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The 3-(4-carboxyl­atophen­oxy)propionate dianion in the title compound, [Cd2(C10H8O5)2(C10H8N2)2]·C7H6O3·H2O, links adjacent metal atoms into a chain, the dianion chelating through both O atoms of its two –CO2 end groups. One of the carboxylate O atoms (that belonging to the aliphatic carboxylate end) engages in inter­chain coordination, linking two chains into a ribbon. The ribbons are linked to the disordered water mol­ecule and 4-hydroxy­benzoic acid by O—H...O hydrogen bonds, further consolidating the ribbon motif. The CdII atom exists in a seven-coordinate CdN2O5 enviroment that approximates to a monocapped octa­hedron. The dinuclear repeat unit is centrosymmetric.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807054669/hb2610sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807054669/hb2610Isup2.hkl
Contains datablock I

CCDC reference: 672611

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.007 Å
  • Disorder in main residue
  • R factor = 0.040
  • wR factor = 0.120
  • Data-to-parameter ratio = 14.7

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT432_ALERT_2_A Short Inter X...Y Contact O8 .. C25 .. 1.38 Ang.
Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a center-of-inversion. The treatement of the disoder is described in the refinement.
PLAT432_ALERT_2_A Short Inter X...Y Contact  O8     ..  C26     ..       2.36 Ang.
Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a center-of-inversion. The treatement of the disoder is described in the refinement.
PLAT432_ALERT_2_A Short Inter X...Y Contact  O8     ..  C24     ..       2.43 Ang.
Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a center-of-inversion. The treatement of the disoder is described in the refinement.
PLAT432_ALERT_2_A Short Inter X...Y Contact  C22    ..  C24     ..       2.41 Ang.
Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a center-of-inversion. The treatement of the disoder is described in the refinement.
PLAT432_ALERT_2_A Short Inter X...Y Contact  C22    ..  C25     ..       2.78 Ang.
Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a center-of-inversion. The treatement of the disoder is described in the refinement.
PLAT432_ALERT_2_A Short Inter X...Y Contact  C23    ..  C24     ..       1.39 Ang.
Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a center-of-inversion. The treatement of the disoder is described in the refinement.
PLAT432_ALERT_2_A Short Inter X...Y Contact  C23    ..  C25     ..       2.41 Ang.
Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a center-of-inversion. The treatement of the disoder is described in the refinement.
PLAT432_ALERT_2_A Short Inter X...Y Contact  C24    ..  C25     ..       1.39 Ang.
Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a center-of-inversion. The treatement of the disoder is described in the refinement.
PLAT432_ALERT_2_A Short Inter X...Y Contact  C24    ..  C26     ..       2.41 Ang.
Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a center-of-inversion. The treatement of the disoder is described in the refinement.
PLAT432_ALERT_2_A Short Inter X...Y Contact  C24    ..  C27     ..       2.78 Ang.
Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a center-of-inversion. The treatement of the disoder is described in the refinement.
PLAT432_ALERT_2_A Short Inter X...Y Contact  C25    ..  C26     ..       1.39 Ang.
Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a center-of-inversion. The treatement of the disoder is described in the refinement.
PLAT432_ALERT_2_A Short Inter X...Y Contact  C25    ..  C27     ..       2.41 Ang.
Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a center-of-inversion. The treatement of the disoder is described in the refinement.

Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.542 0.852 Tmin(prime) and Tmax expected: 0.714 0.848 RR(prime) = 0.756 Please check that your absorption correction is appropriate. PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.75 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.67 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O1 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C13 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C22 PLAT301_ALERT_3_C Main Residue Disorder ......................... 3.00 Perc. PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.17 Ratio
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 4
12 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 11 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 17 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

Comment top

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.

Related literature top

For the 2,2'-bipyridine chelated transition metal derivatives of 3-(4-carboxylatophenoxy)propionic acid, see: Kong et al. (2007a,b).

Experimental top

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.

Refinement top

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.

Computing details top

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).

