metal-organic compounds
catena-Poly[[bis(dimethylammonium) [cadmate(II)-bis(μ-1,1′:4′,1′′-terphenyl-3,3′′-dicarboxylato)]] dimethylformamide disolvate]
aDepartment of Chemistry and Protein Research Center for Bio-Industry, Hankuk University of Foreign Studies, Yongin 449-791, Republic of Korea, and bDepartment of Chemistry and Nano Science, Ewha Womans University, Seoul 120-750, Republic of Korea
*Correspondence e-mail: shuh@hufs.ac.kr
In the title compound, {(C2H8N)2[Cd(C20H12O4)2]·2C3H7NO}n, the CdII ion lies on a twofold rotation axis and is in a distorted octahedral CdO6 environment, defined by four O atoms of two μ2-coordinated 1,1′:4′,1′′-terphenyl-3,3′′-dicarboxylate (DCT) ligands and two O atoms of two μ1-coordinated DCT ligands. Both types of DCT ligands act as bridging, forming a one-dimensional polymeric structure propagating parallel to [10].
Related literature
For background information on metal-organic frameworks (MOFs), see: Li & Zhou (2009); Huh et al. (2009, 2010); Youm et al. (2004); Gu et al. (2010).
Experimental
Crystal data
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Data collection: SMART (Bruker, 1997); cell SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.
Supporting information
https://doi.org/10.1107/S1600536810051366/lh5182sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810051366/lh5182Isup2.hkl
The reaction mixture of Cd(NO3)2.H2O (30.8 mg, 0.1 mmol) and 3,3"-dicarboxy-1,1':4',1"-terphenyl (DCT, 32 mg, 0.1 mmol) in 10 ml of DMF was heated at 130 °C for 4 d. The resulting clear solution was storedat room temperature for few days gave colorless crystals.
H atoms were placed incalculated positions with C—H distances of 0.93 Å (phenyl) 0.96 Å (methyl) and N—H distances of 0.90 Å (ammonium). They were included in the
in riding-motion approximation with Uiso(H) = 1.2Ueq(C and N) and 1.5Ueq(C).The role of bridging ligands in the formation of structurally interesting metal-organic frameworks (MOFs) is of significant importance for the design of multi-functional MOFs and coordination polymers (Li & Zhou, 2009; Huh et al., 2010; Huh et al., 2009; Youm et al., 2004). For instance, the reaction between a Zn(II) ion and a new C2 h-symmetric bridging ligand, 3,3"-dicarboxy-1,1':4',1"-terphenyl (DCT), in the presence of 1,4-diazacyclo[2,2,2]octane (DABCO) afforded a new nanoporous Zn-MOF containing DABCO ligands with an uncoordinated nitrogen atom towards one-dimensional channels. The resulting DABCO-functionalized Zn-MOF showed a better adsorption of CO2 over H2 and N2 with an exceptionally high CO2 adsorption
(Gu et al., 2010).To prepare new functional MOFs and coordination polymers, a reaction between Cd(NO3)2.H2O and the DCT ligand was investigated. A new one-dimensional coordination polymer, [H2N(CH3)2]2[Cd(DCT)2].2DMF (I), was obtained as colorless crystals and the
of (I) is reported herein. In the of the title compound the Cd atom is coordinated by four oxygen atoms of two µ2-coordinated DCT ligands and two oxygen atoms of two µ1-coordinated DCT ligands (Fig. 1). Two DCT ligands bridging two Cd atoms and the title compound forms an extended one-dimensional coordination polymer (Fig. 2). The overall coordination environment of a Cd atom is a distorted octahedral geometry. The title compound possesses periodically arranged CdII ions with two negative charges per Cd center because of the charge mismatching between CdII ions and the DCT ligands. Therefore two dimethylammonium cations are required for charge balancing. In addtion there are two dimethylformamide solvent molecules in the formula unit.For background information on metal-organic frameworks (MOFs), see: Li & Zhou (2009); Huh et al. (2009, 2010); Youm et al. (2004); Gu et al. (2010).
