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The one- and two-dimensional polymorphic cadmium poly­carboxyl­ate coordination polymers, catena-poly[bis[[mu]2-2-(2-methyl-1H-benzimidazol-1-yl)acetato-[kappa]3N3:O,O']cadmium(II)], [Cd(C10H9N2O2)2]n, and poly[bis[[mu]2-2-(2-methyl-1H-benzimidazol-1-yl)acetato-[kappa]3N3:O,O']cadmium(II)], also [Cd(C10H9N2O2)2]n, were prepared under solvothermal conditions. In each structure, each CdII atom is coordinated by four O atoms and two N atoms from four different ligands. In the former structure, two crystallographically independent CdII atoms are located on twofold symmetry axes and doubly bridged in a [mu]2-N:O,O'-mode by the ligands into correspondingly independent chains that run in the [100] and [010] directions. Chains containing crystallographically related CdII atoms are linked into sheets via [pi]-[pi] stacking inter­actions. Sheets containing one of the distinct types of CdII atom are stacked perpendicular to [001] and alternate with sheets containing the other type of CdII atom. The second complex is a two-dimensional homometallic CdII (4,4) net structure in which each CdII atom is singly bridged to four neighbouring CdII atoms by four ligands also acting in a [mu]2-N:O,O'-mode. A square-grid network results and the three-dimensional supra­molecular framework is completed by [pi]-[pi] stacking inter­actions between the aromatic ring systems.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229614020853/wq3072sup1.cif
Contains datablocks I, II, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229614020853/wq3072Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229614020853/wq3072IIsup3.hkl
Contains datablock II

CCDC references: 1024752; 1024513

Introduction top

A great deal of attention has been paid to the crystal engineering of metal–organic coordination polymers in recent years, due to a conbination of their fascinating molecular structures and their potential applications as functional materials (Kahn & Martinez, 1998; Xiong et al., 2001; Batten et al., 2009; Liao et al., 2004). A series of cadmium coordination polymers containing carboxyl­ate ligands have been reported (Yang et al., 2009; Zheng et al., 2012; Zhou et al., 2011; Nie & Wang, 2011; Han et al., 2012; Wang et al., 2012). According to previous reports, asymmetric bridging ligands containing carb­oxy­lic acid and nitro­gen groups with a variety of properties are excellent candidates for the construction of highly connected topological frameworks. The structural topologies of these polymers are affected by the coordination geometries of both the organic ligands and the metal atoms. Bridging ligands with N- and O-donor atoms play an instrumental role in building coordination polymers. Among the various ligands, the versatile carb­oxy­lic acid ligands display diverse coordination modes. In particular, the aromatic carb­oxy­lic acids, such as benzene- and naphthalene-based derivatives, have been used and well documented in the preparation of numerous carboxyl­ate-containing coordination complexes. In order to explore new coordination polymers using rigid building blocks, we synthesized a novel benzimidazole-derivative ligand containing a carb­oxy­lic acid group, namely, (2-methyl­benzimidazol-l-yl)acetate, L, which is formed in situ from the corresponding cyano-substituted derivative under solvothermal conditions in the presence of CdII cations. We report here the crystal structure of two new `polymorphic' CdII coordination polymers based on this ligand, (I) and (II), which show some inter­esting structural features.

Experimental top

Synthesis and crystallization top

(2-Methyl­benzimidazol-1-yl)aceto­nitrile was prepared by an adaptation of the literature method of Ramla et al. (2006) for the synthesis of 2-(2-methyl-5-nitro-1H-benzimidazol-1-yl)aceto­nitrile. To a solution of 2-methyl­benzimidazole (7.48g, 56.6 mmol) and sodium hydride (1.5g, 56.6 mmol) in tetra­hydro­furan (30 ml), bromo­aceto­nitrile (3.96 ml, 56.6 mmol) was added dropwise. The reaction mixture was stirred for 8 h at room temperature and then poured onto iced water. The obtained precipitate was filtered off, dried and recrystallized from ethanol (yield 8.24 g, 85%).

For the synthesis of (I), a mixture of (2-methyl­benzimidazol-1-yl)aceto­nitrile (0.0274g, 0.16mmol), Cd(ClO4)2·6H2O (0.0336g, 0.08 mmol) and pyridine (0.0312 g, 0.2 mmol) was dissolved in deionized water and stirred for 30 min in air. The mixture was sealed in a 25 ml Teflon-lined stainless steel vessel, heated at 453 K for 3 d under autogenous pressure and then cooled to room temperature. Highly pure and well shaped colourless block crystals of (I) were collected in 67% yield. During the reaction under solvothermal conditions, the nitrile group of (I) is hydrolysed to a carboxyl­ate group (Liu & Ye, 2013).

For the synthesis of (II), a mixture of Cd(CH3COO)2.2H2O (0.053 g, 0.2 mmol), (2-methyl­benzimidazol-1-yl)aceto­nitrile (0.068 g, 0.4 mmol) and distilled water (9 ml) was stirred to homogeneity for 10 min in air. The mixture was then transferred to a 20 ml Teflon-lined steel autoclave and heated at 433 K for 5 d under autogenously controlled pressure, followed by slow cooling to room temperature. Colourless blocks of complex (II) were collected (yield ca 65%, based on Cd).

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1. All H atoms were positioned geometrically and refined using a riding model, with C—H = 0.93 (aromatic), 0.96 (methyl) or 0.97 Å (methyl­ene), and with Uiso(H) = 1.5Ueq(C) for methyl groups or 1.2Ueq(C) otherwise.

Results and discussion top

The asymmetric unit of complex (I) contains two independent Cd atoms located on twofold symmetry axes and (2-methyl­benzimidazol-l-yl)acetate ligands in general positions. In this context, the cyano group of (2-methyl­benzimidazol-1-yl)aceto­nitrile has been hydrolysed to a carboxyl­ate group under hydro­thermal conditions. As shown in Fig. 1, each of the central Cd atoms (Cd1 and Cd2) is six-coordinated by four O atoms from two L carboxyl­ate groups and two N atoms from imidazole rings of two further L ligands. Both Cd atoms adopt a distorted o­cta­hedral coordination geometry, brought about mainly by the small bite angles of the bidentate carboxyl­ate groups (Table 2). All the carboxyl­ate groups maintain approximate equivalence of their C—O bonds, with lengths in the range 1.23–1.27 Å. The ranges shown by the Cd—O and Cd—N bond lengths (Table 2) are in good agreement with those found in other Cd complexes with six-coordinated geometries (Dai et al., 2002). The O1—Cd1—O2 and O3—Cd2—O4 angles (Table 2) are similar to those reported in other cadmium polymers coordinated by two O atoms from a carboxyl­ate group (Luo et al., 2004).

