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The title cadmium(II) coordination polymer, [Cd2(C4H2O4)Cl2(C19H12N4)2]n, (I), was obtained by the reaction of CdCl2·2.5H2O, fumaric acid (H2fum) and 2-phenyl-1H-1,3,7,8-tetra­azacyclo­penta­[l]phenanthrene (L) under hydro­thermal conditions. The fum dianion is situated across an inversion centre in the space group P \overline 1. The CdII atom is six-coordinated by two L N atoms, two fum O atoms and two Cl atoms in a distorted octa­hedral geometry. The μ2-Cl atoms and the bis-chelating fum dianions bridge neighbouring CdII centres, yielding a coordination polymer chain structure along the c axis. N—H...O hydrogen bonds between the N atoms of L and the carboxyl­ate O atoms of fum lead to a sheet structure in the bc plane. Compound (I) represents a rare example of a supra­molecular structure constructed by a chloride anion, a dicarboxyl­ate anion and a 1,10-phenanthroline derivative. This work may further the development of the coordination chemistry of 1,10-phenanthroline derivatives.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270108026760/gd3238sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270108026760/gd3238Isup2.hkl
Contains datablock I

CCDC reference: 707197

Comment top

Generally, two different types of interactions (covalent bonds and non-covalent intermolecular forces) can be used to construct varied supramolecular architectures. The ππ interaction, as one of the most powerful non-covalent intermolecular interactions, is operative in determining supramolecular architectures (Chen & Liu, 2002). On this basis, a number of coordination polymers have been prepared from one-dimensional covalently bonded chains or layers, yielding extended two- or three-dimensional supramolecular structures through these interactions (Zhang et al., 2005; Wang et al., 2007).

To date, 1,10-phenanthroline (phen) and 2,2-bipyridyl have been widely used to build supramolecular architectures, due to their excellent coordinating ability and large conjugated systems that can easily form ππ interactions (Wang et al., 2008; Tong et al., 2000; Zheng et al., 2001). However, far less attention has been given to their derivatives (Yang, Li et al., 2007; Yang, Ma et al., 2007). For example, the rare phen derivative 2-phenyl-1H-1,3,7,8,-tetraazacyclopenta[l]phenanthrene (L) possesses a promising aromatic system and is a good candidate for the construction of metal–organic supramolecular architectures (Wang et al., 2007). In this contribution, we selected fumaric acid (H2fum) as a linker and L as a secondary ligand, generating the title new CdII coordination polymer, (I), which displays a two-dimensional supramolecular architecture interlinked through hydrogen bonds.

As shown in Fig. 1, the asymmetric unit of (I) contains one unique CdII cation, one unique Cl- anion and one-half of a fum dianionic ligand. The fum dianion is situated across an inversion centre. Each CdII atom is six-coordinated by two N atoms (N1 and N2) from one L ligand, two O atoms (O1 and O2) from one fum ligand and two Cl- anions [Cl1 and Cl1i; symmetry code: (i) 1 - x, 1 - y, -z Please check added symop] in a distorted octahedral geometry. The average Cd—O and Cd—N distances in (I) (Table 1) are comparable twith those observed for [Cd4(OH)2(H2O)2(sip)2(4,4'-bpy)4].H2O (sip = 5-sulfoisophthalate and 4,4'-bpy = 4,4'-bipyridyl; Li et al., 2005).

As depicted in Fig. 2, two µ2-Cl atoms bridge two CdII centres to yield a [Cd2Cl2]2- unit. The fum dianions link neighbouring [Cd2Cl2]2- units in a bis-chelating mode, to give a one-dimensional chain structure along the c axis. The L ligands are extended on both sides of the chain, and the planes of adjacent L ligands are nearly parallel [Dihedral angle between the best planes?]. The secondary L ligand plays an important role in the formation of the chain structure. Two N atoms from the secondary L ligand occupy two coordination positions of the CdII atom, while the remaining coordination positions are available for fum ligands, allowing the formation of the chain structure. N—H···O hydrogen bonds between the N atoms of L and the carboxylate O atoms of fum lead to a sheet structure of (I) in the bc plane (Table 2, Fig. 3).

