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The CdII atom in the title complex, [Cd(C8H5O3)2(C12H8N2)(H2O)], is coordinated by three O atoms of two formyl­benzoate ligands, two N atoms of a 1,10-phenanthroline ligand and one water mol­ecule, giving rise to a trigonal–prismatic coordination geometry. Adjacent complex mol­ecules are linked into a two-dimensional layer structure via hydrogen-bonding inter­actions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807048787/im2036sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807048787/im2036Isup2.hkl
Contains datablock I

CCDC reference: 667136

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.025
  • wR factor = 0.063
  • Data-to-parameter ratio = 13.8

checkCIF/PLATON results

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Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.27 PLAT230_ALERT_2_C Hirshfeld Test Diff for O1 - C1 .. 5.92 su PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 27.44 From the CIF: _reflns_number_total 4825 Count of symmetry unique reflns 2872 Completeness (_total/calc) 168.00% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1953 Fraction of Friedel pairs measured 0.680 Are heavy atom types Z>Si present yes PLAT794_ALERT_5_G Check Predicted Bond Valency for Cd1 (2) 2.16 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 4
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 0 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 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Comment top

An earlier report (Deng et al., 2006a) detailed the synthesis and crystal structure of a zinc complex with 1,10-phenanthroline and 4-formylbenzoato ligands. Replacing zinc by cadmium in a similar reaction leads to the formation of the title complex, (I) (Fig. 1). The Cd(II) atom displays a trigonal prismatic geometry, which is different from the zinc complex and another cadmium phenanthroline adduct, (II) (Deng et al., 2006b). The two basal planes of the trigonal prism are built up by O1, O1, N2 and O2, O4, N1, respectively. The Cd—O and Cd—N bond lengths are similar to complex (II). Interestingly, one of the 4-formylbenzoato ligands shows a coordination to cadmium only via one of the oxygen atoms whereas the other oxygen atom is engaged in a strong intramolecular hydrogen bond toward the aqua ligand. Adjacent complex molecules are linked into a two-dimensional layer structure via hydrogen-bonding interactions (Table 1, Fig. 2).

Related literature top

For the zinc phenanthroline adduct, see Deng, Gao, Huo et al. (2006), and for the cadmium phenanthroline complex, see Deng, Gao & Ng (2006).

Experimental top

Cadmium(II) diacetate trihydrate (0.14 g, 0.5 mmol) was added to an H2O/EtOH solution (1:1 v/v) of 4-formylbenzoic acid (0.15 g, 1 mmol) and 1,10-phenanthroline (0.099 g 0.5 mmol). Sodium hydroxide (0.1 M) was added dropwise until the solution registered a pH of 5. Pale yellow single crystals separated from the filtered solution after several days. Elemental analysis: calcd. for C28H20N2O7Cd: C 55.23, H 3.31, N 4.60. Found: C 55.25, H 3.24, N 4.62.

Refinement top

Carbon-bound H atoms were placed in calculated positions, with C—H = 0.93 and Uiso(H) = 1.2Ueq (C), and were included in the refinement in the riding model approximation. The H atoms of water molecules were located in difference Fourier maps and refined with the O—H and H···H distance restraints to 0.85 (1) and 1.39 (1) Å, and with Uiso(H) = 1.5Ueq(O).

Structure description top

An earlier report (Deng et al., 2006a) detailed the synthesis and crystal structure of a zinc complex with 1,10-phenanthroline and 4-formylbenzoato ligands. Replacing zinc by cadmium in a similar reaction leads to the formation of the title complex, (I) (Fig. 1). The Cd(II) atom displays a trigonal prismatic geometry, which is different from the zinc complex and another cadmium phenanthroline adduct, (II) (Deng et al., 2006b). The two basal planes of the trigonal prism are built up by O1, O1, N2 and O2, O4, N1, respectively. The Cd—O and Cd—N bond lengths are similar to complex (II). Interestingly, one of the 4-formylbenzoato ligands shows a coordination to cadmium only via one of the oxygen atoms whereas the other oxygen atom is engaged in a strong intramolecular hydrogen bond toward the aqua ligand. Adjacent complex molecules are linked into a two-dimensional layer structure via hydrogen-bonding interactions (Table 1, Fig. 2).

