Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807054669/hb2610sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807054669/hb2610Isup2.hkl |
CCDC reference: 672611
Cadmium dinitrate tetrahydrate (2 mmol), 2,2'-bipyridine (2 mmol) and 3-(4-carboxylatophenoxy)propionic acid (2 mmol) and water were sealed in a 25-ml, Teflon-lined, stainless steel bomb and heated at 413 K for 20 h. The bomb was cooled to room temperature; the colorless crystals that separated was picked out manually.
The water and 4-hydroxybenzoic acid molecules are disordered about a center-of-inversion; the molecules were assigned half-occupancy each. The phenylene ring was refined as a rigid hexagon of 1.39 Å sides. The four-atom –C(=O)–O fragment was restrained to be nearly planar; the two C–O distances were restrained to 1.25±0.01 Å and the C–C single-bond distance to 1.50±-0.01 Å.
Carbon-bound H atoms were placed in calculated positions [C—H 0.93–0.97 Å and Uiso(H) 1.2Ueq(C)], and were included in the refinement in the riding-model approximation. The carboxylic acid and water H-atoms were similarly generated [O–H 0.82 Å and and Uiso(H) 1.2Ueq(O)].
The final difference Fourier map had a large peak near Cd1, but was otherwise essentially featureless.
Data collection: RAPID-AUTO (Rigaku Corporation, 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: X-SEED (Barbour, 2001), OLEX (Dolomanov et al., 2003); software used to prepare material for publication: publCIF (Westrip, 2007).
[Cd2(C10H8O5)2(C10H8N2)2]·C7H6O3·H2O | Z = 1 |
Mr = 1109.63 | F(000) = 558 |
Triclinic, P1 | Dx = 1.659 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.1615 (5) Å | Cell parameters from 8754 reflections |
b = 10.6255 (5) Å | θ = 3.0–27.5° |
c = 10.8507 (6) Å | µ = 1.03 mm−1 |
α = 73.147 (2)° | T = 295 K |
β = 82.174 (1)° | Block, colorless |
γ = 88.734 (1)° | 0.32 × 0.24 × 0.16 mm |
V = 1110.6 (1) Å3 |
Rigaku RAXIS-RAPID diffractometer | 5010 independent reflections |
Radiation source: fine-focus sealed tube | 3997 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.042 |
Detector resolution: 10.000 pixels mm-1 | θmax = 27.5°, θmin = 3.0° |
ω–scans | h = −13→13 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −11→13 |
Tmin = 0.542, Tmax = 0.852 | l = −14→14 |
10857 measured reflections |
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) = 0.120 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.048P)2 + 1.4148P] where P = (Fo2 + 2Fc2)/3 |
5010 reflections | (Δ/σ)max = 0.001 |
341 parameters | Δρmax = 1.13 e Å−3 |
