The pyromellitate tetraanion in the title polymeric complex, [Zn2(C10H2O8)(C12H8N2)2(H2O)2]n, uses only one O atom from each carboxylate group to bind to one Zn atom, which is also chelated by the heterocycle; the fifth coordination site of the trigonal bipyramid around the Zn atom is occupied by a water molecule. The ribbons are linked by hydrogen bonds into sheets. The pyromellitate tetranion lies on an inversion center.
Supporting information
CCDC reference: 263551
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.004 Å
- R factor = 0.040
- wR factor = 0.105
- Data-to-parameter ratio = 14.0
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: 0.490 0.844
Tmin' and Tmax expected: 0.584 0.839
RR' = 0.834
Please check that your absorption correction is appropriate.
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.82
PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.50 Ratio
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H1W1 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H1# 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 1.95(3), Rep 1.940(10) ...... 3.00 su-Rat
H1# -O2 1.555 4.666
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
10 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
0 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
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 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[bis[aqua(1,10-phenanthroline)zinc(II)]-µ
4-1,2,4,5-
benzenetetracarboxylato]
top
Crystal data top
C34H22N4O10Zn2 | F(000) = 788 |
Mr = 777.30 | Dx = 1.810 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 10914 reflections |
a = 7.9612 (2) Å | θ = 2.6–27.5° |
b = 11.8020 (3) Å | µ = 1.76 mm−1 |
c = 15.3935 (4) Å | T = 295 K |
β = 99.614 (1)° | Block, colorless |
V = 1426.03 (6) Å3 | 0.3 × 0.2 × 0.1 mm |
Z = 2 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 3276 independent reflections |
Radiation source: fine-focus sealed tube | 2830 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.066 |
ω scans | θmax = 27.5°, θmin = 2.2° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −10→10 |
Tmin = 0.490, Tmax = 0.844 | k = −15→15 |
6341 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)] = 0.040 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.105 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0444P)2 + 0.7927P] where P = (Fo2 + 2Fc2)/3 |
