The carboxylate dianion in the polymeric title compound, [Zn(C9H6O5)(H2O)2]n, which is disordered over a centre of inversion, links diaquazinc(II) units into a zigzag chain; the chains interact through hydrogen bonds to form layers. The six-coordinate metal atom lies on a special position of site symmetry 2.
Supporting information
CCDC reference: 222209
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (O-C) = 0.005 Å
- Disorder in main residue
- R factor = 0.045
- wR factor = 0.114
- Data-to-parameter ratio = 11.0
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT301_ALERT_3_B Main Residue Disorder ......................... 32.00 Perc.
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.97
PLAT165_ALERT_3_C Nr. of Status R Flagged Non-Hydrogen Atoms ..... 6
PLAT215_ALERT_3_C Disordered C6 has ADP max/min Ratio ....... 3.50
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O1
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.28
PLAT415_ALERT_2_C Short Inter D-H..H-X H1W1 .. H7 .. 2.11 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H1W1 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Rat
O1W -H1W2 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H1# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Rat
O1W -H2# 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 1.82(3), Rep 1.830(10) ...... 3.00 su-Rat
H1# -O1 1.555 3.555
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
13 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
3 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: CrystalStructure (Rigaku/MSC & Rigaku Corporation, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
catena-Poly[-diaquazinc(II)]-µ-4-carboxylatophenoxyacetato]
top
Crystal data top
[Zn(C9H6O5)(H2O)2] | F(000) = 600 |
Mr = 295.54 | Dx = 1.905 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 4330 reflections |
a = 11.853 (2) Å | θ = 3.8–27.4° |
b = 5.0520 (9) Å | µ = 2.41 mm−1 |
c = 17.641 (3) Å | T = 295 K |
β = 102.720 (9)° | Block, colorless |
V = 1030.5 (3) Å3 | 0.34 × 0.25 × 0.18 mm |
Z = 4 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 1192 independent reflections |
Radiation source: fine-focus sealed tube | 1048 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
ω scan | θmax = 27.5°, θmin = 3.5° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −15→15 |
Tmin = 0.441, Tmax = 0.671 | k = −6→6 |
4588 measured reflections | l = −22→22 |
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) = 0.114 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0475P)2 + 5.0313P] where P = (Fo2 + 2Fc2)/3 |
