In the complex molecule of the title compound, [Zn(C
9H
5O
6)
2(H
2O)
4]·2H
2O, zinc(II) is six-coordinated by two O atoms from two monodentate 2,4-dicarboxybenzoate ligands and four O atoms from water molecules. The complex possesses a crystallographically imposed centre of symmetry. In the crystal packing, complex molecules and water molecules are connected by strong intermolecular O—H
O hydrogen bonds, resulting in an extended three-dimensional network. A zigzag chain of hydrogen-bonded water molecules running along the
c axis is observed.
Supporting information
CCDC reference: 298526
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.004 Å
- R factor = 0.033
- wR factor = 0.102
- Data-to-parameter ratio = 12.2
checkCIF/PLATON results
No syntax errors found
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
Tmin and Tmax reported: 0.556 0.691
Tmin(prime) and Tmax expected: 0.647 0.695
RR(prime) = 0.864
Please check that your absorption correction is appropriate.
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.85
PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 3
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.17 Ratio
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.03
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2
H2 O
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
9 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
3 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: RAPID-AUTO (Rigaku Corporation, 1998); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL/PC (Sheldrick, 1993); software used to prepare material for publication: SHELXL97-2 (Sheldrick, 1997).
Tetraaquabis(2,4-dicarboxybenzoato)zinc(II) dihydrate
top
Crystal data top
[Zn(C9H5O6)2(H2O)4]·2H2O | F(000) = 608 |
Mr = 591.73 | Dx = 1.730 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 8978 reflections |
a = 12.3211 (7) Å | θ = 2.4–27.5° |
b = 12.6398 (9) Å | µ = 1.17 mm−1 |
c = 7.5043 (5) Å | T = 293 K |
β = 103.597 (3)° | Block, colourless |
V = 1135.94 (13) Å3 | 0.36 × 0.35 × 0.31 mm |
Z = 2 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 2598 independent reflections |
Radiation source: fine-focus sealed tube | 1836 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.043 |
Oscillation scans | θmax = 27.5°, θmin = 1.7° |
Absorption correction: multi-scan (RAPID-AUTO; Rigaku Corporation, 1998) | h = −15→15 |
Tmin = 0.556, Tmax = 0.691 | k = −16→16 |
10257 measured reflections | l = −9→9 |
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)] = 0.033 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.102 | All H-atom parameters refined |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0564P)2] where P = (Fo2 + 2Fc2)/3 |
2598 reflections | (Δ/σ)max < 0.001 |
213 parameters | Δρmax = 0.48 e Å−3 |
3 restraints | Δρmin = −0.69 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 | |
Zn1 | 0.5000 | 0.5000 | 0.5000 | 0.02492 (14) | |
O1 | 0.36160 (15) | 0.45840 (16) | 0.6018 (3) | 0.0269 (4) | |
