The title compound, [Cd(C
8H
4O
4)(C
5H
5N)(H
2O)
2]
n, is a one-dimensional spiral polymer in which the organic species act in bis-monodentate and bis-bidentate coordination modes. The two crystallographically independent terephthalate ligands lie on centers of symmetry. The Cd
2+ cation is hexacoordinated in a distorted octahedral geometry by five O atoms [Cd—O = 2.2370 (16)–2.4928 (17) Å] and one N atom [Cd—N = 2.316 (2) Å]. The water molecules and carboxylate O atoms are involved in O—H
O hydrogen bonds, which link adjacent polymeric chains into a three-dimensional supramolecular network.
Supporting information
CCDC reference: 298013
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.004 Å
- R factor = 0.022
- wR factor = 0.059
- Data-to-parameter ratio = 14.7
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.51 Ratio
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O3
Alert level G
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
2 ALERT level C = Check and explain
2 ALERT level G = General alerts; check
2 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
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
catena-Poly[[diaquapyridinecadmium(II)]-µ-terephthalato]
top
Crystal data top
[Cd(C8H4O4)(C5H5N)(H2O)2] | F(000) = 776 |
Mr = 391.64 | Dx = 1.872 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 4986 reflections |
a = 8.639 (2) Å | θ = 2.9–27.0° |
b = 9.617 (3) Å | µ = 1.60 mm−1 |
c = 16.951 (4) Å | T = 293 K |
β = 99.324 (5)° | Block, colourless |
V = 1389.6 (6) Å3 | 0.42 × 0.31 × 0.28 mm |
Z = 4 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 3034 independent reflections |
Radiation source: fine-focus sealed tube | 2326 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.019 |
ω scans | θmax = 27.0°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | h = −11→10 |
Tmin = 0.549, Tmax = 0.639 | k = −12→5 |
7409 measured reflections | l = −19→21 |
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)] = 0.022 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.059 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0324P)2 + 0.1996P] where P = (Fo2 + 2Fc2)/3 |
3034 reflections | (Δ/σ)max = 0.045 |
206 parameters | Δρmax = 0.31 e Å−3 |
0 restraints | Δρmin = −0.70 e Å−3 |
Special details top
Experimental. Selected data for 1. IR (KBr pellet) (ν/cm-1): 3434.46m, 2927.29w,
1601.66m, 1573.70 s, 1502.79m, 1446.81m, 1395.96 s,
1379.56 s, 745.49m, 691.99w, 524.59w. Anal. Calcd for C13H13NO6Cd
(391.64): C, 39.83; H, 3.32; N, 3.57. Found: C, 40.12; H, 3.50; N, 3.30. |
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 | |
Cd1 | 0.275301 (17) | 0.000529 (16) | 0.131012 (9) | 0.02442 (7) | |
N1 | 0.5271 (2) | 0.0839 (2) | 0.17162 (12) | 0.0327 (5) | |
O1 | 0.2477 (3) | −0.0241 (2) | 0.26060 (11) | 0.0416 (5) | |
H11 | 0.277 (3) | −0.096 (3) | 0.2897 (16) | 0.045 (8)* | |
H12 | 0.233 (4) | 0.040 (3) | 0.2964 (19) | 0.055 (10)* | |
O2 | 0.0439 (2) | −0.1302 (2) | 0.11065 (13) | 0.0387 (4) | |
H21 | 0.084 (4) | −0.205 (4) | 0.1076 (19) | 0.065 (11)* | |
H22 | −0.012 (5) | −0.129 (4) | 0.072 (2) | 0.086 (15)* | |