1192 reflections | (Δ/σ)max = 0.001 |
108 parameters | Δρmax = 0.51 e Å−3 |
11 restraints | Δρmin = −0.39 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Zn1 | 0.5000 | 1.1101 (1) | 0.7500 | 0.0356 (2) | |
O1 | 0.3054 (3) | 0.9418 (7) | 0.6962 (2) | 0.054 (1) | |
O2 | 0.4655 (2) | 0.8399 (5) | 0.66111 (15) | 0.038 (1) | |
O3 | 0.3449 (6) | 0.464 (2) | 0.5715 (5) | 0.045 (2) | 0.50 |
O1w | 0.5858 (3) | 1.3869 (6) | 0.7068 (2) | 0.050 (1) | |
C1 | 0.3576 (4) | 0.8052 (7) | 0.6548 (2) | 0.040 (1) | |
C2 | 0.2721 (7) | 0.602 (2) | 0.6099 (6) | 0.040 (2) | 0.50 |
C3 | 0.2861 (4) | 0.281 (1) | 0.5183 (3) | 0.034 (2) | 0.50 |
C4 | 0.1684 (4) | 0.226 (1) | 0.5046 (4) | 0.032 (2) | 0.50 |
C5 | 0.1205 (3) | 0.037 (1) | 0.4498 (4) | 0.031 (2) | 0.50 |
C6 | 0.1901 (5) | −0.098 (1) | 0.4087 (3) | 0.032 (2) | 0.50 |
C7 | 0.3078 (5) | −0.042 (1) | 0.4224 (3) | 0.045 (2) | 0.50 |
C8 | 0.3557 (3) | 0.147 (1) | 0.4772 (3) | 0.052 (2) | 0.50 |
H1w1 | 0.655 (2) | 1.388 (9) | 0.701 (3) | 0.060* | |
H1w2 | 0.550 (3) | 1.522 (7) | 0.685 (3) | 0.060* | |
H2a | 0.2412 | 0.4874 | 0.6446 | 0.048* | 0.50 |
H2b | 0.2090 | 0.6862 | 0.5737 | 0.048* | 0.50 |
H4 | 0.1218 | 0.3160 | 0.5321 | 0.039* | 0.50 |
H5 | 0.0418 | −0.0003 | 0.4407 | 0.037* | 0.50 |
H7 | 0.3544 | −0.1323 | 0.3949 | 0.054* | 0.50 |
H8 | 0.4344 | 0.1840 | 0.4863 | 0.062* | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Zn1 | 0.0447 (4) | 0.0220 (3) | 0.0358 (4) | 0.000 | −0.0008 (3) | 0.000 |
O1 | 0.042 (2) | 0.046 (2) | 0.068 (2) | 0.002 (1) | 0.001 (2) | 0.005 (2) |
O2 | 0.043 (2) | 0.029 (1) | 0.035 (1) | −0.006 (1) | −0.004 (1) | −0.002 (1) |
O3 | 0.022 (3) | 0.047 (4) | 0.061 (5) | −0.008 (3) | −0.001 (3) | −0.013 (4) |
O1w | 0.039 (2) | 0.033 (2) | 0.082 (2) | 0.005 (1) | 0.018 (2) | 0.0083 (16) |
C1 | 0.041 (2) | 0.024 (2) | 0.045 (2) | −0.006 (2) | −0.014 (2) | 0.0115 (17) |
C2 | 0.021 (5) | 0.043 (5) | 0.053 (5) | −0.005 (4) | 0.000 (4) | 0.000 (5) |
C3 | 0.016 (4) | 0.035 (4) | 0.048 (5) | −0.010 (3) | 0.003 (3) | 0.000 (4) |
C4 | 0.019 (4) | 0.033 (4) | 0.042 (5) | −0.005 (4) | 0.002 (3) | 0.000 (4) |
C5 | 0.023 (5) | 0.035 (4) | 0.032 (4) | −0.012 (4) | −0.001 (3) | 0.001 (3) |
C6 | 0.013 (4) | 0.026 (4) | 0.047 (5) | −0.009 (4) | −0.015 (4) | 0.015 (4) |
C7 | 0.024 (4) | 0.058 (5) | 0.049 (5) | 0.003 (4) | 0.000 (4) | −0.023 (4) |
C8 | 0.026 (4) | 0.065 (7) | 0.057 (5) | −0.007 (4) | −0.004 (4) | −0.025 (5) |
Geometric parameters (Å, º) top
Zn1—O1 | 2.445 (3) | C4—C5 | 1.3900 |
Zn1—O1i | 2.445 (3) | C5—C6 | 1.3900 |
Zn1—O2 | 2.051 (3) | C6—C7 | 1.3900 |
Zn1—O2i | 2.051 (3) | C6—C1ii | 1.548 (2) |