Figures top
[Figure 1] Fig. 1. View of a fragment of (I); displacement ellipsoids are drawn at the 50% probability level, and H atoms as spheres of arbitrary radius. Symmetry codes are given in Table 1.
[Figure 2] Fig. 2. A representation of the polymeric double ribbon structure in (I).
[Figure 3] Fig. 3. Seven-coordinate geometry of cadmium in (I).
Poly[[[bis[(2,2'-bipyridine-κ2N,N')cadmium(II)]- bis[µ3-3-(4-carboxylatophenoxy)propionato- κ5O,O':O':O'',O''']] 4-hydroxybenzoic acid monohydrate] top
Crystal data top
[Cd2(C10H8O5)2(C10H8N2)2]·C7H6O3·H2OZ = 1
Mr = 1109.63F(000) = 558
Triclinic, P1Dx = 1.659 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.1615 (5) ÅCell parameters from 8754 reflections
b = 10.6255 (5) Åθ = 3.0–27.5°
c = 10.8507 (6) ŵ = 1.03 mm1
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
Data collection top
Rigaku RAXIS-RAPID
diffractometer
5010 independent reflections
Radiation source: fine-focus sealed tube3997 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
Detector resolution: 10.000 pixels mm-1θmax = 27.5°, θmin = 3.0°
ω–scansh = 1313
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 1113
Tmin = 0.542, Tmax = 0.852l = 1414
10857 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.120H-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 parametersΔρmax = 1.13 e Å3
4 restraintsΔρmin = 0.87 e Å3
Crystal data top
[Cd2(C10H8O5)2(C10H8N2)2]·C7H6O3·H2Oγ = 88.734 (1)°
Mr = 1109.63V = 1110.6 (1) Å3
Triclinic, P1Z = 1
a = 10.1615 (5) ÅMo Kα radiation
b = 10.6255 (5) ŵ = 1.03 mm1
c = 10.8507 (6) ÅT = 295 K
α = 73.147 (2)°0.32 × 0.24 × 0.16 mm
β = 82.174 (1)°
Data collection top
Rigaku RAXIS-RAPID
diffractometer
5010 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
3997 reflections with I > 2σ(I)
Tmin = 0.542, Tmax = 0.852Rint = 0.042
10857 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0404 restraints
wR(F2) = 0.120H-atom parameters constrained
S = 1.06Δρmax = 1.13 e Å3
5010 reflectionsΔρmin = 0.87 e Å3
341 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cd10.42672 (3)0.67472 (3)0.96257 (3)0.04096 (12)
O10.4806 (4)0.6852 (4)0.7269 (3)0.0713 (11)
O20.4891 (3)0.5017 (3)0.8745 (3)0.0503 (7)
O30.7194 (3)0.5162 (4)0.4709 (3)0.0528 (8)
O41.2813 (3)0.7051 (3)0.1393 (3)0.0524 (8)
O51.1998 (3)0.6081 (3)0.0120 (3)0.0501 (8)
N10.6322 (3)0.7835 (4)0.9263 (3)0.0422 (8)
N20.3986 (3)0.8980 (4)0.8686 (4)0.0506 (9)
C10.5078 (4)0.5672 (5)0.7584 (4)0.0423 (10)
C20.5637 (4)0.5052 (6)0.6544 (4)0.0544 (12)
H2A0.49730.50690.59760.065*
H2B0.58310.41390.69480.065*
C30.6886 (4)0.5747 (5)0.5741 (4)0.0501 (11)
H3A0.67380.66810.53990.060*