Compound (I) is a new coordination polymer in which both of the six-coordinated Cd centres adopt a distorted o­cta­hedral coordination geometry. It displays a novel coordination architecture compared with a similar compound, {[Cd(H2PIMDC)2]}n (Zhai et al., 2013), in which the central CdII cation is coordinated by only one O atom of one carboxyl­ate group of each of four 2-propyl-1H-imidazole-4,5-di­carboxyl­ate (H2PIMDC) ligands, rather than two O atoms of a carboxyl­ate group, plus the N atoms from just two of these ligands. Compound (I) also differs from another Cd complex with H2PIDMC, [Cd(H2PIMDC)2(H2O)2]·4H2O (Deng et al., 2012), where the central Cd cation is again coordinated by one O atom of one carboxyl­ate group and an N atom of each of two H2PIMDC ligands, plus two O atoms from two coordinated water molecules, resulting in a distorted o­cta­hedral geometry.

The (2-methyl­benzimidazol-l-yl)acetate ligand in (I) is tridentate and links two Cd centres in chelate and chelate-bridged (µ3-N:O,O) modes to form one-dimensional chains, in which two L ligands bridge each Cd atom (Figs. 2 and 3). In our notation, the letters A, B, C, D and A', B', C', D' denote imidazole rings in adjacent parallel sets of one-dimensional chains involving atoms Cd1 and Cd2, respectively. Within the chains containing Cd1, the dihedral angles between the planes of A and B, and between the symmetry-related pair C and D, are 53.07 (14)°, whereas within the chains containing Cd2, the dihedral angles between the planes of A' and B', and between C' and D', are 57.98 (14)°. Planes B and C, which are in adjacent chains composed of Cd1 atoms, and planes B' and C' from adjacent chains composed of Cd2 atoms, are close to being parallel, with dihedral angles of 3.73 (14) and 6.30 (14)°, respectively. Thus, for each of the two independent polymeric chains, there are weak ππ stacking inter­actions between adjacent imidazole rings, which leads to stacks of chains containing just one of the independent types of Cd atom. They are characterized by ring B–C and B'–C' centroid-to-centroid distances of 3.8446 (14) and 3.9664 (15) Å, respectively. The perpendicular displacement from the ring centroid of plane B to the mean plane C is 3.7096 (10) Å, and the perpendicular distance from the ring centroid of plane B' to the mean plane C' is 3.4548 (10) Å. In addition, it is likely that the steric inter­action resulting from the optimization of this stacking inter­action may explain the difference in the dihedral angles between adjacent imidazole rings, and the effect of this inter­action is to link molecules related by translation into chains.

A noteworthy feature of this structure is that the chains containing the Cd1 atoms run perpendicular to those containing the Cd2 atoms (Figs. 2 and 3). The chains containing the Cd1 atoms run parallel to the [100] direction with an intra­chain Cd···Cd distance of 7.3521 (4) Å, while the chains containing the Cd2 atoms run parallel to the [010] direction with an intra­chain Cd···Cd distance of 7.0037 (4) Å. In both cases, the ππ inter­actions link the chains into layers which lie parallel to the (001) plane (Fig. 4), but the two types are turned through 90° in this plane with respect to each other. These layers containing atoms Cd1 then stack along the [001] direction in an alternating fashion with those containing atoms Cd2.

The asymmetric unit of complex (II) contains one CdII cation and one L ligand, both in general positions (Fig. 5). As shown in Fig. 6, the central CdII cation is coordinated by four O atoms from the carboxyl­ate group of two L ligands and two benzimidazole N atoms from another two L ligands, forming a highly distorted CdO4N2 o­cta­hedral coordination geometry. Each L ligand acts in a µ3-N:O,O mode to bridge two CdII cations through one chelating carboxyl­ate group and one benzimidazole N atom.

The six-coordinate geometry of (II) is similar to that in other carboxyl­ate-containing CdII complexes, e.g. [Cd(4-pyridyl­acrylate)2].H2O (Evans & Lin, 2001) and [Cd(oba)(1,4-bix)] [oba = 4,4'-oxybis(benzoate) and 1,4-bix = 1,4-bis­(imidazol-1-yl­methyl)­benzene; Yang et al., 2009]. The Cd—O and Cd—N bond lengths (Table 3), with the bond angles around each CdII centre ranging from 54.39 (18) to 154.3 (2)°, are fundamentally consistent with those in the above-mentioned CdII complexes. In contrast, the crystal structure of {Cd[4-(4-pyridyl)­benzoate]2}.H2O exhibits two distinct metal-atom coordination geometries; one is o­cta­hedral and similar to that in (II), while the other is trigonal–bipyramidal, with one of the carboxyl­ate groups only coordinating in a monodentate fashion (Evans & Lin, 2001).

In contrast with the structure of (I), where double bridges of L exist between adjacent Cd atoms to give a chain structure, each Cd atom in (II) is singly bridged by four L ligands to four different Cd atoms, which generates a two-dimensional (4,4) net structure that extends parallel to the (001) plane (Fig. 7). This connectivity leads to square-grid sheets, with a Cd···Cd distance along each grid side of 8.173 (4) Å. In each grid of two-dimensional sheets there are two benzimidazole rings projecting above and two below the plane defined by the Cd atoms. These benzimidazole rings participate in ππ inter­actions with benzimidazole rings from adjacent layers, with an inter­planar spacing of 3.415 (3) Å and a centroid separation of 3.564 (5) Å. These weak ππ stacking inter­actions between symmetry-related benzimidazole rings complete the three-dimensional supra­molecular structure of (II) (Fig. 8). The cavities in the (4,4) grid apparent in Fig. 7 are occupied by the benzene rings of L ligands in the adjacent layers on either side.

In conclusion, to the best of our knowledge, complexes (I) and (II) are new one- and two-dimensional cadmium coordination polymers of a new (2-methyl­benzimidazol-l-yl)acetate ligand. The complexes are polymorphs which form under solvothermal conditions involving slightly different components; for (I), pyridine was included in the reaction mixure, whereas no pyridine was used for the synthesis of (II). This work suggests that this carboxyl­ate-based ligand will be a rich source of new coordination polymers.

