37297 (17) | −0.36100 (11) | 0.0213 (3) | |
O6 | −0.3471 (3) | −0.69872 (18) | −0.00678 (11) | 0.0434 (3) | |
C11 | −0.1242 (2) | −0.44311 (19) | −0.32867 (12) | 0.0260 (3) | |
H11A | −0.2448 | −0.3790 | −0.3098 | 0.031* | |
C7 | 0.2668 (3) | −0.46689 (19) | −0.39006 (12) | 0.0258 (3) | |
H7A | 0.4112 | −0.4181 | −0.4141 | 0.031* | |
C10 | −0.1594 (3) | −0.6065 (2) | −0.32425 (14) | 0.0333 (3) | |
H10A | −0.3046 | −0.6539 | −0.3034 | 0.040* | |
C9 | 0.0185 (3) | −0.7012 (2) | −0.35041 (13) | 0.0328 (3) | |
H9A | −0.0058 | −0.8141 | −0.3455 | 0.039* | |
C8 | 0.2309 (3) | −0.6318 (2) | −0.38364 (13) | 0.0310 (3) | |
H8A | 0.3511 | −0.6967 | −0.4019 | 0.037* | |
C2 | 0.4877 (2) | −0.03769 (16) | −0.39079 (10) | 0.0189 (2) | |
H6B1 | −0.338 (5) | −0.748 (4) | 0.057 (3) | 0.059 (8)* | |
H6B2 | −0.297 (6) | −0.772 (5) | −0.034 (3) | 0.083 (11)* | |
H7B1 | 0.234 (5) | 0.102 (4) | −0.059 (3) | 0.060 (8)* | |
H7B2 | 0.306 (5) | 0.122 (3) | −0.160 (2) | 0.053 (7)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0368 (2) | 0.0338 (2) | 0.02366 (18) | 0.00491 (14) | −0.00168 (13) | −0.00347 (13) |
O1 | 0.0318 (5) | 0.0280 (5) | 0.0220 (5) | −0.0038 (4) | −0.0045 (4) | −0.0120 (4) |
O2 | 0.0341 (6) | 0.0243 (5) | 0.0193 (5) | −0.0046 (4) | −0.0036 (4) | −0.0023 (4) |
O3 | 0.0264 (5) | 0.0261 (5) | 0.0260 (5) | −0.0016 (4) | 0.0028 (4) | −0.0108 (4) |
O7 | 0.0349 (6) | 0.0365 (6) | 0.0265 (6) | 0.0036 (5) | −0.0041 (5) | −0.0121 (5) |
O4 | 0.0383 (6) | 0.0297 (6) | 0.0270 (6) | −0.0031 (5) | −0.0026 (5) | −0.0081 (5) |
C1 | 0.0217 (6) | 0.0235 (6) | 0.0168 (5) | −0.0003 (5) | −0.0021 (4) | −0.0068 (5) |
C3 | 0.0222 (6) | 0.0202 (6) | 0.0182 (6) | −0.0024 (5) | −0.0038 (5) | −0.0066 (5) |
O5 | 0.0361 (7) | 0.0581 (9) | 0.0240 (6) | −0.0095 (6) | −0.0066 (5) | −0.0087 (6) |
C4 | 0.0208 (6) | 0.0175 (6) | 0.0177 (6) | −0.0016 (4) | −0.0011 (4) | −0.0055 (4) |
C5 | 0.0203 (6) | 0.0202 (6) | 0.0159 (5) | −0.0021 (5) | −0.0021 (4) | −0.0044 (4) |
C6 | 0.0245 (6) | 0.0196 (6) | 0.0185 (6) | −0.0031 (5) | −0.0030 (5) | −0.0049 (5) |
O6 | 0.0621 (9) | 0.0354 (7) | 0.0279 (6) | 0.0006 (6) | 0.0016 (6) | −0.0098 (5) |
C11 | 0.0242 (7) | 0.0250 (7) | 0.0271 (7) | −0.0033 (5) | −0.0046 (5) | −0.0065 (5) |
C7 | 0.0285 (7) | 0.0236 (7) | 0.0235 (6) | −0.0019 (5) | −0.0007 (5) | −0.0076 (5) |
C10 | 0.0333 (8) | 0.0270 (7) | 0.0380 (8) | −0.0096 (6) | −0.0116 (6) | −0.0056 (6) |
C9 | 0.0480 (10) | 0.0210 (7) | 0.0314 (8) | −0.0043 (6) | −0.0131 (7) | −0.0081 (6) |