H3B0.76060.56270.62640.060*
C40.8339 (4)0.5545 (4)0.3857 (4)0.0366 (8)
C50.9291 (4)0.6386 (5)0.4003 (4)0.0470 (10)
H50.91630.67510.46920.056*
C61.0433 (4)0.6675 (5)0.3111 (4)0.0450 (10)
H61.10870.72190.32180.054*
C71.0620 (4)0.6166 (4)0.2057 (4)0.0357 (8)
C80.9646 (4)0.5349 (4)0.1924 (4)0.0407 (9)
H80.97580.49970.12270.049*
C90.8502 (4)0.5047 (5)0.2819 (4)0.0466 (10)
H90.78460.45060.27120.056*
C101.1891 (4)0.6454 (4)0.1128 (4)0.0383 (9)
C110.7459 (4)0.7223 (5)0.9483 (5)0.0507 (11)
H110.74360.63170.98600.061*
C120.8668 (5)0.7873 (6)0.9178 (6)0.0690 (15)
H120.94490.74160.93330.083*
C130.8693 (5)0.9193 (6)0.8645 (8)0.096 (3)
H130.94980.96570.84260.115*
C140.7518 (5)0.9853 (5)0.8427 (7)0.0749 (18)
H140.75211.07640.80900.090*
C150.6343 (4)0.9139 (4)0.8718 (4)0.0405 (9)
C160.5054 (4)0.9786 (4)0.8424 (4)0.0391 (9)
C170.4953 (5)1.1124 (5)0.7919 (5)0.0555 (12)
H170.57021.16670.77540.067*
C180.3730 (5)1.1661 (5)0.7658 (6)0.0638 (14)
H180.36441.25650.73220.077*
C190.2654 (5)1.0838 (6)0.7902 (6)0.0750 (17)
H190.18251.11690.77170.090*
C200.2812 (5)0.9547 (5)0.8413 (6)0.0717 (17)
H200.20640.90010.85940.086*
O1w0.6482 (8)1.1595 (8)0.4750 (9)0.077 (2)0.50
H1w0.61621.21130.41510.092*0.50
H2w0.60571.09010.49590.092*0.50
O60.1473 (12)0.9220 (11)0.5206 (16)0.089 (4)0.50
O70.1003 (11)1.1321 (8)0.4495 (14)0.078 (5)0.50
H7O0.17901.14870.44480.117*0.50
O80.4798 (7)0.9246 (7)0.5287 (8)0.0657 (19)0.50
H8O0.49070.85280.58040.099*0.50
C210.0645 (10)1.0142 (12)0.4888 (14)0.071 (8)0.50
C220.0799 (7)0.9884 (13)0.4960 (19)0.059 (6)0.50
C230.1194 (8)0.8635 (11)0.5611 (16)0.127 (14)0.50
H230.05640.79640.59830.153*0.50
C240.2532 (9)0.8391 (6)0.5707 (10)0.074 (3)0.50
H240.27960.75550.61430.089*0.50
C250.3473 (6)0.9395 (7)0.5152 (8)0.054 (2)0.50
C260.3077 (8)1.0643 (6)0.4500 (8)0.055 (2)0.50
H260.37071.13150.41280.066*0.50
C270.1740 (9)1.0888 (9)0.4404 (14)0.066 (5)0.50
H270.14761.17240.39680.079*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.03119 (16)0.04466 (19)0.04179 (19)0.00141 (12)0.00713 (11)0.00967 (14)
O10.081 (2)0.080 (3)0.040 (2)0.030 (2)0.0032 (17)0.0039 (18)
O20.0553 (17)0.0601 (19)0.0309 (16)0.0082 (15)0.0077 (13)0.0127 (14)
O30.0361 (15)0.083 (2)0.0409 (17)0.0108 (15)0.0124 (12)0.0284 (17)
O40.0339 (15)0.066 (2)0.058 (2)0.0112 (15)0.0079 (13)0.0255 (17)
O50.0414 (16)0.064 (2)0.0483 (18)0.0108 (15)0.0130 (13)0.0295 (16)
N10.0361 (17)0.046 (2)0.044 (2)0.0026 (15)0.0018 (14)0.0144 (16)
N20.0370 (18)0.051 (2)0.057 (2)0.0029 (17)0.0016 (16)0.0078 (19)
C10.0290 (18)0.063 (3)0.035 (2)0.0069 (19)0.0027 (15)0.015 (2)
C20.039 (2)0.091 (4)0.033 (2)0.005 (2)0.0071 (17)0.022 (2)
