Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229614022852/lg3147sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229614022852/lg3147Isup2.hkl |
CCDC reference: 1029730
During the past decade coordination polymers have attracted great interest, not only owing to their intriguing variety of topologies but also because of their potential applications in many fields, such as ion-exchange media, heterogeneous catalysts, optical devices, molecular magnets and gas-storage devices (Du et al., 2013; Li et al., 2010; Luo et al., 2010; Ma et al., 2009; Su et al., 2010). Generally, the assembly of coordination polymers is mainly affected by the combination of a few factors including temperature, the neutral ligands, the organic anions and the metal atoms (Cook et al., 2013; Almeida Paz et al., 2012). Among these factors, great effort has been devoted to the design of suitable organic ligands to construct new coordination polymers.
Organic ligands that contain carboxylic groups are frequently used for coordination polymers since the carboxylate group has an excellent coordination capability and flexible coordination patterns, which result in a large diversity of structures. Benzophenone-2,4'-dicarboxylic acid (H2bpdc), an asymmetrically V-shaped aromatic polycarboxylic acid derivative, has been used as a bridging ligand in the synthesis of novel coordination polymers (Chen et al., 2012; Hu et al., 2011, 2009; Xu et al., 2012). Taking inspiration from the points mentioned above, we explored the self-assembly of the CdII cation and H2bpdc under hydrothermal conditions, and obtained a novel two-dimensional coordination polymer, [Cd(bpdc)·H2O]n, (I), and we now report its synthesis, crystal structure and physical properties.
All chemicals used in the experiment were purchased from commercial sources (Sigma–Aldrich) and used without further purification. The C and H elemental analysis was performed on a Vario EL III elemental analyser (Elementar Analysensysteme GmbH). The IR spectrum was recorded from a KBr pellet in the range 4000–400 cm-1 on a VECTOR 22 spectrometer (Bruker). The fluorescence spectrum was recorded on a Fluoro Max-P spectrophotometer (Perkin–Elmer). Thermogravimetric analysis was performed on a Perkin–Elmer Pyris 1 TGA analyser from 298 to 1123 K with a heating rate of 20 K min-1 under nitrogen (TA Instruments). The electric hysteresis loop was measured with a Premier II ferroelectric tester at room temperature (Radiant Technology Inc.).
A mixture of Cd(NO3)2·6H2O (0.0346 g, 0.1 mmol), H2bpdc (0.0271 g, 0.1 mmol) and KOH (0.0112 g, 0.2 mmol) in H2O (10 ml) was sealed in a 16 ml Teflon-lined stainless steel container and heated at 493 K for 72 h. After cooling to room temperature, colourless block crystals of (I) were collected by filtration and washed in water and ethanol several times (yield 22.9%, based on H2bpdc). Elemental analysis for C15H10CdO6 (Mr = 398.63): C 45.19, H 2.53; found: C 45.28, H 2.54. IR (KBr, ν, cm-1) : 3439 (m), 3057 (m), 1661 (s), 1578 (s), 1424 (vs), 1274 (s), 1234 (s), 841 (s), 771 (s), 722 (s).
Crystal data, data collection and structure refinement details are summarized in Table 1. C-bound H atoms were placed in calculated positions and treated using a riding-model approximation, with C—H = 0.93 Å (aromatic) and with Uiso(H) = 1.2Ueq(C). Water H atoms were located in a difference Fourier map and refined with Uiso(H) = 1.2Ueq(O) and with the O—H distance restrained to 0.85 (2) Å.
X-ray crystallography reveals that the asymmetric unit of (I) consists of a divalent cadmium cation, one fully deprotonated bpdc ligand and one aqua ligand. As shown in Fig. 1, atom Cd1 is six-coordinated by two O atoms from one bpdc2- ligand in a chelating mode, three O donor atoms from three individual bpdc anions and one O atom from a coordinated aqua molecule in an octahedral coordination environment (Table 2). The average of the Cd—O distances [2.31 (4) Å] is indeed comparable with those for other structures containing CdII (Wang et al., 2013; Wang, 2014).