3276 reflections | (Δ/σ)max = 0.001 |
234 parameters | Δρmax = 0.67 e Å−3 |
2 restraints | Δρmin = −0.62 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Zn1 | 0.08941 (3) | 0.58751 (3) | 0.25379 (2) | 0.0186 (1) | |
O1 | 0.2173 (2) | 0.5804 (2) | 0.1546 (1) | 0.0258 (4) | |
O2 | 0.3963 (2) | 0.4486 (2) | 0.2198 (1) | 0.0279 (4) | |
O3 | 0.6641 (2) | 0.6426 (2) | 0.2060 (1) | 0.0275 (4) | |
O4 | 0.8693 (2) | 0.5247 (2) | 0.1791 (1) | 0.0277 (4) | |
O1w | −0.0421 (3) | 0.7341 (2) | 0.2760 (2) | 0.0352 (5) | |
N1 | 0.0981 (3) | 0.4768 (2) | 0.3607 (1) | 0.0191 (4) | |
N2 | 0.2857 (3) | 0.6640 (2) | 0.3477 (1) | 0.0216 (4) | |
C1 | 0.2031 (3) | 0.5140 (2) | 0.4348 (2) | 0.0186 (5) | |
C2 | 0.0138 (3) | 0.3813 (3) | 0.3653 (2) | 0.0269 (6) | |
C3 | 0.0261 (4) | 0.3171 (2) | 0.4421 (2) | 0.0325 (6) | |
C4 | 0.1279 (4) | 0.3542 (3) | 0.5173 (2) | 0.0308 (6) | |
C5 | 0.2199 (3) | 0.4554 (3) | 0.5155 (2) | 0.0239 (5) | |
C6 | 0.3309 (4) | 0.5014 (3) | 0.5904 (2) | 0.0303 (6) | |
C7 | 0.4173 (4) | 0.5985 (3) | 0.5846 (2) | 0.0304 (7) | |
C8 | 0.4041 (3) | 0.6597 (2) | 0.5033 (2) | 0.0246 (5) | |
C9 | 0.4967 (4) | 0.7582 (3) | 0.4920 (2) | 0.0327 (6) | |
C10 | 0.4848 (4) | 0.8050 (3) | 0.4102 (2) | 0.0358 (7) | |
C11 | 0.3775 (4) | 0.7553 (3) | 0.3396 (2) | 0.0297 (6) | |
C12 | 0.2983 (3) | 0.6152 (2) | 0.4283 (2) | 0.0189 (5) | |
C13 | 0.3447 (3) | 0.5136 (2) | 0.1585 (1) | 0.0174 (5) | |
C14 | 0.4288 (3) | 0.5117 (2) | 0.0769 (1) | 0.0152 (4) | |
C15 | 0.6048 (3) | 0.5244 (2) | 0.0809 (1) | 0.0151 (4) | |
C16 | 0.6734 (3) | 0.5117 (2) | 0.0039 (1) | 0.0163 (5) | |
C17 | 0.7202 (3) | 0.5667 (2) | 0.1635 (2) | 0.0169 (5) | |
H1w1 | −0.009 (6) | 0.802 (2) | 0.277 (3) | 0.07 (1)* | |
H1w2 | −0.146 (2) | 0.727 (4) | 0.254 (2) | 0.06 (1)* | |
H2 | −0.0572 | 0.3556 | 0.3150 | 0.032* | |
H3 | −0.0342 | 0.2496 | 0.4423 | 0.039* | |
H4 | 0.1360 | 0.3127 | 0.5691 | 0.037* | |
H6 | 0.3434 | 0.4633 | 0.6440 | 0.036* | |
H7 | 0.4870 | 0.6266 | 0.6345 | 0.036* | |
H9 | 0.5658 | 0.7914 | 0.5399 | 0.039* | |
H10 | 0.5474 | 0.8694 | 0.4016 | 0.043* | |
H11 | 0.3704 | 0.7880 | 0.2841 | 0.036* | |
H16 | 0.7904 | 0.5190 | 0.0064 | 0.020* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Zn1 | 0.0150 (2) | 0.0272 (2) | 0.0126 (2) | 0.0003 (1) | −0.0004 (1) | −0.0015 (1) |