C30.037 (2)0.077 (3)0.035 (2)0.003 (2)0.0047 (17)0.018 (2)
C40.0277 (17)0.045 (2)0.034 (2)0.0036 (16)0.0028 (14)0.0099 (17)
C50.038 (2)0.065 (3)0.042 (2)0.004 (2)0.0039 (17)0.025 (2)
C60.035 (2)0.058 (3)0.045 (2)0.0091 (19)0.0054 (17)0.025 (2)
C70.0322 (18)0.036 (2)0.036 (2)0.0016 (16)0.0032 (15)0.0087 (17)
C80.041 (2)0.048 (2)0.034 (2)0.0034 (18)0.0062 (16)0.0185 (18)
C90.037 (2)0.059 (3)0.046 (3)0.011 (2)0.0058 (17)0.022 (2)
C100.0299 (18)0.038 (2)0.043 (2)0.0038 (16)0.0025 (16)0.0093 (18)
C110.043 (2)0.046 (2)0.060 (3)0.006 (2)0.010 (2)0.010 (2)
C120.039 (2)0.063 (3)0.102 (5)0.004 (2)0.010 (3)0.020 (3)
C130.039 (3)0.063 (4)0.176 (8)0.007 (3)0.012 (4)0.019 (4)
C140.047 (3)0.040 (3)0.126 (6)0.002 (2)0.010 (3)0.009 (3)
C150.040 (2)0.038 (2)0.045 (2)0.0003 (17)0.0021 (17)0.0174 (19)
C160.044 (2)0.039 (2)0.034 (2)0.0084 (18)0.0026 (16)0.0125 (17)
C170.057 (3)0.041 (2)0.068 (3)0.002 (2)0.014 (2)0.013 (2)
C180.064 (3)0.055 (3)0.067 (4)0.010 (3)0.018 (3)0.005 (3)
C190.051 (3)0.074 (4)0.084 (4)0.017 (3)0.022 (3)0.007 (3)
C200.042 (2)0.055 (3)0.104 (5)0.003 (2)0.017 (3)0.002 (3)
O1w0.071 (5)0.061 (5)0.082 (6)0.008 (5)0.024 (5)0.011 (4)
O60.068 (6)0.077 (8)0.132 (12)0.000 (6)0.044 (8)0.032 (7)
O70.065 (6)0.035 (5)0.134 (13)0.010 (5)0.022 (7)0.021 (7)
O80.060 (4)0.060 (4)0.066 (5)0.003 (4)0.008 (3)0.000 (4)
C210.068 (10)0.069 (19)0.082 (17)0.005 (11)0.027 (10)0.025 (13)
C220.059 (10)0.065 (17)0.053 (10)0.009 (10)0.011 (8)0.013 (10)
C230.12 (2)0.14 (2)0.092 (18)0.026 (17)0.050 (17)0.025 (16)
C240.069 (7)0.048 (6)0.098 (10)0.004 (6)0.035 (7)0.000 (6)
C250.062 (6)0.050 (6)0.044 (5)0.002 (5)0.007 (4)0.004 (5)
C260.060 (6)0.044 (5)0.056 (6)0.003 (4)0.004 (5)0.009 (4)
C270.079 (11)0.045 (8)0.066 (9)0.001 (7)0.007 (7)0.004 (6)
Geometric parameters (Å, º) top
Cd1—O12.511 (4)C9—H90.9300
Cd1—O22.345 (3)C11—C121.375 (7)
Cd1—O2i2.406 (3)C11—H110.9300
Cd1—O4ii2.351 (3)C12—C131.353 (8)
Cd1—O5ii2.370 (3)C12—H120.9300
Cd1—N12.339 (3)C13—C141.385 (7)
Cd1—N22.323 (4)C13—H130.9300
O1—C11.236 (6)C14—C151.378 (6)
O2—C11.241 (5)C14—H140.9300
O2—Cd1i2.406 (3)C15—C161.496 (6)
O3—C41.373 (4)C16—C171.375 (6)
O3—C31.428 (5)C17—C181.387 (7)
O4—C101.253 (5)C17—H170.9300
O4—Cd1iii2.351 (3)C18—C191.363 (8)
O5—C101.257 (5)C18—H180.9300
O5—Cd1iii2.370 (3)C19—C201.338 (8)
N1—C111.329 (5)C19—H190.9300
N1—C151.339 (5)C20—H200.9300
N2—C161.345 (5)O1w—H1w0.8200
N2—C201.354 (6)O1w—H2w0.8200
C1—C21.507 (6)O6—C211.244 (9)
C2—C31.511 (6)O7—C211.263 (9)
C2—H2A0.9700O7—H7O0.8200
C2—H2B0.9700O8—C251.375 (9)
C3—H3A0.9700O8—H8O0.8200
C3—H3B0.9700C21—C221.495 (8)
C4—C91.366 (6)C22—C231.3900
C4—C51.386 (6)C22—C271.3900