In the bpdc2- ligand in (I), the dihedral angle between the two benzene rings is 79.8 (2)° and the C5—C8—C9 angle is 118.6 (3)°. The dihedral angles between the carboxylate groups at C1 and C15 and their adjacent benzene rings are 19.7 (3) and 17.5 (3)°, respectively. Each bpdc anion in (I) acts in a µ4-mode (µ2-η1:η1 and µ2-η2:η1), with one carboxylate group bridging two CdII cations in a bis-monodentate mode and the other carboxylate group bridging two other CdII cations in a briding mode. Two crystallographically equivalent CdII cations are bridged by one carboxylate group (O4–C15–O5) and the carboxylate group containing atoms O1, O2 and C1 to form a binuclear [(Cd1)2(O1)(O4–C15–O5)] secondary building unit (SBU) with a Cd···Cd separation of 3.805 (2) Å. As shown in Fig 2, adjacent SBUs are interlinked to form a one-dimensional [Cd(OCO)2]n chain extending along the c axis. The bpdc2- ligands link these rod-shaped SBUs to give rise to a complicated two-dimensional [Cd(bpdc)]n framework parallel to the (010) crystal plane (Fig 3).
The topology of this neutral [Cd(bpdc)]n two-dimensional framework can be simplified by regarding both the CdII cations and the bpdc2- ligands as 4-connected nodes. The resulting network thus has a 4,4-connected binodal net topology of point symbol {43.62.8} (Fig. 4). To the best of our knowledge, this 4,4-connected binodal lattice has not yet been reported in coordination polymer chemistry.
Interlayer interactions are fostered by weak O—H···O and C—H···O hydrogen bonds (see Table 3), constructing a three-dimensional supramolecular architecture.
To test the thermal stability of (I), thermogravimetric analysis (TGA) was conducted. As shown in Fig. 5, the coordination water molecule was lost between 373 and 433 K (observed 3.98%, calculated 4.52%). The anhydrous substance was stable upon heating to 483 K. The decomposition of the organic ligand is observed between 483 and 1063 K, and the remaining weight corresponds to the formation of CdO (observed 32.03%, calculated 32.21%).
Due to the excellent fluorescence properties of d10 metal compounds, the solid-state photoluminescent properties of (I) were investigated at room temperature. The H2bpdc ligand exhibits a broad weak fluorescent emission centred at 394 nm with an excitation maximum at 280 nm, which are probably attributed to π*–n or π*–π transitions, as previously reported (Xu et al., 2012). Compound (I) exhibits a relatively [strong? Text missing] emission band centred on ~410 nm upon excitation at 290 nm (Fig. 6). Because the CdII cation is difficult to oxidize or reduce, due to its d10 configuration, the emissive behaviour of (I) can be attributed to ligand-centred electronic transitions (Guo et al., 2011; Wen et al., 2007).
Since (I) crystallizes in the non-centrosymmetric space group Aba2, which belongs to one of the ten polar point groups, its ferroelectric features were investigated (Hang et al., 2011; Zhang & Xiong, 2012). Fig. 7 clearly indicates that (I) does indeed display ferroelectric behaviour, with a remnant polarization (Pr) of ca 0.67 µC cm-2 and a coercive field (Ec) of 475.35 V cm-1. The saturation value of the spontaneous polarization (Ps) is ~1.23 µC cm-2.