It is noteworthy that the structure of (I) presented here is clearly different from that of the previously reported compound [Pb(ndc)(L)].0.5H2O (ndc = 1,4-naphthalenedicarboxylate; Yang, Li et al., 2007). In the latter compound, the ndc ligand links the PbII atoms to yield a single chain. The L ligands extend solely on one side of the chain in a slanted fashion, and ππ interactions between the L ligands result in a final wavy layer structure. The structure of (I) is also entirely different from that of [Pb(fum)(dpdp)].H2O (dpdp = dipyrido[3,2-a:2',3'-c]phenazine; Yang, Ma et al., 2007). In that structure, each fum ligand bridges four PbII centres in a tetradentate mode, generating a novel layer structure. These layers are decorated with dpdp ligands alternating on the two sides of each layer. ππ interactions between the dpdp ligands lead to a unique three-dimensional supramolecular structure.

It should be pointed out that the complex structure of (I) is not sensitive to the CdII:L ratio. The same compound (I), with a CdII:L ratio of 1:1, can always be isolated using CdII:L reaction stoichiometries of 1, 2, or 3. We have also tried to investigate the effects of different cadmium(II) salts on the structure of the complex through reaction with Cd(NO3)2, Cd(CH3COOH)2 or CdSO4, but single crystals of their products have not been obtained. Therefore, the Cl- anion probably plays an important role in the formation of complex (I). To the best of our knowledge, compound (I), featuring a fascinating two-dimensional superamolecular structure, is the first solid entity constructed by a Cl- anion, a dicarboxylate anion and a phen derivative.

Related literature top

For related literature, see: Chen & Liu (2002); Hiort et al. (1993); Li et al. (2005); Tong et al. (2000); Wang et al. (2007, 2008); Yang, Li, Cao, Yue, Li & Chen (2007); Yang, Ma, Liu, Ma & Batten (2007); Zhang et al. (2005); Zheng et al. (2001).

Experimental top

1,10-Phenanthroline was oxidized to 1,10-phenanthroline-5,6-dione according to the reported procedure of Hiort et al. (1993). For the preparation of L, a mixture of 1,10-phenanthroline-5,6-dione (2 mmol), benzaldehyde (2.2 mmol), glacial acetic acid (15 ml) and ammonium acetate (3.2 g) was heated under reflux for 2 h, resulting in a yellow precipitate. After cooling, the mixture was diluted with water (25 ml) and the pH value of the solution was adjusted with concentrated aqueous ammonia to 5.5. The yellow product was filtered off from the mixture, washed with water and acetone, and oven-dried at 333 K. For the preparation of (I), CdCl2.2.5H2O (0.114 g, 0.5 mmol), H2fum (0.058 g, 0.5 mmol) and L (0.148 g, 0.5 mmol) were dissolved in distilled water (12 ml), followed by addition of triethylamine until the pH of the system was about 5.3. The resulting solution was stirred for about 3 h at room temperature, sealed in a 23 ml Teflon-lined stainless steel autoclave and heated at 463 K for 7 d under autogenous pressure. The reaction system was then cooled slowly to room temperature. Pale-yellow block crystals of (I) suitable for single-crystal X-ray diffraction analysis were collected from the final reaction system by filtration, washed several times with distilled water and dried in air at ambient temperature (yield: 39% based on CdII). Spectroscopic analysis: IR (ν, cm-1, KBr): 3115 (s), 3056 (s), 2914 (vs), 1611 (vs), 1389 (s), 1340 (s), 1113 (s), 753 (s), 654 (s).

Refinement top

All H atoms were positioned geometrically (N—H = 0.86 Å and C—H = 0.93 Å) and refined as riding, with Uiso(H)=1.2Ueq(C,N).