Related literature top

For related literature, see: Batten et al. (2009); Evans & Lin (2001); Han et al. (2012); Kahn & Martinez (1998); Liao et al. (2004); Nie & Wang (2011); Ramla et al. (2006); Wang et al. (2012); Xiong et al. (2001); Yang et al. (2009); Zheng et al. (2012); Zhou et al. (2011).

Computing details top

For both compounds, data collection: CrystalClear (Rigaku, 2005); cell refinement: CrystalClear (Rigaku, 2005); data reduction: CrystalClear (Rigaku, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. (a) The local coordination environment of Cd1 in (I), viewed down the b axis and showing the atom-numbering scheme. (b) The coordination environment of Cd2 in (I), viewed down the a axis. [Symmetry codes: (i) x - 1/2, -y + 1, z; (ii) -x + 1/2, y + 1/2, z; (iii) x - 1/2, y, -z + 1/2; (iv) x, y + 1/2, -z; (v) -x + 1/2, y, -z; (vi) x, -y + 1, -z + 1/2.]
[Figure 2] Fig. 2. The two-dimensional network layer in (I) lying perpendicular to [001], formed via ππ stacking interactions (dashed lines) between Cd1-based polymeric chains running in the [100] direction. H atoms have been omitted for clarity.
[Figure 3] Fig. 3. The two-dimensional network layer in (I) perpendicular to [001], formed via ππ stacking interactions (dashed lines) between Cd2-based polymeric chains running in the [010] direction. H atoms have been omitted for clarity.
[Figure 4] Fig. 4. (a) A packing view of (I), showing the mutually perpendicular coordination polymer chains. H atoms have been omitted for clarity. (b) A schematic view of the topology of (I). The orange rods represent one type of coordination polymer chain and the blue dots represent the other chain running into the page.
[Figure 5] Fig. 5. The asymmetric unit of (II), showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. H atoms have been omitted.
[Figure 6] Fig. 6. A view of complex (II), depicting the coordination environment around the Cd centre. H atoms have been omitted for clarity. [Symmetry codes: (i) 1/2 + x, -1/2 + y, z; (ii) 3/2 - x, -1/2 + y, 1/2 - z; (iii) 2 - x, y, 1/2 - z.]
[Figure 7] Fig. 7. The square grid-like structure of complex (II) formed by the CdII centres, viewed in the (001) plane.
[Figure 8] Fig. 8. An illustration of the three-dimensional supramolecular network of (II), formed by ππ stacking interactions (indicated by dashed lines) between benzimidazole rings of parallel sheets, viewed along (left) the [001] direction and (right) the [100] direction.
(I) catena-poly[bis[µ3-(2-methylbenzimidazol-1-yl)acetato]cadmium(II)] top
Crystal data top
[Cd(C10H9N2O2)2]F(000) = 3936
Mr = 490.79Dx = 1.668 Mg m3
Orthorhombic, IbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -I 2b 2cCell parameters from 26640 reflections
a = 14.7042 (4) Åθ = 3.0–27.6°
b = 14.0074 (4) ŵ = 1.15 mm1
c = 37.9500 (9) ÅT = 293 K
V = 7816.5 (4) Å3Block, colourless
Z = 160.38 × 0.34 × 0.3 mm
Data collection top
Rigaku SCXmini
diffractometer
3781 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.041
Graphite monochromatorθmax = 27.5°, θmin = 3.1°
ω scansh = 1819
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2005)
k = 1818
Tmin = 0.652, Tmax = 0.708l = 4843
29375 measured reflections3 standard reflections every 180 reflections
4479 independent reflections intensity decay: none
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)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.068H-atom parameters constrained
S = 1.14 w = 1/[σ2(Fo2) + (0.022P)2 + 9.7962P]
where P = (Fo2 + 2Fc2)/3
4479 reflections(Δ/σ)max = 0.001
265 parametersΔρmax = 0.43 e Å3
0 restraintsΔρmin = 0.37 e Å3
Crystal data top
[Cd(C10H9N2O2)2]V = 7816.5 (4) Å3
Mr = 490.79Z = 16
Orthorhombic, IbcaMo Kα radiation
a = 14.7042 (4) ŵ = 1.15 mm1
b = 14.0074 (4) ÅT = 293 K
c = 37.9500 (9) Å0.38 × 0.34 × 0.3 mm
Data collection top
Rigaku SCXmini
diffractometer
3781 reflections with I > 2σ(I)
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2005)
Rint = 0.041
Tmin = 0.652, Tmax = 0.7083 standard reflections every 180 reflections
29375 measured reflections intensity decay: none
4479 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0300 restraints
wR(F2) = 0.068H-atom parameters constrained