Data collection: SMART (Bruker, 1997); cell
SAINT (Bruker, 1997); data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).(C2H8N)2[Cd(C20H12O4)2]·2C3H7NO | F(000) = 2040 |
Mr = 983.37 | Dx = 1.314 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 2049 reflections |
a = 28.525 (4) Å | θ = 2.3–27.0° |
b = 9.3267 (13) Å | µ = 0.50 mm−1 |
c = 20.580 (3) Å | T = 293 K |
β = 114.752 (2)° | Block, colorless |
V = 4972.1 (11) Å3 | 0.08 × 0.08 × 0.05 mm |
Z = 4 |
Bruker SMART CCD area-detector diffractometer | 2861 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.068 |
Graphite monochromator | θmax = 26.0°, θmin = 1.6° |
φ and ω scans | h = −35→32 |
13515 measured reflections | k = −8→11 |
4888 independent reflections | l = −25→18 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.046 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.116 | H-atom parameters constrained |
S = 0.90 | w = 1/[σ2(Fo2) + (0.0481P)2] where P = (Fo2 + 2Fc2)/3 |
4888 reflections | (Δ/σ)max < 0.001 |
298 parameters | Δρmax = 1.47 e Å−3 |
0 restraints | Δρmin = −0.76 e Å−3 |
(C2H8N)2[Cd(C20H12O4)2]·2C3H7NO | V = 4972.1 (11) Å3 |
Mr = 983.37 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 28.525 (4) Å | µ = 0.50 mm−1 |
b = 9.3267 (13) Å | T = 293 K |
c = 20.580 (3) Å | 0.08 × 0.08 × 0.05 mm |
β = 114.752 (2)° |
Bruker SMART CCD area-detector diffractometer | 2861 reflections with I > 2σ(I) |
13515 measured reflections | Rint = 0.068 |
4888 independent reflections |
R[F2 > 2σ(F2)] = 0.046 | 0 restraints |
wR(F2) = 0.116 | H-atom parameters constrained |
S = 0.90 | Δρmax = 1.47 e Å−3 |
4888 reflections | Δρmin = −0.76 e Å−3 |
298 parameters |
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 | ||
Cd1 | 1.0000 | 0.22586 (5) | 0.7500 | 0.03992 (17) | |
O1 | 1.08028 (11) | 0.3209 (3) | 0.77314 (16) | 0.0572 (9) | |
O2 | 1.01785 (11) | 0.4040 (3) | 0.67570 (16) | 0.0621 (9) | |
O3 | 0.95903 (10) | 0.0827 (3) | 0.65658 (14) | 0.0505 (8) | |
O4 | 1.03902 (12) | 0.0114 (4) | 0.68232 (16) | 0.0719 (10) | |
C1 | 1.06411 (17) | 0.4007 (5) | 0.7194 (2) | 0.0449 (11) | |
C2 | 1.10258 (15) | 0.4955 (4) | 0.7074 (2) | 0.0389 (10) | |
C3 | 1.15225 (14) | 0.5095 (4) | 0.7608 (2) | 0.0390 (10) | |
H3 | 1.1610 | 0.4619 | 0.8040 | 0.047* | |
C4 | 1.18932 (14) | 0.5936 (4) | 0.7510 (2) | 0.0382 (10) | |
C5 | 1.17464 (16) | 0.6611 (5) | 0.6854 (2) | 0.0482 (12) | |
H5 | 1.1987 | 0.7164 | 0.6770 | 0.058* | |
C6 | 1.12548 (16) | 0.6485 (5) | 0.6323 (2) | 0.0534 (12) | |