O3 | 0.3748 (2) | −0.15712 (16) | 0.05608 (10) | 0.0422 (4) | |
O4 | 0.3129 (2) | −0.30375 (19) | 0.14639 (10) | 0.0440 (5) | |
O5 | 0.1741 (2) | 0.23971 (17) | 0.14765 (10) | 0.0360 (4) | |
O6 | 0.1678 (2) | 0.14968 (17) | 0.02808 (9) | 0.0380 (4) | |
C1 | 0.5533 (3) | 0.1730 (3) | 0.23243 (16) | 0.0507 (7) | |
H1A | 0.4691 | 0.1998 | 0.2569 | 0.061* | |
C2 | 0.6987 (4) | 0.2273 (4) | 0.26082 (18) | 0.0633 (9) | |
H2A | 0.7128 | 0.2885 | 0.3038 | 0.076* | |
C3 | 0.8229 (3) | 0.1889 (4) | 0.2242 (2) | 0.0611 (9) | |
H3A | 0.9230 | 0.2233 | 0.2423 | 0.073* | |
C4 | 0.7974 (3) | 0.1001 (3) | 0.1612 (2) | 0.0604 (9) | |
H4A | 0.8798 | 0.0741 | 0.1352 | 0.072* | |
C5 | 0.6482 (3) | 0.0483 (3) | 0.13573 (18) | 0.0434 (6) | |
H5A | 0.6318 | −0.0128 | 0.0927 | 0.052* | |
C6 | 0.3714 (3) | −0.2773 (2) | 0.08481 (13) | 0.0285 (5) | |
C7 | 0.4401 (2) | −0.3928 (2) | 0.04179 (13) | 0.0251 (5) | |
C8 | 0.4639 (3) | −0.3735 (2) | −0.03601 (14) | 0.0335 (5) | |
H8A | 0.4402 | −0.2880 | −0.0606 | 0.040* | |
C9 | 0.5226 (3) | −0.4799 (2) | −0.07813 (15) | 0.0328 (5) | |
H9A | 0.5368 | −0.4656 | −0.1307 | 0.039* | |
C10 | 0.1414 (3) | 0.2488 (2) | 0.07319 (14) | 0.0281 (5) | |
C11 | 0.0680 (2) | 0.3793 (2) | 0.03542 (13) | 0.0264 (5) | |
C12 | 0.1034 (3) | 0.4245 (2) | −0.03750 (14) | 0.0301 (5) | |
H12A | 0.1735 | 0.3742 | −0.0626 | 0.036* | |
C13 | −0.0347 (3) | 0.4558 (3) | 0.07308 (15) | 0.0300 (5) | |
H13A | −0.0576 | 0.4269 | 0.1223 | 0.036* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.02914 (10) | 0.02076 (10) | 0.02279 (10) | 0.00510 (7) | 0.00246 (6) | −0.00002 (7) |
N1 | 0.0333 (11) | 0.0312 (11) | 0.0337 (11) | 0.0009 (9) | 0.0056 (9) | 0.0005 (9) |
O1 | 0.0671 (13) | 0.0337 (11) | 0.0250 (9) | 0.0053 (9) | 0.0107 (9) | 0.0028 (8) |
O2 | 0.0364 (10) | 0.0357 (11) | 0.0420 (11) | 0.0012 (9) | 0.0005 (8) | −0.0053 (9) |
O3 | 0.0593 (11) | 0.0199 (8) | 0.0535 (11) | 0.0053 (8) | 0.0274 (9) | −0.0029 (8) |
O4 | 0.0626 (11) | 0.0397 (10) | 0.0334 (9) | 0.0241 (9) | 0.0193 (8) | 0.0051 (8) |
O5 | 0.0458 (10) | 0.0273 (9) | 0.0323 (9) | 0.0069 (8) | −0.0016 (7) | 0.0068 (7) |
O6 | 0.0514 (10) | 0.0234 (8) | 0.0349 (9) | 0.0112 (8) | −0.0059 (8) | −0.0023 (7) |
C1 | 0.0498 (16) | 0.0629 (19) | 0.0420 (15) | −0.0155 (15) | 0.0150 (13) | −0.0142 (14) |
C2 | 0.065 (2) | 0.075 (2) | 0.0486 (17) | −0.0309 (18) | 0.0049 (15) | −0.0110 (17) |
C3 | 0.0387 (16) | 0.059 (2) | 0.080 (2) | −0.0115 (15) | −0.0070 (15) | 0.0130 (19) |
C4 | 0.0351 (15) | 0.0446 (17) | 0.105 (3) | 0.0072 (13) | 0.0208 (16) | 0.0045 (19) |
C5 | 0.0414 (15) | 0.0324 (13) | 0.0589 (18) | 0.0068 (12) | 0.0153 (13) | 0.0001 (14) |
C6 | 0.0307 (12) | 0.0227 (11) | 0.0314 (12) | 0.0063 (9) | 0.0029 (9) | −0.0058 (10) |
C7 | 0.0253 (11) | 0.0198 (11) | 0.0306 (11) | 0.0022 (9) | 0.0053 (9) | −0.0027 (9) |
C8 | 0.0452 (14) | 0.0215 (11) | 0.0364 (13) | 0.0114 (11) | 0.0145 (11) | 0.0065 (10) |
C9 | 0.0437 (14) | 0.0296 (13) | 0.0272 (11) | 0.0104 (10) | 0.0126 (10) | 0.0045 (10) |
C10 | 0.0283 (11) | 0.0200 (11) | 0.0341 (12) | 0.0007 (9) | −0.0008 (9) | 0.0042 (10) |
