metal-organic compounds
Poly[[aqua(μ2-4,4′-bipyridine-κ2N:N′)[μ3-3-bromo-2-(carboxylatomethyl)benzoato-κ3O1:O1′:O2]cadmium] monohydrate]
aNational Food Packaging Products Quality Supervision and Inspection Center, Jiangsu Provincial Supervising and Testing Research Institute for Products Quality, Nanjing 210007, Jiangsu, People's Republic of China, and bSchool of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210093, Jiangsu, People's Republic of China
*Correspondence e-mail: hare1014@163.com
In the title compound, {[Cd(C9H5BrO4)(C10H8N2)(H2O)]·H2O}n, the CdII atom has a distorted octahedral coordination geometry. Two N atoms from two 4,4′-bipyridine (bipy) ligands occupy the axial positions, while the equatorial positions are furnished by three carboxylate O atoms from three 3-bromo-2-(carboxylatomethyl)benzoate (bcb) ligands and one O atom from a water molecule. The bipy and bcb ligands link the CdII atoms into a three-dimensional network. O—H⋯O hydrogen bonds and π–π interactions between the pyridine and benzene rings [centroid–centroid distance = 3.736 (4) Å] are present in the crystal.
Experimental
Crystal data
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Data collection: APEX2 (Bruker, 2007); cell SAINT (Bruker, 2007); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL; molecular graphics: XP in SHELXTL and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL.
Supporting information
https://doi.org/10.1107/S1600536812031297/hy2559sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536812031297/hy2559Isup2.hkl
A mixture of 3-bromo-2-(carboxymethyl)benzoic acid (0.1 mmol, 25.9 mg), 4,4'-bipyridine (0.1 mmol, 19.5 mg), Cd(NO3)2.4H2O (0.1 mmol, 30.9 mg) and 8 ml water was sealed in a 23 ml Teflon-lined autoclave. The pH value of the mixture was adjusted to 7.0 with NaOH solution. The autoclave was kept at 393 K for 3 days. After the mixture was slowly cooled to room temperature, colorless crystals of the title compound were obtained.
H atoms bonded to C atoms were positioned geometrically and refined as riding atoms, with C—H = 0.93 (aromatic) and 0.97 (CH2) Å and with Uiso(H) = 1.2Ueq(C). Water H atoms were located in a difference Fourier map and refined as riding, with O—H = 0.85 Å and with Uiso(H) = 1.2(1.5 for O5)Ueq(O).
In the title complex (Fig. 1), the carboxylate group containing O1 and O2 is monocoordinated and the other carboxylate group containing O3 and O4 is bidentate and bridging. Therefore, the 3-bromo-2-(carboxymethyl)benzoate (bcb) ligand coordinates with three Cd atoms. The Cd atom is coordinated by three bcb ligands, forming a two-dimensional polymeric layer parallel to (1 1 0). Since each Cd atom is coordinated by three bcb ligands, from a topology viewpoint the Cd atom can be considered as a 3-connecting node and the center of benzene ring of the bcb ligand also acts as a 3-connecting node. In this way, the polymeric layer can be simplified to a 63 network (Fig. 2). The 4,4'-bipyridine ligands act as bridges to connect the neighboring Cd atoms which come from different layers, forming a three-dimensional rigid porous network. This three-dimensional topology can be defined with Schläfli symbol (63)(69.8) (Fig. 3).
For related structures, see: Liu et al. (2010).