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO (Rigaku, 1998); data reduction: PROCESS-AUTO (Rigaku, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL-Plus (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. A view of the local coordination of the CdII cation in (I), showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level and H atoms are shown as small spheres of arbitrary radii. [Symmetry codes: (i) 1 - x, 1 - y, -z; (ii) 1 - x, 1 - y, 1 - z.]
[Figure 2] Fig. 2. A view of the coordination polymer chain structure of (I), along the c axis.
[Figure 3] Fig. 3. A view of the sheet formed by the linking of the coordination polymer chains by N—H···O hydrogen bonds.
catena-Poly[[(2-phenyl-1H-1,3,7,8- tetraazacyclopenteno[l]phenanthrene- κ2N7,N8)cadmium(II)]-di-µ-chlorido-[(2-phenyl-1H- 1,3,7,8-tetraazacyclopenteno[l]phenanthrene- κ2N7,N8)cadmium(II)]-µ-fumarato- κ4O1,O1':O4,O4'] top
Crystal data top
[Cd2(C4H2O4)Cl2(C19H12N4)2]Z = 1
Mr = 1002.40F(000) = 496
Triclinic, P1Dx = 1.726 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.069 (3) ÅCell parameters from 8106 reflections
b = 10.480 (2) Åθ = 3.0–27.5°
c = 10.749 (4) ŵ = 1.30 mm1
α = 88.59 (3)°T = 293 K
β = 63.20 (3)°Block, pale yellow
γ = 73.59 (5)°0.33 × 0.25 × 0.21 mm
V = 964.2 (6) Å3
Data collection top
Rigaku R-AXIS RAPID
diffractometer
4365 independent reflections
Radiation source: rotating anode3755 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.029
Detector resolution: 10.0 pixels mm-1θmax = 27.5°, θmin = 3.4°
ω scansh = 1312
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 1313
Tmin = 0.642, Tmax = 0.760l = 1313
9502 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)] = 0.029Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.062H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.0229P)2 + 0.382P]
where P = (Fo2 + 2Fc2)/3
4365 reflections(Δ/σ)max = 0.001
262 parametersΔρmax = 0.42 e Å3
0 restraintsΔρmin = 0.39 e Å3
Crystal data top
[Cd2(C4H2O4)Cl2(C19H12N4)2]γ = 73.59 (5)°
Mr = 1002.40V = 964.2 (6) Å3
Triclinic, P1Z = 1
a = 10.069 (3) ÅMo Kα radiation
b = 10.480 (2) ŵ = 1.30 mm1
c = 10.749 (4) ÅT = 293 K
α = 88.59 (3)°0.33 × 0.25 × 0.21 mm
β = 63.20 (3)°
Data collection top
Rigaku R-AXIS RAPID
diffractometer
4365 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
3755 reflections with I > 2σ(I)
Tmin = 0.642, Tmax = 0.760Rint = 0.029
9502 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0290 restraints
wR(F2) = 0.062H-atom parameters constrained
S = 1.06Δρmax = 0.42 e Å3
4365 reflectionsΔρmin = 0.39 e Å3
262 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.

