The title one-dimensional coordination polymer, {[Zn2(C8H4O4)2(C10H8N2)(H2O)2]·2H2O}n, was synthesized by hydrothermal synthesis. Two asymmetric units, C13H10NO5Zn·H2O, make up each monomer, such that the benzene-1,3-dicarboxylate ligands link ZnII atoms, forming a one-dimensional linear chain, with two adjacent chains bridged by bpy ligands into a ladder running along the b axis. These ladders are assembled into three-dimensional networks via hydrogen bonds between the coordinated water and the carboxylate O atoms in adjacent ladders. Further hydrogen bonding connects uncoordinated water molecules to the coordinated water, carboxyl O atoms and other solvent water molecules.
Supporting information
CCDC reference: 620965
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.010 Å
- R factor = 0.072
- wR factor = 0.216
- Data-to-parameter ratio = 13.8
checkCIF/PLATON results
No syntax errors found
Alert level C
RINTA01_ALERT_3_C The value of Rint is greater than 0.10
Rint given 0.118
PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.12
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.89
PLAT150_ALERT_1_C Volume as Calculated Differs from that Given ... 1336.00 Ang-3
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 11
PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C6 - C8 ... 1.53 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
Alert level G
ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be
replaced by the scaled T values. Since the ratio of scaled T's
is identical to the ratio of reported T values, the scaling
does not imply a change to the absorption corrections used in
the study.
Ratio of Tmax expected/reported 0.891
Tmax scaled 0.440 Tmin scaled 0.406
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
8 ALERT level C = Check and explain
3 ALERT level G = General alerts; check
4 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
4 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: R3m Software (Siemens, 1990); cell refinement: R3m Software; data reduction: R3m Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXTL (Bruker, 2000); molecular graphics: SHELXTL and OLEX (Dolomanov et al., 2003); software used to prepare material for publication: SHELXTL and OLEX.
catena-Poly[[[µ-4,4'-bipyridine-bis[aquazinc(II)]]-di-µ-
benzene-1,3-dicarboxylato] dihydrate]
top
Crystal data top
[Zn2(C8H4O4)2(C10H8N2)(H2O)2]·2H2O | F(000) = 700 |
Mr = 343.61 | Dx = 1.708 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 25 reflections |
a = 11.73 (1) Å | θ = 2–27° |
b = 9.863 (6) Å | µ = 1.87 mm−1 |
c = 12.23 (1) Å | T = 293 K |
β = 109.07 (2)° | Block, colorless |
V = 1336 (2) Å3 | 0.50 × 0.46 × 0.44 mm |
Z = 4 | |
Data collection top
Siemens R3m diffractometer | 1533 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.118 |
Graphite monochromator | θmax = 26.0°, θmin = 2.1° |
ω scans | h = 0→14 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→12 |
Tmin = 0.456, Tmax = 0.494 | l = −15→14 |
2757 measured reflections | 2 standard reflections every 200 reflections |
2628 independent reflections | intensity decay: none |
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)] = 0.072 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.216 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.1095P)2 + 1.2922P] where P = (Fo2 + 2Fc2)/3 |