H6 | 1.1167 | 0.6951 | 0.5888 | 0.064* | |
C7 | 1.08924 (16) | 0.5672 (5) | 0.6433 (2) | 0.0471 (11) | |
H7 | 1.0558 | 0.5605 | 0.6077 | 0.056* | |
C8 | 0.74239 (14) | −0.1084 (4) | 0.3083 (2) | 0.0377 (10) | |
C9 | 0.76565 (15) | 0.0007 (5) | 0.3571 (2) | 0.0452 (11) | |
H9 | 0.7467 | 0.0827 | 0.3560 | 0.054* | |
C10 | 0.81649 (16) | −0.0094 (5) | 0.4076 (2) | 0.0465 (11) | |
H10 | 0.8308 | 0.0657 | 0.4395 | 0.056* | |
C11 | 0.84628 (15) | −0.1288 (5) | 0.4114 (2) | 0.0379 (10) | |
C12 | 0.82222 (15) | −0.2418 (5) | 0.3648 (2) | 0.0443 (11) | |
H12 | 0.8404 | −0.3260 | 0.3677 | 0.053* | |
C13 | 0.77171 (15) | −0.2300 (5) | 0.3145 (2) | 0.0463 (11) | |
H13 | 0.7569 | −0.3066 | 0.2837 | 0.056* | |
C14 | 0.90158 (15) | −0.1368 (4) | 0.4619 (2) | 0.0385 (10) | |
C15 | 0.92021 (15) | −0.0652 (4) | 0.5273 (2) | 0.0408 (10) | |
H15 | 0.8975 | −0.0131 | 0.5400 | 0.049* | |
C16 | 0.97212 (15) | −0.0706 (4) | 0.5738 (2) | 0.0396 (10) | |
C17 | 1.00572 (16) | −0.1481 (5) | 0.5552 (2) | 0.0506 (12) | |
H17 | 1.0406 | −0.1523 | 0.5861 | 0.061* | |
C18 | 0.98748 (16) | −0.2195 (5) | 0.4906 (2) | 0.0541 (12) | |
H18 | 1.0102 | −0.2724 | 0.4782 | 0.065* | |
C19 | 0.93633 (16) | −0.2132 (5) | 0.4445 (2) | 0.0480 (11) | |
H19 | 0.9248 | −0.2609 | 0.4009 | 0.058* | |
C20 | 0.99169 (17) | 0.0116 (5) | 0.6434 (2) | 0.0473 (11) | |
N21 | 0.1478 (2) | 0.4189 (6) | 0.9596 (2) | 0.0814 (14) | |
O21 | 0.16600 (16) | 0.1981 (4) | 0.9324 (2) | 0.0925 (13) | |
C21 | 0.1350 (2) | 0.2929 (7) | 0.9302 (3) | 0.0737 (16) | |
H21 | 0.1000 | 0.2727 | 0.9057 | 0.088* | |
C22 | 0.2015 (3) | 0.4610 (9) | 0.9988 (4) | 0.146 (3) | |
H22A | 0.2235 | 0.3826 | 0.9996 | 0.220* | |
H22B | 0.2077 | 0.4863 | 1.0469 | 0.220* | |
H22C | 0.2088 | 0.5420 | 0.9757 | 0.220* | |
C23 | 0.1082 (3) | 0.5226 (8) | 0.9496 (3) | 0.126 (3) | |
H23A | 0.1143 | 0.6068 | 0.9275 | 0.189* | |
H23B | 0.1088 | 0.5475 | 0.9952 | 0.189* | |
H23C | 0.0752 | 0.4828 | 0.9196 | 0.189* | |
N31 | 0.12647 (13) | 1.0202 (4) | 0.80646 (18) | 0.0537 (10) | |
H31A | 0.1302 | 1.0770 | 0.8436 | 0.064* | |
H31B | 0.0943 | 1.0331 | 0.7724 | 0.064* | |
C31 | 0.16355 (19) | 1.0657 (7) | 0.7781 (3) | 0.0912 (19) | |
H31C | 0.1980 | 1.0579 | 0.8149 | 0.137* | |
H31D | 0.1568 | 1.1634 | 0.7623 | 0.137* | |
H31E | 0.1601 | 1.0055 | 0.7385 | 0.137* | |
C32 | 0.1320 (2) | 0.8719 (6) | 0.8299 (3) | 0.101 (2) | |
H32A | 0.1310 | 0.8107 | 0.7919 | 0.152* | |
H32B | 0.1042 | 0.8471 | 0.8426 | 0.152* | |