C8 | 0.0415 (9) | 0.0235 (7) | 0.0285 (7) | 0.0033 (6) | −0.0057 (6) | −0.0102 (6) |
C2 | 0.0222 (6) | 0.0177 (6) | 0.0166 (5) | −0.0009 (4) | −0.0025 (4) | −0.0059 (4) |
Geometric parameters (Å, º) top
K1—O4 | 2.7263 (16) | C3—C4 | 1.3938 (18) |
K1—O4i | 2.7375 (15) | C3—C2v | 1.3964 (18) |
K1—O6 | 2.8042 (18) | C3—H3A | 0.9500 |
K1—O3 | 2.8803 (14) | O5—H5B2 | 0.88 (3) |
K1—O2ii | 2.8918 (14) | O5—H5B1 | 0.77 (3) |
K1—O6iii | 2.9244 (19) | C4—C2 | 1.4010 (18) |
K1—O5 | 3.143 (2) | C4—C5 | 1.5113 (18) |
K1—C11 | 3.5129 (19) | C5—C6 | 1.4866 (19) |
K1—C1ii | 3.5186 (17) | C6—C7 | 1.400 (2) |
K1—K1i | 4.0406 (13) | C6—C11 | 1.401 (2) |
K1—K1iii | 4.2724 (15) | O6—K1iii | 2.9244 (19) |
K1—H5B2 | 3.09 (3) | O6—H6B1 | 0.84 (3) |
O1—C1 | 1.2574 (17) | O6—H6B2 | 0.84 (4) |
O2—C1 | 1.2583 (18) | C11—C10 | 1.387 (2) |
O2—K1iv | 2.8918 (14) | C11—H11A | 0.9500 |
O3—C5 | 1.2212 (17) | C7—C8 | 1.391 (2) |
O7—H7B1 | 0.86 (3) | C7—H7A | 0.9500 |
O7—H7B2 | 0.81 (3) | C10—C9 | 1.395 (3) |
O4—K1i | 2.7375 (15) | C10—H10A | 0.9500 |
O4—H4B2 | 0.86 (3) | C9—C8 | 1.390 (3) |
O4—H4B1 | 0.86 (3) | C9—H9A | 0.9500 |
C1—C2 | 1.5163 (19) | C8—H8A | 0.9500 |
C1—K1iv | 3.5186 (17) | C2—C3v | 1.3964 (18) |
| | | |
O4—K1—O4i | 84.62 (4) | C11—K1—H5B2 | 108.6 (6) |
O4—K1—O6 | 77.62 (5) | C1ii—K1—H5B2 | 50.2 (6) |
O4i—K1—O6 | 71.86 (4) | K1i—K1—H5B2 | 126.1 (6) |
O4—K1—O3 | 78.31 (4) | K1iii—K1—H5B2 | 110.4 (6) |
O4i—K1—O3 | 143.29 (4) | C1—O2—K1iv | 109.55 (9) |
O6—K1—O3 | 133.66 (4) | C5—O3—K1 | 121.36 (9) |
O4—K1—O2ii | 136.24 (4) | H7B1—O7—H7B2 | 107 (3) |
O4i—K1—O2ii | 135.96 (4) | K1—O4—K1i | 95.38 (4) |
O6—K1—O2ii | 97.85 (5) | K1—O4—H4B2 | 129.4 (17) |
O3—K1—O2ii | 74.11 (4) | K1i—O4—H4B2 | 100.3 (18) |
O4—K1—O6iii | 157.46 (4) | K1—O4—H4B1 | 107.9 (17) |
O4i—K1—O6iii | 77.76 (5) | K1i—O4—H4B1 | 118.1 (17) |
O6—K1—O6iii | 83.57 (5) | H4B2—O4—H4B1 | 106 (2) |
O3—K1—O6iii | 124.09 (4) | O1—C1—O2 | 125.72 (13) |
O2ii—K1—O6iii | 58.36 (4) | O1—C1—C2 | 116.39 (12) |
O4—K1—O5 | 121.85 (4) | O2—C1—C2 | 117.88 (12) |
O4i—K1—O5 | 89.35 (4) | O1—C1—K1iv | 89.12 (9) |
O6—K1—O5 | 152.23 (4) | O2—C1—K1iv | 50.76 (8) |
O3—K1—O5 | 73.10 (4) | C2—C1—K1iv | 134.37 (9) |
O2ii—K1—O5 | 81.34 (4) | C4—C3—C2v | 121.53 (12) |
O6iii—K1—O5 | 72.33 (4) | C4—C3—H3A | 119.2 |
O4—K1—C11 | 68.81 (4) | C2v—C3—H3A | 119.2 |
O4i—K1—C11 | 146.40 (4) | K1—O5—H5B2 | 78 (2) |
O6—K1—C11 | 82.32 (4) | K1—O5—H5B1 | 110 (2) |
O3—K1—C11 | 52.08 (4) | H5B2—O5—H5B1 | 108 (3) |
O2ii—K1—C11 | 67.45 (4) | C3—C4—C2 | 119.96 (12) |