S = 1.14Δρmax = 0.43 e Å3
4479 reflectionsΔρmin = 0.37 e Å3
265 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
Cd10.129398 (16)0.50000.25000.03330 (8)
Cd20.25000.593964 (16)0.00000.03393 (8)
O10.26067 (13)0.46968 (13)0.21094 (6)0.0518 (5)
O20.17001 (13)0.35199 (13)0.22580 (6)0.0506 (5)
O40.08714 (16)0.56909 (13)0.02627 (6)0.0578 (6)
O30.20319 (14)0.47327 (13)0.03579 (5)0.0520 (5)
N10.53243 (13)0.41704 (14)0.21568 (5)0.0335 (4)
N20.40367 (14)0.34711 (14)0.19958 (5)0.0329 (4)
N40.09618 (14)0.32183 (13)0.05082 (5)0.0342 (4)
N30.16944 (15)0.19040 (14)0.03481 (5)0.0356 (5)
C30.4919 (2)0.3809 (2)0.10906 (7)0.0559 (8)
H30.48020.37210.08520.067*
C40.5733 (2)0.4205 (2)0.11924 (8)0.0569 (8)
H40.61570.43630.10200.068*
C50.5944 (2)0.4377 (2)0.15400 (7)0.0469 (7)
H50.64930.46560.16050.056*
C80.42830 (18)0.36733 (19)0.26423 (6)0.0406 (6)
H8A0.48100.37230.27900.061*
H8B0.40040.30600.26760.061*
H8C0.38570.41660.27030.061*
C70.45592 (15)0.37813 (16)0.22664 (6)0.0307 (5)
C100.24304 (17)0.38308 (18)0.21353 (6)0.0351 (5)
C20.4270 (2)0.3537 (2)0.13340 (7)0.0472 (7)
H20.37200.32660.12660.057*
C90.31234 (16)0.30858 (18)0.20261 (7)0.0374 (6)
H9A0.31250.25740.21980.045*
H9B0.29440.28160.18010.045*
C10.44851 (16)0.36892 (17)0.16840 (6)0.0337 (5)
C60.52988 (17)0.41136 (17)0.17888 (6)0.0342 (5)
C200.11966 (19)0.49194 (17)0.03585 (7)0.0389 (6)
C150.1860 (2)0.1231 (2)0.09647 (8)0.0506 (7)
H150.21300.06570.08990.061*
C140.1687 (2)0.1439 (3)0.13138 (8)0.0587 (8)
H140.18400.09950.14860.070*
C190.05368 (18)0.41504 (17)0.04737 (7)0.0394 (6)
H19A0.02730.43300.06980.047*
H19B0.00470.41090.03030.047*
C120.10187 (19)0.2971 (2)0.11700 (7)0.0463 (7)
H120.07480.35430.12370.056*
C130.1286 (2)0.2298 (3)0.14133 (8)0.0565 (8)
H130.11970.24210.16520.068*
C180.12148 (19)0.29955 (18)0.01369 (7)0.0413 (6)
H18A0.17130.34100.01950.062*
H18B0.06510.33300.01700.062*
H18C0.12300.24440.02870.062*
C110.11781 (16)0.27448 (19)0.08191 (7)0.0357 (5)
C160.16161 (17)0.19135 (18)0.07157 (6)0.0363 (5)
C170.12932 (16)0.26905 (17)0.02374 (6)0.0326 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.02637 (13)0.03605 (14)0.03748 (15)0.0000.0000.00250 (11)
Cd20.03733 (15)0.02713 (12)0.03732 (14)0.0000.00199 (11)0.000
O10.0407 (11)0.0396 (10)0.0752 (14)0.0031 (8)0.0003 (10)0.0025 (10)
O20.0367 (11)0.0500 (11)0.0652 (14)0.0004 (8)0.0178 (10)0.0049 (9)
O40.0817 (16)0.0354 (10)0.0562 (13)0.0030 (10)0.0024 (11)0.0125 (9)
O30.0498 (13)0.0408 (11)0.0655 (14)0.0089 (9)0.0116 (10)0.0007 (9)
N10.0280 (11)0.0419 (11)0.0307 (11)0.0014 (9)0.0012 (8)0.0038 (9)
N20.0276 (10)0.0370 (11)0.0341 (11)0.0015 (8)0.0030 (8)0.0029 (9)
N40.0387 (12)0.0283 (10)0.0355 (11)0.0012 (8)0.0042 (9)0.0006 (8)
N30.0424 (12)0.0324 (10)0.0320 (11)0.0026 (9)0.0055 (9)0.0004 (9)
C30.067 (2)0.072 (2)0.0283 (15)0.0027 (16)0.0006 (14)0.0008 (14)
C40.057 (2)0.077 (2)0.0364 (16)0.0037 (16)0.0138 (14)0.0127 (14)
C50.0411 (15)0.0571 (17)0.0424 (16)0.0062 (13)0.0054 (12)0.0096 (13)
C80.0410 (15)0.0480 (15)0.0327 (14)0.0059 (12)0.0042 (11)0.0022 (11)
C70.0272 (12)0.0326 (12)0.0324 (13)0.0028 (9)0.0018 (9)0.0012 (10)
C100.0307 (13)0.0411 (13)0.0336 (13)0.0007 (11)0.0040 (11)0.0037 (10)
C20.0464 (17)0.0543 (17)0.0409 (16)0.0009 (13)0.0051 (13)0.0064 (13)
C90.0303 (13)0.0374 (13)0.0445 (15)0.0030 (10)0.0035 (11)0.0063 (11)
C10.0314 (13)0.0363 (12)0.0332 (13)0.0047 (10)0.0016 (10)0.0001 (10)
C60.0315 (13)0.0378 (13)0.0333 (13)0.0024 (10)0.0017 (10)0.0028 (10)
C200.0562 (18)0.0318 (13)0.0287 (13)0.0073 (12)0.0082 (11)0.0040 (10)
C150.0486 (17)0.0564 (17)0.0467 (18)0.0098 (14)0.0077 (13)0.0074 (14)
C140.055 (2)0.082 (2)0.0387 (17)0.0079 (17)0.0069 (14)0.0173 (15)
C190.0413 (15)0.0320 (13)0.0448 (15)0.0039 (10)0.0108 (12)0.0012 (11)
C120.0467 (16)0.0540 (17)0.0382 (15)0.0086 (13)0.0069 (12)0.0058 (13)
C130.0529 (19)0.085 (2)0.0311 (16)0.0061 (16)0.0006 (13)0.0007 (15)
C180.0507 (17)0.0359 (14)0.0373 (14)0.0055 (12)0.0028 (12)0.0026 (11)
C110.0315 (13)0.0400 (13)0.0356 (14)0.0083 (11)0.0002 (10)0.0006 (11)
C160.0351 (13)0.0399 (13)0.0340 (13)0.0028 (11)0.0028 (10)0.0004 (11)
C170.0342 (13)0.0305 (11)0.0331 (13)0.0034 (10)0.0017 (10)0.0002 (10)
Geometric parameters (Å, º) top
Cd1—N1i2.254 (2)C3—H30.9300
Cd1—N1ii2.254 (2)C4—C51.376 (4)