H32C | 0.1643 | 0.8599 | 0.8708 | 0.152* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.0305 (2) | 0.0450 (3) | 0.0417 (3) | 0.000 | 0.01258 (19) | 0.000 |
O1 | 0.0486 (19) | 0.058 (2) | 0.060 (2) | −0.0061 (16) | 0.0182 (16) | 0.0137 (17) |
O2 | 0.0367 (18) | 0.067 (2) | 0.072 (2) | −0.0066 (16) | 0.0126 (17) | 0.0110 (17) |
O3 | 0.0426 (18) | 0.061 (2) | 0.0476 (18) | 0.0010 (15) | 0.0182 (15) | −0.0085 (15) |
O4 | 0.0410 (19) | 0.101 (3) | 0.055 (2) | 0.0050 (19) | 0.0016 (16) | −0.0156 (19) |
C1 | 0.042 (3) | 0.041 (3) | 0.051 (3) | 0.002 (2) | 0.019 (2) | −0.003 (2) |
C2 | 0.037 (2) | 0.035 (3) | 0.047 (3) | 0.0023 (19) | 0.020 (2) | 0.002 (2) |
C3 | 0.038 (2) | 0.038 (3) | 0.040 (2) | 0.005 (2) | 0.015 (2) | 0.0036 (19) |
C4 | 0.033 (2) | 0.037 (3) | 0.044 (3) | 0.0013 (19) | 0.015 (2) | 0.000 (2) |
C5 | 0.040 (3) | 0.053 (3) | 0.053 (3) | −0.004 (2) | 0.020 (2) | 0.014 (2) |
C6 | 0.043 (3) | 0.064 (3) | 0.048 (3) | 0.002 (2) | 0.014 (2) | 0.016 (2) |
C7 | 0.035 (2) | 0.048 (3) | 0.051 (3) | 0.004 (2) | 0.011 (2) | 0.007 (2) |
C8 | 0.035 (2) | 0.036 (3) | 0.042 (2) | 0.000 (2) | 0.016 (2) | 0.001 (2) |
C9 | 0.041 (3) | 0.041 (3) | 0.052 (3) | 0.006 (2) | 0.017 (2) | −0.006 (2) |
C10 | 0.046 (3) | 0.042 (3) | 0.045 (3) | −0.002 (2) | 0.013 (2) | −0.006 (2) |
C11 | 0.039 (2) | 0.042 (3) | 0.034 (2) | 0.002 (2) | 0.0158 (19) | 0.002 (2) |
C12 | 0.044 (2) | 0.040 (3) | 0.048 (3) | 0.006 (2) | 0.018 (2) | −0.002 (2) |
C13 | 0.045 (2) | 0.040 (3) | 0.052 (3) | −0.003 (2) | 0.018 (2) | −0.011 (2) |
C14 | 0.040 (2) | 0.040 (3) | 0.034 (2) | 0.001 (2) | 0.014 (2) | 0.001 (2) |
C15 | 0.037 (2) | 0.042 (3) | 0.044 (3) | 0.001 (2) | 0.018 (2) | 0.002 (2) |
C16 | 0.038 (2) | 0.040 (3) | 0.038 (2) | 0.002 (2) | 0.012 (2) | −0.001 (2) |
C17 | 0.038 (3) | 0.057 (3) | 0.051 (3) | 0.009 (2) | 0.012 (2) | −0.001 (2) |
C18 | 0.048 (3) | 0.056 (3) | 0.060 (3) | 0.010 (2) | 0.024 (2) | −0.008 (3) |
C19 | 0.045 (3) | 0.051 (3) | 0.045 (3) | 0.002 (2) | 0.015 (2) | −0.010 (2) |
C20 | 0.047 (3) | 0.046 (3) | 0.045 (3) | −0.002 (2) | 0.015 (2) | 0.003 (2) |
N21 | 0.092 (4) | 0.076 (4) | 0.074 (3) | −0.010 (3) | 0.034 (3) | −0.021 (3) |
O21 | 0.095 (3) | 0.086 (3) | 0.078 (3) | 0.011 (2) | 0.018 (2) | −0.011 (2) |
C21 | 0.090 (4) | 0.067 (4) | 0.054 (3) | −0.016 (4) | 0.020 (3) | −0.010 (3) |
C22 | 0.108 (6) | 0.159 (8) | 0.171 (7) | −0.055 (5) | 0.057 (5) | −0.080 (6) |
C23 | 0.151 (7) | 0.092 (6) | 0.130 (6) | 0.007 (5) | 0.054 (5) | −0.012 (4) |