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
xyzUiso*/Ueq
C10.4231 (3)0.8318 (3)0.1039 (3)0.0378 (6)
H10.34510.79050.07350.045*
C20.4198 (3)0.9327 (3)0.1904 (3)0.0425 (6)
H20.34000.95890.21580.051*
C30.5351 (3)0.9927 (3)0.2373 (3)0.0375 (6)
H3A0.53421.06050.29460.045*
C40.6547 (3)0.9514 (2)0.1986 (2)0.0303 (5)
C50.6497 (3)0.8491 (2)0.1100 (2)0.0277 (5)
C60.7708 (3)0.8012 (2)0.0661 (3)0.0320 (5)
C70.8617 (4)0.6646 (3)0.0682 (4)0.0513 (7)
H70.85000.60010.13000.062*
C80.9882 (4)0.7125 (4)0.0284 (4)0.0687 (10)
H81.05920.68170.06350.082*
C91.0061 (4)0.8062 (3)0.0637 (4)0.0598 (9)
H91.09150.83830.09350.072*
C100.8972 (3)0.8537 (3)0.1130 (3)0.0386 (6)
C110.9021 (3)0.9548 (3)0.2042 (3)0.0367 (6)
C120.7848 (3)1.0020 (2)0.2416 (3)0.0327 (5)
C130.9654 (3)1.1033 (3)0.3384 (3)0.0410 (6)
C141.0505 (3)1.1930 (3)0.4231 (3)0.0453 (7)
C151.1828 (4)1.1979 (4)0.4166 (4)0.0636 (10)
H151.21471.14610.35790.076*
C161.2683 (5)1.2790 (4)0.4964 (4)0.0785 (13)
H161.35741.28130.49140.094*
C171.2217 (5)1.3556 (4)0.5827 (4)0.0749 (13)
H171.27921.41030.63610.090*
C181.0911 (5)1.3522 (3)0.5908 (3)0.0671 (11)
H181.05991.40450.64970.081*
C191.0043 (4)1.2701 (3)0.5105 (3)0.0545 (8)
H190.91561.26760.51620.065*
C200.4984 (3)0.5876 (3)0.3413 (3)0.0379 (6)
C210.4637 (3)0.5568 (3)0.4866 (3)0.0402 (6)
H210.38740.62080.56140.048*
N10.7562 (3)0.7065 (2)0.0221 (2)0.0364 (5)
N20.5331 (2)0.79241 (19)0.0635 (2)0.0304 (4)
N30.8268 (3)1.0978 (2)0.3281 (2)0.0378 (5)
H30.77571.14520.36810.045*
N41.0148 (3)1.0182 (2)0.2652 (3)0.0447 (6)
O10.4310 (2)0.70323 (19)0.3250 (2)0.0463 (5)
O20.5921 (3)0.4988 (2)0.2410 (2)0.0497 (5)
Cd10.55367 (2)0.618432 (18)0.072732 (19)0.03153 (7)
Cl10.70589 (7)0.41956 (6)0.12379 (7)0.03761 (14)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0372 (14)0.0411 (14)0.0454 (15)0.0189 (12)0.0241 (12)0.0146 (12)
C20.0439 (15)0.0424 (14)0.0547 (17)0.0143 (13)0.0339 (14)0.0175 (13)
C30.0457 (15)0.0337 (13)0.0396 (14)0.0135 (12)0.0248 (12)0.0140 (11)
C40.0346 (12)0.0274 (11)0.0269 (12)0.0099 (10)0.0123 (10)0.0044 (10)
C50.0296 (12)0.0269 (11)0.0273 (12)0.0092 (10)0.0133 (10)0.0038 (9)
C60.0338 (13)0.0318 (12)0.0315 (13)0.0115 (11)0.0154 (10)0.0068 (10)
C70.0559 (18)0.0568 (17)0.065 (2)0.0268 (15)0.0439 (16)0.0305 (16)
C80.060 (2)0.082 (2)0.101 (3)0.0333 (19)0.062 (2)0.043 (2)
C90.0485 (17)0.070 (2)0.090 (3)0.0356 (17)0.0477 (18)0.0377 (19)
C100.0341 (13)0.0407 (14)0.0476 (16)0.0165 (12)0.0217 (12)0.0106 (12)
C110.0322 (13)0.0345 (13)0.0414 (15)0.0152 (11)0.0127 (11)0.0080 (11)
C120.0362 (13)0.0274 (11)0.0310 (13)0.0124 (11)0.0110 (10)0.0056 (10)