4 restraints | Δρmin = −0.87 e Å−3 |
[Cd2(C10H8O5)2(C10H8N2)2]·C7H6O3·H2O | γ = 88.734 (1)° |
Mr = 1109.63 | V = 1110.6 (1) Å3 |
Triclinic, P1 | Z = 1 |
a = 10.1615 (5) Å | Mo Kα radiation |
b = 10.6255 (5) Å | µ = 1.03 mm−1 |
c = 10.8507 (6) Å | T = 295 K |
α = 73.147 (2)° | 0.32 × 0.24 × 0.16 mm |
β = 82.174 (1)° |
Rigaku RAXIS-RAPID diffractometer | 5010 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 3997 reflections with I > 2σ(I) |
Tmin = 0.542, Tmax = 0.852 | Rint = 0.042 |
10857 measured reflections |
R[F2 > 2σ(F2)] = 0.040 | 4 restraints |
wR(F2) = 0.120 | H-atom parameters constrained |
S = 1.06 | Δρmax = 1.13 e Å−3 |
5010 reflections | Δρmin = −0.87 e Å−3 |
341 parameters |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cd1 | 0.42672 (3) | 0.67472 (3) | 0.96257 (3) | 0.04096 (12) | |
O1 | 0.4806 (4) | 0.6852 (4) | 0.7269 (3) | 0.0713 (11) | |
O2 | 0.4891 (3) | 0.5017 (3) | 0.8745 (3) | 0.0503 (7) | |
O3 | 0.7194 (3) | 0.5162 (4) | 0.4709 (3) | 0.0528 (8) | |
O4 | 1.2813 (3) | 0.7051 (3) | 0.1393 (3) | 0.0524 (8) | |
O5 | 1.1998 (3) | 0.6081 (3) | 0.0120 (3) | 0.0501 (8) | |
N1 | 0.6322 (3) | 0.7835 (4) | 0.9263 (3) | 0.0422 (8) | |
N2 | 0.3986 (3) | 0.8980 (4) | 0.8686 (4) | 0.0506 (9) | |
C1 | 0.5078 (4) | 0.5672 (5) | 0.7584 (4) | 0.0423 (10) | |
C2 | 0.5637 (4) | 0.5052 (6) | 0.6544 (4) | 0.0544 (12) | |
H2A | 0.4973 | 0.5069 | 0.5976 | 0.065* | |
H2B | 0.5831 | 0.4139 | 0.6948 | 0.065* | |
C3 | 0.6886 (4) | 0.5747 (5) | 0.5741 (4) | 0.0501 (11) | |
H3A | 0.6738 | 0.6681 | 0.5399 | 0.060* | |
H3B | 0.7606 | 0.5627 | 0.6264 | 0.060* | |
C4 | 0.8339 (4) | 0.5545 (4) | 0.3857 (4) | 0.0366 (8) | |
C5 | 0.9291 (4) | 0.6386 (5) | 0.4003 (4) | 0.0470 (10) | |
H5 | 0.9163 | 0.6751 | 0.4692 | 0.056* | |
C6 | 1.0433 (4) | 0.6675 (5) | 0.3111 (4) | 0.0450 (10) | |
H6 | 1.1087 | 0.7219 | 0.3218 | 0.054* | |
C7 | 1.0620 (4) | 0.6166 (4) | 0.2057 (4) | 0.0357 (8) | |
C8 | 0.9646 (4) | 0.5349 (4) | 0.1924 (4) | 0.0407 (9) | |
H8 | 0.9758 | 0.4997 | 0.1227 | 0.049* | |
C9 | 0.8502 (4) | 0.5047 (5) | 0.2819 (4) | 0.0466 (10) | |
H9 | 0.7846 | 0.4506 | 0.2712 | 0.056* | |
C10 | 1.1891 (4) | 0.6454 (4) | 0.1128 (4) | 0.0383 (9) | |
C11 | 0.7459 (4) | 0.7223 (5) | 0.9483 (5) | 0.0507 (11) | |
H11 | 0.7436 | 0.6317 | 0.9860 | 0.061* | |
C12 | 0.8668 (5) | 0.7873 (6) | 0.9178 (6) | 0.0690 (15) | |
H12 | 0.9449 | 0.7416 | 0.9333 | 0.083* | |
C13 | 0.8693 (5) | 0.9193 (6) | 0.8645 (8) | 0.096 (3) | |
H13 | 0.9498 | 0.9657 | 0.8426 | 0.115* | |
