Literature DB >> 21588205

Bis(μ-5-carboxyl-atotetra-zolido)bis-[aqua-(2,2'-bipyrid-yl)cadmium(II)].

Shuang-Jiao Sun, Ji-Hua Deng, Ti-Lou Liu.   

Abstract

In the title dinuclear Cd(II) complex, [n class="Chemical">Cd(2)(C(2)N(4)O(2))(2)(C(10)H(8)N(2))(2)(H(2)O)(2)], each Cd atom is in a slightly distorted octa-hedral coordination by two N atoms and one O atom of two 1H-tetra-zole-5-carboxyl-ate (TZC) ligands, two N atoms of a 2,2'-bipyridyl ligand and one water O atom. The TZC ligand acts in a tridentate N,O-chelating N-bridging mode to two symmetry-equivalent Cd(II) atoms. The complex reveals mol-ecular C(i) symmetry. Extensive O-H⋯O hydrogen bonding plays an important role in the crystal packing.

Entities:  

Year:  2010        PMID： 21588205      PMCID： PMC3007395          DOI： 10.1107/S1600536810027613

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


Related literature

For the structural topologies and varied properties such as mol­ecular magnetism, mol­ecular absorption, catalysis, non-linear optics and luminescence of coordination complexes with tetra­zolate-based ligands, see: Zhao et al. (2008 ▶); Cheng et al. (2007 ▶). For related structures, see: Wu et al. (2009 ▶; 2010 ▶) For related literature on n class="Chemical">1H-tetrazoles, see: Jia et al. (2009 ▶); Zhong et al. (2010 ▶).

Experimental

Crystal data

[Cd2(C2n class="Chemical">N4O2)2(C10H8N2)2(H2O)2] M = 797.32 Triclinic, a = 7.5218 (13) Å b = 9.6372 (16) Å c = 9.7335 (16) Å α = 75.628 (3)° β = 89.686 (3)° γ = 74.461 (2)° V = 657.10 (19) Å3 Z = 1 Mo Kα radiation μ = 1.69 mm−1 T = 173 K 0.28 × 0.22 × 0.16 mm

Data collection

Bruker SMART CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Bruker, 1998 ▶) T min = 0.650, T max = 0.774 3760 measured reflections 2168 independent reflections 1930 reflections with I > 2σ(I) R int = 0.019