C5—C61.385 (5)C23—C241.3900
C5—H50.9300C23—H230.9300
C6—C71.390 (6)C24—C251.3900
C6—H60.9300C24—H240.9300
C7—C81.379 (6)C25—C261.3900
C7—C101.505 (5)C26—C271.3900
C8—C91.388 (5)C26—H260.9300
C8—H80.9300C27—H270.9300
N2—Cd1—N171.09 (12)C7—C8—H8119.6
N2—Cd1—O2132.62 (13)C9—C8—H8119.6
N1—Cd1—O299.56 (12)C4—C9—C8120.0 (4)
N2—Cd1—O4ii84.69 (13)C4—C9—H9120.0
N1—Cd1—O4ii114.25 (11)C8—C9—H9120.0
O2—Cd1—O4ii137.28 (11)O4—C10—O5122.2 (4)
N2—Cd1—O5ii98.40 (12)O4—C10—C7118.6 (4)
N1—Cd1—O5ii166.81 (11)O5—C10—C7119.2 (4)
O2—Cd1—O5ii93.44 (11)N1—C11—C12122.8 (5)
O4ii—Cd1—O5ii55.46 (10)N1—C11—H11118.6
N2—Cd1—O2i150.29 (13)C12—C11—H11118.6
N1—Cd1—O2i88.75 (12)C13—C12—C11118.3 (5)
O2—Cd1—O2i70.79 (12)C13—C12—H12120.9
O4ii—Cd1—O2i84.10 (11)C11—C12—H12120.9
O5ii—Cd1—O2i97.67 (11)C12—C13—C14119.9 (5)
N2—Cd1—O180.37 (14)C12—C13—H13120.1
N1—Cd1—O183.43 (13)C14—C13—H13120.1
O2—Cd1—O152.26 (12)C15—C14—C13118.9 (5)
O4ii—Cd1—O1151.63 (12)C15—C14—H14120.5
O5ii—Cd1—O1103.05 (12)C13—C14—H14120.5
O2i—Cd1—O1119.78 (11)N1—C15—C14120.9 (4)
C1—O1—Cd189.9 (3)N1—C15—C16117.7 (4)
C1—O2—Cd197.7 (3)C14—C15—C16121.4 (4)
C1—O2—Cd1i144.3 (3)N2—C16—C17121.5 (4)
Cd1—O2—Cd1i109.21 (12)N2—C16—C15116.1 (4)
C4—O3—C3119.1 (3)C17—C16—C15122.5 (4)
C10—O4—Cd1iii91.5 (2)C16—C17—C18119.6 (5)
C10—O5—Cd1iii90.5 (2)C16—C17—H17120.2
C11—N1—C15119.2 (4)C18—C17—H17120.2
C11—N1—Cd1123.7 (3)C19—C18—C17118.8 (5)
C15—N1—Cd1116.9 (3)C19—C18—H18120.6
C16—N2—C20116.9 (4)C17—C18—H18120.6
C16—N2—Cd1118.1 (3)C20—C19—C18118.8 (5)
C20—N2—Cd1124.9 (3)C20—C19—H19120.6
O1—C1—O2119.9 (4)C18—C19—H19120.6
O1—C1—C2119.1 (4)C19—C20—N2124.5 (5)
O2—C1—C2121.0 (4)C19—C20—H20117.8
C1—C2—C3112.5 (4)N2—C20—H20117.8
C1—C2—H2A109.1H1w—O1w—H2w108.2
C3—C2—H2A109.1C21—O7—H7O120.0
C1—C2—H2B109.1O6—C21—O7120.8 (10)
C3—C2—H2B109.1O6—C21—C22120.9 (9)
H2A—C2—H2B107.8O7—C21—C22118.2 (10)
O3—C3—C2105.8 (4)C23—C22—C27120.0
O3—C3—H3A110.6C23—C22—C21119.5 (6)
C2—C3—H3A110.6C27—C22—C21120.5 (6)
O3—C3—H3B110.6C22—C23—C24120.0
C2—C3—H3B110.6C22—C23—H23120.0
H3A—C3—H3B108.7C24—C23—H23120.0
C9—C4—O3115.8 (4)C25—C24—C23120.0
C9—C4—C5120.5 (4)C25—C24—H24120.0
O3—C4—C5123.7 (4)C23—C24—H24120.0
C6—C5—C4119.1 (4)O8—C25—C26116.9 (6)
C6—C5—H5120.4O8—C25—C24123.0 (6)
C4—C5—H5120.4C26—C25—C24120.0
C5—C6—C7121.0 (4)C25—C26—C27120.0
C5—C6—H6119.5C25—C26—H26120.0
C7—C6—H6119.5C27—C26—H26120.0
C8—C7—C6118.6 (3)C26—C27—C22120.0
C8—C7—C10121.3 (4)C26—C27—H27120.0
C6—C7—C10120.0 (4)C22—C27—H27120.0
C7—C8—C9120.8 (4)
N2—Cd1—O1—C1176.3 (3)C4—C5—C6—C71.8 (7)
N1—Cd1—O1—C1104.5 (3)C5—C6—C7—C80.7 (7)
O2—Cd1—O1—C13.0 (2)C5—C6—C7—C10177.8 (4)
O4ii—Cd1—O1—C1124.5 (3)C6—C7—C8—C90.3 (7)