C14 | 0.7518 (5) | 0.9853 (5) | 0.8427 (7) | 0.0749 (18) | |
H14 | 0.7521 | 1.0764 | 0.8090 | 0.090* | |
C15 | 0.6343 (4) | 0.9139 (4) | 0.8718 (4) | 0.0405 (9) | |
C16 | 0.5054 (4) | 0.9786 (4) | 0.8424 (4) | 0.0391 (9) | |
C17 | 0.4953 (5) | 1.1124 (5) | 0.7919 (5) | 0.0555 (12) | |
H17 | 0.5702 | 1.1667 | 0.7754 | 0.067* | |
C18 | 0.3730 (5) | 1.1661 (5) | 0.7658 (6) | 0.0638 (14) | |
H18 | 0.3644 | 1.2565 | 0.7322 | 0.077* | |
C19 | 0.2654 (5) | 1.0838 (6) | 0.7902 (6) | 0.0750 (17) | |
H19 | 0.1825 | 1.1169 | 0.7717 | 0.090* | |
C20 | 0.2812 (5) | 0.9547 (5) | 0.8413 (6) | 0.0717 (17) | |
H20 | 0.2064 | 0.9001 | 0.8594 | 0.086* | |
O1w | 0.6482 (8) | 1.1595 (8) | 0.4750 (9) | 0.077 (2) | 0.50 |
H1w | 0.6162 | 1.2113 | 0.4151 | 0.092* | 0.50 |
H2w | 0.6057 | 1.0901 | 0.4959 | 0.092* | 0.50 |
O6 | −0.1473 (12) | 0.9220 (11) | 0.5206 (16) | 0.089 (4) | 0.50 |
O7 | −0.1003 (11) | 1.1321 (8) | 0.4495 (14) | 0.078 (5) | 0.50 |
H7O | −0.1790 | 1.1487 | 0.4448 | 0.117* | 0.50 |
O8 | 0.4798 (7) | 0.9246 (7) | 0.5287 (8) | 0.0657 (19) | 0.50 |
H8O | 0.4907 | 0.8528 | 0.5804 | 0.099* | 0.50 |
C21 | −0.0645 (10) | 1.0142 (12) | 0.4888 (14) | 0.071 (8) | 0.50 |
C22 | 0.0799 (7) | 0.9884 (13) | 0.4960 (19) | 0.059 (6) | 0.50 |
C23 | 0.1194 (8) | 0.8635 (11) | 0.5611 (16) | 0.127 (14) | 0.50 |
H23 | 0.0564 | 0.7964 | 0.5983 | 0.153* | 0.50 |
C24 | 0.2532 (9) | 0.8391 (6) | 0.5707 (10) | 0.074 (3) | 0.50 |
H24 | 0.2796 | 0.7555 | 0.6143 | 0.089* | 0.50 |
C25 | 0.3473 (6) | 0.9395 (7) | 0.5152 (8) | 0.054 (2) | 0.50 |
C26 | 0.3077 (8) | 1.0643 (6) | 0.4500 (8) | 0.055 (2) | 0.50 |
H26 | 0.3707 | 1.1315 | 0.4128 | 0.066* | 0.50 |
C27 | 0.1740 (9) | 1.0888 (9) | 0.4404 (14) | 0.066 (5) | 0.50 |
H27 | 0.1476 | 1.1724 | 0.3968 | 0.079* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.03119 (16) | 0.04466 (19) | 0.04179 (19) | −0.00141 (12) | 0.00713 (11) | −0.00967 (14) |
O1 | 0.081 (2) | 0.080 (3) | 0.040 (2) | 0.030 (2) | 0.0032 (17) | −0.0039 (18) |
O2 | 0.0553 (17) | 0.0601 (19) | 0.0309 (16) | 0.0082 (15) | 0.0077 (13) | −0.0127 (14) |
O3 | 0.0361 (15) | 0.083 (2) | 0.0409 (17) | −0.0108 (15) | 0.0124 (12) | −0.0284 (17) |
O4 | 0.0339 (15) | 0.066 (2) | 0.058 (2) | −0.0112 (15) | 0.0079 (13) | −0.0255 (17) |
O5 | 0.0414 (16) | 0.064 (2) | 0.0483 (18) | −0.0108 (15) | 0.0130 (13) | −0.0295 (16) |
N1 | 0.0361 (17) | 0.046 (2) | 0.044 (2) | 0.0026 (15) | −0.0018 (14) | −0.0144 (16) |
N2 | 0.0370 (18) | 0.051 (2) | 0.057 (2) | −0.0029 (17) | 0.0016 (16) | −0.0078 (19) |