For the zinc phenanthroline adduct, see Deng, Gao, Huo et al. (2006), and for the cadmium phenanthroline complex, see Deng, Gao & Ng (2006).

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO (Rigaku, 1998); 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 (Sheldrick, 1997).

Figures top
[Figure 1] Fig. 1. Molecular structure of the title compound with 30% probability ellipsoid for the non-H atoms. Dashed lines indicate O—H···O hydrogen bonds.
[Figure 2] Fig. 2. Two-dimensional-layer structure of the title complex along the ab plane formed by hydrogen-bonding, with the O—H···O hydrogen bonds denoted by dashed lines. H atoms not involved in hydrogen bonding have been omitted.
Aquabis(4-formylbenzoato)-κ2O,O';κO- (1,10-phenanthroline-κ2N,N')cadmium(II) top
Crystal data top
[Cd(C8H5O3)2(C12H8N2)(H2O)]F(000) = 612
Mr = 608.86Dx = 1.656 Mg m3
Monoclinic, P21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ybCell parameters from 11052 reflections
a = 6.357 (1) Åθ = 3.2–27.4°
b = 19.668 (4) ŵ = 0.95 mm1
c = 9.766 (2) ÅT = 295 K
β = 90.11 (3)°Prism, pale yellow
V = 1221.0 (4) Å30.34 × 0.21 × 0.18 mm
Z = 2
Data collection top
Rigaku R-AXIS RAPID
diffractometer
4825 independent reflections
Radiation source: fine-focus sealed tube4537 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
Detector resolution: 10.000 pixels mm-1θmax = 27.4°, θmin = 3.2°
ω scansh = 88
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 2521
Tmin = 0.739, Tmax = 0.848l = 1212
11897 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.025H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.063 w = 1/[σ2(Fo2) + (0.0347P)2 + 0.1062P]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max < 0.001
4825 reflectionsΔρmax = 0.56 e Å3
349 parametersΔρmin = 0.25 e Å3
4 restraintsAbsolute structure: Flack (1983), from 1957 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.01 (2)
Crystal data top
[Cd(C8H5O3)2(C12H8N2)(H2O)]V = 1221.0 (4) Å3
Mr = 608.86Z = 2
Monoclinic, P21Mo Kα radiation
a = 6.357 (1) ŵ = 0.95 mm1
b = 19.668 (4) ÅT = 295 K
c = 9.766 (2) Å0.34 × 0.21 × 0.18 mm
β = 90.11 (3)°
Data collection top
Rigaku R-AXIS RAPID
diffractometer
4825 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
4537 reflections with I > 2σ(I)
Tmin = 0.739, Tmax = 0.848Rint = 0.024
11897 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.025H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.063Δρmax = 0.56 e Å3
S = 1.05Δρmin = 0.25 e Å3