Data collection: SMART (Bruker 2000); cell refinement: SAINT (Bruker 2000); data reduction: SAINT (Bruker 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
[Cd(C15H8O5)(H2O)] | Z = 8 |
Mr = 398.63 | F(000) = 1568 |
Orthorhombic, Aba2 | Dx = 1.953 Mg m−3 |
Hall symbol: A 2 -2ac | Mo Kα radiation, λ = 0.71073 Å |
a = 12.664 (6) Å | µ = 1.64 mm−1 |
b = 30.334 (15) Å | T = 296 K |
c = 7.060 (4) Å | Block, colourless |
V = 2712 (2) Å3 | 0.21 × 0.19 × 0.17 mm |
Bruker SMART CCD area-detector diffractometer | 3061 independent reflections |
Radiation source: fine-focus sealed tube | 2511 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
ϕ and ω scans | θmax = 27.6°, θmin = 2.1° |
Absorption correction: multi-scan SADABS (Bruker, 2000) | h = −8→16 |
Tmin = 0.725, Tmax = 0.768 | k = −39→25 |
8238 measured reflections | l = −9→9 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.028 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.055 | w = 1/[σ2(Fo2) + (0.0207P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.99 | (Δ/σ)max = 0.002 |
3061 reflections | Δρmax = 0.36 e Å−3 |
205 parameters | Δρmin = −0.89 e Å−3 |
3 restraints | Absolute structure: Flack (1983), with 1218 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.02 (3) |
[Cd(C15H8O5)(H2O)] | V = 2712 (2) Å3 |
Mr = 398.63 | Z = 8 |
Orthorhombic, Aba2 | Mo Kα radiation |
a = 12.664 (6) Å | µ = 1.64 mm−1 |
b = 30.334 (15) Å | T = 296 K |
c = 7.060 (4) Å | 0.21 × 0.19 × 0.17 mm |
Bruker SMART CCD area-detector diffractometer | 3061 independent reflections |
Absorption correction: multi-scan SADABS (Bruker, 2000) | 2511 reflections with I > 2σ(I) |
Tmin = 0.725, Tmax = 0.768 | Rint = 0.034 |
8238 measured reflections |
R[F2 > 2σ(F2)] = 0.028 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.055 | Δρmax = 0.36 e Å−3 |
S = 0.99 | Δρmin = −0.89 e Å−3 |
3061 reflections | Absolute structure: Flack (1983), with 1218 Friedel pairs |
205 parameters | Absolute structure parameter: 0.02 (3) |
3 restraints |
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. |
x | y | z | Uiso*/Ueq | ||
C1 | 0.1456 (3) | 0.46675 (13) | 0.3340 (5) | 0.0247 (9) | |
C2 | 0.1314 (3) | 0.50502 (15) | 0.4667 (6) | 0.0221 (10) | |
C3 | 0.1242 (4) | 0.54738 (15) | 0.3946 (7) | 0.0293 (12) | |
H3 | 0.1260 | 0.5520 | 0.2644 | 0.035* | |
C4 | 0.1143 (4) | 0.58270 (17) | 0.5164 (6) | 0.0286 (12) | |
H4 | 0.1118 | 0.6112 | 0.4675 | 0.034* | |
C5 | 0.1080 (4) | 0.57638 (16) | 0.7112 (6) | 0.0233 (10) | |
C6 | 0.1151 (4) | 0.53324 (15) | 0.7841 (6) | 0.0255 (11) | |