O1 | 0.020 (1) | 0.042 (1) | 0.016 (1) | 0.011 (1) | 0.003 (1) | 0.001 (1) |
O2 | 0.034 (1) | 0.032 (1) | 0.018 (1) | 0.007 (1) | 0.004 (1) | 0.005 (1) |
O3 | 0.020 (1) | 0.034 (1) | 0.026 (1) | 0.003 (1) | −0.003 (1) | −0.014 (1) |
O4 | 0.016 (1) | 0.037 (1) | 0.026 (1) | 0.006 (1) | −0.009 (1) | −0.012 (1) |
O1w | 0.022 (1) | 0.028 (1) | 0.051 (1) | 0.001 (1) | −0.006 (1) | −0.007 (1) |
N1 | 0.017 (1) | 0.022 (1) | 0.018 (1) | −0.002 (1) | 0.002 (1) | −0.001 (1) |
N2 | 0.020 (1) | 0.026 (1) | 0.019 (1) | 0.000 (1) | 0.001 (1) | 0.003 (1) |
C1 | 0.018 (1) | 0.023 (1) | 0.015 (1) | 0.002 (1) | 0.003 (1) | −0.001 (1) |
C2 | 0.026 (1) | 0.026 (1) | 0.030 (1) | −0.004 (1) | 0.007 (1) | −0.009 (1) |
C3 | 0.036 (2) | 0.018 (1) | 0.046 (2) | −0.002 (1) | 0.015 (1) | 0.001 (1) |
C4 | 0.035 (2) | 0.028 (2) | 0.032 (1) | 0.008 (1) | 0.013 (1) | 0.010 (1) |
C5 | 0.024 (1) | 0.029 (2) | 0.019 (1) | 0.006 (1) | 0.004 (1) | 0.006 (1) |
C6 | 0.033 (2) | 0.041 (2) | 0.015 (1) | 0.012 (1) | 0.000 (1) | 0.006 (1) |
C7 | 0.030 (1) | 0.043 (2) | 0.015 (1) | 0.004 (1) | −0.007 (1) | −0.007 (1) |
C8 | 0.020 (1) | 0.030 (2) | 0.022 (1) | 0.003 (1) | −0.002 (1) | −0.008 (1) |
C9 | 0.026 (1) | 0.030 (2) | 0.038 (2) | −0.003 (1) | −0.007 (1) | −0.013 (1) |
C10 | 0.029 (1) | 0.028 (2) | 0.049 (2) | −0.009 (1) | −0.001 (1) | 0.001 (1) |
C11 | 0.026 (1) | 0.032 (2) | 0.030 (1) | −0.005 (1) | 0.000 (1) | 0.007 (1) |
C12 | 0.015 (1) | 0.023 (1) | 0.018 (1) | 0.003 (1) | −0.001 (1) | 0.000 (1) |
C13 | 0.015 (1) | 0.024 (1) | 0.012 (1) | −0.004 (1) | −0.001 (1) | −0.004 (1) |
C14 | 0.013 (1) | 0.018 (1) | 0.015 (1) | 0.001 (1) | 0.001 (1) | 0.001 (1) |
C15 | 0.013 (1) | 0.016 (1) | 0.014 (1) | 0.001 (1) | −0.003 (1) | 0.001 (1) |
C16 | 0.011 (1) | 0.020 (1) | 0.017 (1) | 0.000 (1) | −0.001 (1) | 0.000 (1) |
C17 | 0.013 (1) | 0.023 (1) | 0.013 (1) | −0.001 (1) | −0.001 (1) | 0.001 (1) |
Geometric parameters (Å, º) top
Zn1—O1 | 1.973 (2) | C8—C9 | 1.403 (4) |
Zn1—O4i | 2.066 (2) | C8—C12 | 1.412 (3) |
Zn1—O1w | 2.080 (2) | C9—C10 | 1.363 (5) |
Zn1—N1 | 2.094 (2) | C10—C11 | 1.395 (4) |
Zn1—N2 | 2.142 (2) | C13—C14 | 1.518 (3) |
O1—C13 | 1.278 (3) | C14—C16ii | 1.395 (3) |
O2—C13 | 1.233 (3) | C14—C15 | 1.400 (3) |