O8 | 0.59863 (19) | 0.54607 (19) | 0.7475 (3) | 0.0317 (5) | |
O3 | 0.37543 (16) | 0.29956 (17) | 0.9182 (3) | 0.0399 (5) | |
O7 | 0.54864 (19) | 0.34129 (17) | 0.5484 (4) | 0.0304 (5) | |
O4 | 0.23167 (19) | 0.19689 (18) | 0.9345 (4) | 0.0465 (7) | |
O5 | −0.1336 (2) | 0.31884 (18) | 0.8656 (4) | 0.0516 (7) | |
O2 | 0.39377 (17) | 0.55511 (19) | 0.8551 (3) | 0.0424 (6) | |
O6 | −0.18319 (17) | 0.48420 (18) | 0.7843 (4) | 0.0452 (6) | |
O9 | −0.33792 (19) | 0.3080 (2) | 0.9034 (3) | 0.0345 (5) | |
H5B | −0.028 (3) | 0.586 (3) | 0.696 (4) | 0.038 (9)* | |
H3 | 0.064 (2) | 0.289 (2) | 0.894 (4) | 0.023 (7)* | |
H6 | 0.154 (2) | 0.607 (3) | 0.676 (4) | 0.034 (9)* | |
H5A | −0.195 (4) | 0.316 (3) | 0.876 (6) | 0.073 (15)* | |
H8A | 0.659 (3) | 0.525 (3) | 0.776 (6) | 0.056 (13)* | |
H7A | 0.494 (3) | 0.309 (3) | 0.510 (6) | 0.061 (14)* | |
H9A | −0.348 (3) | 0.350 (3) | 0.970 (5) | 0.038 (11)* | |
H8B | 0.577 (3) | 0.553 (3) | 0.835 (4) | 0.062 (13)* | |
H9B | −0.354 (3) | 0.255 (2) | 0.938 (5) | 0.049 (12)* | |
H4 | 0.277 (3) | 0.154 (3) | 0.973 (6) | 0.059 (13)* | |
H7B | 0.576 (3) | 0.331 (3) | 0.648 (5) | 0.051 (13)* | |
C1 | 0.2202 (2) | 0.4668 (2) | 0.7677 (4) | 0.0233 (6) | |
C2 | 0.1916 (2) | 0.3703 (2) | 0.8343 (4) | 0.0239 (6) | |
C3 | 0.0818 (2) | 0.3538 (2) | 0.8461 (4) | 0.0286 (6) | |
C4 | 0.0023 (2) | 0.4316 (2) | 0.7952 (4) | 0.0269 (6) | |
C5 | 0.0307 (2) | 0.5276 (2) | 0.7304 (4) | 0.0313 (7) | |
C6 | 0.1392 (2) | 0.5447 (2) | 0.7177 (4) | 0.0299 (6) | |
C7 | 0.3357 (2) | 0.4947 (2) | 0.7447 (4) | 0.0247 (5) | |
C8 | 0.2762 (2) | 0.2862 (2) | 0.8986 (4) | 0.0266 (6) | |
C9 | −0.1144 (2) | 0.4148 (2) | 0.8128 (4) | 0.0316 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Zn1 | 0.0200 (2) | 0.0271 (2) | 0.0281 (2) | −0.00264 (19) | 0.00651 (17) | −0.0021 (2) |
O1 | 0.0229 (10) | 0.0316 (10) | 0.0292 (10) | −0.0050 (8) | 0.0122 (8) | −0.0068 (8) |
O8 | 0.0236 (11) | 0.0455 (13) | 0.0264 (11) | −0.0006 (10) | 0.0063 (9) | −0.0056 (10) |
O3 | 0.0219 (10) | 0.0339 (11) | 0.0638 (16) | 0.0064 (8) | 0.0097 (10) | 0.0114 (11) |
O7 | 0.0246 (11) | 0.0299 (11) | 0.0358 (13) | 0.0009 (9) | 0.0051 (10) | −0.0049 (10) |
O4 | 0.0309 (12) | 0.0290 (12) | 0.0827 (19) | 0.0077 (10) | 0.0194 (12) | 0.0193 (13) |
O5 | 0.0311 (13) | 0.0346 (13) | 0.098 (2) | −0.0020 (10) | 0.0325 (14) | 0.0049 (13) |
O2 | 0.0291 (11) | 0.0584 (14) | 0.0441 (13) | −0.0159 (11) | 0.0176 (10) | −0.0256 (12) |
O6 | 0.0211 (10) | 0.0484 (15) | 0.0681 (16) | 0.0099 (10) | 0.0144 (11) | 0.0142 (12) |
O9 | 0.0351 (12) | 0.0299 (12) | 0.0433 (14) | −0.0061 (10) | 0.0189 (10) | −0.0010 (11) |
C1 | 0.0204 (13) | 0.0276 (13) | 0.0229 (13) | −0.0016 (10) | 0.0074 (11) | −0.0028 (10) |
C2 | 0.0194 (13) | 0.0255 (13) | 0.0284 (14) | 0.0038 (10) | 0.0091 (11) | −0.0001 (11) |
C3 | 0.0229 (14) | 0.0269 (14) | 0.0384 (16) | 0.0000 (11) | 0.0117 (12) | 0.0035 (13) |
C4 | 0.0181 (12) | 0.0316 (15) | 0.0324 (15) | 0.0022 (11) | 0.0087 (11) | 0.0003 (12) |