C1 | 0.0290 (18) | 0.063 (3) | 0.035 (2) | 0.0069 (19) | −0.0027 (15) | −0.015 (2) |
C2 | 0.039 (2) | 0.091 (4) | 0.033 (2) | −0.005 (2) | 0.0071 (17) | −0.022 (2) |
C3 | 0.037 (2) | 0.077 (3) | 0.035 (2) | 0.003 (2) | 0.0047 (17) | −0.018 (2) |
C4 | 0.0277 (17) | 0.045 (2) | 0.034 (2) | 0.0036 (16) | 0.0028 (14) | −0.0099 (17) |
C5 | 0.038 (2) | 0.065 (3) | 0.042 (2) | 0.004 (2) | 0.0039 (17) | −0.025 (2) |
C6 | 0.035 (2) | 0.058 (3) | 0.045 (2) | −0.0091 (19) | 0.0054 (17) | −0.025 (2) |
C7 | 0.0322 (18) | 0.036 (2) | 0.036 (2) | 0.0016 (16) | 0.0032 (15) | −0.0087 (17) |
C8 | 0.041 (2) | 0.048 (2) | 0.034 (2) | −0.0034 (18) | 0.0062 (16) | −0.0185 (18) |
C9 | 0.037 (2) | 0.059 (3) | 0.046 (3) | −0.011 (2) | 0.0058 (17) | −0.022 (2) |
C10 | 0.0299 (18) | 0.038 (2) | 0.043 (2) | 0.0038 (16) | 0.0025 (16) | −0.0093 (18) |
C11 | 0.043 (2) | 0.046 (2) | 0.060 (3) | 0.006 (2) | −0.010 (2) | −0.010 (2) |
C12 | 0.039 (2) | 0.063 (3) | 0.102 (5) | 0.004 (2) | −0.010 (3) | −0.020 (3) |
C13 | 0.039 (3) | 0.063 (4) | 0.176 (8) | −0.007 (3) | −0.012 (4) | −0.019 (4) |
C14 | 0.047 (3) | 0.040 (3) | 0.126 (6) | −0.002 (2) | −0.010 (3) | −0.009 (3) |
C15 | 0.040 (2) | 0.038 (2) | 0.045 (2) | 0.0003 (17) | −0.0021 (17) | −0.0174 (19) |
C16 | 0.044 (2) | 0.039 (2) | 0.034 (2) | 0.0084 (18) | −0.0026 (16) | −0.0125 (17) |
C17 | 0.057 (3) | 0.041 (2) | 0.068 (3) | 0.002 (2) | −0.014 (2) | −0.013 (2) |
C18 | 0.064 (3) | 0.055 (3) | 0.067 (4) | 0.010 (3) | −0.018 (3) | −0.005 (3) |
C19 | 0.051 (3) | 0.074 (4) | 0.084 (4) | 0.017 (3) | −0.022 (3) | 0.007 (3) |
C20 | 0.042 (2) | 0.055 (3) | 0.104 (5) | 0.003 (2) | −0.017 (3) | 0.002 (3) |
O1w | 0.071 (5) | 0.061 (5) | 0.082 (6) | 0.008 (5) | −0.024 (5) | 0.011 (4) |
O6 | 0.068 (6) | 0.077 (8) | 0.132 (12) | 0.000 (6) | −0.044 (8) | −0.032 (7) |
O7 | 0.065 (6) | 0.035 (5) | 0.134 (13) | 0.010 (5) | −0.022 (7) | −0.021 (7) |
O8 | 0.060 (4) | 0.060 (4) | 0.066 (5) | 0.003 (4) | −0.008 (3) | 0.000 (4) |
C21 | 0.068 (10) | 0.069 (19) | 0.082 (17) | 0.005 (11) | −0.027 (10) | −0.025 (13) |
C22 | 0.059 (10) | 0.065 (17) | 0.053 (10) | −0.009 (10) | −0.011 (8) | −0.013 (10) |
C23 | 0.12 (2) | 0.14 (2) | 0.092 (18) | −0.026 (17) | −0.050 (17) | 0.025 (16) |
C24 | 0.069 (7) | 0.048 (6) | 0.098 (10) | 0.004 (6) | −0.035 (7) | 0.000 (6) |
C25 | 0.062 (6) | 0.050 (6) | 0.044 (5) | 0.002 (5) | −0.007 (4) | −0.004 (5) |
C26 | 0.060 (6) | 0.044 (5) | 0.056 (6) | 0.003 (4) | −0.004 (5) | −0.009 (4) |
C27 | 0.079 (11) | 0.045 (8) | 0.066 (9) | 0.001 (7) | −0.007 (7) | −0.004 (6) |
