Literature DB >> 21836888

Poly[bis[μ-1,3-bis-(imidazol-1-ylmeth-yl)benzene-κN:N]bis-(nitrato-κO)cadmium].

Xi-Ying Hu1, Guang-Rui Yang, Wen-Wen Shan.   

Abstract

A novel metal-organic framework based on 1,3-bis-(imidazol-1-ylmeth-yl)benzene (1,3-bimb), [Cd(NO(3))(2)(C(14)H(14)N(4))(2)](n), has been synthesized hydro-thermally. The structure exhibits a two-dimensional metal-organic (4,4)-net composed of Cd(II) atoms and bimb ligands, and such layers are further joined through inter-layer C-H⋯O hydrogen bonds to generate a three-dimensional supra-molecular structure.

Entities:  

Year:  2011        PMID： 21836888      PMCID： PMC3151839          DOI： 10.1107/S1600536811021027

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For background to the network topologies and applications of coordination polymers, see: Maspoch et al. (2007 ▶); Ockwig et al. (2005 ▶); Zang et al. (2006 ▶); Zhang et al. (2009 ▶). For synthesis and related structures with the bimb ligand, see: Hoskins et al. (1997 ▶). For C—H⋯O hydrogen bonds, see: Desiraju (1996 ▶); Broder et al. (2002 ▶).

Experimental

Crystal data

[Cd(NO3)2(C14H14N4)2] M = 713.00 Monoclinic, a = 8.4542 (8) Å b = 19.3910 (18) Å c = 9.2222 (8) Å β = 102.415 (10)° V = 1476.5 (2) Å3 Z = 2 Mo Kα radiation μ = 0.80 mm−1 T = 296 K 0.21 × 0.20 × 0.19 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2005 ▶) T min = 0.850, T max = 0.863 5606 measured reflections 2578 independent reflections 2253 reflections with I > 2σ(I) R int = 0.017