C5 | 0.0238 (14) | 0.0297 (16) | 0.0410 (17) | 0.0076 (11) | 0.0087 (13) | 0.0044 (12) |
C6 | 0.0264 (15) | 0.0259 (14) | 0.0400 (17) | 0.0017 (12) | 0.0128 (13) | 0.0075 (14) |
C7 | 0.0193 (12) | 0.0268 (13) | 0.0293 (13) | 0.0005 (12) | 0.0086 (11) | 0.0008 (13) |
C8 | 0.0258 (14) | 0.0246 (13) | 0.0318 (15) | 0.0029 (11) | 0.0115 (12) | 0.0013 (11) |
C9 | 0.0200 (13) | 0.0398 (18) | 0.0355 (16) | 0.0002 (12) | 0.0078 (12) | 0.0002 (13) |
Geometric parameters (Å, º) top
Zn1—O8i | 2.050 (2) | O2—C7 | 1.226 (3) |
Zn1—O8 | 2.050 (2) | O6—C9 | 1.204 (3) |
Zn1—O1 | 2.0927 (17) | O9—H9A | 0.76 (4) |
Zn1—O1i | 2.0927 (17) | O9—H9B | 0.76 (2) |
Zn1—O7 | 2.101 (2) | C1—C6 | 1.388 (4) |
Zn1—O7i | 2.101 (2) | C1—C2 | 1.395 (4) |
O1—C7 | 1.274 (3) | C1—C7 | 1.515 (3) |
O8—H8A | 0.77 (4) | C2—C3 | 1.392 (4) |
O8—H8B | 0.77 (3) | C2—C8 | 1.488 (4) |
O3—C8 | 1.209 (3) | C3—C4 | 1.377 (4) |
O7—H7A | 0.78 (3) | C3—H3 | 0.93 (3) |
O7—H7B | 0.75 (4) | C4—C5 | 1.382 (4) |
O4—C8 | 1.310 (3) | C4—C9 | 1.490 (4) |
O4—H4 | 0.79 (4) | C5—C6 | 1.381 (4) |
O5—C9 | 1.314 (4) | C5—H5B | 1.02 (3) |
O5—H5A | 0.78 (4) | C6—H6 | 0.88 (3) |
| | | |
O8i—Zn1—O8 | 180.000 (1) | C6—C1—C7 | 116.1 (2) |
O8i—Zn1—O1 | 84.20 (8) | C2—C1—C7 | 124.5 (2) |
O8—Zn1—O1 | 95.80 (8) | C3—C2—C1 | 119.0 (2) |
O8i—Zn1—O1i | 95.80 (8) | C3—C2—C8 | 119.3 (2) |
O8—Zn1—O1i | 84.20 (8) | C1—C2—C8 | 121.7 (2) |
O1—Zn1—O1i | 180.0 | C4—C3—C2 | 120.9 (3) |
O8i—Zn1—O7 | 88.26 (10) | C4—C3—H3 | 120.9 (17) |
O8—Zn1—O7 | 91.74 (10) | C2—C3—H3 | 118.2 (17) |
O1—Zn1—O7 | 85.45 (8) | C3—C4—C5 | 120.2 (2) |
O1i—Zn1—O7 | 94.55 (8) | C3—C4—C9 | 120.8 (3) |
O8i—Zn1—O7i | 91.74 (10) | C5—C4—C9 | 119.0 (2) |
O8—Zn1—O7i | 88.26 (10) | C6—C5—C4 | 119.4 (3) |
O1—Zn1—O7i | 94.55 (8) | C6—C5—H5B | 120.4 (18) |
O1i—Zn1—O7i | 85.45 (8) | C4—C5—H5B | 120.2 (18) |
O7—Zn1—O7i | 180.000 (1) | C5—C6—C1 | 121.1 (3) |
C7—O1—Zn1 | 127.13 (17) | C5—C6—H6 | 116 (2) |
Zn1—O8—H8A | 119 (3) | C1—C6—H6 | 123 (2) |
Zn1—O8—H8B | 124 (3) | O2—C7—O1 | 124.8 (2) |
H8A—O8—H8B | 108 (4) | O2—C7—C1 | 118.9 (2) |
Zn1—O7—H7A | 104 (3) | O1—C7—C1 | 116.1 (2) |
Zn1—O7—H7B | 112 (3) | O3—C8—O4 | 123.8 (3) |
H7A—O7—H7B | 115 (4) | O3—C8—C2 | 123.4 (2) |
C8—O4—H4 | 112 (3) | O4—C8—C2 | 112.8 (2) |
C9—O5—H5A | 109 (3) | O6—C9—O5 | 123.9 (3) |
H9A—O9—H9B | 107 (4) | O6—C9—C4 | 122.3 (3) |
C6—C1—C2 | 119.4 (3) | O5—C9—C4 | 113.8 (2) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5A···O9 | 0.78 (4) | 1.83 (4) | 2.603 (3) | 179 (5) |
O8—H8A···O6ii | 0.77 (4) | 2.00 (4) | 2.751 (3) | 165 (4) |
O7—H7A···O3iii | 0.78 (3) | 2.01 (3) | 2.775 (3) | 168 (4) |
O9—H9A···O2iv | 0.76 (4) | 1.96 (4) | 2.709 (3) | 171 (4) |
O9—H9B···O7v | 0.76 (2) | 2.02 (3) | 2.722 (3) | 154 (4) |
O4—H4···O1vi | 0.79 (4) | 1.88 (4) | 2.654 (3) | 166 (4) |
O7—H7B···O9ii | 0.75 (4) | 1.99 (4) | 2.735 (4) | 174 (4) |
Symmetry codes: (ii) x+1, y, z; (iii) x, −y+1/2, z−1/2; (iv) −x, −y+1, −z+2; (v) x−1, −y+1/2, z+1/2; (vi) x, −y+1/2, z+1/2. |