H6 | 0.1117 | 0.5285 | 0.9141 | 0.031* | |
C7 | 0.1269 (4) | 0.49802 (16) | 0.6622 (6) | 0.0240 (11) | |
H7 | 0.1318 | 0.4695 | 0.7103 | 0.029* | |
C8 | 0.0973 (3) | 0.61466 (13) | 0.8439 (6) | 0.0288 (9) | |
C9 | 0.0826 (3) | 0.65986 (13) | 0.7619 (5) | 0.0275 (9) | |
C10 | 0.1692 (3) | 0.68747 (16) | 0.7589 (7) | 0.0443 (12) | |
H10 | 0.2327 | 0.6782 | 0.8118 | 0.053* | |
C11 | 0.1619 (4) | 0.72935 (16) | 0.6764 (7) | 0.0543 (14) | |
H11 | 0.2207 | 0.7477 | 0.6751 | 0.065* | |
C12 | 0.0700 (4) | 0.74334 (12) | 0.5987 (13) | 0.0513 (11) | |
H12 | 0.0661 | 0.7710 | 0.5424 | 0.062* | |
C13 | −0.0181 (3) | 0.71616 (11) | 0.6034 (9) | 0.0367 (9) | |
H13 | −0.0812 | 0.7259 | 0.5509 | 0.044* | |
C14 | −0.0134 (3) | 0.67491 (13) | 0.6849 (5) | 0.0262 (9) | |
C15 | −0.1114 (3) | 0.64644 (13) | 0.6943 (5) | 0.0274 (9) | |
Cd1 | 0.193946 (18) | 0.400042 (7) | 0.09130 (6) | 0.02709 (7) | |
O1 | 0.1826 (2) | 0.43005 (9) | 0.3988 (4) | 0.0327 (6) | |
O2 | 0.1235 (2) | 0.47011 (9) | 0.1631 (4) | 0.0344 (7) | |
O3 | 0.1084 (3) | 0.61025 (9) | 1.0158 (4) | 0.0460 (8) | |
O4 | −0.1117 (2) | 0.61486 (9) | 0.8091 (4) | 0.0369 (7) | |
O5 | −0.1862 (2) | 0.65611 (8) | 0.5860 (10) | 0.0484 (7) | |
O6 | 0.0677 (3) | 0.35110 (12) | 0.1977 (4) | 0.0470 (8) | |
H6A | 0.074 (4) | 0.3446 (15) | 0.312 (3) | 0.056* | |
H6B | 0.0031 (18) | 0.3508 (16) | 0.168 (6) | 0.056* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.020 (2) | 0.025 (2) | 0.028 (2) | −0.0015 (16) | 0.0025 (16) | −0.0026 (16) |
C2 | 0.020 (2) | 0.025 (3) | 0.021 (2) | 0.0005 (18) | 0.0006 (17) | 0.0037 (18) |
C3 | 0.040 (3) | 0.024 (3) | 0.023 (2) | 0.006 (2) | 0.0028 (19) | 0.0031 (19) |
C4 | 0.039 (3) | 0.019 (2) | 0.027 (2) | 0.000 (2) | 0.0004 (18) | 0.0010 (18) |
C5 | 0.024 (2) | 0.024 (3) | 0.022 (2) | 0.004 (2) | 0.0022 (17) | −0.0033 (18) |
C6 | 0.027 (2) | 0.027 (3) | 0.022 (2) | 0.003 (2) | −0.0026 (18) | 0.004 (2) |
C7 | 0.031 (2) | 0.018 (2) | 0.0229 (19) | 0.0073 (19) | −0.0050 (16) | −0.0007 (16) |
C8 | 0.025 (2) | 0.030 (2) | 0.031 (2) | 0.0004 (17) | −0.0027 (17) | 0.0001 (17) |
C9 | 0.033 (2) | 0.025 (2) | 0.0249 (19) | −0.0001 (19) | 0.0022 (17) | −0.0073 (16) |
C10 | 0.034 (3) | 0.041 (3) | 0.057 (3) | −0.006 (2) | −0.005 (2) | −0.010 (2) |
C11 | 0.057 (3) | 0.038 (3) | 0.068 (3) | −0.020 (3) | 0.016 (3) | −0.013 (2) |
C12 | 0.079 (3) | 0.027 (2) | 0.048 (2) | −0.008 (2) | 0.008 (4) | 0.010 (4) |
C13 | 0.054 (2) | 0.0240 (19) | 0.032 (2) | 0.0026 (16) | −0.001 (3) | 0.001 (3) |
