Literature DB >> 22219843

catena-Poly[diaqua-(cis-cyclo-hexane-1,2-dicarboxyl-ato)cadmium].

Xiao-Hong Zhu1, Xiao-Chun Cheng.   

Abstract

In the title polymer, [Cd(C(8)H(10)O(4))(H(2)O)(2)](n), the Cd(II) cation is coordinated by five carboxyl-ate O atoms from three different cyclo-hexane-1,2-dicarboxyl-ate anions and two O atoms from two water mol-ecules, displaying a distorted CdO(7) pentagonal-bipyramidal geometry. Each anion acts as a μ(3)-bridge, linking symmetry-related Cd(II) ions into a layer parallel to (010). In the crystal, numerous O-H⋯O and C-H⋯O hydrogen bonds occur. The coordinated water mol-ecules and carboxyl-ate O atoms act as donors or acceptors in the formation of these hydrogen-bonding inter-actions.

Entities:  

Year:  2011        PMID： 22219843      PMCID： PMC3247538          DOI： 10.1107/S1600536811044187

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


Related literature

For related structures, see: Thirumurugan et al. (2006 ▶).

Experimental

Crystal data

[Cd(C8H10O4)(H2O)2] M = 318.59 Monoclinic, a = 6.0585 (9) Å b = 23.544 (3) Å c = 8.3308 (9) Å β = 118.787 (8)° V = 1041.5 (2) Å3 Z = 4 Mo Kα radiation μ = 2.10 mm−1 T = 293 K 0.20 × 0.20 × 0.18 mm

Data collection

Bruker SMART APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.678, T max = 0.703 5908 measured reflections 2250 independent reflections 2214 reflections with I > 2σ(I) R int = 0.021