O3—C17 | 1.235 (3) | C15—C16 | 1.394 (3) |
O4—C17 | 1.273 (3) | C15—C17 | 1.524 (3) |
N1—C2 | 1.320 (4) | C16—C14ii | 1.395 (3) |
N1—C1 | 1.369 (3) | O1w—H1w1 | 0.85 (1) |
N2—C11 | 1.320 (4) | O1w—H1w2 | 0.84 (1) |
N2—C12 | 1.357 (3) | C2—H2 | 0.93 |
C1—C5 | 1.408 (3) | C3—H3 | 0.93 |
C1—C12 | 1.427 (4) | C4—H4 | 0.93 |
C2—C3 | 1.394 (4) | C6—H6 | 0.93 |
C3—C4 | 1.368 (4) | C7—H7 | 0.93 |
C4—C5 | 1.404 (4) | C9—H9 | 0.93 |
C5—C6 | 1.438 (4) | C10—H10 | 0.93 |
C6—C7 | 1.348 (4) | C11—H11 | 0.93 |
C7—C8 | 1.433 (4) | C16—H16 | 0.93 |
| | | |
O1—Zn1—O4i | 93.1 (1) | N2—C12—C1 | 117.4 (2) |
O1—Zn1—O1w | 120.1 (1) | C8—C12—C1 | 120.4 (2) |
O1—Zn1—N1 | 128.9 (1) | O2—C13—O1 | 125.5 (2) |
O1—Zn1—N2 | 97.3 (1) | O2—C13—C14 | 119.2 (2) |
O4i—Zn1—O1w | 89.3 (1) | O1—C13—C14 | 115.2 (2) |
O4i—Zn1—N1 | 97.3 (1) | C16ii—C14—C15 | 119.3 (2) |
O4i—Zn1—N2 | 169.0 (1) | C16ii—C14—C13 | 117.9 (2) |
O1w—Zn1—N1 | 110.0 (1) | C15—C14—C13 | 122.6 (2) |
O1w—Zn1—N2 | 82.5 (1) | C16—C15—C14 | 118.9 (2) |
N1—Zn1—N2 | 78.9 (1) | C16—C15—C17 | 118.6 (2) |
C13—O1—Zn1 | 119.9 (2) | C14—C15—C17 | 122.0 (2) |
C17—O4—Zn1iii | 130 (3) | C14ii—C16—C15 | 121.8 (2) |
C2—N1—C1 | 118.3 (2) | O3—C17—O4 | 126.3 (2) |
C2—N1—Zn1 | 128.7 (2) | O3—C17—C15 | 117.3 (2) |
C1—N1—Zn1 | 112.9 (2) | O4—C17—C15 | 116.3 (2) |
C11—N2—C12 | 118.4 (2) | Zn1—O1w—H1w1 | 129 (3) |
C11—N2—Zn1 | 129.3 (2) | Zn1—O1w—H1w2 | 109 (3) |
C12—N2—Zn1 | 111.9 (2) | H1w1—O1w—H1w2 | 113 (4) |
N1—C1—C5 | 122.1 (2) | N1—C2—H2 | 118.5 |
N1—C1—C12 | 117.9 (2) | C3—C2—H2 | 118.5 |
C5—C1—C12 | 120.0 (2) | C4—C3—H3 | 120.3 |
N1—C2—C3 | 123.1 (3) | C2—C3—H3 | 120.3 |
C4—C3—C2 | 119.4 (3) | C3—C4—H4 | 120.2 |
C3—C4—C5 | 119.5 (3) | C5—C4—H4 | 120.2 |
C1—C5—C4 | 117.5 (2) | C7—C6—H6 | 119.3 |
C1—C5—C6 | 118.5 (3) | C5—C6—H6 | 119.3 |
C4—C5—C6 | 123.9 (2) | C6—C7—H7 | 119.2 |
C7—C6—C5 | 121.3 (2) | C8—C7—H7 | 119.2 |
C6—C7—C8 | 121.5 (3) | C10—C9—H9 | 120.2 |
C9—C8—C12 | 117.4 (2) | C8—C9—H9 | 120.2 |
C9—C8—C7 | 124.2 (3) | C9—C10—H10 | 120.4 |
C12—C8—C7 | 118.3 (3) | C11—C10—H10 | 120.4 |
C10—C9—C8 | 119.6 (3) | N2—C11—H11 | 118.4 |
C9—C10—C11 | 119.2 (3) | C10—C11—H11 | 118.4 |
N2—C11—C10 | 123.2 (3) | C14ii—C16—H16 | 119.1 |
N2—C12—C8 | 122.2 (2) | C15—C16—H16 | 119.1 |
| | | |
O4i—Zn1—O1—C13 | −115.3 (2) | C6—C7—C8—C12 | −0.4 (4) |