Data collection: APEX2 (Bruker, 2007); cell
SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).[Cd(C9H5BrO4)(C10H8N2)(H2O)]·H2O | F(000) = 552 |
Mr = 561.66 | Dx = 1.918 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2yb | Cell parameters from 1319 reflections |
a = 9.3257 (19) Å | θ = 2.6–21.3° |
b = 9.1312 (18) Å | µ = 3.22 mm−1 |
c = 11.652 (2) Å | T = 291 K |
β = 101.344 (4)° | Block, colorless |
V = 972.8 (3) Å3 | 0.29 × 0.26 × 0.23 mm |
Z = 2 |
Bruker APEXII CCD diffractometer | 3122 independent reflections |
Radiation source: sealed tube | 2807 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
φ and ω scans | θmax = 26.0°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −11→8 |
Tmin = 0.466, Tmax = 0.538 | k = −11→10 |
5248 measured reflections | l = −14→13 |
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)] = 0.049 | H-atom parameters constrained |
wR(F2) = 0.118 | w = 1/[σ2(Fo2) + (0.07P)2 + 1.99P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max < 0.001 |
3122 reflections | Δρmax = 0.49 e Å−3 |
251 parameters | Δρmin = −0.93 e Å−3 |
1 restraint | Absolute structure: Flack (1983), 1096 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.07 (2) |
[Cd(C9H5BrO4)(C10H8N2)(H2O)]·H2O | V = 972.8 (3) Å3 |
Mr = 561.66 | Z = 2 |
Monoclinic, P21 | Mo Kα radiation |
a = 9.3257 (19) Å | µ = 3.22 mm−1 |
b = 9.1312 (18) Å | T = 291 K |
c = 11.652 (2) Å | 0.29 × 0.26 × 0.23 mm |
β = 101.344 (4)° |
Bruker APEXII CCD diffractometer | 3122 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | 2807 reflections with I > 2σ(I) |
Tmin = 0.466, Tmax = 0.538 | Rint = 0.033 |
5248 measured reflections |
R[F2 > 2σ(F2)] = 0.049 | H-atom parameters constrained |
wR(F2) = 0.118 | Δρmax = 0.49 e Å−3 |
S = 1.05 | Δρmin = −0.93 e Å−3 |
3122 reflections | Absolute structure: Flack (1983), 1096 Friedel pairs |
251 parameters | Absolute structure parameter: 0.07 (2) |
1 restraint |
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 | ||
Br1 | 0.78647 (11) | 0.15671 (12) | 1.36696 (9) | 0.0477 (3) | |
C1 | 0.9844 (6) | 0.3672 (6) | 1.1234 (3) | 0.038 (2) | |
C2 | 0.9014 (6) | 0.2688 (5) | 1.1738 (4) | 0.040 (2) | |
C3 | 0.8909 (6) | 0.2844 (6) | 1.2905 (4) | 0.043 (2) | |
C4 | 0.9634 (6) | 0.3984 (7) | 1.3568 (3) | 0.0325 (18) | |
H4 | 0.9595 | 0.4095 | 1.4322 | 0.039* | |
C5 | 1.0464 (6) | 0.4968 (6) | 1.3064 (4) | 0.037 (2) | |
H5 | 1.0956 | 0.5725 | 1.3513 | 0.045* | |
C6 | 1.0569 (6) | 0.4812 (6) | 1.1896 (4) | 0.044 (2) | |
