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catena-Poly[[tetra-aqua-cadmium]-μ-5,5'-(1,4-phenyl-ene)di(tetra-zol-2-ido)-κ(2) N (2):N (2')].
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MedLine Citation:
PMID:  23723784     Owner:  NLM     Status:  PubMed-not-MEDLINE    
Abstract/OtherAbstract:
In the title compound, [Cd(C8H4N8)(H2O)4] n , 5,5'-(1,4-phenyl-ene)di(tetra-zol-2-ide) (L) ligands bridge Cd(II) atoms into polymeric chains along [201]. The Cd(II) atom is situated on an inversion centre and is coordinated by two N atoms from two L ligands and by four water O atoms in a distorted octa-hedral geometry. In the L ligand, the benzene ring resides on an inversion centre and the tetra-zole rings are twisted from its plane by 22.3 (1)°. An extensive hydrogen-bonding network formed by classical O-H⋯N and O-H⋯O inter-actions consolidates the crystal packing, linking the poymeric chains into a three-dimensional structure.
Authors:
Qinqin Dang; Han Caiyun
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Publication Detail:
Type:  Journal Article     Date:  2013-04-20
Journal Detail:
Title:  Acta crystallographica. Section E, Structure reports online     Volume:  69     ISSN:  1600-5368     ISO Abbreviation:  Acta Crystallogr Sect E Struct Rep Online     Publication Date:  2013 May 
Date Detail:
Created Date:  2013-05-31     Completed Date:  2013-06-03     Revised Date:  2013-06-04    
Medline Journal Info:
Nlm Unique ID:  101089178     Medline TA:  Acta Crystallogr Sect E Struct Rep Online     Country:  United States    
Other Details:
Languages:  eng     Pagination:  m283     Citation Subset:  -    
Affiliation:
School of Chemistry & Material Science, Shanxi Normal University, Linfen 041004, People's Republic of China.
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Journal Information
Journal ID (nlm-ta): Acta Crystallogr Sect E Struct Rep Online
Journal ID (iso-abbrev): Acta Crystallogr Sect E Struct Rep Online
Journal ID (publisher-id): Acta Cryst. E
ISSN: 1600-5368
Publisher: International Union of Crystallography
Article Information
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A full version of this article is available from Crystallography Journals Online.© Dang and Caiyun 2013
open-access:
Received Day: 09 Month: 4 Year: 2013
Accepted Day: 17 Month: 4 Year: 2013
collection publication date: Day: 01 Month: 5 Year: 2013
Electronic publication date: Day: 20 Month: 4 Year: 2013
pmc-release publication date: Day: 20 Month: 4 Year: 2013
Volume: 69 Issue: Pt 5
First Page: m283 Last Page: m283
PubMed Id: 23723784
ID: 3647818
Publisher Id: cv5403
DOI: 10.1107/S1600536813010441
Coden: ACSEBH
Publisher Item Identifier: S1600536813010441

catena-Poly[[tetra­aqua­cadmium]-μ-5,5′-(1,4-phenyl­ene)di(tetra­zol-2-ido)-κ2N2:N2′] Alternate Title:[Cd(C8H4N8)(H2O)4]
Qinqin Danga*
Han Caiyuna
aSchool of Chemistry & Material Science, Shanxi Normal University, Linfen 041004, People’s Republic of China
Correspondence: Correspondence e-mail: dangqq820116@yahoo.cn

Related literature  

For background to coordination frameworks, see: Yaghi et al. (2003); Kitagawa et al. (2004); Ockwig et al. (2005). For details of the synthesis of 1,4-bis­(tetra­zole-5-yl)benzene, see: Tao et al. (2004). For the crystal structures of coordination polymers containing the 1,4-bis­(tetra­zole-5-yl)benzene ligand, see: Dinca et al. (2006); Ouellette et al. (2009); Liu et al. (2012).[Chemical Structure ID: scheme1]


Experimental  
Crystal data  

  • [Cd(C8H4N8)(H2O)4]
  • Mr = 396.66
  • Monoclinic,
  • a = 5.3188 (4) Å
  • b = 11.1525 (14) Å
  • c = 12.0279 (8) Å
  • β = 101.256 (7)°
  • V = 699.75 (11) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 1.59 mm−1
  • T = 293 K
  • 0.25 × 0.20 × 0.15 mm