Cd1—O1iii2.471 (2)C4—H40.9300
Cd1—O12.471 (2)C5—C61.388 (3)
Cd1—O2iii2.3448 (19)C5—H50.9300
Cd1—O22.3448 (19)C8—C71.491 (3)
Cd1—C10iii2.718 (2)C8—H8A0.9600
Cd2—N3iv2.230 (2)C8—H8B0.9600
Cd2—N3v2.230 (2)C8—H8C0.9600
Cd2—O3vi2.2753 (19)C10—C91.516 (3)
Cd2—O32.2753 (19)C2—C11.382 (4)
Cd2—O4vi2.617 (2)C2—H20.9300
Cd2—O42.617 (2)C9—H9A0.9700
Cd2—C20vi2.751 (3)C9—H9B0.9700
O1—C101.244 (3)C1—C61.394 (3)
O2—C101.249 (3)C20—C191.514 (3)
O4—C201.236 (3)C15—C141.381 (4)
O3—C201.256 (3)C15—C161.392 (4)
N1—C71.317 (3)C15—H150.9300
N1—C61.400 (3)C14—C131.392 (5)
N1—Cd1vii2.254 (2)C14—H140.9300
N2—C71.354 (3)C19—H19A0.9700
N2—C11.389 (3)C19—H19B0.9700
N2—C91.452 (3)C12—C131.377 (4)
N4—C171.356 (3)C12—C111.389 (4)
N4—C111.390 (3)C12—H120.9300
N4—C191.453 (3)C13—H130.9300
N3—C171.318 (3)C18—C171.488 (3)
N3—C161.400 (3)C18—H18A0.9600
N3—Cd2viii2.230 (2)C18—H18B0.9600
C3—C41.375 (5)C18—H18C0.9600
C3—C21.381 (4)C11—C161.387 (4)
N1i—Cd1—N1ii101.51 (10)C4—C5—H5121.6
N1i—Cd1—O2iii86.07 (7)C6—C5—H5121.6
N1ii—Cd1—O2iii113.00 (7)C7—C8—H8A109.5
N1i—Cd1—O2113.00 (7)C7—C8—H8B109.5
N1ii—Cd1—O286.07 (7)H8A—C8—H8B109.5
O2iii—Cd1—O2150.49 (10)C7—C8—H8C109.5
N1i—Cd1—O1iii138.79 (7)H8A—C8—H8C109.5
N1ii—Cd1—O1iii103.66 (7)H8B—C8—H8C109.5
O2iii—Cd1—O1iii54.13 (6)N1—C7—N2112.2 (2)
O2—Cd1—O1iii100.84 (7)N1—C7—C8125.2 (2)
N1i—Cd1—O1103.66 (7)N2—C7—C8122.6 (2)
N1ii—Cd1—O1138.79 (7)O1—C10—O2123.3 (2)
O2iii—Cd1—O1100.84 (7)O1—C10—C9120.6 (2)
O2—Cd1—O154.13 (6)O2—C10—C9116.1 (2)
O1iii—Cd1—O177.24 (10)C3—C2—C1116.3 (3)
N1i—Cd1—C10iii111.87 (7)C3—C2—H2121.9
N1ii—Cd1—C10iii113.91 (7)C1—C2—H2121.9
O2iii—Cd1—C10iii27.30 (7)N2—C9—C10112.8 (2)
O2—Cd1—C10iii125.13 (7)N2—C9—H9A109.0
O1iii—Cd1—C10iii27.21 (7)C10—C9—H9A109.0
O1—Cd1—C10iii85.91 (7)N2—C9—H9B109.0
N3iv—Cd2—N3v105.44 (10)C10—C9—H9B109.0
N3iv—Cd2—O3vi130.02 (8)H9A—C9—H9B107.8
N3v—Cd2—O3vi104.90 (7)C2—C1—N2132.6 (2)
N3iv—Cd2—O3104.90 (7)C2—C1—C6122.4 (2)
N3v—Cd2—O3130.02 (8)N2—C1—C6105.0 (2)
O3vi—Cd2—O384.02 (10)C5—C6—C1120.4 (2)
N3iv—Cd2—O4vi79.65 (7)C5—C6—N1130.2 (2)
N3v—Cd2—O4vi109.94 (7)C1—C6—N1109.4 (2)
O3vi—Cd2—O4vi52.90 (7)O4—C20—O3124.0 (2)
O3—Cd2—O4vi113.91 (7)O4—C20—C19117.3 (3)
N3iv—Cd2—O4109.94 (7)O3—C20—C19118.6 (2)
N3v—Cd2—O479.65 (7)C14—C15—C16117.3 (3)
O3vi—Cd2—O4113.91 (7)C14—C15—H15121.3
O3—Cd2—O452.90 (7)C16—C15—H15121.3
O4vi—Cd2—O4164.70 (8)C15—C14—C13121.4 (3)
N3iv—Cd2—C20vi103.75 (8)C15—C14—H14119.3
N3v—Cd2—C20vi113.06 (7)C13—C14—H14119.3
O3vi—Cd2—C20vi26.86 (7)N4—C19—C20112.9 (2)
O3—Cd2—C20vi96.90 (7)N4—C19—H19A109.0
O4vi—Cd2—C20vi26.48 (7)C20—C19—H19A109.0
O4—Cd2—C20vi139.18 (7)N4—C19—H19B109.0
C10—O1—Cd187.56 (15)C20—C19—H19B109.0
C10—O2—Cd193.25 (15)H19A—C19—H19B107.8
C20—O4—Cd282.79 (17)C13—C12—C11116.0 (3)
C20—O3—Cd298.18 (16)C13—C12—H12122.0
C7—N1—C6105.6 (2)C11—C12—H12122.0
C7—N1—Cd1vii124.82 (16)C12—C13—C14122.1 (3)
C6—N1—Cd1vii128.54 (15)C12—C13—H13119.0
C7—N2—C1107.83 (19)C14—C13—H13119.0
C7—N2—C9125.7 (2)C17—C18—H18A109.5
C1—N2—C9126.0 (2)C17—C18—H18B109.5
C17—N4—C11107.5 (2)H18A—C18—H18B109.5
C17—N4—C19125.1 (2)C17—C18—H18C109.5
C11—N4—C19127.1 (2)H18A—C18—H18C109.5
C17—N3—C16105.8 (2)H18B—C18—H18C109.5
C17—N3—Cd2viii123.71 (17)C16—C11—C12122.8 (3)
C16—N3—Cd2viii129.78 (16)C16—C11—N4105.4 (2)
C4—C3—C2121.6 (3)C12—C11—N4131.8 (3)
C4—C3—H3119.2C11—C16—C15120.3 (2)
C2—C3—H3119.2C11—C16—N3109.2 (2)
C3—C4—C5122.4 (3)C15—C16—N3130.5 (2)
C3—C4—H4118.8N3—C17—N4112.0 (2)
C5—C4—H4118.8N3—C17—C18125.4 (2)
C4—C5—C6116.8 (3)N4—C17—C18122.6 (2)
N1i—Cd1—O1—C10116.07 (15)C7—N2—C1—C61.6 (3)
N1ii—Cd1—O1—C1010.0 (2)C9—N2—C1—C6174.8 (2)
O2iii—Cd1—O1—C10155.38 (15)C4—C5—C6—C10.6 (4)
O2—Cd1—O1—C107.38 (14)C4—C5—C6—N1178.0 (3)
O1iii—Cd1—O1—C10106.30 (17)C2—C1—C6—C51.9 (4)
C10iii—Cd1—O1—C10132.41 (14)N2—C1—C6—C5176.4 (2)
N1i—Cd1—O2—C1097.92 (16)C2—C1—C6—N1179.9 (2)
N1ii—Cd1—O2—C10161.24 (16)N2—C1—C6—N11.5 (3)
O2iii—Cd1—O2—C1028.88 (15)C7—N1—C6—C5176.8 (3)
O1iii—Cd1—O2—C1058.06 (16)Cd1vii—N1—C6—C514.6 (4)
O1—Cd1—O2—C107.36 (14)C7—N1—C6—C10.8 (3)
C10iii—Cd1—O2—C1044.6 (2)Cd1vii—N1—C6—C1167.70 (16)
N3iv—Cd2—O4—C20101.91 (16)Cd2—O4—C20—O314.0 (3)
N3v—Cd2—O4—C20155.28 (17)Cd2—O4—C20—C19164.3 (2)
O3vi—Cd2—O4—C2053.46 (17)Cd2—O3—C20—O416.2 (3)
O3—Cd2—O4—C207.98 (15)Cd2—O3—C20—C19162.1 (2)