H6 | 1.1103 | 0.5453 | 1.1582 | 0.053* | |
C7 | 0.9925 (10) | 0.3554 (11) | 0.9975 (8) | 0.043 (2) | |
C8 | 0.8249 (10) | 0.1429 (14) | 1.0972 (8) | 0.048 (2) | |
H8A | 0.8339 | 0.0584 | 1.1486 | 0.058* | |
H8B | 0.8795 | 0.1215 | 1.0365 | 0.058* | |
C9 | 0.6697 (10) | 0.1577 (12) | 1.0473 (8) | 0.039 (2) | |
C10 | 0.4900 (9) | 0.3415 (11) | 0.7781 (7) | 0.042 (3) | |
H10 | 0.5714 | 0.3723 | 0.8322 | 0.050* | |
C11 | 0.4933 (11) | 0.3408 (11) | 0.6554 (8) | 0.047 (3) | |
H11 | 0.5784 | 0.3712 | 0.6321 | 0.056* | |
C12 | 0.3785 (8) | 0.2859 (10) | 0.5800 (7) | 0.0316 (17) | |
C13 | 0.2515 (10) | 0.2495 (11) | 0.6235 (8) | 0.040 (2) | |
H13 | 0.1689 | 0.2156 | 0.5723 | 0.048* | |
C14 | 0.2516 (11) | 0.2538 (12) | 0.7434 (7) | 0.043 (2) | |
H14 | 0.1700 | 0.2206 | 0.7705 | 0.051* | |
C15 | 0.3746 (8) | 0.2923 (14) | 0.4498 (6) | 0.039 (2) | |
C16 | 0.4478 (10) | 0.4038 (11) | 0.4039 (8) | 0.040 (2) | |
H16 | 0.5014 | 0.4746 | 0.4514 | 0.048* | |
C17 | 0.4438 (11) | 0.4024 (11) | 0.2825 (8) | 0.043 (2) | |
H17 | 0.4953 | 0.4739 | 0.2506 | 0.051* | |
C18 | 0.2976 (10) | 0.2033 (13) | 0.2613 (9) | 0.048 (3) | |
H18 | 0.2452 | 0.1331 | 0.2123 | 0.057* | |
C19 | 0.3039 (11) | 0.1901 (11) | 0.3853 (9) | 0.046 (2) | |
H19 | 0.2529 | 0.1157 | 0.4142 | 0.055* | |
Cd1 | 0.35516 (6) | 0.30525 (7) | 1.01349 (5) | 0.03236 (17) | |
N1 | 0.3714 (7) | 0.3032 (12) | 0.8186 (5) | 0.0387 (15) | |
N2 | 0.3662 (8) | 0.3106 (13) | 0.2123 (6) | 0.0440 (16) | |
O1 | 1.1007 (6) | 0.3167 (10) | 0.9680 (5) | 0.0450 (15) | |
O2 | 0.8816 (8) | 0.3873 (8) | 0.9228 (6) | 0.0454 (16) | |
O3 | 0.6015 (7) | 0.2669 (7) | 1.0621 (5) | 0.0374 (15) | |
O4 | 0.6104 (7) | 0.0555 (8) | 0.9904 (5) | 0.0385 (15) | |
O5 | 0.3078 (7) | 0.0660 (7) | 0.9920 (6) | 0.0367 (15) | |
H5Y | 0.2159 | 0.0524 | 0.9757 | 0.055* | |
H5X | 0.3462 | 0.0320 | 0.9372 | 0.055* | |
O6 | 0.9272 (8) | 0.3735 (8) | 0.7062 (5) | 0.0464 (17) | |
H6X | 0.9963 | 0.3969 | 0.7624 | 0.056* | |
H6Y | 0.8510 | 0.3716 | 0.7360 | 0.056* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Br1 | 0.0485 (6) | 0.0441 (6) | 0.0474 (5) | −0.0073 (4) | 0.0018 (4) | 0.0159 (5) |
C1 | 0.029 (4) | 0.049 (5) | 0.030 (4) | 0.003 (3) | −0.008 (3) | 0.013 (4) |
C2 | 0.048 (5) | 0.026 (5) | 0.042 (4) | −0.005 (3) | −0.003 (4) | −0.002 (4) |
C3 | 0.037 (4) | 0.037 (6) | 0.047 (4) | 0.002 (4) | −0.010 (3) | 0.010 (4) |
C4 | 0.030 (4) | 0.037 (5) | 0.026 (4) | 0.006 (3) | −0.004 (3) | 0.012 (4) |
C5 | 0.042 (4) | 0.031 (5) | 0.032 (4) | −0.008 (4) | −0.010 (4) | −0.014 (4) |
