Literature DB >> 21578592

Poly[triaqua-(μ-butane-1,2,3,4-tetra-carboxyl-ato)dicadmium(II)].

Chun-Hong Ma, Yong-Sheng Yan.   

Abstract

The asymmetric unit of the title Cd(II) coordination polymer, [Cd(2)(C(8)H(6)O(8))(H(2)O)(3)](n), contains two crystallographically independent Cd(II) cations, one-half each of two independent anionic butane-1,2,3,4-tetra-carboxyl-ate units (L) and three water mol-ecules. Both anionic units lie on inversion centers. One of the Cd(II) ions is six-coordinated by four carboxyl-ate O atoms from four L anions and two water O atoms in a distorted octa-hedral coordination environment. The other Cd(II) ion is eight-coordinated by seven carboxyl-ate O atoms from four L anions and one water O atom. The anionic units bridge neighboring Cd(II) centers, forming a three-dimensional framework. O-H⋯O hydrogen-bonding inter-actions between the water mol-ecules and carboxyl-ate O atoms further stabilize the structure.

Entities:  

Year:  2009        PMID： 21578592      PMCID： PMC2971854          DOI： 10.1107/S1600536809045255

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


Related literature

For coordination polymers with tetra­carboxyl­ate ligands, see: Liu et al. (2008 ▶); Yang et al. (2008 ▶).

Experimental

Crystal data

[Cd2(C8H6O8)(H2O)3] M = 508.98 Triclinic, a = 7.499 (4) Å b = 7.928 (4) Å c = 11.982 (5) Å α = 72.886 (4)° β = 85.748 (4)° γ = 65.666 (5)° V = 619.4 (6) Å3 Z = 2 Mo Kα radiation μ = 3.49 mm−1 T = 293 K 0.27 × 0.22 × 0.20 mm

Data collection

Bruker APEX CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.812, T max = 0.910 4846 measured reflections 2847 independent reflections 2225 reflections with I > 2σ(I) R int = 0.024