Refinement

R[F 2 > 2σ(F 2)] = 0.044 wR(F 2) = 0.123 S = 1.06 2578 reflections 199 parameters 1 restraint H-atom parameters constrained Δρmax = 1.95 e Å−3 Δρmin = −0.86 e Å−3 Data collection: APEX2 (Bruker, 2005 ▶); cell refinement: SAINT (Bruker, 2005 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 2010 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶). Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811021027/hp2007sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811021027/hp2007Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cd(NO3)2(C14H14N4)2]F(000) = 724
Mr = 713.00Dx = 1.604 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3957 reflections
a = 8.4542 (8) Åθ = 3.1–29.1°
b = 19.3910 (18) ŵ = 0.80 mm−1
c = 9.2222 (8) ÅT = 296 K
β = 102.415 (10)°Needle, colourless
V = 1476.5 (2) Å30.21 × 0.20 × 0.19 mm
Z = 2
Bruker SMART APEXII CCD area-detector diffractometer2578 independent reflections
Radiation source: fine-focus sealed tube2253 reflections with I > 2σ(I)
graphiteRint = 0.017
ω scansθmax = 25.0°, θmin = 3.1°
Absorption correction: multi-scan (SADABS; Bruker, 2005)h = −10→6
Tmin = 0.850, Tmax = 0.863k = −21→23
5606 measured reflectionsl = −10→10
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.123H-atom parameters constrained
S = 1.06w = 1/[σ2(Fo2) + (0.0689P)2 + 2.589P] where P = (Fo2 + 2Fc2)/3
2578 reflections(Δ/σ)max < 0.001
199 parametersΔρmax = 1.95 e Å−3
1 restraintΔρmin = −0.86 e Å−3
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.
xyzUiso*/Ueq
Cd10.50000.50000.00000.03330 (18)
O10.9948 (4)0.4485 (2)0.2556 (4)0.0657 (10)
O20.8878 (9)0.5415 (3)0.1617 (11)0.183 (4)
O30.7504 (4)0.45152 (19)0.1259 (4)0.0626 (7)
N10.4529 (4)0.55084 (17)0.2160 (4)0.0364 (7)
N20.3328 (4)0.57252 (16)0.4000 (3)0.0322 (7)
N3−0.2702 (4)0.81383 (18)0.3469 (4)0.0401 (8)
N4−0.4073 (4)0.89430 (17)0.4339 (4)0.0379 (8)
N50.8818 (5)0.4775 (3)0.1699 (6)0.0626 (7)
C10.5664 (5)0.5731 (2)0.3353 (5)0.0419 (10)
H10.67630.57810.33740.050*
C20.4946 (5)0.5868 (2)0.4507 (5)0.0463 (11)
H20.54460.60260.54460.056*
C30.3138 (5)0.5521 (2)0.2602 (4)0.0342 (8)
H30.21450.54000.20020.041*
C40.2053 (6)0.5788 (2)0.4856 (5)0.0414 (10)
H4A0.24430.55980.58410.050*
H4B0.11160.55210.43730.050*
C50.1556 (5)0.6528 (2)0.4988 (4)0.0335 (8)
C60.2395 (5)0.6941 (2)0.6119 (5)0.0436 (10)
H60.32240.67530.68390.052*
C70.2009 (5)0.7630 (2)0.6186 (5)0.0469 (11)
H70.25870.79040.69470.056*
C80.0777 (6)0.7914 (2)0.5137 (5)0.0440 (10)
H80.05380.83810.51780.053*
C9−0.0113 (5)0.7503 (2)0.4012 (4)0.0379 (9)
C100.0285 (5)0.6813 (2)0.3951 (4)0.0348 (8)
H10−0.03070.65350.32060.042*
C11−0.1437 (6)0.7816 (3)0.2829 (5)0.0509 (12)
H11A−0.09690.81600.22830.061*
H11B−0.19190.74590.21360.061*
C12−0.2881 (5)0.8817 (2)0.3668 (5)0.0410 (10)
H12−0.22410.91550.33680.049*
C13−0.4682 (5)0.8310 (2)0.4589 (5)0.0430 (10)
H13−0.55390.82360.50560.052*
C14−0.3855 (5)0.7810 (2)0.4059 (5)0.0469 (11)
H14−0.40310.73370.40880.056*
U11U22U33U12U13U23
Cd10.0367 (3)0.0294 (3)0.0390 (3)−0.00351 (15)0.01983 (19)−0.00143 (16)
O10.0330 (16)0.089 (3)0.072 (2)0.0071 (17)0.0045 (16)0.018 (2)
O20.124 (5)0.077 (2)0.302 (10)−0.021 (4)−0.058 (6)0.044 (5)
O30.0348 (12)0.0655 (16)0.082 (2)−0.0069 (12)0.0001 (13)0.0074 (15)
N10.0393 (18)0.0353 (17)0.0387 (18)0.0008 (15)0.0175 (15)−0.0031 (15)
N20.0369 (17)0.0287 (16)0.0330 (17)0.0082 (14)0.0121 (14)0.0015 (13)
N30.0437 (19)0.0371 (18)0.0404 (19)0.0151 (16)0.0112 (16)−0.0011 (15)
N40.0347 (17)0.0343 (18)0.049 (2)0.0069 (14)0.0172 (15)−0.0008 (15)
N50.0348 (12)0.0655 (16)0.082 (2)−0.0069 (12)0.0001 (13)0.0074 (15)
C10.031 (2)0.040 (2)0.056 (3)0.0006 (18)0.0114 (19)−0.007 (2)
C20.045 (3)0.051 (3)0.039 (2)0.005 (2)0.0020 (19)−0.013 (2)
C30.035 (2)0.032 (2)0.037 (2)0.0019 (16)0.0102 (16)0.0000 (16)
C40.054 (3)0.037 (2)0.040 (2)0.0109 (19)0.025 (2)0.0086 (18)
C50.037 (2)0.037 (2)0.032 (2)0.0080 (17)0.0188 (16)0.0031 (16)
C60.039 (2)0.060 (3)0.033 (2)0.011 (2)0.0090 (18)−0.0037 (19)
C70.043 (2)0.050 (3)0.049 (3)−0.003 (2)0.013 (2)−0.018 (2)