N31 | 0.046 (2) | 0.060 (3) | 0.049 (2) | 0.010 (2) | 0.0142 (19) | −0.0055 (19) |
C31 | 0.069 (4) | 0.108 (5) | 0.113 (5) | 0.000 (3) | 0.055 (4) | −0.002 (4) |
C32 | 0.134 (6) | 0.064 (4) | 0.127 (5) | 0.021 (4) | 0.075 (5) | 0.014 (4) |
Cd1—O3 | 2.228 (3) | C12—H12 | 0.9300 |
Cd1—O3i | 2.228 (3) | C13—H13 | 0.9300 |
Cd1—O1 | 2.312 (3) | C14—C19 | 1.383 (5) |
Cd1—O1i | 2.312 (3) | C14—C15 | 1.394 (5) |
Cd1—O2 | 2.451 (3) | C15—C16 | 1.387 (5) |
Cd1—O2i | 2.451 (3) | C15—H15 | 0.9300 |
Cd1—C1i | 2.714 (4) | C16—C17 | 1.376 (5) |
Cd1—C1 | 2.714 (4) | C16—C20 | 1.510 (6) |
O1—C1 | 1.250 (5) | C17—C18 | 1.380 (6) |
O2—C1 | 1.248 (4) | C17—H17 | 0.9300 |
O3—C20 | 1.262 (5) | C18—C19 | 1.369 (5) |
O4—C20 | 1.249 (5) | C18—H18 | 0.9300 |
C1—C2 | 1.508 (6) | C19—H19 | 0.9300 |
C2—C7 | 1.383 (5) | N21—C21 | 1.302 (6) |
C2—C3 | 1.389 (5) | N21—C23 | 1.434 (7) |
C3—C4 | 1.397 (5) | N21—C22 | 1.455 (7) |
C3—H3 | 0.9300 | O21—C21 | 1.238 (6) |
C4—C5 | 1.386 (5) | C21—H21 | 0.9300 |
C4—C8ii | 1.485 (5) | C22—H22A | 0.9600 |
C5—C6 | 1.375 (5) | C22—H22B | 0.9600 |
C5—H5 | 0.9300 | C22—H22C | 0.9600 |
C6—C7 | 1.375 (5) | C23—H23A | 0.9600 |
C6—H6 | 0.9300 | C23—H23B | 0.9600 |
C7—H7 | 0.9300 | C23—H23C | 0.9600 |
C8—C13 | 1.383 (5) | N31—C32 | 1.452 (6) |
C8—C9 | 1.388 (5) | N31—C31 | 1.469 (6) |
C8—C4iii | 1.485 (5) | N31—H31A | 0.9000 |
C9—C10 | 1.389 (5) | N31—H31B | 0.9000 |
C9—H9 | 0.9300 | C31—H31C | 0.9600 |
C10—C11 | 1.383 (5) | C31—H31D | 0.9600 |
C10—H10 | 0.9300 | C31—H31E | 0.9600 |
C11—C12 | 1.396 (5) | C32—H32A | 0.9600 |
C11—C14 | 1.484 (5) | C32—H32B | 0.9600 |
C12—C13 | 1.383 (5) | C32—H32C | 0.9600 |
O3—Cd1—O3i | 106.36 (15) | C10—C11—C14 | 121.9 (4) |
O3—Cd1—O1 | 121.60 (10) | C12—C11—C14 | 121.0 (4) |
O3i—Cd1—O1 | 86.31 (11) | C13—C12—C11 | 120.9 (4) |
O3—Cd1—O1i | 86.31 (11) | C13—C12—H12 | 119.6 |
O3i—Cd1—O1i | 121.60 (10) | C11—C12—H12 | 119.6 |
O1—Cd1—O1i | 134.91 (16) | C12—C13—C8 | 122.3 (4) |
O3—Cd1—O2 | 92.22 (10) | C12—C13—H13 | 118.9 |
O3i—Cd1—O2 | 140.68 (10) | C8—C13—H13 | 118.9 |
O1—Cd1—O2 | 54.70 (10) | C19—C14—C15 | 118.1 (4) |
O1i—Cd1—O2 | 93.34 (10) | C19—C14—C11 | 120.8 (4) |
O3—Cd1—O2i | 140.68 (10) | C15—C14—C11 | 121.0 (4) |
O3i—Cd1—O2i | 92.22 (10) | C16—C15—C14 | 121.0 (4) |
O1—Cd1—O2i | 93.34 (11) | C16—C15—H15 | 119.5 |
O1i—Cd1—O2i | 54.69 (10) | C14—C15—H15 | 119.5 |
O2—Cd1—O2i | 94.67 (15) | C17—C16—C15 | 119.6 (4) |
O3—Cd1—C1i | 113.54 (12) | C17—C16—C20 | 120.4 (4) |