Cd1—O1 | 2.511 (4) | C9—H9 | 0.9300 |
Cd1—O2 | 2.345 (3) | C11—C12 | 1.375 (7) |
Cd1—O2i | 2.406 (3) | C11—H11 | 0.9300 |
Cd1—O4ii | 2.351 (3) | C12—C13 | 1.353 (8) |
Cd1—O5ii | 2.370 (3) | C12—H12 | 0.9300 |
Cd1—N1 | 2.339 (3) | C13—C14 | 1.385 (7) |
Cd1—N2 | 2.323 (4) | C13—H13 | 0.9300 |
O1—C1 | 1.236 (6) | C14—C15 | 1.378 (6) |
O2—C1 | 1.241 (5) | C14—H14 | 0.9300 |
O2—Cd1i | 2.406 (3) | C15—C16 | 1.496 (6) |
O3—C4 | 1.373 (4) | C16—C17 | 1.375 (6) |
O3—C3 | 1.428 (5) | C17—C18 | 1.387 (7) |
O4—C10 | 1.253 (5) | C17—H17 | 0.9300 |
O4—Cd1iii | 2.351 (3) | C18—C19 | 1.363 (8) |
O5—C10 | 1.257 (5) | C18—H18 | 0.9300 |
O5—Cd1iii | 2.370 (3) | C19—C20 | 1.338 (8) |
N1—C11 | 1.329 (5) | C19—H19 | 0.9300 |
N1—C15 | 1.339 (5) | C20—H20 | 0.9300 |
N2—C16 | 1.345 (5) | O1w—H1w | 0.8200 |
N2—C20 | 1.354 (6) | O1w—H2w | 0.8200 |
C1—C2 | 1.507 (6) | O6—C21 | 1.244 (9) |
C2—C3 | 1.511 (6) | O7—C21 | 1.263 (9) |
C2—H2A | 0.9700 | O7—H7O | 0.8200 |
C2—H2B | 0.9700 | O8—C25 | 1.375 (9) |
C3—H3A | 0.9700 | O8—H8O | 0.8200 |
C3—H3B | 0.9700 | C21—C22 | 1.495 (8) |
C4—C9 | 1.366 (6) | C22—C23 | 1.3900 |
C4—C5 | 1.386 (6) | C22—C27 | 1.3900 |
C5—C6 | 1.385 (5) | C23—C24 | 1.3900 |
C5—H5 | 0.9300 | C23—H23 | 0.9300 |
C6—C7 | 1.390 (6) | C24—C25 | 1.3900 |
C6—H6 | 0.9300 | C24—H24 | 0.9300 |
C7—C8 | 1.379 (6) | C25—C26 | 1.3900 |
C7—C10 | 1.505 (5) | C26—C27 | 1.3900 |
C8—C9 | 1.388 (5) | C26—H26 | 0.9300 |
C8—H8 | 0.9300 | C27—H27 | 0.9300 |
N2—Cd1—N1 | 71.09 (12) | C7—C8—H8 | 119.6 |
N2—Cd1—O2 | 132.62 (13) | C9—C8—H8 | 119.6 |
N1—Cd1—O2 | 99.56 (12) | C4—C9—C8 | 120.0 (4) |
N2—Cd1—O4ii | 84.69 (13) | C4—C9—H9 | 120.0 |
N1—Cd1—O4ii | 114.25 (11) | C8—C9—H9 | 120.0 |
O2—Cd1—O4ii | 137.28 (11) | O4—C10—O5 | 122.2 (4) |
N2—Cd1—O5ii | 98.40 (12) | O4—C10—C7 | 118.6 (4) |
N1—Cd1—O5ii | 166.81 (11) | O5—C10—C7 | 119.2 (4) |
O2—Cd1—O5ii | 93.44 (11) | N1—C11—C12 | 122.8 (5) |
O4ii—Cd1—O5ii | 55.46 (10) | N1—C11—H11 | 118.6 |
N2—Cd1—O2i | 150.29 (13) | C12—C11—H11 | 118.6 |
N1—Cd1—O2i | 88.75 (12) | C13—C12—C11 | 118.3 (5) |
O2—Cd1—O2i | 70.79 (12) | C13—C12—H12 | 120.9 |
O4ii—Cd1—O2i | 84.10 (11) | C11—C12—H12 | 120.9 |
O5ii—Cd1—O2i | 97.67 (11) | C12—C13—C14 | 119.9 (5) |
N2—Cd1—O1 | 80.37 (14) | C12—C13—H13 | 120.1 |
N1—Cd1—O1 | 83.43 (13) | C14—C13—H13 | 120.1 |
O2—Cd1—O1 | 52.26 (12) | C15—C14—C13 | 118.9 (5) |
O4ii—Cd1—O1 | 151.63 (12) | C15—C14—H14 | 120.5 |
O5ii—Cd1—O1 | 103.05 (12) | C13—C14—H14 | 120.5 |
O2i—Cd1—O1 | 119.78 (11) | N1—C15—C14 | 120.9 (4) |
C1—O1—Cd1 | 89.9 (3) | N1—C15—C16 | 117.7 (4) |