2628 reflections | (Δ/σ)max < 0.001 |
190 parameters | Δρmax = 0.56 e Å−3 |
0 restraints | Δρmin = −0.78 e Å−3 |
Special details top
Experimental. IR (KBr, cm-1): ν 3403 (s), 3211 (s), 3123 (s), 3038
(m), 2211 (s), 2167 (m), 1982 (m), 1623
(s), 1566 (s), 1516 (s), 1432 (s), 1391
(s), 1349 (w), 1145 (s), 1102 (m), 912 (w),
904 (m), 860 (s), 826 (m), 783 (s), 726 (s)
and 596 (m). |
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 | 0.12741 (10) | 0.10062 (9) | 0.09783 (8) | 0.0528 (4) | |
N1 | 0.0729 (5) | 0.0677 (6) | 0.2403 (5) | 0.0434 (15) | |
O1 | 0.1100 (5) | −0.0832 (4) | 0.0237 (5) | 0.0475 (13) | |
O2 | 0.2697 (6) | −0.0458 (6) | −0.0368 (6) | 0.076 (2) | |
O3 | 0.1392 (5) | −0.6052 (5) | 0.1471 (5) | 0.0511 (13) | |
O4 | 0.1256 (5) | −0.7459 (5) | −0.0025 (5) | 0.0527 (14) | |
C1 | 0.1909 (7) | −0.1238 (7) | −0.0238 (6) | 0.0412 (17) | |
C2 | 0.1846 (6) | −0.2693 (7) | −0.0614 (6) | 0.0381 (16) | |
C3 | 0.2114 (7) | −0.3015 (8) | −0.1631 (6) | 0.0479 (19) | |
H3A | 0.2319 | −0.2326 | −0.2053 | 0.058* | |
C4 | 0.2076 (8) | −0.4355 (8) | −0.2009 (7) | 0.052 (2) | |
H4A | 0.2230 | −0.4561 | −0.2689 | 0.062* | |
C5 | 0.1799 (7) | −0.5393 (7) | −0.1341 (6) | 0.0476 (19) | |
H5A | 0.1759 | −0.6287 | −0.1593 | 0.057* | |
C6 | 0.1582 (6) | −0.5097 (6) | −0.0295 (6) | 0.0358 (16) | |
C7 | 0.1557 (6) | −0.3738 (6) | 0.0037 (6) | 0.0360 (16) | |
H7A | 0.1350 | −0.3527 | 0.0689 | 0.043* | |
C8 | 0.1375 (7) | −0.6265 (7) | 0.0439 (7) | 0.0438 (18) | |
C9 | 0.0587 (8) | −0.0604 (8) | 0.2724 (6) | 0.052 (2) | |
H9A | 0.0684 | −0.1311 | 0.2260 | 0.063* | |
C10 | 0.0302 (8) | −0.0922 (8) | 0.3720 (7) | 0.056 (2) | |
H10A | 0.0212 | −0.1822 | 0.3905 | 0.067* | |
C11 | 0.0148 (7) | 0.0146 (8) | 0.4452 (6) | 0.0456 (18) | |
C12 | 0.0274 (7) | 0.1486 (8) | 0.4089 (6) | 0.0473 (19) | |
H12A | 0.0157 | 0.2220 | 0.4518 | 0.057* | |
C13 | 0.0571 (7) | 0.1706 (8) | 0.3091 (6) | 0.0465 (19) | |
H13A | 0.0666 | 0.2594 | 0.2882 | 0.056* | |
O1W | 0.3153 (5) | 0.0962 (5) | 0.1934 (5) | 0.0554 (14) | |
H1WA | 0.3636 | 0.0894 | 0.1548 | 0.083* | |
H1WB | 0.3312 | 0.0290 | 0.2394 | 0.083* | |
O2W | 0.4785 (12) | 0.0710 (14) | 0.0620 (11) | 0.194 (5) | |
H2WB | 0.4680 | 0.0230 | 0.0018 | 0.292* | |
H2WA | 0.5506 | 0.0703 | 0.1082 | 0.292* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Zn1 | 0.0833 (8) | 0.0394 (5) | 0.0481 (6) | −0.0119 (5) | 0.0383 (5) | −0.0040 (4) |
N1 | 0.049 (4) | 0.047 (4) | 0.036 (3) | −0.005 (3) | 0.017 (3) | 0.002 (3) |
O1 | 0.053 (3) | 0.034 (3) | 0.063 (3) | −0.001 (2) | 0.029 (3) | −0.005 (2) |
O2 | 0.104 (5) | 0.039 (3) | 0.120 (5) | −0.017 (3) | 0.086 (5) | −0.007 (3) |
O3 | 0.068 (4) | 0.040 (3) | 0.055 (3) | −0.007 (3) | 0.033 (3) | 0.003 (2) |
O4 | 0.067 (4) | 0.031 (3) | 0.068 (3) | −0.006 (2) | 0.033 (3) | −0.005 (2) |
C1 | 0.049 (5) | 0.038 (4) | 0.043 (4) | −0.004 (3) | 0.023 (4) | 0.000 (3) |
C2 | 0.040 (4) | 0.039 (4) | 0.039 (4) | 0.000 (3) | 0.019 (3) | 0.001 (3) |
C3 | 0.055 (5) | 0.046 (4) | 0.051 (4) | 0.003 (4) | 0.028 (4) | 0.006 (4) |
C4 | 0.071 (6) | 0.047 (4) | 0.045 (4) | 0.008 (4) | 0.030 (4) | 0.001 (3) |
C5 | 0.062 (5) | 0.031 (4) | 0.054 (4) | 0.004 (4) | 0.024 (4) | −0.006 (3) |