O3i—Cd1—C1i | 108.72 (12) | C15—C16—C20 | 120.0 (4) |
O1—Cd1—C1i | 115.31 (12) | C16—C17—C18 | 119.7 (4) |
O1i—Cd1—C1i | 27.33 (10) | C16—C17—H17 | 120.1 |
O2—Cd1—C1i | 94.22 (11) | C18—C17—H17 | 120.1 |
O2i—Cd1—C1i | 27.36 (10) | C19—C18—C17 | 120.6 (4) |
O3—Cd1—C1 | 108.72 (12) | C19—C18—H18 | 119.7 |
O3i—Cd1—C1 | 113.54 (12) | C17—C18—H18 | 119.7 |
O1—Cd1—C1 | 27.34 (10) | C18—C19—C14 | 121.0 (4) |
O1i—Cd1—C1 | 115.31 (12) | C18—C19—H19 | 119.5 |
O2—Cd1—C1 | 27.36 (10) | C14—C19—H19 | 119.5 |
O2i—Cd1—C1 | 94.22 (11) | O4—C20—O3 | 124.1 (4) |
C1i—Cd1—C1 | 106.12 (18) | O4—C20—C16 | 118.6 (4) |
C1—O1—Cd1 | 94.5 (3) | O3—C20—C16 | 117.2 (4) |
C1—O2—Cd1 | 88.1 (3) | C21—N21—C23 | 119.5 (6) |
C20—O3—Cd1 | 109.4 (3) | C21—N21—C22 | 121.7 (6) |
O2—C1—O1 | 122.7 (4) | C23—N21—C22 | 118.7 (6) |
O2—C1—C2 | 119.3 (4) | O21—C21—N21 | 124.9 (6) |
O1—C1—C2 | 118.0 (4) | O21—C21—H21 | 117.5 |
O2—C1—Cd1 | 64.5 (2) | N21—C21—H21 | 117.5 |
O1—C1—Cd1 | 58.1 (2) | N21—C22—H22A | 109.5 |
C2—C1—Cd1 | 176.1 (3) | N21—C22—H22B | 109.5 |
C7—C2—C3 | 119.4 (4) | H22A—C22—H22B | 109.5 |
C7—C2—C1 | 120.8 (4) | N21—C22—H22C | 109.5 |
C3—C2—C1 | 119.8 (4) | H22A—C22—H22C | 109.5 |
C2—C3—C4 | 121.4 (4) | H22B—C22—H22C | 109.5 |
C2—C3—H3 | 119.3 | N21—C23—H23A | 109.5 |
C4—C3—H3 | 119.3 | N21—C23—H23B | 109.5 |
C5—C4—C3 | 117.2 (4) | H23A—C23—H23B | 109.5 |
C5—C4—C8ii | 121.5 (4) | N21—C23—H23C | 109.5 |
C3—C4—C8ii | 121.3 (4) | H23A—C23—H23C | 109.5 |
C6—C5—C4 | 121.8 (4) | H23B—C23—H23C | 109.5 |
C6—C5—H5 | 119.1 | C32—N31—C31 | 114.3 (4) |
C4—C5—H5 | 119.1 | C32—N31—H31A | 108.7 |
C7—C6—C5 | 120.2 (4) | C31—N31—H31A | 108.7 |
C7—C6—H6 | 119.9 | C32—N31—H31B | 108.7 |
C5—C6—H6 | 119.9 | C31—N31—H31B | 108.7 |
C6—C7—C2 | 119.9 (4) | H31A—N31—H31B | 107.6 |
C6—C7—H7 | 120.1 | N31—C31—H31C | 109.5 |
C2—C7—H7 | 120.1 | N31—C31—H31D | 109.5 |
C13—C8—C9 | 116.6 (4) | H31C—C31—H31D | 109.5 |
C13—C8—C4iii | 121.7 (4) | N31—C31—H31E | 109.5 |
C9—C8—C4iii | 121.7 (4) | H31C—C31—H31E | 109.5 |
C8—C9—C10 | 121.6 (4) | H31D—C31—H31E | 109.5 |
C8—C9—H9 | 119.2 | N31—C32—H32A | 109.5 |
C10—C9—H9 | 119.2 | N31—C32—H32B | 109.5 |
C11—C10—C9 | 121.5 (4) | H32A—C32—H32B | 109.5 |
C11—C10—H10 | 119.3 | N31—C32—H32C | 109.5 |
C9—C10—H10 | 119.3 | H32A—C32—H32C | 109.5 |
C10—C11—C12 | 117.0 (4) | H32B—C32—H32C | 109.5 |
O3—Cd1—O1—C1 | 68.3 (3) | C2—C3—C4—C5 | −0.8 (6) |
O3i—Cd1—O1—C1 | 175.3 (3) | C2—C3—C4—C8ii | 180.0 (4) |
O1i—Cd1—O1—C1 | −52.1 (2) | C3—C4—C5—C6 | 1.1 (6) |