Refinement

R[F 2 > 2σ(F 2)] = 0.025 wR(F 2) = 0.066 S = 1.11 2168 reflections 207 parameters 3 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.70 e Å−3 Δρmin = −0.47 e Å−3 Data collection: SMART (Bruker, 1998 ▶); cell refinement: SAINT (Bruker, 1998 ▶); data reduction: SAIn class="Chemical">NT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810027613/kp2269sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810027613/kp2269Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cd2(C2N4O2)2(C10H8N2)2(H2O)2]Z = 1
Mr = 797.32F(000) = 392
Triclinic, P1Dx = 2.015 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.5218 (13) ÅCell parameters from 2926 reflections
b = 9.6372 (16) Åθ = 2.7–27.0°
c = 9.7335 (16) ŵ = 1.69 mm−1
α = 75.628 (3)°T = 173 K
β = 89.686 (3)°Block, colourless
γ = 74.461 (2)°0.28 × 0.22 × 0.16 mm
V = 657.10 (19) Å3
Bruker SMART CCD area-detector diffractometer2268 independent reflections
Radiation source: fine-focus sealed tube1930 reflections with I > 2σ(I)
graphiteRint = 0.019
phi and ω scansθmax = 25.0°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Bruker, 1998)h = −8→8
Tmin = 0.650, Tmax = 0.774k = −11→11
3760 measured reflectionsl = −11→11
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.025Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.066H atoms treated by a mixture of independent and constrained refinement
S = 1.11w = 1/[σ2(Fo2) + (0.0331P)2 + 0.4626P] where P = (Fo2 + 2Fc2)/3
2168 reflections(Δ/σ)max < 0.001
207 parametersΔρmax = 0.70 e Å−3
3 restraintsΔρmin = −0.47 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
Cd10.40965 (3)0.23221 (3)0.36929 (3)0.01494 (11)
O10.6019 (3)0.3838 (3)0.3780 (3)0.0205 (6)
O20.8715 (3)0.3914 (3)0.4648 (3)0.0212 (6)
O30.2432 (3)0.3036 (3)0.5528 (3)0.0199 (6)
N10.6687 (4)0.0890 (3)0.5152 (3)0.0145 (6)
N20.7360 (4)−0.0460 (3)0.6050 (3)0.0150 (6)
N30.8896 (4)−0.0486 (4)0.6726 (3)0.0187 (7)
N40.9234 (4)0.0835 (3)0.6289 (3)0.0181 (7)
N90.2429 (4)0.4286 (3)0.1938 (3)0.0151 (6)
N100.5150 (4)0.1995 (3)0.1484 (3)0.0167 (7)
C10.7862 (5)0.1654 (4)0.5330 (4)0.0142 (8)
C20.7527 (5)0.3265 (4)0.4521 (4)0.0174 (8)
C30.1195 (5)0.5462 (4)0.2218 (4)0.0190 (8)
H30.06960.52300.31730.023*
C40.0345 (5)0.6728 (4)0.1188 (4)0.0230 (9)
H4−0.05260.75320.14320.028*
C50.0777 (5)0.6817 (4)−0.0214 (4)0.0232 (9)
H50.01960.7672−0.09510.028*
C60.2080 (5)0.5619 (4)−0.0508 (4)0.0189 (8)
H60.24270.5655−0.14540.023*
C70.2875 (5)0.4368 (4)0.0589 (4)0.0156 (8)
C80.4293 (5)0.3049 (4)0.0329 (4)0.0157 (8)
C90.4693 (5)0.2928 (5)−0.1038 (4)0.0240 (9)
H90.40560.3679−0.18420.029*
C100.6035 (6)0.1695 (5)−0.1209 (4)0.0289 (10)
H100.63160.1582−0.21340.035*
C110.6960 (6)0.0634 (5)−0.0029 (4)0.0282 (9)
H110.7911−0.0205−0.01280.034*
C120.6479 (5)0.0810 (4)0.1307 (4)0.0243 (9)
H120.71060.00720.21230.029*
H3A0.149 (5)0.288 (5)0.531 (5)0.037 (14)*
H3B0.234 (6)0.388 (4)0.563 (5)0.045 (15)*
U11U22U33U12U13U23
Cd10.01564 (15)0.01420 (16)0.01338 (16)−0.00440 (11)−0.00143 (10)−0.00027 (11)
O10.0236 (14)0.0146 (13)0.0214 (14)−0.0080 (11)−0.0036 (11)0.0020 (11)
O20.0216 (13)0.0211 (14)0.0258 (15)−0.0135 (12)0.0028 (11)−0.0069 (12)
O30.0193 (14)0.0196 (15)0.0226 (15)−0.0068 (12)0.0009 (11)−0.0071 (12)
N10.0158 (15)0.0149 (16)0.0129 (16)−0.0050 (13)0.0013 (12)−0.0028 (13)
N20.0163 (15)0.0139 (16)0.0122 (16)−0.0035 (13)0.0010 (12)0.0008 (13)