C130.0419 (15)0.0348 (13)0.0389 (15)0.0190 (12)0.0081 (12)0.0023 (12)
C140.0475 (16)0.0360 (14)0.0361 (15)0.0213 (13)0.0005 (12)0.0009 (12)
C150.067 (2)0.066 (2)0.057 (2)0.0416 (19)0.0156 (17)0.0102 (17)
C160.085 (3)0.081 (3)0.069 (3)0.063 (2)0.013 (2)0.007 (2)
C170.085 (3)0.055 (2)0.056 (2)0.046 (2)0.005 (2)0.0013 (18)
C180.085 (3)0.0380 (16)0.0434 (18)0.0201 (17)0.0007 (17)0.0036 (14)
C190.0556 (18)0.0404 (15)0.0443 (17)0.0161 (14)0.0028 (14)0.0033 (14)
C200.0488 (15)0.0463 (15)0.0387 (15)0.0280 (13)0.0301 (13)0.0234 (13)
C210.0515 (16)0.0483 (15)0.0355 (14)0.0254 (14)0.0272 (13)0.0207 (12)
N10.0413 (12)0.0372 (11)0.0405 (12)0.0138 (10)0.0264 (10)0.0131 (10)
N20.0320 (10)0.0329 (10)0.0313 (11)0.0138 (9)0.0169 (9)0.0095 (9)
N30.0454 (13)0.0309 (10)0.0354 (12)0.0159 (10)0.0151 (10)0.0111 (9)
N40.0394 (12)0.0424 (12)0.0513 (14)0.0230 (11)0.0142 (11)0.0117 (11)
O10.0621 (12)0.0440 (11)0.0438 (11)0.0197 (10)0.0325 (10)0.0215 (9)
O20.0626 (13)0.0510 (12)0.0382 (11)0.0149 (11)0.0276 (10)0.0179 (10)
Cd10.03937 (11)0.03465 (10)0.03032 (10)0.01762 (8)0.02106 (8)0.01408 (7)
Cl10.0315 (3)0.0424 (3)0.0385 (3)0.0118 (3)0.0155 (3)0.0031 (3)
Geometric parameters (Å, º) top
C1—N21.323 (3)C13—C141.468 (4)
C1—C21.394 (4)C14—C191.377 (5)
C1—H10.9300C14—C151.380 (5)
C2—C31.367 (4)C15—C161.382 (5)
C2—H20.9300C15—H150.9300
C3—C41.400 (4)C16—C171.366 (6)
C3—H3A0.9300C16—H160.9300
C4—C51.413 (3)C17—C181.368 (6)
C4—C121.430 (4)C17—H170.9300
C5—N21.354 (3)C18—C191.399 (4)
C5—C61.457 (3)C18—H180.9300
C6—N11.347 (3)C19—H190.9300
C6—C101.407 (4)C20—O21.247 (3)
C7—N11.328 (4)C20—O11.261 (3)
C7—C81.384 (5)C20—C211.487 (4)
C7—H70.9300C20—Cd12.712 (3)
C8—C91.366 (5)C21—C21i1.311 (5)
C8—H80.9300C21—H210.9300
C9—C101.390 (4)N3—H30.8600
C9—H90.9300Cd1—N12.312 (2)
C10—C111.422 (4)Cd1—N22.333 (2)
C11—C121.373 (4)Cd1—O12.479 (2)
C11—N41.376 (3)Cd1—O22.289 (2)
C12—N31.376 (3)Cd1—Cl1ii2.5640 (9)
C13—N41.315 (4)Cd1—Cl12.5782 (14)
C13—N31.367 (4)
N2—C1—C2122.5 (3)C18—C17—H17119.9
N2—C1—H1118.7C17—C18—C19120.0 (4)
C2—C1—H1118.7C17—C18—H18120.0
C3—C2—C1119.2 (3)C19—C18—H18120.0
C3—C2—H2120.4C14—C19—C18119.9 (4)
C1—C2—H2120.4C14—C19—H19120.0
C2—C3—C4119.6 (2)C18—C19—H19120.0
C2—C3—H3A120.2O2—C20—O1122.7 (3)
C4—C3—H3A120.2O2—C20—C21119.0 (2)
C3—C4—C5118.0 (2)O1—C20—C21118.2 (3)
C3—C4—C12126.2 (2)O2—C20—Cd157.13 (14)
C5—C4—C12115.9 (2)O1—C20—Cd165.85 (15)
N2—C5—C4121.3 (2)C21—C20—Cd1173.51 (19)
N2—C5—C6118.0 (2)C21i—C21—C20122.7 (3)
C4—C5—C6120.8 (2)C21i—C21—H21118.7
N1—C6—C10121.4 (2)C20—C21—H21118.7