C1—O2—Cd1 | 97.7 (3) | C14—C15—C16 | 121.4 (4) |
C1—O2—Cd1i | 144.3 (3) | N2—C16—C17 | 121.5 (4) |
Cd1—O2—Cd1i | 109.21 (12) | N2—C16—C15 | 116.1 (4) |
C4—O3—C3 | 119.1 (3) | C17—C16—C15 | 122.5 (4) |
C10—O4—Cd1iii | 91.5 (2) | C16—C17—C18 | 119.6 (5) |
C10—O5—Cd1iii | 90.5 (2) | C16—C17—H17 | 120.2 |
C11—N1—C15 | 119.2 (4) | C18—C17—H17 | 120.2 |
C11—N1—Cd1 | 123.7 (3) | C19—C18—C17 | 118.8 (5) |
C15—N1—Cd1 | 116.9 (3) | C19—C18—H18 | 120.6 |
C16—N2—C20 | 116.9 (4) | C17—C18—H18 | 120.6 |
C16—N2—Cd1 | 118.1 (3) | C20—C19—C18 | 118.8 (5) |
C20—N2—Cd1 | 124.9 (3) | C20—C19—H19 | 120.6 |
O1—C1—O2 | 119.9 (4) | C18—C19—H19 | 120.6 |
O1—C1—C2 | 119.1 (4) | C19—C20—N2 | 124.5 (5) |
O2—C1—C2 | 121.0 (4) | C19—C20—H20 | 117.8 |
C1—C2—C3 | 112.5 (4) | N2—C20—H20 | 117.8 |
C1—C2—H2A | 109.1 | H1w—O1w—H2w | 108.2 |
C3—C2—H2A | 109.1 | C21—O7—H7O | 120.0 |
C1—C2—H2B | 109.1 | O6—C21—O7 | 120.8 (10) |
C3—C2—H2B | 109.1 | O6—C21—C22 | 120.9 (9) |
H2A—C2—H2B | 107.8 | O7—C21—C22 | 118.2 (10) |
O3—C3—C2 | 105.8 (4) | C23—C22—C27 | 120.0 |
O3—C3—H3A | 110.6 | C23—C22—C21 | 119.5 (6) |
C2—C3—H3A | 110.6 | C27—C22—C21 | 120.5 (6) |
O3—C3—H3B | 110.6 | C22—C23—C24 | 120.0 |
C2—C3—H3B | 110.6 | C22—C23—H23 | 120.0 |
H3A—C3—H3B | 108.7 | C24—C23—H23 | 120.0 |
C9—C4—O3 | 115.8 (4) | C25—C24—C23 | 120.0 |
C9—C4—C5 | 120.5 (4) | C25—C24—H24 | 120.0 |
O3—C4—C5 | 123.7 (4) | C23—C24—H24 | 120.0 |
C6—C5—C4 | 119.1 (4) | O8—C25—C26 | 116.9 (6) |
C6—C5—H5 | 120.4 | O8—C25—C24 | 123.0 (6) |
C4—C5—H5 | 120.4 | C26—C25—C24 | 120.0 |
C5—C6—C7 | 121.0 (4) | C25—C26—C27 | 120.0 |
C5—C6—H6 | 119.5 | C25—C26—H26 | 120.0 |
C7—C6—H6 | 119.5 | C27—C26—H26 | 120.0 |
C8—C7—C6 | 118.6 (3) | C26—C27—C22 | 120.0 |
C8—C7—C10 | 121.3 (4) | C26—C27—H27 | 120.0 |
C6—C7—C10 | 120.0 (4) | C22—C27—H27 | 120.0 |
C7—C8—C9 | 120.8 (4) | ||
N2—Cd1—O1—C1 | 176.3 (3) | C4—C5—C6—C7 | 1.8 (7) |
N1—Cd1—O1—C1 | 104.5 (3) | C5—C6—C7—C8 | −0.7 (7) |
O2—Cd1—O1—C1 | −3.0 (2) | C5—C6—C7—C10 | −177.8 (4) |
O4ii—Cd1—O1—C1 | −124.5 (3) | C6—C7—C8—C9 | 0.3 (7) |
O5ii—Cd1—O1—C1 | −87.2 (3) | C10—C7—C8—C9 | 177.3 (4) |
O2i—Cd1—O1—C1 | 19.7 (3) | O3—C4—C9—C8 | −178.2 (4) |
N2—Cd1—O2—C1 | 2.2 (3) | C5—C4—C9—C8 | 2.1 (7) |
N1—Cd1—O2—C1 | −70.9 (3) | C7—C8—C9—C4 | −1.0 (7) |
O4ii—Cd1—O2—C1 | 146.4 (2) | Cd1iii—O4—C10—O5 | −6.1 (4) |
O5ii—Cd1—O2—C1 | 106.9 (3) | Cd1iii—O4—C10—C7 | 173.3 (3) |
O2i—Cd1—O2—C1 | −156.2 (3) | Cd1iii—O5—C10—O4 | 6.0 (4) |
O1—Cd1—O2—C1 | 3.0 (2) | Cd1iii—O5—C10—C7 | −173.3 (3) |
N2—Cd1—O2—Cd1i | 158.33 (13) | C8—C7—C10—O4 | −170.3 (4) |