N30.0174 (15)0.0203 (17)0.0183 (17)−0.0062 (14)0.0006 (13)−0.0037 (14)
N40.0158 (15)0.0193 (17)0.0186 (17)−0.0039 (13)0.0000 (13)−0.0048 (14)
N90.0146 (14)0.0157 (16)0.0154 (16)−0.0054 (13)0.0004 (12)−0.0035 (13)
N100.0159 (15)0.0134 (16)0.0204 (17)−0.0047 (13)0.0021 (13)−0.0027 (13)
C10.0130 (16)0.019 (2)0.0132 (18)−0.0056 (15)0.0047 (14)−0.0077 (16)
C20.0219 (19)0.022 (2)0.0133 (19)−0.0091 (17)0.0087 (16)−0.0108 (16)
C30.0181 (18)0.020 (2)0.017 (2)−0.0035 (16)0.0011 (16)−0.0034 (16)
C40.0218 (19)0.018 (2)0.025 (2)−0.0004 (17)−0.0010 (17)−0.0043 (17)
C50.0231 (19)0.017 (2)0.023 (2)−0.0026 (17)−0.0066 (17)0.0033 (17)
C60.0233 (19)0.020 (2)0.0126 (19)−0.0088 (17)0.0002 (16)0.0000 (16)
C70.0150 (17)0.0170 (19)0.0151 (19)−0.0071 (15)−0.0031 (15)−0.0018 (16)
C80.0146 (17)0.0166 (19)0.0159 (19)−0.0058 (15)0.0015 (15)−0.0027 (16)
C90.028 (2)0.027 (2)0.017 (2)−0.0085 (18)0.0041 (17)−0.0045 (17)
C100.034 (2)0.031 (2)0.022 (2)−0.007 (2)0.0113 (19)−0.0107 (19)
C110.033 (2)0.018 (2)0.029 (2)−0.0001 (18)0.0075 (19)−0.0059 (18)
C120.024 (2)0.016 (2)0.029 (2)−0.0026 (17)0.0019 (17)−0.0024 (17)
Cd1—N92.285 (3)N10—C121.349 (5)
Cd1—N2i2.304 (3)C1—C21.510 (5)
Cd1—N12.310 (3)C3—C41.372 (5)
Cd1—O32.314 (3)C3—H30.9966
Cd1—O12.330 (2)C4—C51.388 (6)
Cd1—N102.352 (3)C4—H40.9500
O1—C21.260 (4)C5—C61.389 (5)
O2—C21.242 (4)C5—H50.9500
O3—H3A0.80 (2)C6—C71.390 (5)
O3—H3B0.83 (2)C6—H60.9500
N1—C11.329 (5)C7—C81.500 (5)
N1—N21.342 (4)C8—C91.389 (5)
N2—N31.324 (4)C9—C101.382 (5)
N2—Cd1i2.304 (3)C9—H90.9500
N3—N41.330 (4)C10—C111.376 (6)
N4—C11.330 (5)C10—H100.9500
N9—C71.342 (5)C11—C121.386 (6)
N9—C31.344 (5)C11—H110.9500
N10—C81.342 (5)C12—H120.9500
N9—Cd1—N2i106.72 (10)N4—C1—C2127.8 (3)
N9—Cd1—N1155.62 (10)O2—C2—O1125.7 (4)
N2i—Cd1—N196.01 (10)O2—C2—C1118.7 (3)
N9—Cd1—O395.41 (10)O1—C2—C1115.6 (3)
N2i—Cd1—O387.65 (10)N9—C3—C4123.2 (3)
N1—Cd1—O394.18 (9)N9—C3—H3113.3
N9—Cd1—O185.09 (10)C4—C3—H3121.4
N2i—Cd1—O1168.16 (9)C3—C4—C5119.0 (4)
N1—Cd1—O172.19 (10)C3—C4—H4120.5
O3—Cd1—O192.14 (9)C5—C4—H4120.5
N9—Cd1—N1071.32 (10)C4—C5—C6118.2 (4)
N2i—Cd1—N1091.88 (10)C4—C5—H5120.9
N1—Cd1—N1099.78 (10)C6—C5—H5120.9
O3—Cd1—N10166.00 (10)C5—C6—C7119.6 (3)
O1—Cd1—N1091.16 (10)C5—C6—H6120.2
C2—O1—Cd1118.0 (2)C7—C6—H6120.2
Cd1—O3—H3A96 (3)N9—C7—C6121.7 (3)
Cd1—O3—H3B119 (3)N9—C7—C8116.5 (3)
H3A—O3—H3B117 (3)C6—C7—C8121.7 (3)
C1—N1—N2104.9 (3)N10—C8—C9121.9 (3)
C1—N1—Cd1113.4 (2)N10—C8—C7116.5 (3)
N2—N1—Cd1141.1 (2)C9—C8—C7121.5 (3)
N3—N2—N1108.9 (3)C10—C9—C8118.8 (4)
N3—N2—Cd1i128.6 (2)C10—C9—H9120.6
N1—N2—Cd1i122.5 (2)C8—C9—H9120.6
N2—N3—N4109.4 (3)C11—C10—C9119.5 (4)
N3—N4—C1105.2 (3)C11—C10—H10120.2
C7—N9—C3118.2 (3)C9—C10—H10120.2
C7—N9—Cd1118.7 (2)C10—C11—C12118.8 (4)
C3—N9—Cd1122.4 (2)C10—C11—H11120.6
C8—N10—C12118.8 (3)C12—C11—H11120.6
C8—N10—Cd1116.4 (2)N10—C12—C11122.1 (4)
C12—N10—Cd1124.7 (3)N10—C12—H12119.0
N1—C1—N4111.6 (3)C11—C12—H12119.0
N1—C1—C2120.6 (3)
D—H···AD—HH···AD···AD—H···A
O3—H3B···O2ii0.83 (2)2.01 (3)2.794 (4)158 (4)
O3—H3A···O2iii0.80 (2)2.09 (4)2.769 (4)143 (4)
Table 1

Selected bond lengths (Å)

Cd1—N92.285 (3)
Cd1—N2i2.304 (3)
Cd1—N12.310 (3)
Cd1—O32.314 (3)
Cd1—O12.330 (2)
Cd1—N102.352 (3)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O3—H3B⋯O2ii0.83 (2)2.01 (3)2.794 (4)158 (4)
O3—H3A⋯O2iii0.80 (2)2.09 (4)2.769 (4)143 (4)

Symmetry codes: (ii) ; (iii) .

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