O4vi—Cd2—O4—C2025.06 (15)C16—C15—C14—C130.2 (5)
C20vi—Cd2—O4—C2041.8 (2)C17—N4—C19—C2067.7 (3)
N3iv—Cd2—O3—C20111.83 (16)C11—N4—C19—C20106.0 (3)
N3v—Cd2—O3—C2013.8 (2)O4—C20—C19—N4167.6 (2)
O3vi—Cd2—O3—C20118.29 (19)O3—C20—C19—N410.8 (4)
O4vi—Cd2—O3—C20163.07 (15)C11—C12—C13—C140.4 (4)
O4—Cd2—O3—C207.88 (15)C15—C14—C13—C121.9 (5)
C20vi—Cd2—O3—C20141.91 (14)C13—C12—C11—C162.8 (4)
C2—C3—C4—C51.6 (5)C13—C12—C11—N4176.3 (3)
C3—C4—C5—C61.2 (5)C17—N4—C11—C162.0 (3)
C6—N1—C7—N20.2 (3)C19—N4—C11—C16176.6 (2)
Cd1vii—N1—C7—N2169.31 (15)C17—N4—C11—C12178.8 (3)
C6—N1—C7—C8179.6 (2)C19—N4—C11—C124.2 (4)
Cd1vii—N1—C7—C811.3 (3)C12—C11—C16—C154.6 (4)
C1—N2—C7—N11.2 (3)N4—C11—C16—C15174.7 (2)
C9—N2—C7—N1174.4 (2)C12—C11—C16—N3178.4 (2)
C1—N2—C7—C8179.4 (2)N4—C11—C16—N32.3 (3)
C9—N2—C7—C86.2 (4)C14—C15—C16—C112.9 (4)
Cd1—O1—C10—O213.5 (3)C14—C15—C16—N3179.1 (3)
Cd1—O1—C10—C9164.6 (2)C17—N3—C16—C111.7 (3)
Cd1—O2—C10—O114.3 (3)Cd2viii—N3—C16—C11169.00 (17)
Cd1—O2—C10—C9163.97 (19)C17—N3—C16—C15174.9 (3)
C4—C3—C2—C10.2 (5)Cd2viii—N3—C16—C1514.4 (4)
C7—N2—C9—C1068.6 (3)C16—N3—C17—N40.4 (3)
C1—N2—C9—C10103.4 (3)Cd2viii—N3—C17—N4171.01 (15)
O1—C10—C9—N217.0 (3)C16—N3—C17—C18179.3 (2)
O2—C10—C9—N2161.3 (2)Cd2viii—N3—C17—C187.9 (3)
C3—C2—C1—N2176.4 (3)C11—N4—C17—N31.0 (3)
C3—C2—C1—C61.5 (4)C19—N4—C17—N3175.8 (2)
C7—N2—C1—C2179.7 (3)C11—N4—C17—C18177.9 (2)
C9—N2—C1—C27.1 (4)C19—N4—C17—C183.2 (4)
Symmetry codes: (i) x1/2, y+1, z; (ii) x1/2, y, z+1/2; (iii) x, y+1, z+1/2; (iv) x+1/2, y+1/2, z; (v) x, y+1/2, z; (vi) x+1/2, y, z; (vii) x+1/2, y, z+1/2; (viii) x, y1/2, z.
(II) poly[bis[µ3-(2-methylbenzimidazol-1-yl)acetato]cadmium(II)] top
Crystal data top
[Cd(C10H9N2O2)2]F(000) = 984
Mr = 490.79Dx = 1.735 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 2201 reflections
a = 11.476 (7) Åθ = 3.5–27.5°
b = 11.641 (7) ŵ = 1.20 mm1
c = 14.064 (13) ÅT = 293 K
β = 90.701 (14)°Block, colourless
V = 1879 (2) Å30.20 × 0.20 × 0.20 mm
Z = 4
Data collection top
Rigaku SCXmini
diffractometer
2168 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.061
Graphite monochromatorθmax = 28.7°, θmin = 2.5°
ω scansh = 1515
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2005)
k = 1515
Tmin = 0.787, Tmax = 0.787l = 1819
9836 measured reflections3 standard reflections every 180 reflections
2421 independent reflections intensity decay: none
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)] = 0.066Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.195H-atom parameters constrained
S = 1.23 w = 1/[σ2(Fo2) + (0.0827P)2 + 8.5997P]
where P = (Fo2 + 2Fc2)/3
2421 reflections(Δ/σ)max = 0.007
133 parametersΔρmax = 0.90 e Å3
0 restraintsΔρmin = 1.42 e Å3
Crystal data top
[Cd(C10H9N2O2)2]V = 1879 (2) Å3
Mr = 490.79Z = 4
Monoclinic, C2/cMo Kα radiation
a = 11.476 (7) ŵ = 1.20 mm1
b = 11.641 (7) ÅT = 293 K
c = 14.064 (13) Å0.20 × 0.20 × 0.20 mm
β = 90.701 (14)°
Data collection top
Rigaku SCXmini
diffractometer
2168 reflections with I > 2σ(I)
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2005)
Rint = 0.061
Tmin = 0.787, Tmax = 0.7873 standard reflections every 180 reflections
9836 measured reflections intensity decay: none
2421 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0660 restraints
wR(F2) = 0.195H-atom parameters constrained
S = 1.23Δρmax = 0.90 e Å3
2421 reflectionsΔρmin = 1.42 e Å3
133 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
Cd11.00000.19978 (5)0.25000.0358 (2)
O20.4757 (5)0.5517 (5)0.3602 (4)0.0522 (13)
O10.6585 (5)0.5978 (4)0.3348 (4)0.0504 (12)
N10.7357 (4)0.3863 (5)0.4092 (4)0.0366 (11)
N30.8943 (5)0.3183 (5)0.3423 (4)0.0362 (11)
C70.8174 (7)0.4160 (6)0.5756 (5)0.0486 (16)
H70.74980.44230.60410.058*
C60.9206 (8)0.4061 (7)0.6259 (5)0.0535 (18)
H60.92240.42570.69000.064*
C51.0228 (8)0.3675 (7)0.5834 (6)0.0543 (19)
H51.09170.36580.61880.065*
C41.0234 (6)0.3321 (6)0.4900 (5)0.0444 (15)
H41.09090.30320.46280.053*
C3A0.9202 (5)0.3407 (5)0.4375 (5)0.0359 (12)
C7A0.8189 (6)0.3852 (5)0.4805 (4)0.0363 (12)
C20.7836 (6)0.3459 (5)0.3291 (4)0.0361 (13)
C80.6168 (6)0.4225 (6)0.4193 (5)0.0450 (15)
H8A0.60150.43300.48640.054*
H8B0.56630.36130.39650.054*
C90.5842 (6)0.5333 (6)0.3667 (5)0.0394 (13)
C100.7180 (7)0.3343 (7)0.2375 (5)0.0496 (17)
H10A0.76220.28820.19430.074*