N1—Cd1—O2—Cd1i | 85.29 (14) | C6—C7—C10—O4 | 6.7 (6) |
O4ii—Cd1—O2—Cd1i | −57.5 (2) | C8—C7—C10—O5 | 9.1 (6) |
O5ii—Cd1—O2—Cd1i | −96.93 (14) | C6—C7—C10—O5 | −173.9 (4) |
O2i—Cd1—O2—Cd1i | 0.0 | C15—N1—C11—C12 | 0.2 (7) |
O1—Cd1—O2—Cd1i | 159.2 (2) | Cd1—N1—C11—C12 | 175.3 (4) |
N2—Cd1—N1—C11 | −175.4 (4) | N1—C11—C12—C13 | 0.8 (9) |
O2—Cd1—N1—C11 | −43.5 (4) | C11—C12—C13—C14 | 0.2 (11) |
O4ii—Cd1—N1—C11 | 109.8 (4) | C12—C13—C14—C15 | −2.2 (12) |
O5ii—Cd1—N1—C11 | 146.3 (5) | C11—N1—C15—C14 | −2.3 (7) |
O2i—Cd1—N1—C11 | 26.8 (4) | Cd1—N1—C15—C14 | −177.7 (4) |
O1—Cd1—N1—C11 | −93.4 (4) | C11—N1—C15—C16 | 177.0 (4) |
N2—Cd1—N1—C15 | −0.2 (3) | Cd1—N1—C15—C16 | 1.6 (5) |
O2—Cd1—N1—C15 | 131.7 (3) | C13—C14—C15—N1 | 3.3 (9) |
O4ii—Cd1—N1—C15 | −75.1 (3) | C13—C14—C15—C16 | −176.0 (6) |
O5ii—Cd1—N1—C15 | −38.5 (7) | C20—N2—C16—C17 | 0.8 (7) |
O2i—Cd1—N1—C15 | −158.0 (3) | Cd1—N2—C16—C17 | −177.2 (3) |
O1—Cd1—N1—C15 | 81.8 (3) | C20—N2—C16—C15 | −179.3 (5) |
N1—Cd1—N2—C16 | −1.4 (3) | Cd1—N2—C16—C15 | 2.6 (5) |
O2—Cd1—N2—C16 | −87.0 (3) | N1—C15—C16—N2 | −2.9 (6) |
O4ii—Cd1—N2—C16 | 116.5 (3) | C14—C15—C16—N2 | 176.5 (5) |
O5ii—Cd1—N2—C16 | 170.4 (3) | N1—C15—C16—C17 | 177.0 (4) |
O2i—Cd1—N2—C16 | 48.3 (4) | C14—C15—C16—C17 | −3.7 (7) |
O1—Cd1—N2—C16 | −87.7 (3) | N2—C16—C17—C18 | −0.8 (7) |
N1—Cd1—N2—C20 | −179.2 (5) | C15—C16—C17—C18 | 179.4 (5) |
O2—Cd1—N2—C20 | 95.2 (5) | C16—C17—C18—C19 | −0.4 (8) |
O4ii—Cd1—N2—C20 | −61.3 (5) | C17—C18—C19—C20 | 1.5 (10) |
O5ii—Cd1—N2—C20 | −7.4 (5) | C18—C19—C20—N2 | −1.5 (11) |
O2i—Cd1—N2—C20 | −129.5 (5) | C16—N2—C20—C19 | 0.3 (9) |
O1—Cd1—N2—C20 | 94.5 (5) | Cd1—N2—C20—C19 | 178.2 (5) |
Cd1—O1—C1—O2 | 5.2 (4) | O6—C21—C22—C23 | −12.1 (9) |
Cd1—O1—C1—C2 | −174.7 (3) | O7—C21—C22—C23 | 167.9 (9) |
Cd1—O2—C1—O1 | −5.6 (4) | O6—C21—C22—C27 | 169.2 (9) |
Cd1i—O2—C1—O1 | −144.9 (4) | O7—C21—C22—C27 | −10.8 (9) |
Cd1—O2—C1—C2 | 174.3 (3) | C27—C22—C23—C24 | 0.0 |
Cd1i—O2—C1—C2 | 35.1 (7) | C21—C22—C23—C24 | −178.7 (10) |
O1—C1—C2—C3 | 56.4 (6) | C22—C23—C24—C25 | 0.0 |
O2—C1—C2—C3 | −123.5 (5) | C23—C24—C25—O8 | 175.3 (10) |
C4—O3—C3—C2 | −176.0 (4) | C23—C24—C25—C26 | 0.0 |
C1—C2—C3—O3 | −172.8 (4) | O8—C25—C26—C27 | −175.6 (10) |
C3—O3—C4—C9 | −173.5 (4) | C24—C25—C26—C27 | 0.0 |
C3—O3—C4—C5 | 6.2 (6) | C25—C26—C27—C22 | 0.0 |
C9—C4—C5—C6 | −2.5 (7) | C23—C22—C27—C26 | 0.0 |
O3—C4—C5—C6 | 177.8 (4) | C21—C22—C27—C26 | 178.7 (10) |
Symmetry codes: (i) −x+1, −y+1, −z+2; (ii) x−1, y, z+1; (iii) x+1, y, z−1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7o···O1wiv | 0.82 | 1.75 | 2.55 (1) | 166 |