C14 | 0.036 (2) | 0.023 (2) | 0.0192 (18) | −0.0026 (17) | 0.0028 (16) | −0.0013 (15) |
C15 | 0.031 (2) | 0.022 (2) | 0.029 (2) | −0.0013 (18) | 0.0039 (17) | −0.0063 (17) |
Cd1 | 0.03306 (13) | 0.02638 (13) | 0.02184 (10) | −0.00207 (11) | −0.0006 (2) | −0.0039 (2) |
O1 | 0.0399 (17) | 0.0254 (16) | 0.0328 (14) | 0.0076 (13) | −0.0088 (13) | −0.0024 (12) |
O2 | 0.0449 (18) | 0.0328 (17) | 0.0254 (13) | 0.0077 (13) | 0.0012 (12) | −0.0039 (11) |
O3 | 0.071 (2) | 0.042 (2) | 0.0247 (13) | 0.0157 (16) | −0.0099 (14) | −0.0031 (12) |
O4 | 0.0443 (18) | 0.0330 (17) | 0.0334 (15) | −0.0036 (14) | 0.0100 (13) | 0.0001 (13) |
O5 | 0.0400 (16) | 0.0341 (15) | 0.0711 (19) | 0.0004 (12) | −0.016 (3) | −0.002 (3) |
O6 | 0.060 (2) | 0.049 (2) | 0.0322 (17) | −0.0167 (18) | −0.0028 (16) | 0.0080 (15) |
C1—O2 | 1.243 (4) | C11—C12 | 1.354 (7) |
C1—O1 | 1.291 (4) | C11—H11 | 0.9300 |
C1—C2 | 1.503 (6) | C12—C13 | 1.388 (5) |
C2—C3 | 1.385 (6) | C12—H12 | 0.9300 |
C2—C7 | 1.398 (6) | C13—C14 | 1.378 (5) |
C3—C4 | 1.379 (6) | C13—H13 | 0.9300 |
C3—H3 | 0.9300 | C14—C15 | 1.514 (5) |
C4—C5 | 1.391 (5) | C15—O5 | 1.253 (6) |
C4—H4 | 0.9300 | C15—O4 | 1.255 (5) |
C5—C6 | 1.409 (6) | Cd1—O1i | 2.263 (3) |
C5—C8 | 1.498 (6) | Cd1—O5ii | 2.281 (3) |
C6—C7 | 1.380 (6) | Cd1—O4iii | 2.293 (3) |
C6—H6 | 0.9300 | Cd1—O6 | 2.307 (3) |
C7—H7 | 0.9300 | Cd1—O1 | 2.358 (3) |
C8—O3 | 1.229 (5) | Cd1—O2 | 2.360 (3) |
C8—C9 | 1.500 (5) | O1—Cd1iv | 2.263 (3) |
C9—C10 | 1.380 (6) | O4—Cd1v | 2.293 (3) |
C9—C14 | 1.409 (5) | O5—Cd1vi | 2.281 (3) |
C10—C11 | 1.401 (7) | O6—H6A | 0.836 (19) |
C10—H10 | 0.9300 | O6—H6B | 0.845 (19) |
O2—C1—O1 | 119.7 (3) | C13—C12—H12 | 120.2 |
O2—C1—C2 | 121.0 (4) | C14—C13—C12 | 121.0 (5) |
O1—C1—C2 | 119.3 (3) | C14—C13—H13 | 119.5 |
C3—C2—C7 | 120.1 (5) | C12—C13—H13 | 119.5 |
C3—C2—C1 | 119.7 (4) | C13—C14—C9 | 119.5 (4) |
C7—C2—C1 | 120.2 (4) | C13—C14—C15 | 120.1 (4) |
C4—C3—C2 | 119.8 (5) | C9—C14—C15 | 120.4 (3) |
C4—C3—H3 | 120.1 | O5—C15—O4 | 124.8 (4) |
C2—C3—H3 | 120.1 | O5—C15—C14 | 117.4 (4) |
C3—C4—C5 | 121.0 (5) | O4—C15—C14 | 117.8 (4) |
C3—C4—H4 | 119.5 | O1i—Cd1—O5ii | 80.26 (14) |
C5—C4—H4 | 119.5 | O1i—Cd1—O4iii | 82.62 (10) |
C4—C5—C6 | 119.1 (5) | O5ii—Cd1—O4iii | 98.09 (17) |
C4—C5—C8 | 121.1 (5) | O1i—Cd1—O6 | 158.91 (11) |
C6—C5—C8 | 119.8 (4) | O5ii—Cd1—O6 | 89.18 (13) |
C7—C6—C5 | 119.9 (4) | O4iii—Cd1—O6 | 80.86 (11) |
C7—C6—H6 | 120.1 | O1i—Cd1—O1 | 116.10 (10) |
C5—C6—H6 | 120.1 | O5ii—Cd1—O1 | 110.11 (18) |
C6—C7—C2 | 120.2 (5) | O4iii—Cd1—O1 | 147.99 (10) |