Data collection  

  • Agilent Xcalibur (Eos, Gemini) diffractometer
  • Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2012) Tmin = 0.692, Tmax = 0.796
  • 2351 measured reflections
  • 1237 independent reflections
  • 895 reflections with I > 2σ(I)
  • Rint = 0.033

Refinement  

  • R[F2 > 2σ(F2)] = 0.040
  • wR(F2) = 0.085
  • S = 1.05
  • 1237 reflections
  • 99 parameters
  • H-atom parameters constrained
  • Δρmax = 0.62 e Å−3
  • Δρmin = −0.53 e Å−3

Data collection: CrysAlis PRO (Agilent, 2012); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 2006); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).


Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536813010441/cv5403sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813010441/cv5403Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report


Notes

fnu1Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: CV5403).

The author thank the Shanxi Province Science Foundation for Youths (grant No. 2012021008–2), the National Natural Science Foundation of China (grant No. 21101102) and the National Science Fund for Distinguished Young Scholars (grant No. 20925101).

supplementary crystallographic information
Comment

Over the last decade coordination frameworks with channels or pores have captivated great attention of chemists because of their potential applications in gas storage, separation, ion exchange and catalysis(Yaghi et al., 2003; Kitagawa et al., 2004; Ockwig et al., 2005). 1,4-Bis(tetrazol-5-yl)benzene, firstly synthesized and characterized by Tao et al. (2004), is now widely used for constructing coordination frameworks with channels or pores (Dinca et al., 2006; Ouellette et al., 2009; Liu et al., 2012). This paper concerns the reaction of cadmium(II) and 1,4-bis(tetrazol-5-yl)benzene, and the crystal structure of the product.

In the title compound (Fig. 1), the CdII ion is located at an inversion centre. It has a slightly distorted octahedral coordination geometry formed by four water molecules and two nitrogen atoms from ligands L, where H2L = 1,4-bis(tetrazol-5-yl)benzene. Four oxygen atoms form a planar parallelogram arrangement around the Cd centre, and the other two nitrogen atoms occupy the apical position. Each ligand L coordinates two cadmium atoms in a µ2-bridging mode, thus generating a one-dimension coordination polymer. As far as we known, this coordination mode is currently unknown for L ligand.

In the crystal, polymeric one-dimensional chains are linked via O—H···N hydrogen bonds (Table 1) into a three-dimensional structure. The results show that there are no channels in the crystal structure.

Experimental

Cadmium nitrate tetrahydrate (0.123 g, 0.40 mmol), 1,4-bis(tetrazole-5-yl)benzene (0.042 g, 0.20 mmol) and sodium hydroxide (0.016, 0.40 mmol) were added to 8 ml of water:ammonium hydroxide (v:v=1:1) mixture. The solution was transferred into a Teflon-lined stainless steel autoclave and the autoclave was heated to 393 K and maintained at that temperature for 72 h. After cooling to room temperature, crystals suitable for X-ray diffraction were collected.

Refinement

Water hydrogen atoms were placed in calculated positions [O—H = 0.85–0.87 Å], and refined as riding, with Uiso(H) = 1.5 Ueq(O). The aromatic H atoms were positioned geometrically [C—H = 0.93 Å], and refined using a riding model, with Uiso(H) = 1.2 Ueq(C).

Figures
Crystal data
Data collection
Refinement
Special details
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)
Atomic displacement parameters (Å2)
Geometric parameters (Å, º)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x−1, −y+1, −z.

Hydrogen-bond geometry (Å, º)

Symmetry codes: (i) −x+1, −y+1, −z+1; (iii) x+1, y, z; (iv) −x+1/2, y+1/2, −z+1/2; (v) x−1, y, z.