C6 | 0.049 (5) | 0.048 (6) | 0.033 (4) | −0.002 (4) | −0.001 (4) | 0.008 (4) |
C7 | 0.037 (5) | 0.052 (6) | 0.042 (5) | −0.022 (4) | 0.014 (4) | −0.004 (4) |
C8 | 0.036 (5) | 0.064 (7) | 0.037 (5) | −0.013 (5) | −0.014 (4) | 0.009 (5) |
C9 | 0.037 (4) | 0.043 (5) | 0.040 (5) | −0.006 (4) | 0.011 (4) | −0.004 (5) |
C10 | 0.032 (4) | 0.059 (8) | 0.032 (4) | −0.010 (4) | −0.001 (3) | −0.016 (4) |
C11 | 0.045 (5) | 0.049 (7) | 0.045 (5) | −0.005 (4) | 0.007 (4) | 0.018 (5) |
C12 | 0.034 (4) | 0.023 (5) | 0.036 (4) | −0.002 (3) | 0.002 (3) | 0.003 (4) |
C13 | 0.031 (4) | 0.044 (5) | 0.042 (5) | −0.004 (4) | 0.002 (4) | −0.006 (4) |
C14 | 0.046 (5) | 0.055 (6) | 0.025 (4) | −0.022 (4) | 0.001 (4) | 0.014 (4) |
C15 | 0.035 (4) | 0.051 (6) | 0.026 (3) | 0.021 (5) | −0.007 (3) | 0.006 (5) |
C16 | 0.030 (4) | 0.043 (6) | 0.046 (5) | −0.013 (4) | 0.001 (4) | −0.012 (4) |
C17 | 0.064 (6) | 0.032 (5) | 0.035 (4) | −0.025 (4) | 0.014 (4) | 0.004 (4) |
C18 | 0.029 (4) | 0.063 (7) | 0.050 (6) | −0.011 (4) | 0.004 (4) | −0.019 (5) |
C19 | 0.044 (5) | 0.037 (5) | 0.057 (6) | −0.018 (4) | 0.008 (4) | 0.013 (5) |
Cd1 | 0.0292 (3) | 0.0353 (3) | 0.0319 (3) | −0.0075 (3) | 0.00435 (19) | −0.0014 (3) |
N1 | 0.048 (4) | 0.038 (4) | 0.033 (3) | −0.019 (5) | 0.016 (3) | −0.013 (5) |
N2 | 0.043 (4) | 0.038 (4) | 0.046 (4) | 0.002 (5) | −0.004 (3) | 0.005 (5) |
O1 | 0.038 (3) | 0.049 (4) | 0.052 (3) | −0.007 (4) | 0.017 (3) | −0.013 (4) |
O2 | 0.054 (4) | 0.044 (4) | 0.041 (3) | 0.011 (3) | 0.015 (3) | 0.000 (3) |
O3 | 0.041 (3) | 0.035 (4) | 0.034 (3) | −0.003 (3) | 0.000 (2) | 0.003 (3) |
O4 | 0.032 (3) | 0.048 (4) | 0.033 (3) | −0.004 (3) | −0.001 (3) | −0.008 (3) |
O5 | 0.026 (3) | 0.037 (4) | 0.048 (3) | 0.014 (3) | 0.007 (3) | −0.019 (3) |
O6 | 0.060 (4) | 0.048 (4) | 0.029 (3) | −0.015 (3) | 0.004 (3) | −0.008 (3) |
Br1—C3 | 1.855 (4) | C13—H13 | 0.9299 |
C1—C2 | 1.3900 | C14—N1 | 1.355 (11) |
C1—C6 | 1.3900 | C14—H14 | 0.9299 |
C1—C7 | 1.487 (10) | C15—C19 | 1.294 (15) |
C2—C3 | 1.3900 | C15—C16 | 1.390 (15) |
C2—C8 | 1.541 (11) | C16—C17 | 1.408 (13) |
C3—C4 | 1.3900 | C16—H16 | 0.9300 |
C4—C5 | 1.3900 | C17—N2 | 1.290 (13) |
C4—H4 | 0.8922 | C17—H17 | 0.9300 |
C5—C6 | 1.3900 | C18—N2 | 1.356 (15) |
C5—H5 | 0.9318 | C18—C19 | 1.440 (15) |
C6—H6 | 0.8918 | C18—H18 | 0.9300 |
C7—O1 | 1.182 (11) | C19—H19 | 0.9300 |
C7—O2 | 1.248 (12) | Cd1—O5 | 2.233 (7) |
C8—C9 | 1.455 (13) | Cd1—O3 | 2.282 (6) |
C8—H8A | 0.9700 | Cd1—N2i | 2.298 (7) |