C6—C7—H7 | 119.9 | O6—Cd1—O1 | 84.63 (11) |
C2—C7—H7 | 119.9 | O1i—Cd1—O2 | 91.61 (10) |
O3—C8—C9 | 119.7 (4) | O5ii—Cd1—O2 | 158.02 (13) |
O3—C8—C5 | 121.5 (4) | O4iii—Cd1—O2 | 101.09 (10) |
C9—C8—C5 | 118.6 (3) | O6—Cd1—O2 | 104.34 (12) |
C10—C9—C14 | 118.9 (4) | O1—Cd1—O2 | 55.37 (9) |
C10—C9—C8 | 117.5 (4) | C1—O1—Cd1iv | 144.1 (2) |
C14—C9—C8 | 123.5 (3) | C1—O1—Cd1 | 91.7 (2) |
C9—C10—C11 | 120.3 (4) | Cd1iv—O1—Cd1 | 110.81 (11) |
C9—C10—H10 | 119.9 | C1—O2—Cd1 | 92.8 (2) |
C11—C10—H10 | 119.9 | C15—O4—Cd1v | 135.5 (3) |
C12—C11—C10 | 120.6 (4) | C15—O5—Cd1vi | 108.6 (3) |
C12—C11—H11 | 119.7 | Cd1—O6—H6A | 114 (3) |
C10—C11—H11 | 119.7 | Cd1—O6—H6B | 127 (3) |
C11—C12—C13 | 119.7 (5) | H6A—O6—H6B | 109 (4) |
C11—C12—H12 | 120.2 | ||
O2—C1—C2—C3 | −19.3 (6) | C10—C9—C14—C15 | −177.0 (4) |
O1—C1—C2—C3 | 159.9 (4) | C8—C9—C14—C15 | 4.6 (5) |
O2—C1—C2—C7 | 161.5 (5) | C13—C14—C15—O5 | 18.1 (6) |
O1—C1—C2—C7 | −19.3 (7) | C9—C14—C15—O5 | −163.0 (4) |
C7—C2—C3—C4 | 1.1 (8) | C13—C14—C15—O4 | −162.2 (4) |
C1—C2—C3—C4 | −178.1 (4) | C9—C14—C15—O4 | 16.7 (5) |
C2—C3—C4—C5 | −2.1 (9) | O2—C1—O1—Cd1iv | 136.6 (3) |
C3—C4—C5—C6 | 1.9 (10) | C2—C1—O1—Cd1iv | −42.6 (6) |
C3—C4—C5—C8 | −180.0 (4) | O2—C1—O1—Cd1 | 6.4 (4) |
C4—C5—C6—C7 | −0.7 (8) | C2—C1—O1—Cd1 | −172.8 (3) |
C8—C5—C6—C7 | −178.8 (4) | O1i—Cd1—O1—C1 | 68.99 (19) |
C5—C6—C7—C2 | −0.3 (8) | O5ii—Cd1—O1—C1 | 157.8 (2) |
C3—C2—C7—C6 | 0.1 (9) | O4iii—Cd1—O1—C1 | −51.9 (3) |
C1—C2—C7—C6 | 179.3 (4) | O6—Cd1—O1—C1 | −115.1 (2) |
C4—C5—C8—O3 | −168.3 (5) | O2—Cd1—O1—C1 | −3.5 (2) |
C6—C5—C8—O3 | 9.8 (7) | O1i—Cd1—O1—Cd1iv | −82.36 (19) |
C4—C5—C8—C9 | 5.9 (7) | O5ii—Cd1—O1—Cd1iv | 6.42 (15) |
C6—C5—C8—C9 | −175.9 (4) | O4iii—Cd1—O1—Cd1iv | 156.72 (14) |
O3—C8—C9—C10 | 72.0 (5) | O6—Cd1—O1—Cd1iv | 93.56 (14) |
C5—C8—C9—C10 | −102.4 (5) | O2—Cd1—O1—Cd1iv | −154.89 (17) |
O3—C8—C9—C14 | −109.6 (5) | O1—C1—O2—Cd1 | −6.4 (4) |
C5—C8—C9—C14 | 76.1 (5) | C2—C1—O2—Cd1 | 172.8 (3) |
C14—C9—C10—C11 | −1.4 (6) | O1i—Cd1—O2—C1 | −117.3 (2) |
C8—C9—C10—C11 | 177.1 (4) | O5ii—Cd1—O2—C1 | −49.8 (5) |
C9—C10—C11—C12 | 0.0 (8) | O4iii—Cd1—O2—C1 | 159.9 (2) |
C10—C11—C12—C13 | 1.0 (10) | O6—Cd1—O2—C1 | 76.6 (3) |
C11—C12—C13—C14 | −0.5 (11) | O1—Cd1—O2—C1 | 3.7 (2) |
C12—C13—C14—C9 | −0.9 (8) | O5—C15—O4—Cd1v | −72.4 (6) |
C12—C13—C14—C15 | 177.9 (6) | C14—C15—O4—Cd1v | 107.9 (4) |
C10—C9—C14—C13 | 1.9 (6) | O4—C15—O5—Cd1vi | −10.9 (6) |
C8—C9—C14—C13 | −176.6 (4) | C14—C15—O5—Cd1vi | 168.8 (3) |