O2—Cd1—O1—C1 | 0.6 (2) | C8ii—C4—C5—C6 | −179.6 (4) |
O2i—Cd1—O1—C1 | −92.7 (3) | C4—C5—C6—C7 | 0.0 (7) |
C1i—Cd1—O1—C1 | −75.8 (3) | C5—C6—C7—C2 | −1.4 (7) |
O3—Cd1—O2—C1 | −128.6 (3) | C3—C2—C7—C6 | 1.7 (6) |
O3i—Cd1—O2—C1 | −9.1 (3) | C1—C2—C7—C6 | −177.4 (4) |
O1—Cd1—O2—C1 | −0.6 (2) | C13—C8—C9—C10 | 2.6 (6) |
O1i—Cd1—O2—C1 | 145.0 (3) | C4iii—C8—C9—C10 | −175.6 (4) |
O2i—Cd1—O2—C1 | 90.1 (3) | C8—C9—C10—C11 | 0.1 (6) |
C1i—Cd1—O2—C1 | 117.6 (3) | C9—C10—C11—C12 | −3.3 (6) |
O3i—Cd1—O3—C20 | −64.4 (3) | C9—C10—C11—C14 | 175.9 (4) |
O1—Cd1—O3—C20 | 31.4 (3) | C10—C11—C12—C13 | 3.7 (6) |
O1i—Cd1—O3—C20 | 173.7 (3) | C14—C11—C12—C13 | −175.5 (4) |
O2—Cd1—O3—C20 | 80.5 (3) | C11—C12—C13—C8 | −1.0 (6) |
O2i—Cd1—O3—C20 | −179.4 (2) | C9—C8—C13—C12 | −2.2 (6) |
C1i—Cd1—O3—C20 | 176.1 (3) | C4iii—C8—C13—C12 | 176.1 (4) |
C1—Cd1—O3—C20 | 58.2 (3) | C10—C11—C14—C19 | −148.1 (4) |
Cd1—O2—C1—O1 | 1.1 (4) | C12—C11—C14—C19 | 31.1 (6) |
Cd1—O2—C1—C2 | −179.3 (3) | C10—C11—C14—C15 | 30.5 (6) |
Cd1—O1—C1—O2 | −1.2 (5) | C12—C11—C14—C15 | −150.4 (4) |
Cd1—O1—C1—C2 | 179.2 (3) | C19—C14—C15—C16 | −0.1 (6) |
O3—Cd1—C1—O2 | 55.5 (3) | C11—C14—C15—C16 | −178.7 (4) |
O3i—Cd1—C1—O2 | 173.7 (2) | C14—C15—C16—C17 | −0.2 (6) |
O1—Cd1—C1—O2 | 178.9 (4) | C14—C15—C16—C20 | 178.1 (4) |
O1i—Cd1—C1—O2 | −39.3 (3) | C15—C16—C17—C18 | 0.0 (7) |
O2i—Cd1—C1—O2 | −92.0 (3) | C20—C16—C17—C18 | −178.3 (4) |
C1i—Cd1—C1—O2 | −66.9 (2) | C16—C17—C18—C19 | 0.5 (7) |
O3—Cd1—C1—O1 | −123.3 (3) | C17—C18—C19—C14 | −0.8 (7) |
O3i—Cd1—C1—O1 | −5.2 (3) | C15—C14—C19—C18 | 0.6 (6) |
O1i—Cd1—C1—O1 | 141.8 (2) | C11—C14—C19—C18 | 179.2 (4) |
O2—Cd1—C1—O1 | −178.9 (4) | Cd1—O3—C20—O4 | 7.4 (5) |
O2i—Cd1—C1—O1 | 89.1 (3) | Cd1—O3—C20—C16 | −168.7 (3) |
C1i—Cd1—C1—O1 | 114.2 (3) | C17—C16—C20—O4 | 2.3 (6) |
O2—C1—C2—C7 | −10.8 (6) | C15—C16—C20—O4 | −176.0 (4) |
O1—C1—C2—C7 | 168.7 (4) | C17—C16—C20—O3 | 178.6 (4) |
O2—C1—C2—C3 | 170.1 (4) | C15—C16—C20—O3 | 0.4 (6) |
O1—C1—C2—C3 | −10.3 (6) | C23—N21—C21—O21 | 176.3 (6) |
C7—C2—C3—C4 | −0.6 (6) | C22—N21—C21—O21 | 0.3 (9) |
C1—C2—C3—C4 | 178.5 (4) |
Symmetry codes: (i) −x+2, y, −z+3/2; (ii) x+1/2, −y+1/2, z+1/2; (iii) x−1/2, −y+1/2, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | (C2H8N)2[Cd(C20H12O4)2]·2C3H7NO |
Mr | 983.37 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 293 |
a, b, c (Å) | 28.525 (4), 9.3267 (13), 20.580 (3) |
β (°) | 114.752 (2) |
V (Å3) | 4972.1 (11) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.50 |