C80.049 (3)0.033 (2)0.056 (3)0.0035 (19)0.025 (2)−0.0064 (19)
C90.042 (2)0.041 (2)0.035 (2)0.0125 (18)0.0183 (18)−0.0013 (18)
C100.038 (2)0.035 (2)0.035 (2)0.0029 (17)0.0160 (17)−0.0055 (17)
C110.062 (3)0.055 (3)0.039 (2)0.031 (2)0.018 (2)−0.001 (2)
C120.042 (2)0.033 (2)0.054 (3)0.0082 (18)0.022 (2)0.0057 (19)
C130.036 (2)0.041 (2)0.054 (3)0.0010 (18)0.0125 (19)0.004 (2)
C140.047 (2)0.033 (2)0.057 (3)0.0044 (19)0.004 (2)0.001 (2)
Cd1—N4i2.322 (3)C2—H20.9300
Cd1—N4ii2.322 (3)C3—H30.9300
Cd1—N1iii2.332 (3)C4—C51.508 (5)
Cd1—N12.332 (3)C4—H4A0.9700
Cd1—O32.378 (3)C4—H4B0.9700
Cd1—O3iii2.378 (3)C5—C61.384 (6)
O1—N51.236 (6)C5—C101.389 (6)
O2—N51.247 (8)C6—C71.379 (6)
O3—N51.207 (5)C6—H60.9300
N1—C31.326 (5)C7—C81.376 (7)
N1—C11.365 (5)C7—H70.9300
N2—C31.326 (5)C8—C91.394 (6)
N2—C21.375 (5)C8—H80.9300
N2—C41.472 (5)C9—C101.384 (6)
N3—C121.341 (5)C9—C111.512 (6)
N3—C141.371 (6)C10—H100.9300
N3—C111.468 (5)C11—H11A0.9700
N4—C121.314 (5)C11—H11B0.9700
N4—C131.369 (6)C12—H120.9300
N4—Cd1iv2.322 (3)C13—C141.347 (6)
C1—C21.360 (6)C13—H130.9300
C1—H10.9300C14—H140.9300
N4i—Cd1—N4ii180.0N2—C4—C5111.8 (3)
N4i—Cd1—N1iii91.13 (12)N2—C4—H4A109.3
N4ii—Cd1—N1iii88.87 (12)C5—C4—H4A109.3
N4i—Cd1—N188.87 (12)N2—C4—H4B109.3
N4ii—Cd1—N191.13 (12)C5—C4—H4B109.3
N1iii—Cd1—N1180.00 (15)H4A—C4—H4B107.9
N4i—Cd1—O399.31 (12)C6—C5—C10118.9 (4)
N4ii—Cd1—O380.69 (12)C6—C5—C4120.4 (4)
N1iii—Cd1—O387.27 (13)C10—C5—C4120.7 (4)
N1—Cd1—O392.73 (13)C7—C6—C5120.5 (4)
N4i—Cd1—O3iii80.69 (12)C7—C6—H6119.8
N4ii—Cd1—O3iii99.31 (12)C5—C6—H6119.8
N1iii—Cd1—O3iii92.73 (13)C8—C7—C6120.5 (4)
N1—Cd1—O3iii87.27 (13)C8—C7—H7119.8
O3—Cd1—O3iii180.0C6—C7—H7119.8
N5—O3—Cd1131.1 (3)C7—C8—C9120.0 (4)
C3—N1—C1105.2 (3)C7—C8—H8120.0
C3—N1—Cd1126.6 (3)C9—C8—H8120.0
C1—N1—Cd1127.1 (3)C10—C9—C8119.1 (4)
C3—N2—C2107.2 (3)C10—C9—C11120.5 (4)
C3—N2—C4126.6 (4)C8—C9—C11120.3 (4)
C2—N2—C4126.2 (4)C9—C10—C5121.0 (4)
C12—N3—C14106.9 (3)C9—C10—H10119.5
C12—N3—C11125.9 (4)C5—C10—H10119.5
C14—N3—C11127.1 (4)N3—C11—C9111.8 (3)
C12—N4—C13105.4 (3)N3—C11—H11A109.3
C12—N4—Cd1iv128.7 (3)C9—C11—H11A109.3
C13—N4—Cd1iv125.9 (3)N3—C11—H11B109.3
O3—N5—O1123.7 (5)C9—C11—H11B109.3
O3—N5—O2116.2 (5)H11A—C11—H11B107.9
O1—N5—O2117.1 (5)N4—C12—N3111.6 (4)
C2—C1—N1109.8 (4)N4—C12—H12124.2
C2—C1—H1125.1N3—C12—H12124.2
N1—C1—H1125.1C14—C13—N4109.9 (4)
C1—C2—N2105.9 (4)C14—C13—H13125.0
C1—C2—H2127.1N4—C13—H13125.0
N2—C2—H2127.1C13—C14—N3106.2 (4)
N1—C3—N2112.0 (4)C13—C14—H14126.9
N1—C3—H3124.0N3—C14—H14126.9
N2—C3—H3124.0
N4i—Cd1—O3—N513.2 (5)N2—C4—C5—C6−86.3 (5)
N4ii—Cd1—O3—N5−166.8 (5)N2—C4—C5—C1091.6 (5)
N1iii—Cd1—O3—N5103.9 (5)C10—C5—C6—C7−2.1 (6)
N1—Cd1—O3—N5−76.1 (5)C4—C5—C6—C7175.8 (4)
N4i—Cd1—N1—C3124.0 (3)C5—C6—C7—C80.5 (7)
N4ii—Cd1—N1—C3−56.0 (3)C6—C7—C8—C91.3 (7)
O3—Cd1—N1—C3−136.7 (3)C7—C8—C9—C10−1.4 (6)
O3iii—Cd1—N1—C343.3 (3)C7—C8—C9—C11−178.2 (4)
N4i—Cd1—N1—C1−69.9 (3)C8—C9—C10—C5−0.2 (6)
N4ii—Cd1—N1—C1110.1 (3)C11—C9—C10—C5176.6 (4)
O3—Cd1—N1—C129.4 (3)C6—C5—C10—C92.0 (6)
O3iii—Cd1—N1—C1−150.6 (3)C4—C5—C10—C9−175.9 (4)
Cd1—O3—N5—O1167.3 (4)C12—N3—C11—C9102.7 (5)
Cd1—O3—N5—O27.5 (9)C14—N3—C11—C9−72.9 (6)
C3—N1—C1—C20.6 (5)C10—C9—C11—N3123.7 (4)
Cd1—N1—C1—C2−167.8 (3)C8—C9—C11—N3−59.5 (6)
N1—C1—C2—N20.0 (5)C13—N4—C12—N30.3 (5)
C3—N2—C2—C1−0.6 (5)Cd1iv—N4—C12—N3−179.9 (3)
C4—N2—C2—C1179.4 (4)C14—N3—C12—N4−0.2 (5)
C1—N1—C3—N2−1.0 (4)C11—N3—C12—N4−176.6 (4)
Cd1—N1—C3—N2167.5 (2)C12—N4—C13—C14−0.3 (5)
C2—N2—C3—N11.0 (5)Cd1iv—N4—C13—C14179.9 (3)
C4—N2—C3—N1−178.9 (3)N4—C13—C14—N30.2 (5)
C3—N2—C4—C5−102.7 (5)C12—N3—C14—C130.0 (5)
C2—N2—C4—C577.3 (5)C11—N3—C14—C13176.3 (4)
D—H···AD—HH···AD···AD—H···A
C3—H3···O2v0.932.713.525 (8)147.
C4—H4B···O1v0.972.673.525 (6)148.
C4—H4B···O2v0.972.833.633 (9)141.
C10—H10···O2v0.932.633.506 (9)158.
C11—H11A···O1vi0.972.703.518 (7)142.
C12—H12···O1vi0.932.373.210 (6)151.
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
C3—H3⋯O2i0.932.713.525 (8)147
C4—H4B⋯O1i0.972.673.525 (6)148
C4—H4B⋯O2i0.972.833.633 (9)141
C10—H10⋯O2i0.932.633.506 (9)158
C11—H11A⋯O1ii0.972.703.518 (7)142
C12—H12⋯O1ii0.932.373.210 (6)151

