Literature DB >> 22807740

Poly[diaqua-bis-(nitrato-κ²O,O')bis-(1,10-phenanthroline-κ²N,N')-μ₃-succinato-dicadmium].

Hong-Jin Li1, Zhu-Qing Gao, Jin-Zhong Gu.   

Abstract

In the title coordination polymer, [Cd₂(C₄H₄O₄)(NO₃)₂(C₁₂H₈N₂)₂(H₂O)₂](n), the Cd(II) ion is seven-coordinated within a distorted penta-gonal-bipyramidal O₅N₂ environment. The succinate anions, located on an inversion centre, adopt a bis-monodentate bridging mode, leading to the formation of rods along [100]. The rods are connected by O-H⋯O hydrogen bonds between the coordinating water mol-ecules and nitrate O atoms of adjacent rods; the same type of hydrogen bonds are also observed between water and carboxyl-ate O atoms within the rods. π-π stacking inter-actions with a minimum plane-to-plane separation of 3.462 (2) Å occur between phenanthroline ligands.

Entities:  

Year:  2012        PMID： 22807740      PMCID： PMC3393172          DOI： 10.1107/S1600536812025287

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


Related literature

For the structures and properties of other cadmium coordination compounds, see: Montney et al. (2007 ▶); Li et al. (2011 ▶).

Experimental

Crystal data

[Cd2(C4H4O4)(NO3)2(C12H8N2)2(H2O)2] M = 861.33 Triclinic, a = 7.7349 (13) Å b = 9.4467 (16) Å c = 11.2063 (18) Å α = 102.284 (2)° β = 106.059 (2)° γ = 107.003 (2)° V = 713.0 (2) Å3 Z = 1 Mo Kα radiation μ = 1.57 mm−1 T = 110 K 0.40 × 0.34 × 0.32 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2008 ▶) T min = 0.572, T max = 0.633 5357 measured reflections 2617 independent reflections 2333 reflections with I > 2σ(I) R int = 0.021

