Poly[[tetra-μ2-aqua-diaqua-μ2-2,5-dibenzoyl­terephthalato­dipotassium(I)] dihydrate]

Wang, D.-D.; Zhu, H.-J.; Shan, N.; Song, G.-L.; Wang, J.-T.

doi:10.1107/S1600536805042819

Poly[[tetra-μ₂-aqua-diaqua-μ₂-2,5-dibenzoylterephthalatodipotassium(I)] dihydrate]

D.-D. Wang, H.-J. Zhu, N. Shan, G.-L. Song and J.-T. Wang

The title compound, {[K₂(C₂₂H₁₂O₆)(H₂O)₆]·2H₂O}_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.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805042819/sj6185sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536805042819/sj6185Isup2.hkl Contains datablock I

CCDC reference: 298543

checkCIF report

Key indicators

Single-crystal X-ray study
T = 180 K
Mean (C-C) = 0.002 Å
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

Computing details top

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-µ₂-aqua-diaqua-µ₂-2,5-dibenzoylterephthalato dipotassium(I)] dihydrate] top

Crystal data top

[K₂(C₂₂H₁₂O₆)(H₂O)₆]·2H₂O	Z = 1
M_r = 297.32	F(000) = 310.0
Triclinic, P1	D_x = 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	R_int = 0.031
φ and ω scans	θ_max = 31.1°, θ_min = 1.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 2002)	h = −8→8
T_min = 0.827, T_max = 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(F_o²) + (0.0578P)² + 0.4465P] where P = (F_o² + 2F_c²)/3
3699 reflections	(Δ/σ)_max < 0.001
205 parameters	Δρ_max = 0.37 e Å⁻³
0 restraints	Δρ_min = −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	U_iso*/U_eq
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—C2^v	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—K1^iv	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—K1^iv	3.5186 (17)	C2—C3^v	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—K1^iv	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—K1^iv	89.12 (9)
O6—K1—O5	152.23 (4)	O2—C1—K1^iv	50.76 (8)
O3—K1—O5	73.10 (4)	C2—C1—K1^iv	134.37 (9)
O2ⁱⁱ—K1—O5	81.34 (4)	C4—C3—C2^v	121.53 (12)
O6ⁱⁱⁱ—K1—O5	72.33 (4)	C4—C3—H3A	119.2
O4—K1—C11	68.81 (4)	C2^v—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)	C3^v—C2—C4	118.51 (12)
O2ⁱⁱ—K1—H5B2	66.1 (6)	C3^v—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···O5^vi	0.86 (4)	1.93 (4)	2.772 (2)	166 (3)
O4—H4B2···O7^vii	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···O5^vii	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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Poly[[tetra-μ2-aqua-diaqua-μ2-2,5-dibenzoyl­terephthalato­dipotassium(I)] dihydrate]

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Poly[[tetra-μ₂-aqua-diaqua-μ₂-2,5-dibenzoylterephthalatodipotassium(I)] dihydrate]