Refinement

R[F 2 > 2σ(F 2)] = 0.062 wR(F 2) = 0.132 S = 1.51 2250 reflections 136 parameters H-atom parameters constrained Δρmax = 1.31 e Å−3 Δρmin = −2.11 e Å−3 Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT (Bruker, 2008 ▶); 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, 2000 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶). Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811044187/pv2458sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811044187/pv2458Isup2.hkl Supplementary material file. DOI: 10.1107/S1600536811044187/pv2458Isup3.cdx Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cd(C8H10O4)(H2O)2]F(000) = 632
Mr = 318.59Dx = 2.032 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3464 reflections
a = 6.0585 (9) Åθ = 2.9–28.3°
b = 23.544 (3) ŵ = 2.10 mm−1
c = 8.3308 (9) ÅT = 293 K
β = 118.787 (8)°Block, colorless
V = 1041.5 (2) Å30.20 × 0.20 × 0.18 mm
Z = 4
Bruker SMART APEXII CCD diffractometer2250 independent reflections
Radiation source: fine-focus sealed tube2214 reflections with I > 2σ(I)
graphiteRint = 0.021
phi and ω scansθmax = 27.0°, θmin = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −7→7
Tmin = 0.678, Tmax = 0.703k = −30→22
5908 measured reflectionsl = −9→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)] = 0.062Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.132H-atom parameters constrained
S = 1.51w = 1/[σ2(Fo2) + (0.0226P)2 + 8.9495P] where P = (Fo2 + 2Fc2)/3
2250 reflections(Δ/σ)max = 0.001
136 parametersΔρmax = 1.31 e Å−3
0 restraintsΔρmin = −2.11 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
C10.2430 (14)0.8769 (3)0.3235 (9)0.0215 (15)
H10.12390.87310.37100.026*
C20.0977 (14)0.9021 (3)0.1294 (9)0.0217 (15)
H20.01170.93600.14020.026*
C30.2681 (16)0.9226 (4)0.0541 (11)0.0306 (18)
H40.16770.9430−0.05950.037*
H30.34230.89000.02680.037*
C40.4788 (18)0.9615 (4)0.1884 (13)0.040 (2)
H60.59250.97020.14050.048*
H50.40670.99690.20110.048*
C50.6240 (16)0.9336 (4)0.3738 (12)0.038 (2)
H70.75270.95940.45740.046*
H80.70710.89980.36250.046*
C60.4523 (17)0.9175 (3)0.4512 (11)0.0324 (19)
H100.37720.95160.46940.039*
H90.55060.89940.56940.039*
C110.3489 (12)0.8179 (3)0.3255 (9)0.0172 (13)
C21−0.1078 (14)0.8624 (3)0.0000 (10)0.0233 (15)
Cd10.52611 (10)0.71211 (2)0.27582 (7)0.02114 (18)
O10.4616 (10)0.7907 (2)0.4755 (7)0.0292 (12)
O20.3166 (11)0.7961 (2)0.1782 (7)0.0286 (12)
O3−0.2409 (10)0.8354 (2)0.0540 (7)0.0276 (12)
O4−0.1527 (11)0.8576 (3)−0.1638 (7)0.0306 (13)
O50.1442 (11)0.6699 (3)0.1849 (8)0.0420 (16)
H110.03960.68640.08730.050*
H120.06550.65800.23900.050*
O60.8811 (10)0.7702 (2)0.3509 (7)0.0291 (12)
H130.85290.79140.26100.035*
H140.99680.74610.38320.035*
U11U22U33U12U13U23
C10.026 (4)0.018 (4)0.018 (3)0.002 (3)0.009 (3)0.000 (3)
C20.024 (4)0.019 (3)0.016 (3)0.003 (3)0.005 (3)0.000 (3)
C30.034 (4)0.029 (4)0.026 (4)−0.009 (3)0.012 (3)0.003 (3)
C40.042 (5)0.034 (5)0.047 (5)−0.014 (4)0.023 (5)0.002 (4)
C50.021 (4)0.034 (5)0.041 (5)−0.001 (3)0.001 (4)0.000 (4)
C60.039 (5)0.022 (4)0.024 (4)0.002 (3)0.006 (4)−0.005 (3)
C110.015 (3)0.016 (3)0.020 (3)−0.001 (3)0.007 (3)−0.002 (3)
C210.020 (3)0.022 (4)0.019 (3)0.004 (3)0.003 (3)−0.001 (3)
Cd10.0190 (3)0.0229 (3)0.0189 (3)0.0022 (2)0.0070 (2)0.0012 (2)
O10.031 (3)0.031 (3)0.022 (3)0.006 (2)0.011 (2)0.005 (2)
O20.031 (3)0.030 (3)0.021 (3)0.006 (2)0.010 (2)−0.003 (2)
O30.026 (3)0.030 (3)0.030 (3)−0.007 (2)0.017 (2)−0.003 (2)
O40.029 (3)0.039 (3)0.019 (3)0.000 (3)0.007 (2)0.001 (2)
O50.030 (3)0.064 (4)0.027 (3)−0.006 (3)0.010 (3)0.014 (3)
O60.023 (3)0.034 (3)0.028 (3)0.000 (2)0.010 (2)0.007 (2)
C1—C111.528 (9)C11—O11.271 (9)
C1—C61.534 (11)C21—O41.262 (9)
C1—C21.540 (10)C21—O31.266 (9)
C1—H10.9800C21—Cd1i2.737 (7)
C2—C211.515 (10)Cd1—O22.278 (5)
C2—C31.522 (11)Cd1—O52.286 (6)
C2—H20.9800Cd1—O3ii2.337 (5)
C3—C41.531 (11)Cd1—O1iii2.340 (5)
C3—H40.9700Cd1—O62.365 (5)
C3—H30.9700Cd1—O4ii2.407 (6)