Refinement

R[F 2 > 2σ(F 2)] = 0.026 wR(F 2) = 0.086 S = 1.10 2617 reflections 223 parameters 2 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.82 e Å−3 Δρmin = −0.74 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: XP in SHELXTL (Sheldrick, 2008 ▶) and DIAMOND (Brandenburg, 2006 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶). Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812025287/wm2640sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812025287/wm2640Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cd2(C4H4O4)(NO3)2(C12H8N2)2(H2O)2]Z = 1
Mr = 861.33F(000) = 426
Triclinic, P1Dx = 2.006 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.7349 (13) ÅCell parameters from 4041 reflections
b = 9.4467 (16) Åθ = 2.4–25.5°
c = 11.2063 (18) ŵ = 1.57 mm−1
α = 102.284 (2)°T = 110 K
β = 106.059 (2)°Block, colorless
γ = 107.003 (2)°0.40 × 0.34 × 0.32 mm
V = 713.0 (2) Å3
Bruker APEXII CCD diffractometer2617 independent reflections
Radiation source: fine-focus sealed tube2333 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.021
φ and ω scansθmax = 25.5°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2008)h = −9→9
Tmin = 0.572, Tmax = 0.633k = −11→11
5357 measured reflectionsl = −13→13
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) = 0.086H atoms treated by a mixture of independent and constrained refinement
S = 1.10w = 1/[σ2(Fo2) + (0.0381P)2 + 3.2233P] where P = (Fo2 + 2Fc2)/3
2617 reflections(Δ/σ)max = 0.001
223 parametersΔρmax = 0.82 e Å−3
2 restraintsΔρmin = −0.74 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
Cd10.04544 (4)0.84510 (4)0.07477 (3)0.01071 (12)
N20.2174 (5)1.0166 (4)0.2915 (4)0.0132 (8)
N1−0.0501 (5)0.7203 (4)0.2200 (4)0.0142 (8)
C5−0.1372 (7)0.5878 (6)0.4074 (5)0.0177 (10)
H5−0.16620.54120.47020.021*
C140.3403 (6)1.1629 (5)0.3271 (4)0.0153 (9)
H140.35651.20700.26040.018*
C3−0.1898 (7)0.5807 (5)0.1841 (5)0.0174 (10)
H3−0.26010.52620.09330.021*
C130.4480 (7)1.2563 (5)0.4588 (5)0.0178 (10)
H130.53561.36040.48030.021*
C60.0091 (7)0.7368 (6)0.4475 (4)0.0155 (9)
C70.0472 (6)0.7983 (5)0.3497 (4)0.0123 (9)
C110.1893 (6)0.9555 (5)0.3877 (4)0.0131 (9)
C80.1133 (7)0.8288 (6)0.5828 (4)0.0180 (10)
H80.08850.78630.64870.022*
C90.2449 (7)0.9734 (6)0.6180 (5)0.0200 (10)
H90.31071.03180.70840.024*
C100.2890 (6)1.0423 (5)0.5221 (4)0.0141 (9)
C120.4230 (7)1.1927 (5)0.5559 (5)0.0187 (10)