N1—C6—C5117.7 (2)C7—N1—C6119.0 (2)
C10—C6—C5120.9 (2)C7—N1—Cd1124.2 (2)
N1—C7—C8123.0 (3)C6—N1—Cd1116.66 (17)
N1—C7—H7118.5C1—N2—C5119.4 (2)
C8—C7—H7118.5C1—N2—Cd1124.78 (18)
C9—C8—C7118.4 (3)C5—N2—Cd1115.66 (16)
C9—C8—H8120.8C13—N3—C12106.8 (2)
C7—C8—H8120.8C13—N3—H3126.6
C8—C9—C10120.3 (3)C12—N3—H3126.6
C8—C9—H9119.9C13—N4—C11104.5 (2)
C10—C9—H9119.9C20—O1—Cd186.49 (17)
C9—C10—C6117.8 (3)C20—O2—Cd195.63 (16)
C9—C10—C11124.5 (3)O2—Cd1—N193.76 (8)
C6—C10—C11117.6 (2)O2—Cd1—N2160.78 (7)
C12—C11—N4111.2 (2)N1—Cd1—N271.64 (8)
C12—C11—C10120.9 (2)O2—Cd1—O154.83 (7)
N4—C11—C10127.9 (3)N1—Cd1—O191.37 (8)
C11—C12—N3105.1 (2)N2—Cd1—O1111.63 (7)
C11—C12—C4123.9 (2)O2—Cd1—Cl1ii96.92 (6)
N3—C12—C4131.0 (2)N1—Cd1—Cl1ii165.67 (5)
N4—C13—N3112.4 (2)N2—Cd1—Cl1ii95.72 (6)
N4—C13—C14123.8 (3)O1—Cd1—Cl1ii87.03 (6)
N3—C13—C14123.7 (3)O2—Cd1—Cl195.16 (6)
C19—C14—C15119.1 (3)N1—Cd1—Cl197.60 (6)
C19—C14—C13122.2 (3)N2—Cd1—Cl199.06 (6)
C15—C14—C13118.7 (3)O1—Cd1—Cl1149.30 (5)
C14—C15—C16120.7 (4)Cl1ii—Cd1—Cl190.93 (4)
C14—C15—H15119.6O2—Cd1—C2027.24 (8)
C16—C15—H15119.6N1—Cd1—C2094.33 (8)
C17—C16—C15119.9 (4)N2—Cd1—C20138.40 (8)
C17—C16—H16120.0O1—Cd1—C2027.66 (7)
C15—C16—H16120.0Cl1ii—Cd1—C2090.86 (7)
C16—C17—C18120.3 (3)Cl1—Cd1—C20121.92 (7)
C16—C17—H17119.9Cd1ii—Cl1—Cd189.07 (4)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N3—H3···O1iii0.862.092.820 (3)142
Symmetry code: (iii) x+1, y+2, z.

Experimental details

Crystal data
Chemical formula[Cd2(C4H2O4)Cl2(C19H12N4)2]
Mr1002.40
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)10.069 (3), 10.480 (2), 10.749 (4)
α, β, γ (°)88.59 (3), 63.20 (3), 73.59 (5)
V3)964.2 (6)
Z1
Radiation typeMo Kα
µ (mm1)1.30
Crystal size (mm)0.33 × 0.25 × 0.21
Data collection
DiffractometerRigaku R-AXIS RAPID
diffractometer
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.642, 0.760
No. of measured, independent and
observed [I > 2σ(I)] reflections
9502, 4365, 3755
Rint0.029
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.029, 0.062, 1.06
No. of reflections4365
No. of parameters262
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.42, 0.39

Computer programs: PROCESS-AUTO (Rigaku, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL-Plus (Sheldrick, 2008).

Selected bond lengths (Å) top
Cd1—N12.312 (2)Cd1—O22.289 (2)
Cd1—N22.333 (2)Cd1—Cl1i2.5640 (9)
Cd1—O12.479 (2)Cd1—Cl12.5782 (14)
Symmetry code: (i) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N3—H3···O1ii0.862.092.820 (3)142.3
Symmetry code: (ii) x+1, y+2, z.
 

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