Refinement

R[F 2 > 2σ(F 2)] = 0.026 wR(F 2) = 0.053 S = 0.92 2847 reflections 208 parameters 4 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.75 e Å−3 Δρmin = −0.85 e Å−3 Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1999 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL-Plus (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809045255/ci2945sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809045255/ci2945Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cd2(C8H6O8)(H2O)3]Z = 2
Mr = 508.98F(000) = 488
Triclinic, P1Dx = 2.729 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.499 (4) ÅCell parameters from 2847 reflections
b = 7.928 (4) Åθ = 3.0–29.1°
c = 11.982 (5) ŵ = 3.49 mm−1
α = 72.886 (4)°T = 293 K
β = 85.748 (4)°Block, colourless
γ = 65.666 (5)°0.27 × 0.22 × 0.20 mm
V = 619.4 (6) Å3
Bruker APEX CCD area-detector diffractometer2847 independent reflections
Radiation source: fine-focus sealed tube2225 reflections with I > 2σ(I)
graphiteRint = 0.024
ω scansθmax = 29.1°, θmin = 3.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −10→9
Tmin = 0.812, Tmax = 0.910k = −9→9
4846 measured reflectionsl = −16→12
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.026Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.053H atoms treated by a mixture of independent and constrained refinement
S = 0.92w = 1/[σ2(Fo2) + (0.024P)2] where P = (Fo2 + 2Fc2)/3
2847 reflections(Δ/σ)max = 0.001
208 parametersΔρmax = 0.75 e Å−3
4 restraintsΔρmin = −0.85 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
C1−1.1870 (5)−0.0435 (5)0.8775 (3)0.0222 (8)
C2−1.0228 (5)−0.2392 (5)0.9250 (4)0.0242 (9)
H2A−0.9498−0.23480.98680.029*
H2B−0.9344−0.26750.86320.029*
C3−1.0890 (5)−0.4024 (5)0.9729 (3)0.0195 (8)
H3−1.1514−0.41540.90870.023*
C4−1.2362 (5)−0.3626 (5)1.0672 (3)0.0180 (8)
C5−0.5128 (5)0.1885 (5)0.5710 (3)0.0157 (7)
C6−0.5234 (5)0.1089 (5)0.4728 (3)0.0138 (7)
H6−0.42370.12220.41750.017*
C7−0.7242 (5)0.2187 (5)0.4086 (3)0.0198 (8)
H7A−0.73130.15580.35180.024*
H7B−0.82340.21190.46430.024*
C8−0.7700 (5)0.4286 (5)0.3463 (3)0.0186 (8)
O1−1.1495 (4)0.1055 (4)0.8533 (2)0.0254 (6)
O2−1.3566 (4)−0.0238 (4)0.8590 (3)0.0316 (7)
O1W−0.7754 (4)0.6162 (4)0.6382 (3)0.0295 (7)
HW11−0.847 (7)0.565 (7)0.635 (4)0.044*
HW12−0.721 (7)0.639 (7)0.574 (4)0.044*
O3−0.6391 (4)0.2043 (4)0.6460 (2)0.0230 (6)
O2W−0.9660 (4)0.0105 (5)0.6309 (3)0.0293 (7)
HW22−0.916 (7)−0.104 (7)0.631 (4)0.044*
HW21−1.084 (3)0.058 (6)0.611 (4)0.044*
O4−0.3718 (4)0.2352 (4)0.5789 (2)0.0249 (6)
O3W−0.6465 (4)−0.1422 (4)0.8435 (3)0.0421 (9)
HW31−0.545 (5)−0.136 (6)0.864 (4)0.063*
HW32−0.628 (7)−0.259 (4)0.875 (4)0.063*
O5−1.2174 (4)−0.2778 (4)1.1353 (2)0.0322 (7)
O6−1.3702 (4)−0.4211 (4)1.0774 (2)0.0293 (7)
O7−0.6349 (4)0.4662 (4)0.2971 (3)0.0450 (9)
O8−0.9426 (4)0.5479 (4)0.3476 (3)0.0386 (8)