C11 | 0.0281 (11) | 0.0190 (10) | 0.0292 (11) | 0.0005 (9) | −0.0045 (9) | 0.0012 (9) |
C12 | 0.0327 (12) | 0.0247 (13) | 0.0323 (12) | 0.0051 (10) | 0.0034 (10) | 0.0002 (10) |
C13 | 0.0330 (12) | 0.0260 (11) | 0.0295 (12) | 0.0027 (10) | 0.0008 (10) | 0.0044 (10) |
Geometric parameters (Å, º) top
Cd1—O3 | 2.2370 (16) | C3—C4 | 1.357 (5) |
Cd1—O1 | 2.2600 (19) | C3—H3A | 0.9300 |
Cd1—N1 | 2.316 (2) | C4—C5 | 1.384 (4) |
Cd1—O6 | 2.3323 (16) | C4—H4A | 0.9300 |
Cd1—O2 | 2.339 (2) | C5—H5A | 0.9300 |
Cd1—O5 | 2.4928 (17) | C6—C7 | 1.503 (3) |
N1—C1 | 1.331 (3) | C7—C8 | 1.380 (3) |
N1—C5 | 1.337 (3) | C7—C9i | 1.384 (3) |
O1—H11 | 0.86 (3) | C8—C9 | 1.390 (3) |
O1—H12 | 0.89 (3) | C8—H8A | 0.9300 |
O2—H21 | 0.81 (4) | C9—C7i | 1.384 (3) |
O2—H22 | 0.75 (4) | C9—H9A | 0.9300 |
O3—C6 | 1.256 (3) | C10—C11 | 1.502 (3) |
O4—C6 | 1.257 (3) | C11—C13 | 1.386 (3) |
O5—C10 | 1.251 (3) | C11—C12 | 1.390 (3) |
O6—C10 | 1.265 (3) | C12—C13ii | 1.387 (3) |
C1—C2 | 1.373 (4) | C12—H12A | 0.9300 |
C1—H1A | 0.9300 | C13—C12ii | 1.387 (3) |
C2—C3 | 1.375 (5) | C13—H13A | 0.9300 |
C2—H2A | 0.9300 | | |
| | | |
O3—Cd1—O1 | 126.26 (7) | C4—C3—C2 | 119.0 (3) |
O3—Cd1—N1 | 88.55 (7) | C4—C3—H3A | 120.5 |
O1—Cd1—N1 | 89.38 (7) | C2—C3—H3A | 120.5 |
O3—Cd1—O6 | 97.77 (6) | C3—C4—C5 | 119.8 (3) |
O1—Cd1—O6 | 134.40 (7) | C3—C4—H4A | 120.1 |
N1—Cd1—O6 | 104.51 (7) | C5—C4—H4A | 120.1 |
O3—Cd1—O2 | 87.11 (7) | N1—C5—C4 | 121.6 (3) |
O1—Cd1—O2 | 82.24 (8) | N1—C5—H5A | 119.2 |
N1—Cd1—O2 | 165.69 (8) | C4—C5—H5A | 119.2 |
O6—Cd1—O2 | 89.60 (7) | O3—C6—O4 | 123.1 (2) |
O3—Cd1—O5 | 149.72 (6) | O3—C6—C7 | 117.1 (2) |
O1—Cd1—O5 | 83.84 (7) | O4—C6—C7 | 119.8 (2) |
N1—Cd1—O5 | 88.65 (6) | C8—C7—C9i | 119.0 (2) |
O6—Cd1—O5 | 54.03 (5) | C8—C7—C6 | 119.7 (2) |
O2—Cd1—O5 | 101.88 (7) | C9i—C7—C6 | 121.3 (2) |
C1—N1—C5 | 118.0 (2) | C7—C8—C9 | 121.0 (2) |
C1—N1—Cd1 | 119.14 (16) | C7—C8—H8A | 119.5 |
C5—N1—Cd1 | 122.84 (18) | C9—C8—H8A | 119.5 |
Cd1—O1—H11 | 124.9 (18) | C7i—C9—C8 | 120.0 (2) |
Cd1—O1—H12 | 130 (2) | C7i—C9—H9A | 120.0 |
H11—O1—H12 | 103 (3) | C8—C9—H9A | 120.0 |
Cd1—O2—H21 | 97 (2) | O5—C10—O6 | 121.6 (2) |
Cd1—O2—H22 | 122 (3) | O5—C10—C11 | 119.9 (2) |
H21—O2—H22 | 100 (4) | O6—C10—C11 | 118.5 (2) |
C6—O3—Cd1 | 111.60 (14) | C13—C11—C12 | 119.6 (2) |
C10—O5—Cd1 | 88.65 (13) | C13—C11—C10 | 120.3 (2) |
C10—O6—Cd1 | 95.75 (13) | C12—C11—C10 | 120.1 (2) |
N1—C1—C2 | 123.2 (3) | C13ii—C12—C11 | 120.4 (2) |
N1—C1—H1A | 118.4 | C13ii—C12—H12A | 119.8 |
C2—C1—H1A | 118.4 | C11—C12—H12A | 119.8 |
C1—C2—C3 | 118.4 (3) | C11—C13—C12ii | 120.1 (2) |
C1—C2—H2A | 120.8 | C11—C13—H13A | 120.0 |
C3—C2—H2A | 120.8 | C12ii—C13—H13A | 120.0 |
Symmetry codes: (i) −x+1, −y−1, −z; (ii) −x, −y+1, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H21···O4 | 0.81 (4) | 2.19 (4) | 2.845 (3) | 138 (3) |
O2—H22···O6iii | 0.75 (4) | 1.99 (4) | 2.741 (3) | 173 (4) |
O1—H12···O4iv | 0.89 (3) | 1.87 (3) | 2.742 (3) | 168 (3) |
O1—H11···O5v | 0.86 (3) | 1.91 (3) | 2.774 (3) | 176 (3) |
Symmetry codes: (iii) −x, −y, −z; (iv) −x+1/2, y+1/2, −z+1/2; (v) −x+1/2, y−1/2, −z+1/2. |