O5ii—Cd1—O1—C187.2 (3)C10—C7—C8—C9177.3 (4)
O2i—Cd1—O1—C119.7 (3)O3—C4—C9—C8178.2 (4)
N2—Cd1—O2—C12.2 (3)C5—C4—C9—C82.1 (7)
N1—Cd1—O2—C170.9 (3)C7—C8—C9—C41.0 (7)
O4ii—Cd1—O2—C1146.4 (2)Cd1iii—O4—C10—O56.1 (4)
O5ii—Cd1—O2—C1106.9 (3)Cd1iii—O4—C10—C7173.3 (3)
O2i—Cd1—O2—C1156.2 (3)Cd1iii—O5—C10—O46.0 (4)
O1—Cd1—O2—C13.0 (2)Cd1iii—O5—C10—C7173.3 (3)
N2—Cd1—O2—Cd1i158.33 (13)C8—C7—C10—O4170.3 (4)
N1—Cd1—O2—Cd1i85.29 (14)C6—C7—C10—O46.7 (6)
O4ii—Cd1—O2—Cd1i57.5 (2)C8—C7—C10—O59.1 (6)
O5ii—Cd1—O2—Cd1i96.93 (14)C6—C7—C10—O5173.9 (4)
O2i—Cd1—O2—Cd1i0.0C15—N1—C11—C120.2 (7)
O1—Cd1—O2—Cd1i159.2 (2)Cd1—N1—C11—C12175.3 (4)
N2—Cd1—N1—C11175.4 (4)N1—C11—C12—C130.8 (9)
O2—Cd1—N1—C1143.5 (4)C11—C12—C13—C140.2 (11)
O4ii—Cd1—N1—C11109.8 (4)C12—C13—C14—C152.2 (12)
O5ii—Cd1—N1—C11146.3 (5)C11—N1—C15—C142.3 (7)
O2i—Cd1—N1—C1126.8 (4)Cd1—N1—C15—C14177.7 (4)
O1—Cd1—N1—C1193.4 (4)C11—N1—C15—C16177.0 (4)
N2—Cd1—N1—C150.2 (3)Cd1—N1—C15—C161.6 (5)
O2—Cd1—N1—C15131.7 (3)C13—C14—C15—N13.3 (9)
O4ii—Cd1—N1—C1575.1 (3)C13—C14—C15—C16176.0 (6)
O5ii—Cd1—N1—C1538.5 (7)C20—N2—C16—C170.8 (7)
O2i—Cd1—N1—C15158.0 (3)Cd1—N2—C16—C17177.2 (3)
O1—Cd1—N1—C1581.8 (3)C20—N2—C16—C15179.3 (5)
N1—Cd1—N2—C161.4 (3)Cd1—N2—C16—C152.6 (5)
O2—Cd1—N2—C1687.0 (3)N1—C15—C16—N22.9 (6)
O4ii—Cd1—N2—C16116.5 (3)C14—C15—C16—N2176.5 (5)
O5ii—Cd1—N2—C16170.4 (3)N1—C15—C16—C17177.0 (4)
O2i—Cd1—N2—C1648.3 (4)C14—C15—C16—C173.7 (7)
O1—Cd1—N2—C1687.7 (3)N2—C16—C17—C180.8 (7)
N1—Cd1—N2—C20179.2 (5)C15—C16—C17—C18179.4 (5)
O2—Cd1—N2—C2095.2 (5)C16—C17—C18—C190.4 (8)
O4ii—Cd1—N2—C2061.3 (5)C17—C18—C19—C201.5 (10)
O5ii—Cd1—N2—C207.4 (5)C18—C19—C20—N21.5 (11)
O2i—Cd1—N2—C20129.5 (5)C16—N2—C20—C190.3 (9)
O1—Cd1—N2—C2094.5 (5)Cd1—N2—C20—C19178.2 (5)
Cd1—O1—C1—O25.2 (4)O6—C21—C22—C2312.1 (9)
Cd1—O1—C1—C2174.7 (3)O7—C21—C22—C23167.9 (9)
Cd1—O2—C1—O15.6 (4)O6—C21—C22—C27169.2 (9)
Cd1i—O2—C1—O1144.9 (4)O7—C21—C22—C2710.8 (9)
Cd1—O2—C1—C2174.3 (3)C27—C22—C23—C240.0
Cd1i—O2—C1—C235.1 (7)C21—C22—C23—C24178.7 (10)
O1—C1—C2—C356.4 (6)C22—C23—C24—C250.0
O2—C1—C2—C3123.5 (5)C23—C24—C25—O8175.3 (10)
C4—O3—C3—C2176.0 (4)C23—C24—C25—C260.0
C1—C2—C3—O3172.8 (4)O8—C25—C26—C27175.6 (10)
C3—O3—C4—C9173.5 (4)C24—C25—C26—C270.0
C3—O3—C4—C56.2 (6)C25—C26—C27—C220.0
C9—C4—C5—C62.5 (7)C23—C22—C27—C260.0
O3—C4—C5—C6177.8 (4)C21—C22—C27—C26178.7 (10)
Symmetry codes: (i) x+1, y+1, z+2; (ii) x1, y, z+1; (iii) x+1, y, z1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7o···O1wiv0.821.752.55 (1)166
O8—H8o···O10.822.012.815 (8)168
O1w—H1w···O1v0.821.982.797 (8)171
O1w—H2w···O80.822.112.93 (1)172
Symmetry codes: (iv) x1, y, z; (v) x+1, y+2, z+1.