Symmetry codes: (i) ; (ii) .

  6 in total

1.  Reticular chemistry: occurrence and taxonomy of nets and grammar for the design of frameworks.

Authors:  Nathan W Ockwig; Olaf Delgado-Friedrichs; Michael O'Keeffe; Omar M Yaghi
Journal:  Acc Chem Res       Date:  2005-03       Impact factor: 22.384

2.  Assemblies of a new flexible multicarboxylate ligand and d10 metal centers toward the construction of homochiral helical coordination polymers: structures, luminescence, and NLO-active properties.

Authors:  Shuangquan Zang; Yang Su; Yizhi Li; Zhaoping Ni; Qingjin Meng
Journal:  Inorg Chem       Date:  2006-01-09       Impact factor: 5.165

3.  Old materials with new tricks: multifunctional open-framework materials.

Authors:  Daniel Maspoch; Daniel Ruiz-Molina; Jaume Veciana
Journal:  Chem Soc Rev       Date:  2007-02-08       Impact factor: 54.564

4.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

5.  A highly connected porous coordination polymer with unusual channel structure and sorption properties.

Authors:  Yue-Biao Zhang; Wei-Xiong Zhang; Fei-Yue Feng; Jie-Peng Zhang; Xiao-Ming Chen
Journal:  Angew Chem Int Ed Engl       Date:  2009       Impact factor: 15.336

6.  The C-h···o hydrogen bond:  structural implications and supramolecular design.

Authors:  G R Desiraju
Journal:  Acc Chem Res       Date:  1996-09       Impact factor: 22.384
  6 in total

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