4825 reflectionsAbsolute structure: Flack (1983), from 1957 Friedel pairs
349 parametersAbsolute structure parameter: 0.01 (2)
4 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cd10.77987 (3)0.712516 (17)0.315510 (15)0.04216 (7)
O1W1.1049 (4)0.73572 (17)0.3948 (3)0.0812 (10)
H1W11.211 (7)0.709 (3)0.401 (5)0.122*
H1W21.074 (8)0.749 (3)0.476 (2)0.122*
O10.7527 (4)0.61002 (14)0.4439 (3)0.0509 (6)
O20.4560 (4)0.65579 (13)0.3778 (3)0.0565 (6)
O30.1403 (6)0.3939 (2)0.8716 (4)0.1075 (12)
O40.6851 (4)0.79973 (15)0.4452 (3)0.0553 (7)
O50.9706 (4)0.82545 (17)0.5680 (3)0.0810 (10)
O60.3252 (5)1.0274 (2)0.9929 (3)0.0981 (12)
N10.5860 (4)0.75318 (13)0.1303 (2)0.0437 (6)
N20.9394 (4)0.67398 (13)0.1142 (2)0.0424 (5)
C10.5570 (5)0.61234 (16)0.4443 (3)0.0413 (6)
C20.4344 (5)0.56143 (16)0.5297 (3)0.0404 (6)
C30.5283 (6)0.53018 (18)0.6406 (3)0.0462 (7)
H30.66740.54000.66270.055*
C40.4147 (6)0.48377 (18)0.7196 (4)0.0486 (8)
H40.47740.46340.79530.058*
C50.2109 (5)0.46823 (19)0.6856 (3)0.0478 (7)
C60.1167 (5)0.49958 (18)0.5737 (3)0.0491 (7)
H60.02100.48870.55010.059*
C70.2267 (5)0.54710 (16)0.4970 (3)0.0444 (6)
H70.16160.56920.42420.053*
C80.0849 (7)0.4194 (2)0.7671 (4)0.0691 (10)
H80.04760.40780.73400.083*
C90.7805 (5)0.83037 (17)0.5412 (3)0.0505 (7)
C100.6485 (6)0.87646 (16)0.6317 (3)0.0453 (7)
C110.7320 (5)0.90185 (18)0.7532 (3)0.0499 (7)
H110.86900.89090.77840.060*
C120.6124 (5)0.94315 (18)0.8366 (3)0.0528 (8)
H120.66850.95980.91800.063*
C130.4075 (5)0.95998 (17)0.7986 (4)0.0495 (7)
C140.3249 (6)0.93475 (19)0.6781 (4)0.0500 (8)
H140.18850.94610.65240.060*
C150.4445 (6)0.89241 (18)0.5951 (4)0.0480 (8)
H150.38710.87480.51490.058*
C160.2764 (7)1.0020 (2)0.8867 (5)0.0696 (11)
H160.13971.01000.85680.083*
C170.4134 (6)0.79067 (18)0.1388 (4)0.0572 (8)
H170.37300.80710.22410.069*
C180.2888 (6)0.8067 (2)0.0242 (5)0.0632 (10)
H180.16730.83250.03380.076*
C190.3491 (6)0.78362 (18)0.1008 (4)0.0582 (8)
H190.26900.79400.17780.070*
C200.5308 (5)0.74446 (15)0.1141 (3)0.0467 (7)
C210.6059 (6)0.7193 (3)0.2424 (3)0.0562 (8)
H210.52970.72820.32180.067*
C220.7857 (6)0.68279 (18)0.2503 (3)0.0565 (8)
H220.83180.66800.33550.068*
C230.9054 (5)0.66654 (16)0.1326 (3)0.0455 (7)
C241.0926 (6)0.62859 (17)0.1353 (3)0.0549 (8)
H241.14600.61340.21850.066*
C251.1962 (6)0.61390 (19)0.0170 (4)0.0575 (9)
H251.31950.58850.01860.069*
C261.1154 (5)0.63739 (18)0.1059 (3)0.0510 (7)
H261.18720.62710.18630.061*
C270.8340 (5)0.68927 (14)0.0025 (3)0.0389 (6)