Symmetry codes: (i) −x+1/2, y, z−1/2; (ii) x+1/2, −y+1, z−1/2; (iii) −x, −y+1, z−1; (iv) −x+1/2, y, z+1/2; (v) −x, −y+1, z+1; (vi) x−1/2, −y+1, z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O6—H6A···O5vii | 0.84 (2) | 2.40 (3) | 3.133 (8) | 147 (4) |
O6—H6B···O3iii | 0.85 (2) | 2.13 (3) | 2.828 (5) | 139 (4) |
C3—H3···O3viii | 0.93 | 2.50 | 3.290 (6) | 143 |
C6—H6···O2ix | 0.93 | 2.50 | 3.292 (5) | 143 |
Symmetry codes: (iii) −x, −y+1, z−1; (vii) −x, −y+1, z; (viii) x, y, z−1; (ix) x, y, z+1. |
Experimental details
Crystal data | |
Chemical formula | [Cd(C15H8O5)(H2O)] |
Mr | 398.63 |
Crystal system, space group | Orthorhombic, Aba2 |
Temperature (K) | 296 |
a, b, c (Å) | 12.664 (6), 30.334 (15), 7.060 (4) |
V (Å3) | 2712 (2) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 1.64 |
Crystal size (mm) | 0.21 × 0.19 × 0.17 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector diffractometer |
Absorption correction | Multi-scan SADABS (Bruker, 2000) |
Tmin, Tmax | 0.725, 0.768 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8238, 3061, 2511 |
Rint | 0.034 |
(sin θ/λ)max (Å−1) | 0.652 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.028, 0.055, 0.99 |
No. of reflections | 3061 |
No. of parameters | 205 |
No. of restraints | 3 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.36, −0.89 |
Absolute structure | Flack (1983), with 1218 Friedel pairs |
Absolute structure parameter | 0.02 (3) |
Computer programs: SMART (Bruker 2000), SAINT (Bruker 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 1999), SHELXTL (Sheldrick, 2008).
Cd1—O1i | 2.263 (3) | Cd1—O6 | 2.307 (3) |
Cd1—O5ii | 2.281 (3) | Cd1—O1 | 2.358 (3) |
Cd1—O4iii | 2.293 (3) | Cd1—O2 | 2.360 (3) |
O1i—Cd1—O5ii | 80.26 (14) | O4iii—Cd1—O1 | 147.99 (10) |
O1i—Cd1—O4iii | 82.62 (10) | O6—Cd1—O1 | 84.63 (11) |
O5ii—Cd1—O4iii | 98.09 (17) | O1i—Cd1—O2 | 91.61 (10) |
O1i—Cd1—O6 | 158.91 (11) | O5ii—Cd1—O2 | 158.02 (13) |
O5ii—Cd1—O6 | 89.18 (13) | O4iii—Cd1—O2 | 101.09 (10) |
O4iii—Cd1—O6 | 80.86 (11) | O6—Cd1—O2 | 104.34 (12) |
O1i—Cd1—O1 | 116.10 (10) | O1—Cd1—O2 | 55.37 (9) |
O5ii—Cd1—O1 | 110.11 (18) |
Symmetry codes: (i) −x+1/2, y, z−1/2; (ii) x+1/2, −y+1, z−1/2; (iii) −x, −y+1, z−1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O6—H6A···O5iv | 0.836 (19) | 2.40 (3) | 3.133 (8) | 147 (4) |
O6—H6B···O3iii | 0.845 (19) | 2.13 (3) | 2.828 (5) | 139 (4) |
C3—H3···O3v | 0.93 | 2.50 | 3.290 (6) | 143 |
C6—H6···O2vi | 0.93 | 2.50 | 3.292 (5) | 143 |
Symmetry codes: (iii) −x, −y+1, z−1; (iv) −x, −y+1, z; (v) x, y, z−1; (vi) x, y, z+1. |