H10B0.70540.40900.21050.074*
H10C0.64430.29810.24890.074*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.0359 (4)0.0343 (4)0.0374 (4)0.0000.0061 (3)0.000
O20.049 (3)0.060 (3)0.048 (3)0.019 (2)0.014 (2)0.006 (2)
O10.058 (3)0.040 (2)0.054 (3)0.005 (2)0.001 (2)0.010 (2)
N10.036 (3)0.039 (3)0.036 (3)0.008 (2)0.002 (2)0.004 (2)
N30.039 (3)0.037 (3)0.033 (3)0.007 (2)0.001 (2)0.001 (2)
C70.063 (4)0.043 (4)0.040 (4)0.007 (3)0.008 (3)0.001 (3)
C60.070 (5)0.052 (4)0.039 (4)0.001 (4)0.002 (3)0.005 (3)
C50.061 (5)0.046 (4)0.055 (4)0.004 (3)0.016 (4)0.008 (3)
C40.043 (4)0.043 (3)0.047 (4)0.002 (3)0.000 (3)0.005 (3)
C3A0.036 (3)0.033 (3)0.039 (3)0.002 (2)0.000 (2)0.003 (2)
C7A0.042 (3)0.033 (3)0.034 (3)0.000 (2)0.002 (2)0.005 (2)
C20.042 (3)0.031 (3)0.036 (3)0.009 (2)0.001 (2)0.003 (2)
C80.040 (3)0.040 (3)0.055 (4)0.004 (3)0.013 (3)0.008 (3)
C90.047 (4)0.035 (3)0.037 (3)0.003 (3)0.005 (3)0.004 (2)
C100.054 (4)0.054 (4)0.041 (4)0.014 (3)0.006 (3)0.001 (3)
Geometric parameters (Å, º) top
Cd1—N32.258 (5)C7—C61.377 (11)
Cd1—N3i2.258 (5)C7—H70.9300
Cd1—O2ii2.337 (5)C6—C51.397 (12)
Cd1—O1ii2.467 (5)C6—H60.9300
Cd1—O1iii2.467 (5)C5—C41.377 (11)
Cd1—O2iii2.337 (5)C5—H50.9300
Cd1—C9ii2.710 (7)C4—C3A1.392 (9)
Cd1—C9iii2.710 (7)C4—H40.9300
O2—C91.266 (8)C3A—C7A1.414 (9)
O2—Cd1iv2.337 (5)C2—C101.489 (9)
O1—C91.224 (8)C8—C91.532 (9)
O1—Cd1iv2.467 (5)C8—H8A0.9700
N1—C21.346 (8)C8—H8B0.9700
N1—C7A1.376 (8)C9—Cd1iv2.710 (7)
N1—C81.436 (8)C10—H10A0.9600
N3—C21.321 (8)C10—H10B0.9600
N3—C3A1.394 (8)C10—H10C0.9600
C7—C7A1.385 (9)
O2ii—Cd1—N3i90.03 (19)C6—C7—H7121.5
O2iii—Cd1—N3i154.3 (2)C7—C6—C5121.9 (7)
N3—Cd1—N3i104.7 (3)C7—C6—H6119.1
N3—Cd1—O2ii154.3 (2)C5—C6—H6119.1
N3—Cd1—O2iii90.03 (19)C4—C5—C6121.3 (7)
O2ii—Cd1—O2iii84.9 (3)C4—C5—H5119.4
N3—Cd1—O1ii100.02 (19)C6—C5—H5119.4
N3i—Cd1—O1ii114.47 (19)C5—C4—C3A118.0 (7)
O2ii—Cd1—O1ii54.39 (18)C5—C4—H4121.0
O2iii—Cd1—O1ii82.7 (2)C3A—C4—H4121.0
N3—Cd1—O1iii114.47 (19)N3—C3A—C4131.8 (6)
N3i—Cd1—O1iii100.02 (19)N3—C3A—C7A108.2 (5)
O2ii—Cd1—O1iii82.7 (2)C4—C3A—C7A119.9 (6)
O2iii—Cd1—O1iii54.39 (18)N1—C7A—C7133.2 (6)
O1ii—Cd1—O1iii122.5 (2)N1—C7A—C3A105.0 (5)
N3—Cd1—C9ii126.5 (2)C7—C7A—C3A121.8 (6)
N3i—Cd1—C9ii106.2 (2)N3—C2—N1111.7 (6)
O2ii—Cd1—C9ii27.82 (19)N3—C2—C10125.0 (6)
O2iii—Cd1—C9ii80.2 (2)N1—C2—C10123.3 (6)
O1ii—Cd1—C9ii26.84 (19)N1—C8—C9115.2 (6)
O1iii—Cd1—C9ii101.8 (2)N1—C8—H8A108.5
N3—Cd1—C9iii106.2 (2)C9—C8—H8A108.5
N3i—Cd1—C9iii126.5 (2)N1—C8—H8B108.5
O2ii—Cd1—C9iii80.2 (2)C9—C8—H8B108.5
O2iii—Cd1—C9iii27.82 (19)H8A—C8—H8B107.5
O1ii—Cd1—C9iii101.8 (2)O1—C9—O2123.9 (7)
O1iii—Cd1—C9iii26.84 (19)O1—C9—C8121.8 (6)
C9ii—Cd1—C9iii88.7 (3)O2—C9—C8114.3 (6)
C9—O2—Cd1iv92.7 (4)O1—C9—Cd1iv65.5 (4)
C9—O1—Cd1iv87.7 (4)O2—C9—Cd1iv59.5 (4)
C2—N1—C7A108.7 (5)C8—C9—Cd1iv168.0 (5)
C2—N1—C8125.7 (6)C2—C10—H10A109.5
C7A—N1—C8125.6 (6)C2—C10—H10B109.5
C2—N3—C3A106.4 (5)H10A—C10—H10B109.5
C2—N3—Cd1126.2 (4)C2—C10—H10C109.5
C3A—N3—Cd1123.9 (4)H10A—C10—H10C109.5
C7A—C7—C6117.0 (7)H10B—C10—H10C109.5
C7A—C7—H7121.5
N3i—Cd1—N3—C2100.6 (5)C2—N1—C7A—C3A0.2 (7)
O2ii—Cd1—N3—C222.4 (8)C8—N1—C7A—C3A178.6 (6)
O2iii—Cd1—N3—C2100.7 (5)C6—C7—C7A—N1178.1 (7)
O1ii—Cd1—N3—C218.1 (6)C6—C7—C7A—C3A2.7 (10)
O1iii—Cd1—N3—C2150.9 (5)N3—C3A—C7A—N10.7 (7)
C9ii—Cd1—N3—C222.9 (6)C4—C3A—C7A—N1177.6 (6)
C9iii—Cd1—N3—C2123.6 (5)N3—C3A—C7A—C7179.9 (6)
N3i—Cd1—N3—C3A103.5 (5)C4—C3A—C7A—C73.0 (10)
O2ii—Cd1—N3—C3A133.5 (5)C3A—N3—C2—N10.8 (7)
O2iii—Cd1—N3—C3A55.2 (5)Cd1—N3—C2—N1160.1 (4)
O1ii—Cd1—N3—C3A137.7 (5)C3A—N3—C2—C10179.1 (6)
O1iii—Cd1—N3—C3A4.9 (6)Cd1—N3—C2—C1019.8 (9)
C9ii—Cd1—N3—C3A133.0 (5)C7A—N1—C2—N30.4 (7)
C9iii—Cd1—N3—C3A32.2 (5)C8—N1—C2—N3179.2 (6)
C7A—C7—C6—C50.4 (11)C7A—N1—C2—C10179.5 (6)
C7—C6—C5—C43.3 (12)C8—N1—C2—C100.7 (10)
C6—C5—C4—C3A2.9 (11)C2—N1—C8—C969.4 (9)
C2—N3—C3A—C4177.3 (7)C7A—N1—C8—C9112.0 (7)
Cd1—N3—C3A—C422.8 (10)Cd1iv—O1—C9—O211.4 (7)
C2—N3—C3A—C7A0.9 (7)Cd1iv—O1—C9—C8169.1 (6)
Cd1—N3—C3A—C7A160.8 (4)Cd1iv—O2—C9—O112.0 (7)
C5—C4—C3A—N3176.2 (7)Cd1iv—O2—C9—C8168.4 (5)
C5—C4—C3A—C7A0.2 (10)N1—C8—C9—O113.9 (10)
C2—N1—C7A—C7179.5 (7)N1—C8—C9—O2166.5 (6)
C8—N1—C7A—C70.7 (11)N1—C8—C9—Cd1iv110 (2)
Symmetry codes: (i) x+2, y, z+1/2; (ii) x+3/2, y1/2, z+1/2; (iii) x+1/2, y1/2, z; (iv) x1/2, y+1/2, z.