C280.6459 (5)0.72926 (13)0.0058 (3)0.0399 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.04758 (10)0.04581 (11)0.03311 (9)0.00347 (12)0.00606 (6)0.00381 (13)
O1W0.0490 (14)0.102 (2)0.0932 (19)0.0088 (13)0.0024 (13)0.0504 (17)
O10.0371 (12)0.0630 (16)0.0527 (14)0.0030 (11)0.0002 (10)0.0125 (12)
O20.0487 (13)0.0534 (14)0.0675 (14)0.0010 (10)0.0033 (11)0.0188 (12)
O30.102 (3)0.120 (3)0.100 (3)0.027 (2)0.006 (2)0.045 (2)
O40.0585 (17)0.0584 (16)0.0489 (13)0.0005 (13)0.0046 (12)0.0139 (11)
O50.0510 (15)0.095 (2)0.097 (2)0.0037 (14)0.0073 (14)0.0544 (19)
O60.087 (2)0.116 (3)0.091 (2)0.032 (2)0.0099 (17)0.058 (2)
N10.0517 (14)0.0401 (13)0.0393 (12)0.0007 (11)0.0097 (10)0.0020 (10)
N20.0485 (14)0.0406 (13)0.0381 (12)0.0036 (11)0.0051 (10)0.0012 (10)
C10.0498 (17)0.0401 (15)0.0339 (13)0.0004 (13)0.0027 (12)0.0038 (12)
C20.0404 (15)0.0406 (16)0.0401 (14)0.0019 (12)0.0044 (12)0.0039 (12)
C30.0381 (18)0.0547 (19)0.0460 (17)0.0008 (14)0.0046 (14)0.0011 (15)
C40.0498 (19)0.052 (2)0.0441 (17)0.0009 (15)0.0026 (14)0.0085 (15)
C50.0509 (19)0.0442 (18)0.0482 (17)0.0007 (14)0.0061 (14)0.0020 (13)
C60.0419 (16)0.0565 (19)0.0489 (16)0.0082 (13)0.0008 (13)0.0018 (14)
C70.0418 (15)0.0490 (16)0.0424 (14)0.0003 (13)0.0020 (11)0.0007 (13)
C80.071 (3)0.071 (3)0.066 (2)0.014 (2)0.0047 (19)0.016 (2)
C90.058 (2)0.0454 (18)0.0481 (17)0.0082 (14)0.0107 (14)0.0070 (14)
C100.0492 (18)0.0404 (16)0.0464 (15)0.0092 (13)0.0018 (14)0.0046 (13)
C110.0489 (17)0.0514 (18)0.0494 (17)0.0017 (14)0.0025 (13)0.0106 (15)
C120.0541 (19)0.0557 (19)0.0484 (17)0.0035 (15)0.0063 (14)0.0149 (15)
C130.0521 (18)0.0422 (16)0.0542 (18)0.0016 (14)0.0006 (14)0.0065 (15)
C140.045 (2)0.053 (2)0.0516 (19)0.0052 (15)0.0092 (15)0.0007 (15)
C150.051 (2)0.0509 (19)0.0417 (17)0.0057 (15)0.0059 (14)0.0044 (15)
C160.060 (2)0.071 (3)0.078 (3)0.0143 (19)0.0025 (19)0.026 (2)
C170.065 (2)0.0492 (18)0.0573 (19)0.0038 (16)0.0151 (16)0.0040 (16)
C180.055 (2)0.051 (2)0.083 (3)0.0109 (18)0.0106 (19)0.0154 (19)
C190.063 (2)0.0502 (19)0.062 (2)0.0018 (16)0.0046 (16)0.0161 (16)
C200.0604 (19)0.0378 (15)0.0417 (14)0.0101 (14)0.0002 (13)0.0074 (12)
C210.081 (2)0.051 (2)0.0364 (11)0.010 (2)0.0048 (12)0.0092 (18)
C220.082 (2)0.0528 (18)0.0348 (14)0.0080 (17)0.0051 (14)0.0051 (13)
C230.0585 (18)0.0381 (15)0.0399 (14)0.0081 (13)0.0110 (13)0.0037 (12)
C240.067 (2)0.0455 (18)0.0519 (17)0.0034 (15)0.0189 (15)0.0102 (15)
C250.057 (2)0.0475 (19)0.068 (2)0.0011 (17)0.0150 (18)0.0067 (17)