C8—H8B | 0.9700 | Cd1—N1 | 2.305 (6) |
C9—O4 | 1.213 (12) | Cd1—O4ii | 2.309 (8) |
C9—O3 | 1.213 (12) | Cd1—O1iii | 2.330 (6) |
C10—N1 | 1.332 (11) | N2—Cd1iv | 2.298 (7) |
C10—C11 | 1.435 (13) | O1—Cd1v | 2.330 (6) |
C10—H10 | 0.9300 | O4—Cd1vi | 2.309 (8) |
C11—C12 | 1.341 (13) | O5—H5Y | 0.8500 |
C11—H11 | 0.9299 | O5—H5X | 0.8500 |
C12—C13 | 1.417 (12) | O6—H6X | 0.8500 |
C12—C15 | 1.511 (11) | O6—H6Y | 0.8500 |
C13—C14 | 1.396 (13) | ||
C2—C1—C6 | 120.0 | C13—C14—H14 | 119.4 |
C2—C1—C7 | 120.7 (5) | C19—C15—C16 | 122.5 (8) |
C6—C1—C7 | 119.2 (5) | C19—C15—C12 | 117.7 (9) |
C1—C2—C3 | 120.0 | C16—C15—C12 | 119.8 (9) |
C1—C2—C8 | 118.1 (5) | C15—C16—C17 | 117.5 (8) |
C3—C2—C8 | 121.9 (5) | C15—C16—H16 | 121.9 |
C4—C3—C2 | 120.0 | C17—C16—H16 | 120.6 |
C4—C3—Br1 | 116.6 (3) | N2—C17—C16 | 123.0 (8) |
C2—C3—Br1 | 123.4 (3) | N2—C17—H17 | 118.1 |
C3—C4—C5 | 120.0 | C16—C17—H17 | 118.8 |
C3—C4—H4 | 121.5 | N2—C18—C19 | 123.6 (9) |
C5—C4—H4 | 118.5 | N2—C18—H18 | 118.3 |
C6—C5—C4 | 120.0 | C19—C18—H18 | 118.1 |
C6—C5—H5 | 120.3 | C15—C19—C18 | 116.0 (9) |
C4—C5—H5 | 119.7 | C15—C19—H19 | 123.7 |
C5—C6—C1 | 120.0 | C18—C19—H19 | 120.1 |
C5—C6—H6 | 119.1 | O5—Cd1—O3 | 92.6 (2) |
C1—C6—H6 | 120.9 | O5—Cd1—N2i | 95.9 (3) |
O1—C7—O2 | 120.3 (9) | O3—Cd1—N2i | 84.8 (2) |
O1—C7—C1 | 121.3 (9) | O5—Cd1—N1 | 86.1 (3) |
O2—C7—C1 | 118.4 (8) | O3—Cd1—N1 | 89.1 (2) |
C9—C8—C2 | 118.2 (10) | N2i—Cd1—N1 | 173.8 (2) |
C9—C8—H8A | 106.2 | O5—Cd1—O4ii | 172.3 (2) |
C2—C8—H8A | 105.2 | O3—Cd1—O4ii | 91.1 (2) |
C9—C8—H8B | 110.5 | N2i—Cd1—O4ii | 91.2 (3) |
C2—C8—H8B | 108.9 | N1—Cd1—O4ii | 87.3 (3) |
H8A—C8—H8B | 107.2 | O5—Cd1—O1iii | 81.3 (3) |
O4—C9—O3 | 120.9 (9) | O3—Cd1—O1iii | 173.6 (3) |
O4—C9—C8 | 117.2 (10) | N2i—Cd1—O1iii | 94.0 (2) |
O3—C9—C8 | 121.8 (10) | N1—Cd1—O1iii | 92.1 (2) |
N1—C10—C11 | 122.2 (8) | O4ii—Cd1—O1iii | 95.2 (3) |
N1—C10—H10 | 117.6 | C10—N1—C14 | 119.6 (7) |
C11—C10—H10 | 120.2 | C10—N1—Cd1 | 124.5 (5) |
C12—C11—C10 | 118.9 (8) | C14—N1—Cd1 | 115.8 (5) |
C12—C11—H11 | 122.5 | C17—N2—C18 | 117.0 (8) |
C10—C11—H11 | 118.4 | C17—N2—Cd1iv | 124.2 (7) |
C11—C12—C13 | 117.9 (8) | C18—N2—Cd1iv | 118.5 (7) |
C11—C12—C15 | 120.2 (8) | C7—O1—Cd1v | 146.8 (6) |
C13—C12—C15 | 120.7 (7) | C9—O3—Cd1 | 128.4 (6) |
C14—C13—C12 | 121.0 (8) | C9—O4—Cd1vi | 136.2 (7) |
C14—C13—H13 | 119.2 | Cd1—O5—H5Y | 109.7 |
C12—C13—H13 | 119.6 | Cd1—O5—H5X | 109.7 |
N1—C14—C13 | 119.7 (8) | H5Y—O5—H5X | 109.5 |
N1—C14—H14 | 120.9 | H6X—O6—H6Y | 105.0 |