Experimental details

Crystal data
Chemical formula[Cd2(C10H8O5)2(C10H8N2)2]·C7H6O3·H2O
Mr1109.63
Crystal system, space groupTriclinic, 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)
V3)1110.6 (1)
Z1
Radiation typeMo Kα
µ (mm1)1.03
Crystal size (mm)0.32 × 0.24 × 0.16
Data collection
DiffractometerRigaku RAXIS-RAPID
diffractometer
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.542, 0.852
No. of measured, independent and
observed [I > 2σ(I)] reflections
10857, 5010, 3997
Rint0.042
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.040, 0.120, 1.06
No. of reflections5010
No. of parameters341
No. of restraints4
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)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).

Selected bond lengths (Å) top
Cd1—O12.511 (4)Cd1—O5ii2.370 (3)
Cd1—O22.345 (3)Cd1—N12.339 (3)
Cd1—O2i2.406 (3)Cd1—N22.323 (4)
Cd1—O4ii2.351 (3)
Symmetry codes: (i) x+1, y+1, z+2; (ii) x1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7o···O1wiii0.821.752.55 (1)166
O8—H8o···O10.822.012.815 (8)168
O1w—H1w···O1iv0.821.982.797 (8)171
O1w—H2w···O80.822.112.93 (1)172
Symmetry codes: (iii) x1, y, z; (iv) x+1, y+2, z+1.
 

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