C260.0498 (18)0.0514 (18)0.0519 (17)0.0006 (14)0.0034 (13)0.0008 (15)
C270.0488 (16)0.0327 (13)0.0351 (12)0.0090 (10)0.0049 (11)0.0009 (10)
C280.0488 (15)0.0327 (17)0.0382 (12)0.0085 (10)0.0053 (10)0.0022 (10)
Geometric parameters (Å, º) top
Cd1—O12.381 (3)C10—C151.381 (5)
Cd1—O22.420 (2)C10—C111.392 (5)
Cd1—O1W2.252 (3)C11—C121.379 (5)
Cd1—O42.216 (3)C11—H110.9300
Cd1—N12.328 (3)C12—C131.394 (5)
Cd1—N22.340 (2)C12—H120.9300
Cd1—C12.735 (3)C13—C141.380 (5)
O1W—H1W10.86 (5)C13—C161.457 (5)
O1W—H1W20.86 (3)C14—C151.390 (5)
O1—C11.245 (4)C14—H140.9300
O2—C11.250 (4)C15—H150.9300
O3—C81.190 (5)C16—H160.9300
O4—C91.268 (4)C17—C181.406 (6)
O5—C91.239 (4)C17—H170.9300
O6—C161.191 (5)C18—C191.358 (6)
N1—C171.324 (4)C18—H180.9300
N1—C281.359 (3)C19—C201.395 (5)
N2—C261.333 (4)C19—H190.9300
N2—C271.355 (4)C20—C281.412 (4)
C1—C21.519 (4)C20—C211.430 (4)
C2—C31.380 (4)C21—C221.352 (6)
C2—C71.387 (4)C21—H210.9300
C3—C41.397 (5)C22—C231.414 (5)
C3—H30.9300C22—H220.9300
C4—C51.371 (5)C23—C241.405 (5)
C4—H40.9300C23—C271.422 (4)
C5—C61.389 (5)C24—C251.360 (6)
C5—C81.483 (5)C24—H240.9300
C6—C71.388 (5)C25—C261.386 (5)
C6—H60.9300C25—H250.9300
C7—H70.9300C26—H260.9300
C8—H80.9300C27—C281.434 (4)
C9—C101.520 (5)
O4—Cd1—O1W84.07 (10)O5—C9—O4125.7 (3)
O4—Cd1—N191.94 (10)O5—C9—C10117.6 (3)
O1W—Cd1—N1132.97 (11)O4—C9—C10116.7 (3)
O4—Cd1—N2148.15 (10)C15—C10—C11119.7 (3)
O1W—Cd1—N287.48 (9)C15—C10—C9120.3 (3)
N1—Cd1—N271.84 (9)C11—C10—C9120.0 (3)
O4—Cd1—O1109.54 (9)C12—C11—C10120.3 (3)
O1W—Cd1—O193.32 (11)C12—C11—H11119.8
N1—Cd1—O1131.38 (9)C10—C11—H11119.8
N2—Cd1—O1101.55 (9)C11—C12—C13119.9 (3)
O4—Cd1—O288.91 (10)C11—C12—H12120.0
O1W—Cd1—O2141.94 (10)C13—C12—H12120.0
N1—Cd1—O284.49 (9)C14—C13—C12119.7 (3)
N2—Cd1—O2115.59 (9)C14—C13—C16119.4 (3)
O1—Cd1—O254.18 (8)C12—C13—C16120.9 (3)
O4—Cd1—C198.82 (10)C13—C14—C15120.4 (3)
O1W—Cd1—C1117.62 (12)C13—C14—H14119.8
N1—Cd1—C1109.32 (9)C15—C14—H14119.8
N2—Cd1—C1112.26 (9)C10—C15—C14120.0 (3)
O1—Cd1—C127.05 (9)C10—C15—H15120.0
O2—Cd1—C127.21 (9)C14—C15—H15120.0
Cd1—O1W—H1W1128 (4)O6—C16—C13127.2 (4)
Cd1—O1W—H1W2100 (4)O6—C16—H16116.4
H1W1—O1W—H1W2108 (5)C13—C16—H16116.4
C1—O1—Cd192.5 (2)N1—C17—C18122.7 (3)
C1—O2—Cd190.5 (2)N1—C17—H17118.6
C9—O4—Cd1131.3 (3)C18—C17—H17118.6
C17—N1—C28118.8 (3)C19—C18—C17118.8 (4)
C17—N1—Cd1125.5 (2)C19—C18—H18120.6
C28—N1—Cd1115.28 (19)C17—C18—H18120.6
C26—N2—C27118.8 (3)C18—C19—C20120.2 (3)
C26—N2—Cd1126.2 (2)C18—C19—H19119.9
C27—N2—Cd1114.89 (19)C20—C19—H19119.9