O1w—Zn1—O1—C13 | 153.7 (2) | C12—C8—C9—C10 | −1.6 (4) |
N1—Zn1—O1—C13 | −13.4 (2) | C7—C8—C9—C10 | 174.9 (3) |
N2—Zn1—O1—C13 | 68.2 (2) | C8—C9—C10—C11 | 1.4 (5) |
O1—Zn1—N1—C2 | −84.9 (2) | C12—N2—C11—C10 | −1.1 (4) |
O4i—Zn1—N1—C2 | 15.1 (2) | Zn1—N2—C11—C10 | 170.6 (2) |
O1w—Zn1—N1—C2 | 106.9 (2) | C9—C10—C11—N2 | 0.0 (5) |
N2—Zn1—N1—C2 | −175.4 (2) | C11—N2—C12—C8 | 0.8 (4) |
O1—Zn1—N1—C1 | 97.3 (2) | Zn1—N2—C12—C8 | −172.2 (2) |
O4i—Zn1—N1—C1 | −162.8 (2) | C11—N2—C12—C1 | −177.5 (2) |
O1w—Zn1—N1—C1 | −70.9 (2) | Zn1—N2—C12—C1 | 9.4 (3) |
N2—Zn1—N1—C1 | 6.8 (2) | C9—C8—C12—N2 | 0.5 (4) |
O1—Zn1—N2—C11 | 50.8 (3) | C7—C8—C12—N2 | −176.2 (2) |
O4i—Zn1—N2—C11 | −110.0 (5) | C9—C8—C12—C1 | 178.8 (2) |
O1w—Zn1—N2—C11 | −68.7 (3) | C7—C8—C12—C1 | 2.1 (4) |
N1—Zn1—N2—C11 | 179.2 (3) | N1—C1—C12—N2 | −3.8 (3) |
O1—Zn1—N2—C12 | −137.1 (2) | C5—C1—C12—N2 | 175.7 (2) |
O4i—Zn1—N2—C12 | 62.1 (5) | N1—C1—C12—C8 | 177.8 (2) |
O1w—Zn1—N2—C12 | 103.4 (2) | C5—C1—C12—C8 | −2.6 (4) |
N1—Zn1—N2—C12 | −8.7 (2) | Zn1—O1—C13—O2 | 1.6 (4) |
C2—N1—C1—C5 | −1.7 (4) | Zn1—O1—C13—C14 | 177.6 (2) |
Zn1—N1—C1—C5 | 176.4 (2) | O2—C13—C14—C16ii | 121.3 (3) |
C2—N1—C1—C12 | 177.8 (2) | O1—C13—C14—C16ii | −54.9 (3) |
Zn1—N1—C1—C12 | −4.0 (3) | O2—C13—C14—C15 | −54.0 (3) |
C1—N1—C2—C3 | 0.3 (4) | O1—C13—C14—C15 | 129.7 (3) |
Zn1—N1—C2—C3 | −177.4 (2) | C16ii—C14—C15—C16 | −0.9 (4) |
N1—C2—C3—C4 | 1.0 (4) | C13—C14—C15—C16 | 174.4 (2) |
C2—C3—C4—C5 | −0.9 (4) | C16ii—C14—C15—C17 | 170.9 (2) |
N1—C1—C5—C4 | 1.7 (4) | C13—C14—C15—C17 | −13.8 (4) |
C12—C1—C5—C4 | −177.8 (2) | C14—C15—C16—C14ii | 0.9 (4) |
N1—C1—C5—C6 | −179.0 (2) | C17—C15—C16—C14ii | −171.2 (2) |
C12—C1—C5—C6 | 1.5 (4) | Zn1iii—O4—C17—O3 | −18.0 (4) |
C3—C4—C5—C1 | −0.4 (4) | Zn1iii—O4—C17—C15 | 157.5 (2) |
C3—C4—C5—C6 | −179.6 (3) | C16—C15—C17—O3 | 133.4 (2) |
C1—C5—C6—C7 | 0.2 (4) | C14—C15—C17—O3 | −38.4 (3) |
C4—C5—C6—C7 | 179.5 (3) | C16—C15—C17—O4 | −42.6 (3) |
C5—C6—C7—C8 | −0.8 (4) | C14—C15—C17—O4 | 145.6 (2) |
C6—C7—C8—C9 | −176.8 (3) | | |
Symmetry codes: (i) x−1, y, z; (ii) −x+1, −y+1, −z; (iii) x+1, y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O2iv | 0.85 (1) | 1.94 (1) | 2.781 (3) | 171 (4) |
O1w—H1w2···O3i | 0.84 (1) | 1.86 (2) | 2.638 (3) | 153 (4) |
Symmetry codes: (i) x−1, y, z; (iv) −x+1/2, y+1/2, −z+1/2. |