H120.49731.25150.64540.022*
C4−0.2371 (7)0.5112 (6)0.2757 (5)0.0197 (10)
H4−0.33800.41140.24670.024*
O1W0.2864 (5)0.7375 (4)0.1138 (3)0.0147 (7)
O40.0112 (4)0.7484 (4)−0.1567 (3)0.0166 (7)
O3−0.1556 (5)0.5788 (4)−0.0899 (3)0.0193 (7)
N3−0.1132 (5)0.6148 (4)−0.1844 (4)0.0129 (8)
O5−0.1930 (5)0.5236 (4)−0.2976 (3)0.0226 (8)
O1−0.1906 (4)0.9255 (4)−0.0170 (3)0.0141 (6)
O2−0.3962 (5)0.7674 (4)0.0468 (3)0.0204 (7)
C1−0.3553 (6)0.8680 (5)−0.0059 (4)0.0103 (8)
C2−0.5043 (6)0.9368 (5)−0.0573 (4)0.0118 (9)
H2A−0.63570.8539−0.09780.014*
H2B−0.47580.9823−0.12470.014*
H1B0.238 (7)0.6402 (19)0.106 (5)0.018*
H1A0.373 (5)0.736 (6)0.080 (5)0.018*
U11U22U33U12U13U23
Cd10.01089 (18)0.01093 (18)0.00981 (18)0.00348 (12)0.00347 (12)0.00352 (12)
N20.0124 (18)0.016 (2)0.0127 (18)0.0055 (16)0.0053 (15)0.0070 (15)
N10.0144 (19)0.0113 (19)0.0161 (19)0.0050 (15)0.0048 (15)0.0032 (15)
C50.023 (3)0.019 (2)0.020 (2)0.010 (2)0.014 (2)0.012 (2)
C140.014 (2)0.020 (2)0.015 (2)0.0075 (19)0.0068 (18)0.0064 (18)
C30.019 (2)0.012 (2)0.019 (2)0.0028 (19)0.0079 (19)0.0040 (18)
C130.015 (2)0.007 (2)0.026 (3)−0.0007 (18)0.008 (2)0.0010 (19)
C60.020 (2)0.021 (2)0.016 (2)0.013 (2)0.0106 (19)0.0131 (19)
C70.011 (2)0.015 (2)0.014 (2)0.0058 (18)0.0053 (17)0.0076 (18)
C110.015 (2)0.020 (2)0.011 (2)0.0110 (19)0.0081 (17)0.0057 (18)
C80.023 (2)0.027 (3)0.013 (2)0.014 (2)0.0093 (19)0.012 (2)
C90.020 (2)0.027 (3)0.014 (2)0.011 (2)0.0046 (19)0.006 (2)
C100.015 (2)0.014 (2)0.014 (2)0.0082 (18)0.0056 (18)0.0013 (18)
C120.016 (2)0.015 (2)0.018 (2)0.0037 (19)0.0029 (19)−0.0013 (19)
C40.019 (2)0.017 (2)0.023 (3)0.006 (2)0.011 (2)0.003 (2)
O1W0.0139 (16)0.0115 (16)0.0203 (17)0.0042 (13)0.0083 (13)0.0062 (13)
O40.0154 (16)0.0109 (16)0.0195 (17)−0.0002 (13)0.0063 (13)0.0044 (13)
O30.0243 (18)0.0210 (18)0.0138 (16)0.0057 (15)0.0113 (14)0.0062 (14)
N30.0138 (19)0.0103 (19)0.0136 (19)0.0047 (15)0.0048 (15)0.0019 (15)
O50.0228 (18)0.0244 (19)0.0096 (16)0.0025 (15)0.0019 (14)−0.0015 (14)
O10.0081 (15)0.0195 (17)0.0137 (15)0.0036 (13)0.0037 (12)0.0057 (13)
O20.0181 (17)0.0206 (18)0.036 (2)0.0104 (14)0.0169 (15)0.0219 (16)
C10.015 (2)0.006 (2)0.011 (2)0.0038 (17)0.0065 (17)0.0012 (16)
C20.011 (2)0.011 (2)0.015 (2)0.0026 (17)0.0047 (17)0.0082 (18)
Cd1—O12.253 (3)C7—C111.453 (6)
Cd1—O1W2.355 (3)C11—C101.414 (6)
Cd1—N12.358 (4)C8—C91.340 (7)
Cd1—N22.360 (4)C8—H80.9500