O1—C1—O2122.4 (3)C19—C20—C28117.9 (3)
O1—C1—C2119.4 (3)C19—C20—C21123.4 (3)
O2—C1—C2118.2 (3)C28—C20—C21118.7 (3)
O1—C1—Cd160.42 (18)C22—C21—C20121.2 (3)
O2—C1—Cd162.26 (17)C22—C21—H21119.4
C2—C1—Cd1173.8 (2)C20—C21—H21119.4
C3—C2—C7120.0 (3)C21—C22—C23121.8 (3)
C3—C2—C1120.2 (3)C21—C22—H22119.1
C7—C2—C1119.8 (3)C23—C22—H22119.1
C2—C3—C4120.1 (3)C24—C23—C22124.0 (3)
C2—C3—H3120.0C24—C23—C27117.1 (3)
C4—C3—H3120.0C22—C23—C27118.9 (3)
C5—C4—C3120.0 (3)C25—C24—C23120.4 (3)
C5—C4—H4120.0C25—C24—H24119.8
C3—C4—H4120.0C23—C24—H24119.8
C4—C5—C6119.8 (3)C24—C25—C26119.0 (4)
C4—C5—C8121.7 (3)C24—C25—H25120.5
C6—C5—C8118.5 (3)C26—C25—H25120.5
C7—C6—C5120.4 (3)N2—C26—C25123.0 (3)
C7—C6—H6119.8N2—C26—H26118.5
C5—C6—H6119.8C25—C26—H26118.5
C2—C7—C6119.6 (3)N2—C27—C23121.6 (3)
C2—C7—H7120.2N2—C27—C28119.0 (2)
C6—C7—H7120.2C23—C27—C28119.4 (3)
O3—C8—C5125.0 (4)N1—C28—C20121.6 (3)
O3—C8—H8117.5N1—C28—C27118.4 (3)
C5—C8—H8117.5C20—C28—C27120.0 (2)
O4—Cd1—O1—C170.3 (2)C4—C5—C6—C70.7 (5)
O1W—Cd1—O1—C1155.2 (2)C8—C5—C6—C7178.1 (3)
N1—Cd1—O1—C140.9 (2)C3—C2—C7—C62.1 (4)
N2—Cd1—O1—C1116.7 (2)C1—C2—C7—C6178.7 (3)
O2—Cd1—O1—C13.40 (18)C5—C6—C7—C22.3 (5)
O4—Cd1—O2—C1111.9 (2)C4—C5—C8—O35.8 (7)
O1W—Cd1—O2—C132.9 (3)C6—C5—C8—O3173.0 (5)
N1—Cd1—O2—C1156.09 (19)Cd1—O4—C9—O514.3 (6)
N2—Cd1—O2—C189.3 (2)Cd1—O4—C9—C10165.0 (2)
O1—Cd1—O2—C13.38 (18)O5—C9—C10—C15169.9 (3)
O1W—Cd1—O4—C915.6 (3)O4—C9—C10—C1510.7 (5)
N1—Cd1—O4—C9148.6 (3)O5—C9—C10—C1111.1 (5)
N2—Cd1—O4—C991.0 (4)O4—C9—C10—C11168.2 (3)
O1—Cd1—O4—C975.9 (3)C15—C10—C11—C120.4 (5)
O2—Cd1—O4—C9127.0 (3)C9—C10—C11—C12179.4 (3)
C1—Cd1—O4—C9101.5 (3)C10—C11—C12—C130.4 (5)
O4—Cd1—N1—C1729.0 (3)C11—C12—C13—C140.5 (5)
O1W—Cd1—N1—C17112.7 (3)C11—C12—C13—C16178.4 (4)
N2—Cd1—N1—C17179.0 (3)C12—C13—C14—C150.4 (5)
O1—Cd1—N1—C1789.5 (3)C16—C13—C14—C15177.6 (4)
O2—Cd1—N1—C1759.8 (3)C11—C10—C15—C141.3 (5)
C1—Cd1—N1—C1771.1 (3)C9—C10—C15—C14179.8 (3)
O4—Cd1—N1—C28158.7 (2)C13—C14—C15—C101.3 (5)
O1W—Cd1—N1—C2875.0 (2)C14—C13—C16—O6179.9 (5)
N2—Cd1—N1—C286.61 (19)C12—C13—C16—O62.2 (7)
O1—Cd1—N1—C2882.9 (2)C28—N1—C17—C180.2 (5)
O2—Cd1—N1—C28112.6 (2)Cd1—N1—C17—C18171.9 (3)
C1—Cd1—N1—C28101.3 (2)N1—C17—C18—C191.0 (6)
O4—Cd1—N2—C26115.0 (3)C17—C18—C19—C200.4 (6)
O1W—Cd1—N2—C2640.4 (3)C18—C19—C20—C280.8 (5)
N1—Cd1—N2—C26177.5 (3)C18—C19—C20—C21179.0 (4)
O1—Cd1—N2—C2652.4 (3)C19—C20—C21—C22178.5 (4)
O2—Cd1—N2—C26108.1 (3)C28—C20—C21—C221.3 (6)
C1—Cd1—N2—C2678.5 (3)C20—C21—C22—C231.3 (6)