C4—C51.512 (12)Cd1—O12.639 (6)
C4—H60.9700Cd1—C21ii2.737 (7)
C4—H50.9700O1—Cd1iv2.340 (5)
C5—C61.512 (13)O3—Cd1i2.337 (5)
C5—H70.9700O4—Cd1i2.407 (6)
C5—H80.9700O5—H110.8466
C6—H100.9700O5—H120.8458
C6—H90.9700O6—H130.8460
C11—O21.256 (9)O6—H140.8404
C11—C1—C6110.9 (6)O3—C21—Cd1i58.4 (4)
C11—C1—C2112.8 (6)C2—C21—Cd1i178.1 (5)
C6—C1—C2110.6 (6)O2—Cd1—O587.6 (2)
C11—C1—H1107.4O2—Cd1—O3ii137.40 (19)
C6—C1—H1107.4O5—Cd1—O3ii98.8 (2)
C2—C1—H1107.4O2—Cd1—O1iii82.2 (2)
C21—C2—C3113.0 (6)O5—Cd1—O1iii90.7 (2)
C21—C2—C1111.5 (6)O3ii—Cd1—O1iii139.2 (2)
C3—C2—C1113.4 (6)O2—Cd1—O682.6 (2)
C21—C2—H2106.1O5—Cd1—O6170.2 (2)
C3—C2—H2106.1O3ii—Cd1—O688.65 (19)
C1—C2—H2106.1O1iii—Cd1—O687.78 (19)
C2—C3—C4112.4 (7)O2—Cd1—O4ii157.3 (2)
C2—C3—H4109.1O5—Cd1—O4ii111.1 (2)
C4—C3—H4109.1O3ii—Cd1—O4ii54.90 (18)
C2—C3—H3109.1O1iii—Cd1—O4ii84.63 (19)
C4—C3—H3109.1O6—Cd1—O4ii78.4 (2)
H4—C3—H3107.9O2—Cd1—O152.46 (17)
C5—C4—C3110.9 (7)O5—Cd1—O194.6 (2)
C5—C4—H6109.5O3ii—Cd1—O184.97 (17)
C3—C4—H6109.5O1iii—Cd1—O1133.97 (13)
C5—C4—H5109.5O6—Cd1—O179.61 (19)
C3—C4—H5109.5O4ii—Cd1—O1134.15 (17)
H6—C4—H5108.0O2—Cd1—C21ii158.3 (2)
C4—C5—C6111.3 (7)O5—Cd1—C21ii107.8 (2)
C4—C5—H7109.4O3ii—Cd1—C21ii27.5 (2)
C6—C5—H7109.4O1iii—Cd1—C21ii112.0 (2)
C4—C5—H8109.4O6—Cd1—C21ii81.7 (2)
C6—C5—H8109.4O4ii—Cd1—C21ii27.4 (2)
H7—C5—H8108.0O1—Cd1—C21ii109.6 (2)
C5—C6—C1111.7 (7)C11—O1—Cd1iv143.0 (5)
C5—C6—H10109.3C11—O1—Cd184.6 (4)
C1—C6—H10109.3Cd1iv—O1—Cd1130.9 (2)
C5—C6—H9109.3C11—O2—Cd1102.0 (4)
C1—C6—H9109.3C21—O3—Cd1i94.1 (4)
H10—C6—H9107.9C21—O4—Cd1i91.0 (5)
O2—C11—O1120.8 (6)Cd1—O5—H11106.8
O2—C11—C1119.6 (6)Cd1—O5—H12135.0
O1—C11—C1119.6 (6)H11—O5—H12108.1
O4—C21—O3119.8 (7)Cd1—O6—H13109.7
O4—C21—C2119.9 (7)Cd1—O6—H14101.8
O3—C21—C2120.2 (7)H13—O6—H14117.6
O4—C21—Cd1i61.6 (4)
C11—C1—C2—C2154.4 (8)O3ii—Cd1—O1—C11176.1 (4)
C6—C1—C2—C21179.2 (6)O1iii—Cd1—O1—C119.9 (6)
C11—C1—C2—C3−74.6 (8)O6—Cd1—O1—C1186.6 (4)
C6—C1—C2—C350.2 (9)O4ii—Cd1—O1—C11149.0 (4)
C21—C2—C3—C4−178.5 (7)C21ii—Cd1—O1—C11163.8 (4)
C1—C2—C3—C4−50.3 (9)O2—Cd1—O1—Cd1iv166.6 (4)
C2—C3—C4—C553.1 (11)O5—Cd1—O1—Cd1iv83.2 (3)
C3—C4—C5—C6−57.3 (11)O3ii—Cd1—O1—Cd1iv−15.2 (3)
C4—C5—C6—C158.5 (10)O1iii—Cd1—O1—Cd1iv178.65 (11)
C11—C1—C6—C571.9 (8)O6—Cd1—O1—Cd1iv−104.7 (3)
C2—C1—C6—C5−54.0 (9)O4ii—Cd1—O1—Cd1iv−42.3 (4)
C6—C1—C11—O2−123.1 (7)C21ii—Cd1—O1—Cd1iv−27.5 (4)
C2—C1—C11—O21.5 (10)O1—C11—O2—Cd1−4.1 (8)
C6—C1—C11—O159.1 (9)C1—C11—O2—Cd1178.1 (5)
C2—C1—C11—O1−176.2 (6)O5—Cd1—O2—C1199.8 (5)
C3—C2—C21—O4−12.9 (10)O3ii—Cd1—O2—C11−0.5 (6)
C1—C2—C21—O4−142.0 (7)O1iii—Cd1—O2—C11−169.1 (5)
C3—C2—C21—O3169.7 (7)O6—Cd1—O2—C11−80.4 (5)
C1—C2—C21—O340.5 (9)O4ii—Cd1—O2—C11−113.9 (6)
O2—C11—O1—Cd1iv−162.3 (6)O1—Cd1—O2—C112.1 (4)
C1—C11—O1—Cd1iv15.5 (12)C21ii—Cd1—O2—C11−36.3 (9)
O2—C11—O1—Cd13.5 (7)O4—C21—O3—Cd1i4.1 (7)
C1—C11—O1—Cd1−178.8 (6)C2—C21—O3—Cd1i−178.4 (6)
O2—Cd1—O1—C11−2.1 (4)O3—C21—O4—Cd1i−4.0 (7)
O5—Cd1—O1—C11−85.5 (4)C2—C21—O4—Cd1i178.6 (6)
D—H···AD—HH···AD···AD—H···A
O5—H11···O6i0.852.012.828 (8)164.
O5—H12···O4iv0.851.892.725 (8)169.
O6—H13···O3v0.851.852.694 (8)175.
O6—H14···O2ii0.842.493.147 (8)136.
O6—H14···O4ii0.842.573.016 (8)115.
C3—H3···O20.972.593.120 (10)115.
C6—H9···O4vi0.972.303.257 (10)169.
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O5—H11⋯O6i0.852.012.828 (8)164
O5—H12⋯O4ii0.851.892.725 (8)169
O6—H13⋯O3iii0.851.852.694 (8)175
O6—H14⋯O2iv0.842.493.147 (8)136
O6—H14⋯O4iv0.842.573.016 (8)115
C3—H3⋯O20.972.593.120 (10)115
C6—H9⋯O4v0.972.303.257 (10)169

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

  2 in total

1.  A short history of SHELX.

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

2.  1, 2-, 1, 3- and 1, 4-Cyclohexanedicarboxylates of Cd and Mn with chain and layered structures.

Authors:  A Thirumurugan; M B Avinash; C N R Rao
Journal:  Dalton Trans       Date:  2005-11-24       Impact factor: 4.390
  2 in total

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