C6 | 0.038 (4) | 0.033 (4) | 0.041 (4) | 0.004 (3) | 0.018 (3) | 0.002 (3) |
C7 | 0.039 (4) | 0.034 (4) | 0.042 (4) | 0.002 (3) | 0.022 (3) | −0.002 (3) |
C8 | 0.041 (4) | 0.034 (4) | 0.058 (5) | 0.001 (3) | 0.019 (4) | 0.001 (3) |
C9 | 0.072 (6) | 0.049 (4) | 0.048 (4) | −0.003 (4) | 0.036 (4) | −0.003 (4) |
C10 | 0.071 (6) | 0.053 (5) | 0.055 (5) | −0.005 (4) | 0.038 (4) | 0.001 (4) |
C11 | 0.043 (5) | 0.061 (5) | 0.036 (4) | 0.007 (4) | 0.017 (3) | 0.007 (3) |
C12 | 0.055 (5) | 0.055 (4) | 0.040 (4) | −0.002 (4) | 0.027 (4) | −0.002 (3) |
C13 | 0.059 (5) | 0.047 (4) | 0.040 (4) | −0.004 (4) | 0.024 (4) | −0.002 (3) |
O1W | 0.067 (4) | 0.051 (3) | 0.056 (3) | −0.001 (3) | 0.031 (3) | 0.004 (3) |
O2W | 0.189 (13) | 0.250 (15) | 0.157 (11) | −0.009 (11) | 0.075 (10) | −0.039 (10) |
Geometric parameters (Å, º) top
Zn1—O4i | 1.944 (5) | C5—C6 | 1.413 (9) |
Zn1—O1 | 2.007 (5) | C5—H5A | 0.9300 |
Zn1—N1 | 2.068 (6) | C6—C7 | 1.403 (9) |
Zn1—O1W | 2.130 (6) | C6—C8 | 1.528 (9) |
N1—C9 | 1.349 (9) | C7—H7A | 0.9300 |
N1—C13 | 1.369 (9) | C9—C10 | 1.400 (10) |
O1—C1 | 1.325 (8) | C9—H9A | 0.9300 |
O2—C1 | 1.252 (9) | C10—C11 | 1.431 (10) |
O3—C8 | 1.273 (9) | C10—H10A | 0.9300 |
O4—C8 | 1.295 (8) | C11—C12 | 1.418 (11) |
O4—Zn1ii | 1.944 (5) | C11—C11iii | 1.518 (13) |
C1—C2 | 1.502 (9) | C12—C13 | 1.390 (10) |
C2—C7 | 1.409 (9) | C12—H12A | 0.9300 |
C2—C3 | 1.416 (10) | C13—H13A | 0.9300 |
C3—C4 | 1.396 (10) | O1W—H1WA | 0.8500 |
C3—H3A | 0.9300 | O1W—H1WB | 0.8501 |
C4—C5 | 1.412 (10) | O2W—H2WB | 0.8500 |
C4—H4A | 0.9300 | O2W—H2WA | 0.8500 |
| | | |
O4i—Zn1—O1 | 116.1 (2) | C7—C6—C8 | 121.8 (6) |
O4i—Zn1—N1 | 135.3 (2) | C5—C6—C8 | 119.0 (6) |
O1—Zn1—N1 | 103.0 (2) | C6—C7—C2 | 120.2 (6) |
O4i—Zn1—O1W | 99.1 (2) | C6—C7—H7A | 119.9 |
O1—Zn1—O1W | 99.4 (2) | C2—C7—H7A | 119.9 |
N1—Zn1—O1W | 94.8 (2) | O3—C8—O4 | 123.3 (6) |
C9—N1—C13 | 117.4 (6) | O3—C8—C6 | 120.3 (6) |
C9—N1—Zn1 | 119.6 (5) | O4—C8—C6 | 116.3 (7) |
C13—N1—Zn1 | 122.9 (5) | N1—C9—C10 | 123.4 (7) |
C1—O1—Zn1 | 119.3 (4) | N1—C9—H9A | 118.3 |
C8—O4—Zn1ii | 117.0 (5) | C10—C9—H9A | 118.3 |
O2—C1—O1 | 122.3 (6) | C9—C10—C11 | 119.6 (7) |
O2—C1—C2 | 120.8 (6) | C9—C10—H10A | 120.2 |
O1—C1—C2 | 116.9 (6) | C11—C10—H10A | 120.2 |
C7—C2—C3 | 119.7 (6) | C12—C11—C10 | 116.3 (6) |
C7—C2—C1 | 121.5 (6) | C12—C11—C11iii | 122.0 (8) |
C3—C2—C1 | 118.7 (6) | C10—C11—C11iii | 121.7 (9) |
C4—C3—C2 | 120.7 (6) | C13—C12—C11 | 120.1 (7) |
C4—C3—H3A | 119.7 | C13—C12—H12A | 119.9 |
C2—C3—H3A | 119.7 | C11—C12—H12A | 119.9 |
C3—C4—C5 | 119.0 (7) | N1—C13—C12 | 123.1 (7) |
C3—C4—H4A | 120.5 | N1—C13—H13A | 118.4 |
C5—C4—H4A | 120.5 | C12—C13—H13A | 118.4 |
C4—C5—C6 | 121.1 (6) | Zn1—O1W—H1WA | 117.0 |
C4—C5—H5A | 119.5 | Zn1—O1W—H1WB | 110.1 |
C6—C5—H5A | 119.5 | H1WA—O1W—H1WB | 105.2 |
C7—C6—C5 | 119.1 (6) | H2WB—O2W—H2WA | 113.7 |
Symmetry codes: (i) x, y+1, z; (ii) x, y−1, z; (iii) −x, −y, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O2W | 0.85 | 2.03 | 2.88 (1) | 179 |
O1W—H1WB···O3iv | 0.85 | 1.87 | 2.71 (1) | 173 |
O2W—H2WB···O2 | 0.85 | 2.32 | 2.62 (1) | 101 |
O2W—H2WB···O2Wv | 0.85 | 1.48 | 2.24 (2) | 147 |
O2W—H2WA···O2v | 0.85 | 2.54 | 3.08 (2) | 122 |
Symmetry codes: (iv) −x+1/2, y+1/2, −z+1/2; (v) −x+1, −y, −z. |