O4—Cd1—N2—C2767.5 (3)C21—C22—C23—C24179.8 (4)
O1W—Cd1—N2—C27142.1 (2)C21—C22—C23—C270.1 (5)
N1—Cd1—N2—C274.96 (19)C22—C23—C24—C25178.6 (3)
O1—Cd1—N2—C27125.07 (19)C27—C23—C24—C251.1 (5)
O2—Cd1—N2—C2769.4 (2)C23—C24—C25—C260.5 (5)
C1—Cd1—N2—C2799.0 (2)C27—N2—C26—C250.2 (5)
Cd1—O1—C1—O26.3 (3)Cd1—N2—C26—C25177.2 (3)
Cd1—O1—C1—C2172.9 (2)C24—C25—C26—N20.0 (6)
Cd1—O2—C1—O16.2 (3)C26—N2—C27—C230.8 (4)
Cd1—O2—C1—C2173.0 (2)Cd1—N2—C27—C23176.9 (2)
O4—Cd1—C1—O1116.14 (19)C26—N2—C27—C28179.3 (3)
O1W—Cd1—C1—O128.2 (2)Cd1—N2—C27—C283.0 (3)
N1—Cd1—C1—O1148.7 (2)C24—C23—C27—N21.2 (4)
N2—Cd1—C1—O171.0 (2)C22—C23—C27—N2178.5 (3)
O2—Cd1—C1—O1174.0 (3)C24—C23—C27—C28178.9 (3)
O4—Cd1—C1—O269.9 (2)C22—C23—C27—C281.4 (4)
O1W—Cd1—C1—O2157.79 (18)C17—N1—C28—C201.1 (4)
N1—Cd1—C1—O225.3 (2)Cd1—N1—C28—C20174.1 (2)
N2—Cd1—C1—O2103.0 (2)C17—N1—C28—C27179.4 (3)
O1—Cd1—C1—O2174.0 (3)Cd1—N1—C28—C277.7 (3)
O1—C1—C2—C323.3 (4)C19—C20—C28—N11.6 (4)
O2—C1—C2—C3155.9 (3)C21—C20—C28—N1178.2 (3)
O1—C1—C2—C7157.6 (3)C19—C20—C28—C27179.9 (3)
O2—C1—C2—C723.2 (4)C21—C20—C28—C270.0 (4)
C7—C2—C3—C40.4 (5)N2—C27—C28—N13.2 (4)
C1—C2—C3—C4179.5 (3)C23—C27—C28—N1176.9 (3)
C2—C3—C4—C51.2 (5)N2—C27—C28—C20178.5 (3)
C3—C4—C5—C61.1 (5)C23—C27—C28—C201.4 (4)
C3—C4—C5—C8179.8 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O2i0.86 (5)1.89 (5)2.735 (4)168 (5)
O1W—H1W2···O50.86 (5)1.88 (3)2.590 (4)140 (5)
Symmetry code: (i) x+1, y, z.

Experimental details

Crystal data
Chemical formula[Cd(C8H5O3)2(C12H8N2)(H2O)]
Mr608.86
Crystal system, space groupMonoclinic, P21
Temperature (K)295
a, b, c (Å)6.357 (1), 19.668 (4), 9.766 (2)
β (°) 90.11 (3)
V3)1221.0 (4)
Z2
Radiation typeMo Kα
µ (mm1)0.95
Crystal size (mm)0.34 × 0.21 × 0.18
Data collection
DiffractometerRigaku R-AXIS RAPID
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.739, 0.848
No. of measured, independent and
observed [I > 2σ(I)] reflections
11897, 4825, 4537
Rint0.024
(sin θ/λ)max1)0.648
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.025, 0.063, 1.05
No. of reflections4825
No. of parameters349
No. of restraints4
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.56, 0.25
Absolute structureFlack (1983), from 1957 Friedel pairs
Absolute structure parameter0.01 (2)

Computer programs: RAPID-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O2i0.86 (5)1.89 (5)2.735 (4)168 (5)
O1W—H1W2···O50.86 (5)1.88 (3)2.590 (4)140 (5)
Symmetry code: (i) x+1, y, z.
 

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