Experimental details

(I)(II)
Crystal data
Chemical formula[Cd(C10H9N2O2)2][Cd(C10H9N2O2)2]
Mr490.79490.79
Crystal system, space groupOrthorhombic, IbcaMonoclinic, C2/c
Temperature (K)293293
a, b, c (Å)14.7042 (4), 14.0074 (4), 37.9500 (9)11.476 (7), 11.641 (7), 14.064 (13)
α, β, γ (°)90, 90, 9090, 90.701 (14), 90
V3)7816.5 (4)1879 (2)
Z164
Radiation typeMo KαMo Kα
µ (mm1)1.151.20
Crystal size (mm)0.38 × 0.34 × 0.30.20 × 0.20 × 0.20
Data collection
DiffractometerRigaku SCXmini
diffractometer
Rigaku SCXmini
diffractometer
Absorption correctionMulti-scan
(CrystalClear; Rigaku, 2005)
Multi-scan
(CrystalClear; Rigaku, 2005)
Tmin, Tmax0.652, 0.7080.787, 0.787
No. of measured, independent and
observed [I > 2σ(I)] reflections
29375, 4479, 3781 9836, 2421, 2168
Rint0.0410.061
(sin θ/λ)max1)0.6490.676
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.030, 0.068, 1.14 0.066, 0.195, 1.23
No. of reflections44792421
No. of parameters265133
H-atom treatmentH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.43, 0.370.90, 1.42

Computer programs: CrystalClear (Rigaku, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg & Putz, 2005).

Selected geometric parameters (Å, º) for (I) top
Cd1—N1i2.254 (2)Cd2—N3ii2.230 (2)
Cd1—O12.471 (2)Cd2—O32.2753 (19)
Cd1—O22.3448 (19)Cd2—O42.617 (2)
N1i—Cd1—N1iii101.51 (10)N3ii—Cd2—N3iv105.44 (10)
O2—Cd1—O154.13 (6)O3—Cd2—O452.90 (7)
Symmetry codes: (i) x1/2, y+1, z; (ii) x+1/2, y+1/2, z; (iii) x1/2, y, z+1/2; (iv) x, y+1/2, z.
Selected geometric parameters (Å, º) for (II) top
Cd1—N32.258 (5)Cd1—O2i2.337 (5)
Cd1—O1i2.467 (5)
O2ii—Cd1—N3iii90.03 (19)O2i—Cd1—O1ii82.7 (2)
O2i—Cd1—N3iii154.3 (2)N3—Cd1—O1i114.47 (19)
N3—Cd1—N3iii104.7 (3)N3iii—Cd1—O1i100.02 (19)
O2ii—Cd1—O2i84.9 (3)O2i—Cd1—O1i54.39 (18)
N3iii—Cd1—O1ii114.47 (19)O1ii—Cd1—O1i122.5 (2)
Symmetry codes: (i) x+1/2, y1/2, z; (ii) x+3/2, y1/2, z+1/2; (iii) x+2, y, z+1/2.
 

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