References
Agilent (2012). CrysAlis PRO and CrysAlis RED Agilent Technologies Ltd, Yarnton, England.
Brandenburg, K. & Putz, H. (2006). DIAMOND Crystal Impact, Bonn, Germany.
Dinca, M., Yu, A. F. & Long, J. R. (2006). J. Am. Chem. Soc.128, 8904–8913.
Kitagawa, S., Kitaura, R. & Noro, S. I. (2004). Angew. Chem. Int. Ed.43, 2334–2375.
Liu, W. T., Li, J. Y., Ni, Z. P., Bao, X., Ou, Y. C., Leng, J. D., Liu, J. L. & Tong, M. L. (2012). Cryst. Growth Des.12, 1482–1488.
Ockwig, N. W., Delgado-Friedrichs, O., O’Keeffe, M. & Yaghi, O. M. (2005). Acc. Chem. Res.38, 176–182.
Ouellette, W., Prosvirin, A. V., Whitenack, K., Dunbar, K. R. & Zubieta, J. (2009). Angew. Chem. Int. Ed.48, 2140–2143.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.
Tao, J., Ma, Z. J., Huang, R. B. & Zheng, L. S. (2004). Inorg. Chem.43, 6133–6135.
Yaghi, O. M., O’Keeffe, M., Ockwig, N. W., Chae, H. K., Eddaoudi, M. & Kim, J. (2003). Nature, 423, 705–714.

Figures

[Figure ID: Fap1]
Fig. 1. 

A portion of the polymeric chain in the title compound showing the atomic numbering [symmetry codes: (a) 1-x , 1-y, 1-z; (b) -1-x, 1-y, -z]. Displacement ellipsoids are drawn at the 50% probability level.



Tables
[TableWrap ID: d1e173]
[Cd(C8H4N8)(H2O)4] F(000) = 392
Mr = 396.66 2013-04-07 # Formatted by publCIF
Monoclinic, P21/n Dx = 1.883 Mg m3
Hall symbol: -P 2yn Mo Kα radiation, λ = 0.71073 Å
a = 5.3188 (4) Å Cell parameters from 739 reflections
b = 11.1525 (14) Å θ = 3.5–29.1°
c = 12.0279 (8) Å µ = 1.59 mm1
β = 101.256 (7)° T = 293 K
V = 699.75 (11) Å3 Prism, yellow
Z = 2 0.25 × 0.20 × 0.15 mm

[TableWrap ID: d1e308]
Agilent Xcalibur (Eos, Gemini) diffractometer 1237 independent reflections
Radiation source: fine-focus sealed tube 895 reflections with I > 2σ(I)
Graphite monochromator Rint = 0.033
Detector resolution: 16.0710 pixels mm-1 θmax = 25.0°, θmin = 3.5°
ω scans h = −5→6
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2012) k = −5→13
Tmin = 0.692, Tmax = 0.796 l = −13→14
2351 measured reflections

[TableWrap ID: d1e428]
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)] = 0.040 Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.085 H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0301P)2] where P = (Fo2 + 2Fc2)/3
1237 reflections (Δ/σ)max < 0.001
99 parameters Δρmax = 0.62 e Å3
0 restraints Δρmin = −0.53 e Å3

[TableWrap ID: d1e582]
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.

[TableWrap ID: d1e681]
x y z Uiso*/Ueq
Cd1 0.5000 0.5000 0.5000 0.0273 (2)
O1 0.7271 (6) 0.6312 (4) 0.4040 (3) 0.0365 (10)
H1A 0.6261 0.6859 0.3696 0.055*
H1B 0.7918 0.5921 0.3544 0.055*
N1 0.0067 (7) 0.5049 (4) 0.2701 (3) 0.0266 (10)
N4 0.0598 (8) 0.3375 (4) 0.1802 (4) 0.0369 (12)
C2 −0.2949 (9) 0.4694 (5) 0.0882 (4) 0.0279 (13)
C4 −0.3166 (9) 0.4199 (5) −0.0197 (4) 0.0333 (13)
H4 −0.1933 0.3658 −0.0335 0.040*
N2 0.2066 (7) 0.4426 (4) 0.3287 (4) 0.0327 (11)
C1 −0.0782 (9) 0.4371 (5) 0.1798 (4) 0.0286 (12)
N3 0.2401 (8) 0.3426 (4) 0.2768 (4) 0.0403 (12)
O2 0.2732 (8) 0.6693 (4) 0.5307 (4) 0.0659 (14)
H2A 0.3484 0.7038 0.5914 0.099*
H2B 0.1225 0.6488 0.5376 0.099*
C3 −0.4828 (10) 0.5505 (5) 0.1061 (4) 0.0342 (13)
H3 −0.4724 0.5849 0.1773 0.041*