Zn1—O1w | 1.978 (3) | C7—C8 | 1.3900 |
Zn1—O1wi | 1.978 (3) | O1w—H1w1 | 0.85 (1) |
O1—C1 | 1.262 (5) | O1w—H1w2 | 0.85 (1) |
O2—C1 | 1.271 (5) | C2—H2a | 0.9700 |
C1—C2 | 1.536 (2) | C2—H2b | 0.9700 |
C1—C6ii | 1.548 (3) | C4—H4 | 0.9300 |
O3—C3 | 1.388 (7) | C5—H5 | 0.9300 |
O3—C2 | 1.40 (1) | C7—H7 | 0.9300 |
C3—C4 | 1.3900 | C8—H8 | 0.9300 |
C3—C8 | 1.3900 | | |
| | | |
O1—Zn1—O1i | 139.3 (2) | O3—C3—C8 | 114.1 (4) |
O1—Zn1—O2 | 57.3 (1) | C4—C3—C8 | 120.0 |
O1—Zn1—O2i | 94.4 (1) | C3—C4—C5 | 120.0 |
O1—Zn1—O1w | 128.1 (1) | C4—C5—C6 | 120.0 |
O1—Zn1—O1wi | 82.8 (1) | C5—C6—C7 | 120.0 |
O1i—Zn1—O2 | 94.4 (1) | C5—C6—C1ii | 122.9 (4) |
O1i—Zn1—O2i | 57.3 (1) | C7—C6—C1ii | 117.1 (4) |
O1i—Zn1—O1w | 82.8 (1) | C8—C7—C6 | 120.0 |
O1i—Zn1—O1wi | 128.1 (1) | C7—C8—C3 | 120.0 |
O2—Zn1—O2i | 96.6 (2) | Zn1—O1w—H1w1 | 130 (3) |
O2—Zn1—O1w | 102.0 (1) | Zn1—O1w—H1w2 | 120 (3) |
O2—Zn1—O1wi | 137.1 (1) | H1w1—O1w—H1w2 | 110 (2) |
O2i—Zn1—O1w | 137.1 (1) | O3—C2—H2a | 111.7 |
O2i—Zn1—O1wi | 102.0 (1) | C1—C2—H2a | 111.7 |
O1w—Zn1—O1wi | 90.0 (2) | O3—C2—H2b | 111.7 |
C1—O1—Zn1 | 82.8 (2) | C1—C2—H2b | 111.7 |
C1—O2—Zn1 | 100.7 (2) | H2a—C2—H2b | 109.5 |
O1—C1—O2 | 119.1 (3) | C3—C4—H4 | 120.0 |
O1—C1—C2 | 108.2 (5) | C5—C4—H4 | 120.0 |
O2—C1—C2 | 132.4 (5) | C4—C5—H5 | 120.0 |
O1—C1—C6ii | 129.9 (5) | C6—C5—H5 | 120.0 |
O2—C1—C6ii | 110.9 (5) | C8—C7—H7 | 120.0 |
C3—O3—C2 | 112.8 (5) | C6—C7—H7 | 120.0 |
O3—C2—C1 | 100.2 (6) | C7—C8—H8 | 120.0 |
O3—C3—C4 | 125.9 (4) | C3—C8—H8 | 120.0 |
| | | |
O1w—Zn1—O1—C1 | 81.3 (3) | C3—O3—C2—C1 | −173.1 (8) |
O1wi—Zn1—O1—C1 | 165.6 (3) | O1—C1—C2—O3 | −177.2 (6) |
O2—Zn1—O1—C1 | 2.2 (2) | O2—C1—C2—O3 | −3 (1) |
O2i—Zn1—O1—C1 | −92.8 (2) | C6ii—C1—C2—O3 | 19 (1) |
O1i—Zn1—O1—C1 | −50.5 (2) | C2—O3—C3—C4 | −3 (1) |
O1w—Zn1—O2—C1 | −130.0 (2) | C2—O3—C3—C8 | 178.0 (7) |
O1wi—Zn1—O2—C1 | −26.7 (3) | O3—C3—C4—C5 | −179.5 (8) |
O2i—Zn1—O2—C1 | 88.9 (2) | C8—C3—C4—C5 | 0.0 |
O1—Zn1—O2—C1 | −2.2 (2) | C3—C4—C5—C6 | 0.0 |
O1i—Zn1—O2—C1 | 146.4 (2) | C4—C5—C6—C7 | 0.0 |
Zn1—O1—C1—O2 | −3.4 (3) | C4—C5—C6—C1ii | −178.2 (6) |
Zn1—O1—C1—C2 | 171.3 (5) | C5—C6—C7—C8 | 0.0 |
Zn1—O1—C1—C6ii | 179.6 (8) | C1ii—C6—C7—C8 | 178.3 (6) |
Zn1—O2—C1—O1 | 4.1 (4) | C6—C7—C8—C3 | 0.0 |
Zn1—O2—C1—C2 | −169.1 (7) | O3—C3—C8—C7 | 179.6 (7) |
Zn1—O2—C1—C6ii | −178.4 (6) | C4—C3—C8—C7 | 0.0 |
Symmetry codes: (i) −x+1, y, −z+3/2; (ii) −x+1/2, −y+1/2, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O1iii | 0.85 (1) | 1.83 (1) | 2.665 (4) | 171 (5) |
O1w—H1w2···O2iv | 0.85 (1) | 1.89 (2) | 2.723 (4) | 166 (5) |
Symmetry codes: (iii) x+1/2, y+1/2, z; (iv) x, y+1, z. |