Crystal size (mm) | 0.08 × 0.08 × 0.05 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 13515, 4888, 2861 |
Rint | 0.068 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.046, 0.116, 0.90 |
No. of reflections | 4888 |
No. of parameters | 298 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.47, −0.76 |
Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1997), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
Acknowledgements
This work was supported by the Korea Research Foundation Grant funded by the Korean Government (MOEHRD, Basic ResearchPromotion Fund) (KRF-2008–331-C00149).
References
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The role of bridging ligands in the formation of structurally interesting metal-organic frameworks (MOFs) is of significant importance for the design of multi-functional MOFs and coordination polymers (Li & Zhou, 2009; Huh et al., 2010; Huh et al., 2009; Youm et al., 2004). For instance, the reaction between a Zn(II) ion and a new C2 h-symmetric bridging ligand, 3,3"-dicarboxy-1,1':4',1"-terphenyl (DCT), in the presence of 1,4-diazacyclo[2,2,2]octane (DABCO) afforded a new nanoporous Zn-MOF containing DABCO ligands with an uncoordinated nitrogen atom towards one-dimensional channels. The resulting DABCO-functionalized Zn-MOF showed a better adsorption of CO2 over H2 and N2 with an exceptionally high CO2 adsorption enthalpy (Gu et al., 2010).
To prepare new functional MOFs and coordination polymers, a reaction between Cd(NO3)2.H2O and the DCT ligand was investigated. A new one-dimensional coordination polymer, [H2N(CH3)2]2[Cd(DCT)2].2DMF (I), was obtained as colorless crystals and the crystal structure of (I) is reported herein. In the crystal structure of the title compound the Cd atom is coordinated by four oxygen atoms of two µ2-coordinated DCT ligands and two oxygen atoms of two µ1-coordinated DCT ligands (Fig. 1). Two DCT ligands bridging two Cd atoms and the title compound forms an extended one-dimensional coordination polymer (Fig. 2). The overall coordination environment of a Cd atom is a distorted octahedral geometry. The title compound possesses periodically arranged CdII ions with two negative charges per Cd center because of the charge mismatching between CdII ions and the DCT ligands. Therefore two dimethylammonium cations are required for charge balancing. In addtion there are two dimethylformamide solvent molecules in the formula unit.