O6iii—K1—C11 | 121.03 (4) | C3—C4—C5 | 117.87 (12) |
O5—K1—C11 | 121.77 (4) | C2—C4—C5 | 122.01 (12) |
O4—K1—C1ii | 132.54 (4) | O3—C5—C6 | 122.00 (12) |
O4i—K1—C1ii | 142.13 (4) | O3—C5—C4 | 120.55 (12) |
O6—K1—C1ii | 117.17 (5) | C6—C5—C4 | 117.43 (11) |
O3—K1—C1ii | 58.67 (4) | C7—C6—C11 | 120.01 (13) |
O2ii—K1—C1ii | 19.69 (3) | C7—C6—C5 | 120.26 (12) |
O6iii—K1—C1ii | 67.63 (4) | C11—C6—C5 | 119.55 (13) |
O5—K1—C1ii | 66.32 (4) | K1—O6—K1iii | 96.43 (5) |
C11—K1—C1ii | 69.18 (4) | K1—O6—H6B1 | 116 (2) |
O4—K1—K1i | 42.42 (3) | K1iii—O6—H6B1 | 80 (2) |
O4i—K1—K1i | 42.20 (3) | K1—O6—H6B2 | 123 (2) |
O6—K1—K1i | 69.17 (4) | K1iii—O6—H6B2 | 132 (2) |
O3—K1—K1i | 113.98 (4) | H6B1—O6—H6B2 | 102 (3) |
O2ii—K1—K1i | 167.00 (3) | C10—C11—C6 | 119.74 (15) |
O6iii—K1—K1i | 118.66 (4) | C10—C11—K1 | 118.72 (11) |
O5—K1—K1i | 110.39 (3) | C6—C11—K1 | 93.61 (9) |
C11—K1—K1i | 108.69 (3) | C10—C11—H11A | 120.1 |
C1ii—K1—K1i | 172.31 (3) | C6—C11—H11A | 120.1 |
O4—K1—K1iii | 119.44 (4) | K1—C11—H11A | 57.2 |
O4i—K1—K1iii | 69.54 (3) | C8—C7—C6 | 119.91 (14) |
O6—K1—K1iii | 42.86 (4) | C8—C7—H7A | 120.0 |
O3—K1—K1iii | 146.80 (3) | C6—C7—H7A | 120.0 |
O2ii—K1—K1iii | 74.37 (3) | C11—C10—C9 | 119.98 (15) |
O6iii—K1—K1iii | 40.71 (3) | C11—C10—H10A | 120.0 |
O5—K1—K1iii | 111.90 (3) | C9—C10—H10A | 120.0 |
C11—K1—K1iii | 105.37 (3) | C8—C9—C10 | 120.58 (14) |
C1ii—K1—K1iii | 92.25 (4) | C8—C9—H9A | 119.7 |
K1i—K1—K1iii | 95.44 (3) | C10—C9—H9A | 119.7 |
O4—K1—H5B2 | 129.0 (6) | C9—C8—C7 | 119.74 (15) |
O4i—K1—H5B2 | 104.0 (6) | C9—C8—H8A | 120.1 |
O6—K1—H5B2 | 153.1 (6) | C7—C8—H8A | 120.1 |
O3—K1—H5B2 | 65.0 (6) | C3v—C2—C4 | 118.51 (12) |
O2ii—K1—H5B2 | 66.1 (6) | C3v—C2—C1 | 118.71 (12) |
O6iii—K1—H5B2 | 69.7 (6) | C4—C2—C1 | 122.75 (12) |
O5—K1—H5B2 | 16.2 (6) | | |
Symmetry codes: (i) −x, −y−1, −z; (ii) x−1, y, z; (iii) −x−1, −y−1, −z; (iv) x+1, y, z; (v) −x+1, −y, −z−1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7B1···O5vi | 0.86 (4) | 1.93 (4) | 2.772 (2) | 166 (3) |
O4—H4B2···O7vii | 0.86 (3) | 1.98 (4) | 2.815 (2) | 163 (2) |
O4—H4B1···O2 | 0.86 (3) | 2.02 (3) | 2.810 (2) | 154 (2) |
O5—H5B2···O1ii | 0.88 (4) | 1.89 (4) | 2.764 (2) | 174 (4) |
O5—H5B1···O7 | 0.77 (3) | 2.06 (3) | 2.800 (2) | 162 (3) |
O7—H7B2···O1 | 0.80 (3) | 1.98 (3) | 2.778 (2) | 174 (3) |
O6—H6B2···O5vii | 0.84 (4) | 2.23 (4) | 3.067 (3) | 170 (4) |
Symmetry codes: (ii) x−1, y, z; (vi) −x, −y, −z; (vii) x, y−1, z. |
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