Cd1−0.89424 (4)0.14635 (4)0.75659 (2)0.01890 (8)
Cd2−0.48747 (4)0.31540 (4)0.76500 (2)0.01614 (8)
U11U22U33U12U13U23
C10.019 (2)0.0184 (19)0.021 (2)−0.0033 (16)0.0030 (16)−0.0005 (16)
C20.0179 (19)0.0178 (19)0.032 (2)−0.0057 (16)0.0038 (17)−0.0031 (17)
C30.0173 (19)0.0170 (19)0.020 (2)−0.0034 (16)0.0041 (16)−0.0056 (16)
C40.0171 (18)0.0115 (17)0.0177 (19)−0.0006 (15)0.0044 (15)−0.0020 (15)
C50.0149 (18)0.0066 (15)0.0194 (19)−0.0002 (14)−0.0035 (15)−0.0002 (14)
C60.0117 (17)0.0137 (17)0.0149 (18)−0.0045 (14)0.0010 (14)−0.0037 (14)
C70.0176 (19)0.0157 (18)0.022 (2)−0.0057 (15)−0.0049 (16)−0.0001 (15)
C80.020 (2)0.0136 (18)0.020 (2)−0.0054 (16)−0.0048 (16)−0.0029 (15)
O10.0239 (14)0.0194 (14)0.0319 (16)−0.0115 (12)0.0077 (13)−0.0038 (12)
O20.0195 (15)0.0229 (15)0.0472 (19)−0.0093 (12)−0.0054 (13)−0.0002 (14)
O1W0.0262 (16)0.0263 (16)0.0362 (18)−0.0125 (13)0.0027 (14)−0.0068 (14)
O30.0205 (14)0.0247 (14)0.0276 (15)−0.0101 (12)0.0100 (12)−0.0139 (12)
O2W0.0237 (15)0.0300 (16)0.0406 (18)−0.0120 (14)0.0021 (14)−0.0177 (15)
O40.0241 (14)0.0297 (15)0.0276 (15)−0.0160 (13)0.0017 (12)−0.0104 (12)
O3W0.0237 (17)0.0224 (16)0.073 (3)−0.0105 (14)−0.0142 (16)0.0028 (16)
O50.0320 (16)0.0449 (18)0.0316 (17)−0.0197 (14)0.0097 (13)−0.0241 (15)
O60.0237 (15)0.0331 (16)0.0367 (17)−0.0155 (13)0.0118 (13)−0.0150 (14)
O70.0289 (17)0.0218 (16)0.075 (3)−0.0138 (14)0.0029 (17)0.0039 (16)
O80.0228 (16)0.0213 (15)0.052 (2)0.0002 (13)0.0038 (15)0.0030 (14)
Cd10.01652 (15)0.01605 (14)0.02473 (16)−0.00788 (11)0.00187 (12)−0.00519 (12)
Cd20.01470 (14)0.01407 (14)0.01976 (15)−0.00613 (11)0.00438 (11)−0.00553 (11)
C1—O21.245 (4)O1W—Cd22.601 (3)
C1—O11.272 (4)O1W—HW110.81 (5)
C1—C21.502 (5)O1W—HW120.85 (5)
C2—C31.517 (5)O3—Cd12.370 (3)
C2—H2A0.97O3—Cd22.430 (3)
C2—H2B0.97O2W—Cd12.295 (3)
C3—C41.528 (5)O2W—HW220.83 (5)
C3—C3i1.560 (7)O2W—HW210.831 (19)
C3—H30.98O4—Cd22.495 (3)
C4—O51.247 (4)O3W—Cd12.270 (3)
C4—O61.254 (4)O3W—HW310.842 (19)
C5—O31.251 (4)O3W—HW320.849 (19)
C5—O41.274 (4)O5—Cd1iv2.267 (3)
C5—C61.511 (5)O5—Cd2iv2.521 (3)
C6—C71.522 (5)O6—Cd2iv2.303 (3)
C6—C6ii1.549 (7)O7—Cd2v2.201 (3)
C6—H60.98O8—Cd1vi2.221 (3)
C7—C81.510 (5)Cd1—O8vi2.221 (3)
C7—H7A0.97Cd1—O5iv2.267 (3)
C7—H7B0.97Cd2—O7v2.201 (3)
C8—O71.232 (5)Cd2—O6iv2.303 (3)
C8—O81.252 (4)Cd2—O2vii2.381 (3)
O1—Cd12.252 (3)Cd2—O1vii2.490 (3)
O1—Cd2iii2.490 (3)Cd2—O5iv2.521 (3)
O2—Cd2iii2.381 (3)
O2—C1—O1119.4 (3)Cd1—O3W—HW32139 (3)
O2—C1—C2121.9 (3)HW31—O3W—HW32104 (3)
O1—C1—C2118.7 (3)C4—O5—Cd1iv165.6 (2)
C1—C2—C3114.3 (3)C4—O5—Cd2iv87.7 (2)
C1—C2—H2A108.7Cd1iv—O5—Cd2iv105.79 (11)
C3—C2—H2A108.7C4—O6—Cd2iv97.8 (2)
C1—C2—H2B108.7C8—O7—Cd2v146.3 (3)
C3—C2—H2B108.7C8—O8—Cd1vi132.2 (3)
H2A—C2—H2B107.6O8vi—Cd1—O197.13 (10)
C2—C3—C4111.4 (3)O8vi—Cd1—O5iv83.82 (13)
C2—C3—C3i110.8 (4)O1—Cd1—O5iv104.20 (10)
C4—C3—C3i108.2 (4)O8vi—Cd1—O3W161.95 (11)
C2—C3—H3108.8O1—Cd1—O3W100.36 (11)