Cd1—O1i2.439 (3)C9—C101.437 (7)
Cd1—O42.470 (3)C9—H90.9500
Cd1—O32.511 (3)C10—C121.389 (7)
N2—C141.327 (6)C12—H120.9500
N2—C111.365 (6)C4—H40.9500
N1—C31.330 (6)O1W—H1B0.859 (10)
N1—C71.355 (6)O1W—H1A0.859 (10)
C5—C41.374 (7)O4—N31.254 (5)
C5—C61.407 (7)O3—N31.275 (5)
C5—H50.9500N3—O51.234 (5)
C14—C131.410 (6)O1—C11.282 (5)
C14—H140.9500O1—Cd1i2.439 (3)
C3—C41.405 (7)O2—C11.232 (5)
C3—H30.9500C1—C21.521 (6)
C13—C121.381 (7)C2—C2ii1.528 (9)
C13—H130.9500C2—H2A0.9900
C6—C71.406 (6)C2—H2B0.9900
C6—C81.435 (7)
O1—Cd1—O1W165.04 (11)N1—C7—C6122.8 (4)
O1—Cd1—N1107.49 (12)N1—C7—C11117.9 (4)
O1W—Cd1—N183.07 (12)C6—C7—C11119.3 (4)
O1—Cd1—N2107.06 (12)N2—C11—C10122.0 (4)
O1W—Cd1—N286.20 (12)N2—C11—C7118.5 (4)
N1—Cd1—N270.97 (13)C10—C11—C7119.4 (4)
O1—Cd1—O1i71.54 (12)C9—C8—C6121.2 (4)
O1W—Cd1—O1i103.94 (10)C9—C8—H8119.4
N1—Cd1—O1i153.21 (12)C6—C8—H8119.4
N2—Cd1—O1i83.58 (11)C8—C9—C10121.5 (4)
O1—Cd1—O481.10 (11)C8—C9—H9119.2
O1W—Cd1—O483.94 (11)C10—C9—H9119.2
N1—Cd1—O4133.14 (12)C12—C10—C11118.3 (4)
N2—Cd1—O4152.10 (12)C12—C10—C9122.7 (4)
O1i—Cd1—O473.64 (10)C11—C10—C9119.0 (4)
O1—Cd1—O387.96 (11)C13—C12—C10119.8 (4)
O1W—Cd1—O382.85 (11)C13—C12—H12120.1
N1—Cd1—O382.58 (12)C10—C12—H12120.1
N2—Cd1—O3152.40 (12)C5—C4—C3119.9 (4)
O1i—Cd1—O3123.65 (10)C5—C4—H4120.1
O4—Cd1—O351.17 (10)C3—C4—H4120.1
C14—N2—C11118.1 (4)Cd1—O1W—H1B112 (4)
C14—N2—Cd1126.2 (3)Cd1—O1W—H1A132 (4)
C11—N2—Cd1115.7 (3)H1B—O1W—H1A99 (5)
C3—N1—C7118.5 (4)N3—O4—Cd197.2 (2)
C3—N1—Cd1125.0 (3)N3—O3—Cd194.7 (2)
C7—N1—Cd1116.5 (3)O5—N3—O4121.9 (4)
C4—C5—C6118.8 (4)O5—N3—O3121.5 (4)
C4—C5—H5120.6O4—N3—O3116.6 (3)
C6—C5—H5120.6C1—O1—Cd1117.6 (3)
N2—C14—C13123.4 (4)C1—O1—Cd1i132.2 (3)
N2—C14—H14118.3Cd1—O1—Cd1i108.46 (12)
C13—C14—H14118.3O2—C1—O1124.8 (4)
N1—C3—C4122.3 (4)O2—C1—C2119.1 (4)
N1—C3—H3118.9O1—C1—C2116.0 (4)
C4—C3—H3118.9C1—C2—C2ii108.6 (4)
C12—C13—C14118.3 (4)C1—C2—H2A110.0
C12—C13—H13120.8C2ii—C2—H2A110.0
C14—C13—H13120.8C1—C2—H2B110.0
C7—C6—C5117.9 (4)C2ii—C2—H2B110.0
C7—C6—C8119.6 (4)H2A—C2—H2B108.4
C5—C6—C8122.5 (4)
O1—Cd1—N2—C14−73.4 (4)C5—C6—C8—C9−176.6 (5)
O1W—Cd1—N2—C1499.5 (4)C6—C8—C9—C10−0.6 (7)
N1—Cd1—N2—C14−176.5 (4)N2—C11—C10—C12−1.8 (6)
O1i—Cd1—N2—C14−5.0 (3)C7—C11—C10—C12−179.5 (4)
O4—Cd1—N2—C1430.1 (5)N2—C11—C10—C9176.9 (4)
O3—Cd1—N2—C14166.2 (3)C7—C11—C10—C9−0.9 (6)
O1—Cd1—N2—C11108.4 (3)C8—C9—C10—C12179.2 (4)
O1W—Cd1—N2—C11−78.7 (3)C8—C9—C10—C110.6 (7)