C6—C1—C2—C3 | 0.0 | C19—C15—C16—C17 | −0.3 (15) |
C7—C1—C2—C3 | −177.8 (7) | C12—C15—C16—C17 | 178.4 (9) |
C6—C1—C2—C8 | −179.2 (7) | C15—C16—C17—N2 | 5.9 (16) |
C7—C1—C2—C8 | 3.1 (8) | C16—C15—C19—C18 | −3.8 (15) |
C1—C2—C3—C4 | 0.0 | C12—C15—C19—C18 | 177.5 (8) |
C8—C2—C3—C4 | 179.1 (7) | N2—C18—C19—C15 | 3.3 (16) |
C1—C2—C3—Br1 | −178.6 (5) | C11—C10—N1—C14 | 3.9 (17) |
C8—C2—C3—Br1 | 0.5 (7) | C11—C10—N1—Cd1 | −178.8 (8) |
C2—C3—C4—C5 | 0.0 | C13—C14—N1—C10 | −2.8 (17) |
Br1—C3—C4—C5 | 178.7 (4) | C13—C14—N1—Cd1 | 179.7 (8) |
C3—C4—C5—C6 | 0.0 | O5—Cd1—N1—C10 | −120.4 (10) |
C4—C5—C6—C1 | 0.0 | O3—Cd1—N1—C10 | −27.7 (10) |
C2—C1—C6—C5 | 0.0 | O4ii—Cd1—N1—C10 | 63.4 (10) |
C7—C1—C6—C5 | 177.8 (7) | O1iii—Cd1—N1—C10 | 158.5 (10) |
C2—C1—C7—O1 | −109.3 (9) | O5—Cd1—N1—C14 | 57.1 (9) |
C6—C1—C7—O1 | 73.0 (11) | O3—Cd1—N1—C14 | 149.7 (9) |
C2—C1—C7—O2 | 70.6 (10) | O4ii—Cd1—N1—C14 | −119.1 (9) |
C6—C1—C7—O2 | −107.1 (8) | O1iii—Cd1—N1—C14 | −24.0 (9) |
C1—C2—C8—C9 | −100.5 (9) | C16—C17—N2—C18 | −6.4 (16) |
C3—C2—C8—C9 | 80.4 (9) | C16—C17—N2—Cd1iv | 179.6 (8) |
C2—C8—C9—O4 | −177.7 (8) | C19—C18—N2—C17 | 1.8 (16) |
C2—C8—C9—O3 | 1.9 (14) | C19—C18—N2—Cd1iv | 176.2 (8) |
N1—C10—C11—C12 | −6.9 (16) | O2—C7—O1—Cd1v | 151.1 (10) |
C10—C11—C12—C13 | 8.3 (14) | C1—C7—O1—Cd1v | −29 (2) |
C10—C11—C12—C15 | 176.2 (9) | O4—C9—O3—Cd1 | 8.0 (13) |
C11—C12—C13—C14 | −7.6 (14) | C8—C9—O3—Cd1 | −171.6 (6) |
C15—C12—C13—C14 | −175.3 (9) | O5—Cd1—O3—C9 | 16.6 (8) |
C12—C13—C14—N1 | 4.6 (16) | N2i—Cd1—O3—C9 | 112.2 (8) |
C11—C12—C15—C19 | 150.4 (10) | N1—Cd1—O3—C9 | −69.5 (8) |
C13—C12—C15—C19 | −42.1 (13) | O4ii—Cd1—O3—C9 | −156.7 (8) |
C11—C12—C15—C16 | −28.3 (13) | O3—C9—O4—Cd1vi | −152.0 (7) |
C13—C12—C15—C16 | 139.1 (9) | C8—C9—O4—Cd1vi | 27.7 (13) |
Symmetry codes: (i) x, y, z+1; (ii) −x+1, y+1/2, −z+2; (iii) x−1, y, z; (iv) x, y, z−1; (v) x+1, y, z; (vi) −x+1, y−1/2, −z+2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5X···O3vi | 0.85 | 2.47 | 2.963 (8) | 118 |
O5—H5Y···O2vi | 0.85 | 2.22 | 2.731 (9) | 119 |
O6—H6X···O1 | 0.85 | 2.51 | 3.201 (9) | 139 |
O6—H6Y···O2 | 0.85 | 2.14 | 2.643 (9) | 117 |
Symmetry code: (vi) −x+1, y−1/2, −z+2. |
Experimental details
Crystal data | |
Chemical formula | [Cd(C9H5BrO4)(C10H8N2)(H2O)]·H2O |
Mr | 561.66 |
Crystal system, space group | Monoclinic, P21 |
Temperature (K) | 291 |
a, b, c (Å) | 9.3257 (19), 9.1312 (18), 11.652 (2) |
β (°) | 101.344 (4) |
V (Å3) | 972.8 (3) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 3.22 |