O8—H8o···O1 | 0.82 | 2.01 | 2.815 (8) | 168 |
O1w—H1w···O1v | 0.82 | 1.98 | 2.797 (8) | 171 |
O1w—H2w···O8 | 0.82 | 2.11 | 2.93 (1) | 172 |
Symmetry codes: (iv) x−1, y, z; (v) −x+1, −y+2, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Cd2(C10H8O5)2(C10H8N2)2]·C7H6O3·H2O |
Mr | 1109.63 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 295 |
a, b, c (Å) | 10.1615 (5), 10.6255 (5), 10.8507 (6) |
α, β, γ (°) | 73.147 (2), 82.174 (1), 88.734 (1) |
V (Å3) | 1110.6 (1) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 1.03 |
Crystal size (mm) | 0.32 × 0.24 × 0.16 |
Data collection | |
Diffractometer | Rigaku RAXIS-RAPID diffractometer |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.542, 0.852 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10857, 5010, 3997 |
Rint | 0.042 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.040, 0.120, 1.06 |
No. of reflections | 5010 |
No. of parameters | 341 |
No. of restraints | 4 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.13, −0.87 |
Computer programs: RAPID-AUTO (Rigaku Corporation, 1998), RAPID-AUTO, CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001), OLEX (Dolomanov et al., 2003), publCIF (Westrip, 2007).
Cd1—O1 | 2.511 (4) | Cd1—O5ii | 2.370 (3) |
Cd1—O2 | 2.345 (3) | Cd1—N1 | 2.339 (3) |
Cd1—O2i | 2.406 (3) | Cd1—N2 | 2.323 (4) |
Cd1—O4ii | 2.351 (3) |
Symmetry codes: (i) −x+1, −y+1, −z+2; (ii) x−1, y, z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7o···O1wiii | 0.82 | 1.75 | 2.55 (1) | 166 |
O8—H8o···O1 | 0.82 | 2.01 | 2.815 (8) | 168 |
O1w—H1w···O1iv | 0.82 | 1.98 | 2.797 (8) | 171 |
O1w—H2w···O8 | 0.82 | 2.11 | 2.93 (1) | 172 |
Symmetry codes: (iii) x−1, y, z; (iv) −x+1, −y+2, −z+1. |
The present study on the title compound, (I), follows reports on the transition metal derivatives of 3-(4-carboxylatophenoxy)propionic acid. These (Kong et al., 2007a,b) describe the isostrutural manganese(II) and cobalt(II) adducts with 2,2'-bipyridine. With cadmium nitrate as reactant and by using a hydrothermal method, part of the carboxylic acid is hydrolyzed to give 4-hydroxybenzoic acid, which is then incorporated into the crystal structure (Fig. 1). Topologically, a double ribbon polyer is formed (Fig. 2).
The cadmium(II) atom in (I) exists in a seven-coordinate CdN2O5 enviroment (Fig. 3) that approximates to a monocapped octahedron (Table 1) and a network of O—H···O hydrogen bonds (Table 2) helps to consolidate the structure.