N1—Cd1—N2—C115.3 (3)C14—C13—C12—C10−2.4 (7)
O1i—Cd1—N2—C11176.8 (3)C11—C10—C12—C133.5 (7)
O4—Cd1—N2—C11−148.1 (3)C9—C10—C12—C13−175.1 (4)
O3—Cd1—N2—C11−12.0 (5)C6—C5—C4—C31.2 (7)
O1—Cd1—N1—C372.5 (4)N1—C3—C4—C5−0.1 (7)
O1W—Cd1—N1—C3−96.7 (4)O1—Cd1—O4—N3−91.1 (2)
N2—Cd1—N1—C3175.0 (4)O1W—Cd1—O4—N389.2 (2)
O1i—Cd1—N1—C3156.0 (3)N1—Cd1—O4—N314.6 (3)
O4—Cd1—N1—C3−21.7 (4)N2—Cd1—O4—N3159.1 (3)
O3—Cd1—N1—C3−13.0 (4)O1i—Cd1—O4—N3−164.3 (3)
O1—Cd1—N1—C7−107.8 (3)O3—Cd1—O4—N33.5 (2)
O1W—Cd1—N1—C783.1 (3)O1—Cd1—O3—N376.8 (2)
N2—Cd1—N1—C7−5.3 (3)O1W—Cd1—O3—N3−91.4 (2)
O1i—Cd1—N1—C7−24.3 (5)N1—Cd1—O3—N3−175.3 (3)
O4—Cd1—N1—C7158.0 (3)N2—Cd1—O3—N3−158.8 (3)
O3—Cd1—N1—C7166.7 (3)O1i—Cd1—O3—N310.6 (3)
C11—N2—C14—C132.3 (6)O4—Cd1—O3—N3−3.4 (2)
Cd1—N2—C14—C13−175.8 (3)Cd1—O4—N3—O5172.9 (3)
C7—N1—C3—C4−1.1 (7)Cd1—O4—N3—O3−6.0 (4)
Cd1—N1—C3—C4178.6 (3)Cd1—O3—N3—O5−173.1 (3)
N2—C14—C13—C12−0.6 (7)Cd1—O3—N3—O45.9 (4)
C4—C5—C6—C7−1.0 (7)O1W—Cd1—O1—C1118.5 (4)
C4—C5—C6—C8176.5 (4)N1—Cd1—O1—C1−15.1 (3)
C3—N1—C7—C61.3 (6)N2—Cd1—O1—C1−90.0 (3)
Cd1—N1—C7—C6−178.5 (3)O1i—Cd1—O1—C1−166.9 (4)
C3—N1—C7—C11−175.4 (4)O4—Cd1—O1—C1117.4 (3)
Cd1—N1—C7—C114.8 (5)O3—Cd1—O1—C166.4 (3)
C5—C6—C7—N1−0.2 (7)O1W—Cd1—O1—Cd1i−74.6 (4)
C8—C6—C7—N1−177.8 (4)N1—Cd1—O1—Cd1i151.83 (13)
C5—C6—C7—C11176.4 (4)N2—Cd1—O1—Cd1i76.95 (14)
C8—C6—C7—C11−1.1 (6)O1i—Cd1—O1—Cd1i0.0
C14—N2—C11—C10−1.1 (6)O4—Cd1—O1—Cd1i−75.62 (12)
Cd1—N2—C11—C10177.3 (3)O3—Cd1—O1—Cd1i−126.61 (12)
C14—N2—C11—C7176.7 (4)Cd1—O1—C1—O2−2.9 (6)
Cd1—N2—C11—C7−5.0 (5)Cd1i—O1—C1—O2−166.1 (3)
N1—C7—C11—N20.2 (6)Cd1—O1—C1—C2174.2 (3)
C6—C7—C11—N2−176.7 (4)Cd1i—O1—C1—C211.0 (5)
N1—C7—C11—C10178.0 (4)O2—C1—C2—C2ii81.3 (6)
C6—C7—C11—C101.1 (6)O1—C1—C2—C2ii−96.0 (5)
C7—C6—C8—C90.8 (7)
D—H···AD—HH···AD···AD—H···A
O1W—H1B···O3iii0.86 (1)1.93 (1)2.786 (5)174 (5)
O1W—H1A···O2iv0.86 (1)1.88 (2)2.716 (4)166 (5)
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A D⋯A D—H⋯A
O1W—H1B⋯O3i 0.86 (1)1.93 (1)2.786 (5)174 (5)
O1W—H1A⋯O2ii 0.86 (1)1.88 (2)2.716 (4)166 (5)

Symmetry codes: (i) ; (ii) .

  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.  Di-μ-benzoato-κO,O':O';κO:O,O'-bis-[(benzoato-κO,O')(1,10-phenanthroline-κN,N')cadmium].

Authors:  Hong-Jin Li; Zhu-Qing Gao; Jin-Zhong Gu
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-06-18
  2 in total

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