C4—C3—H3108.8O5iv—Cd1—O3W87.57 (13)
C3i—C3—H3108.8O8vi—Cd1—O2W96.30 (13)
O5—C4—O6121.1 (3)O1—Cd1—O2W84.45 (11)
O5—C4—C3119.4 (3)O5iv—Cd1—O2W171.28 (10)
O6—C4—C3119.5 (3)O3W—Cd1—O2W89.84 (13)
O3—C5—O4119.9 (3)O8vi—Cd1—O379.76 (10)
O3—C5—C6120.3 (3)O1—Cd1—O3176.60 (9)
O4—C5—C6119.8 (3)O5iv—Cd1—O376.92 (10)
C5—C6—C7110.8 (3)O3W—Cd1—O382.86 (11)
C5—C6—C6ii107.5 (3)O2W—Cd1—O394.50 (10)
C7—C6—C6ii111.7 (3)O7v—Cd2—O6iv94.65 (12)
C5—C6—H6108.9O7v—Cd2—O2vii135.30 (11)
C7—C6—H6108.9O6iv—Cd2—O2vii98.61 (10)
C6ii—C6—H6108.9O7v—Cd2—O3127.03 (11)
C8—C7—C6113.6 (3)O6iv—Cd2—O3123.75 (9)
C8—C7—H7A108.8O2vii—Cd2—O378.14 (10)
C6—C7—H7A108.8O7v—Cd2—O1vii82.94 (11)
C8—C7—H7B108.8O6iv—Cd2—O1vii98.91 (10)
C6—C7—H7B108.8O2vii—Cd2—O1vii52.95 (8)
H7A—C7—H7B107.7O3—Cd2—O1vii119.71 (9)
O7—C8—O8126.0 (3)O7v—Cd2—O484.40 (11)
O7—C8—C7117.0 (3)O6iv—Cd2—O4172.55 (9)
O8—C8—C7116.9 (3)O2vii—Cd2—O487.15 (10)
C1—O1—Cd1127.2 (2)O3—Cd2—O452.67 (8)
C1—O1—Cd2iii90.8 (2)O1vii—Cd2—O488.32 (9)
Cd1—O1—Cd2iii118.95 (12)O7v—Cd2—O5iv140.00 (11)
C1—O2—Cd2iii96.6 (2)O6iv—Cd2—O5iv53.43 (9)
Cd2—O1W—HW1199 (3)O2vii—Cd2—O5iv78.81 (10)
Cd2—O1W—HW12101 (3)O3—Cd2—O5iv71.26 (9)
HW11—O1W—HW12111 (5)O1vii—Cd2—O5iv121.41 (10)
C5—O3—Cd1157.2 (2)O4—Cd2—O5iv123.88 (8)
C5—O3—Cd295.5 (2)O7v—Cd2—O1W76.29 (11)
Cd1—O3—Cd2105.53 (10)O6iv—Cd2—O1W86.09 (11)
Cd1—O2W—HW22128 (3)O2vii—Cd2—O1W146.80 (9)
Cd1—O2W—HW21114 (3)O3—Cd2—O1W72.16 (10)
HW22—O2W—HW21109 (5)O1vii—Cd2—O1W158.98 (9)
C5—O4—Cd291.9 (2)O4—Cd2—O1W86.51 (10)
Cd1—O3W—HW31116 (3)O5iv—Cd2—O1W77.91 (11)
D—H···AD—HH···AD···AD—H···A
O1W—HW11···O8vi0.81 (5)2.08 (5)2.877 (4)169 (5)
O1W—HW12···O4v0.85 (5)2.04 (5)2.866 (4)166 (5)
O2W—HW22···O1Wviii0.83 (5)2.00 (5)2.828 (5)175 (5)
O2W—HW21···O4iii0.83 (2)2.02 (2)2.825 (4)163 (4)
O3W—HW31···O2vii0.84 (2)1.95 (2)2.736 (4)156 (4)
O3W—HW32···O6i0.85 (2)2.43 (2)3.260 (5)165 (4)
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A D⋯A D—H⋯A
O1W—HW11⋯O8i 0.81 (5)2.08 (5)2.877 (4)169 (5)
O1W—HW12⋯O4ii 0.85 (5)2.04 (5)2.866 (4)166 (5)
O2W—HW22⋯O1W iii 0.83 (5)2.00 (5)2.828 (5)175 (5)
O2W—HW21⋯O4iv 0.83 (2)2.02 (2)2.825 (4)163 (4)
O3W—HW31⋯O2v 0.84 (2)1.95 (2)2.736 (4)156 (4)
O3W—HW32⋯O6vi 0.85 (2)2.43 (2)3.260 (5)165 (4)

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

  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

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Authors:  Jin Yang; Jian-Fang Ma; Stuart R Batten; Zhong-Min Su
Journal:  Chem Commun (Camb)       Date:  2008-03-10       Impact factor: 6.222
  2 in total
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1.  Poly[tetra-aqua-(μ(8)-butane-1,2,3,4-tetra-carboxyl-ato)distrontium].

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Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-11-05
  1 in total

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