Crystal size (mm) | 0.29 × 0.26 × 0.23 |
Data collection | |
Diffractometer | Bruker APEXII CCD |
Absorption correction | Multi-scan (SADABS; Bruker, 2001) |
Tmin, Tmax | 0.466, 0.538 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5248, 3122, 2807 |
Rint | 0.033 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.049, 0.118, 1.05 |
No. of reflections | 3122 |
No. of parameters | 251 |
No. of restraints | 1 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.49, −0.93 |
Absolute structure | Flack (1983), 1096 Friedel pairs |
Absolute structure parameter | 0.07 (2) |
Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999).
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5X···O3i | 0.85 | 2.47 | 2.963 (8) | 118 |
O5—H5Y···O2i | 0.85 | 2.22 | 2.731 (9) | 119 |
O6—H6X···O1 | 0.85 | 2.51 | 3.201 (9) | 139 |
O6—H6Y···O2 | 0.85 | 2.14 | 2.643 (9) | 117 |
Symmetry code: (i) −x+1, y−1/2, −z+2. |
Acknowledgements
This work was financially supported by the Science and Technology Project of the State General Administration of Quality Supervision, Inspection and Quarantine (grant Nos. 2011QK121 and 2011QK122).
References
Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Flack, H. D. (1983). Acta Cryst. A39, 876–881. CrossRef CAS Web of Science IUCr Journals Google Scholar
Liu, Y., He, R., Wang, F., Lu, C. & Meng, Q. (2010). Inorg. Chem. Commun. 13, 1375–1379. Web of Science CSD CrossRef CAS Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
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In the title complex (Fig. 1), the carboxylate group containing O1 and O2 is monocoordinated and the other carboxylate group containing O3 and O4 is bidentate and bridging. Therefore, the 3-bromo-2-(carboxymethyl)benzoate (bcb) ligand coordinates with three Cd atoms. The Cd atom is coordinated by three bcb ligands, forming a two-dimensional polymeric layer parallel to (1 1 0). Since each Cd atom is coordinated by three bcb ligands, from a topology viewpoint the Cd atom can be considered as a 3-connecting node and the center of benzene ring of the bcb ligand also acts as a 3-connecting node. In this way, the polymeric layer can be simplified to a 63 network (Fig. 2). The 4,4'-bipyridine ligands act as bridges to connect the neighboring Cd atoms which come from different layers, forming a three-dimensional rigid porous network. This three-dimensional topology can be defined with Schläfli symbol (63)(69.8) (Fig. 3).