[TableWrap ID: d1e938]
U11 U22 U33 U12 U13 U23
Cd1 0.0262 (3) 0.0279 (3) 0.0244 (3) 0.0008 (3) −0.0036 (2) −0.0009 (3)
O1 0.034 (2) 0.041 (3) 0.034 (2) 0.0078 (17) 0.0051 (18) 0.0042 (19)
N1 0.021 (2) 0.036 (3) 0.019 (2) 0.005 (2) −0.0059 (17) 0.001 (2)
N4 0.039 (3) 0.033 (3) 0.031 (3) 0.008 (2) −0.013 (2) −0.005 (2)
C2 0.023 (3) 0.034 (4) 0.024 (3) −0.003 (2) −0.002 (2) 0.001 (2)
C4 0.030 (3) 0.036 (4) 0.030 (3) 0.008 (3) −0.004 (2) −0.002 (3)
N2 0.031 (2) 0.039 (3) 0.025 (2) 0.001 (2) −0.004 (2) 0.001 (2)
C1 0.027 (3) 0.035 (3) 0.020 (3) 0.000 (3) −0.002 (2) 0.002 (3)
N3 0.042 (3) 0.036 (3) 0.034 (3) 0.005 (2) −0.014 (2) −0.003 (2)
O2 0.047 (2) 0.062 (3) 0.084 (4) 0.001 (2) 0.001 (2) −0.019 (3)
C3 0.039 (3) 0.041 (4) 0.018 (3) 0.006 (3) −0.006 (2) −0.006 (3)

[TableWrap ID: d1e1181]
Cd1—O2i 2.309 (4) N4—N3 1.355 (5)
Cd1—O2 2.309 (4) C2—C4 1.394 (7)
Cd1—O1 2.340 (3) C2—C3 1.396 (7)
Cd1—O1i 2.340 (3) C2—C1 1.475 (7)
Cd1—N2 2.416 (4) C4—C3ii 1.377 (7)
Cd1—N2i 2.416 (4) C4—H4 0.9300
O1—H1A 0.8631 N2—N3 1.307 (6)
O1—H1B 0.8625 O2—H2A 0.8527
N1—C1 1.328 (6) O2—H2B 0.8526
N1—N2 1.348 (6) C3—C4ii 1.377 (7)
N4—C1 1.331 (6) C3—H3 0.9300
O2i—Cd1—O2 179.999 (1) C4—C2—C3 117.9 (5)
O2i—Cd1—O1 95.51 (15) C4—C2—C1 120.6 (4)
O2—Cd1—O1 84.49 (15) C3—C2—C1 121.4 (5)
O2i—Cd1—O1i 84.49 (15) C3ii—C4—C2 121.3 (5)
O2—Cd1—O1i 95.51 (15) C3ii—C4—H4 119.4
O1—Cd1—O1i 180.0 C2—C4—H4 119.4
O2i—Cd1—N2 85.26 (16) N3—N2—N1 110.9 (4)
O2—Cd1—N2 94.74 (16) N3—N2—Cd1 120.5 (3)
O1—Cd1—N2 93.12 (13) N1—N2—Cd1 128.4 (3)
O1i—Cd1—N2 86.88 (13) N1—C1—N4 111.9 (4)
O2i—Cd1—N2i 94.74 (16) N1—C1—C2 124.3 (5)
O2—Cd1—N2i 85.26 (16) N4—C1—C2 123.8 (5)
O1—Cd1—N2i 86.88 (13) N2—N3—N4 107.8 (4)
O1i—Cd1—N2i 93.12 (13) Cd1—O2—H2A 109.5
N2—Cd1—N2i 180.0 (3) Cd1—O2—H2B 109.1
Cd1—O1—H1A 110.2 H2A—O2—H2B 109.3
Cd1—O1—H1B 109.8 C4ii—C3—C2 120.8 (5)
H1A—O1—H1B 108.7 C4ii—C3—H3 119.6
C1—N1—N2 104.0 (4) C2—C3—H3 119.6
C1—N4—N3 105.4 (4)

[TableWrap ID: d1e1577]
D—H···A D—H H···A D···A D—H···A
O1—H1B···N1iii 0.86 1.93 2.779 (5) 167
O1—H1A···N4iv 0.86 1.99 2.836 (6) 166
O2—H2A···N3i 0.85 2.49 3.121 (6) 131
O2—H2B···O1v 0.85 2.39 3.035 (6) 133


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