Literature DB >> 21580497

Bis[μ-2-(2,4-difluoro-phen-yl)-1,3-bis-(1H-1,2,4-triazol-1-yl)propan-2-olato]dicopper(II) bis-(perchlorate).

Zhi-Rong Luo1, Fei-Long Hu, Yue Zhuang, Xian-Hong Yin, Qiao-Lan Wu.   

Abstract

The title complex, [Cu(2)(C(13)H(11)F(2)N(6)O)(2)](ClO(4))(2), which was hydro-thermally synthesized, contains a binuclear copper cluster (2 symmetry) with a Cu(2)O(2) rhombus [Cu-O = 1.927 (2) Å] formed by donation of two O atoms from two chelate rings. The tridentate function of each ligand is completed by two N atoms coordinated to the two Cu(II) atoms [Cu-N = 1.933 (2) Å]. The separation distance of two Cu(II) atoms in a cluster is 2.988 (1) Å. The dihedral angle between the six-membered chelate rings is 2.13 (9)°. The perchlorate counter-anion is disordered over two sites in a 0.58 (10):0.42 (10) ratio.

Entities:  

Year:  2010        PMID： 21580497      PMCID： PMC2984043          DOI： 10.1107/S1600536810008512

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


Related literature

For the use of 1,2,4-triazole and its derivatives in coordination chemistry, see: Haasnoot et al. (2000 ▶); Zhao et al. (2007 ▶). For 1,2,4-triazole as a bridging ligand, see: Liu et al. (2003 ▶); Park et al. (2006 ▶); Yi et al. (2004 ▶); Garcia et al. (2005 ▶).

Experimental

Crystal data

[Cu2(C13H11F2N6O)2](ClO4)2 M = 936.54 Orthorhombic, a = 15.4464 (18) Å b = 7.9532 (10) Å c = 14.2407 (15) Å V = 1749.4 (4) Å3 Z = 2 Mo Kα radiation μ = 1.46 mm−1 T = 298 K 0.49 × 0.45 × 0.43 mm

Data collection

Bruker SMART 1000 diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.534, T max = 0.572 7867 measured reflections 1618 independent reflections 1169 reflections with I > 2σ(I) R int = 0.024

Refinement

R[F 2 > 2σ(F 2)] = 0.040 wR(F 2) = 0.129 S = 1.09 1618 reflections 162 parameters H-atom parameters constrained Δρmax = 0.55 e Å−3 Δρmin = −0.48 e Å−3 Data collection: SMART (Siemens, 1996 ▶); cell refinement: SAINT (Siemens, 1996 ▶); data reduction: SAINT; 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/S1600536810008512/kp2237sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810008512/kp2237Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cu2(C13H11F2N6O)2](ClO4)2Dx = 1.778 Mg m−3
Mr = 936.54Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PnnmCell parameters from 3901 reflections
a = 15.4464 (18) Åθ = 2.6–26.9°
b = 7.9532 (10) ŵ = 1.46 mm−1
c = 14.2407 (15) ÅT = 298 K
V = 1749.4 (4) Å3Block, blue
Z = 20.49 × 0.45 × 0.43 mm
F(000) = 940
Bruker SMART 1000 diffractometer1618 independent reflections
Radiation source: fine-focus sealed tube1169 reflections with I > 2σ(I)
graphiteRint = 0.024
phi and ω scansθmax = 25.0°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −16→18
Tmin = 0.534, Tmax = 0.572k = −9→9
7867 measured reflectionsl = −16→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)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.129H-atom parameters constrained
S = 1.09w = 1/[σ2(Fo2) + (0.0552P)2 + 3.7317P] where P = (Fo2 + 2Fc2)/3
1618 reflections(Δ/σ)max = 0.001
162 parametersΔρmax = 0.55 e Å−3
0 restraintsΔρmin = −0.48 e Å−3
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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*/UeqOcc. (<1)
Cu10.00000.50000.10491 (4)0.0387 (3)
Cl10.00001.00000.1949 (2)0.0786 (7)
F10.3498 (3)0.3943 (7)0.00000.112 (2)
F20.3994 (4)0.9719 (7)0.00000.110 (2)
N10.1704 (2)0.4153 (4)0.1725 (2)0.0412 (8)
N20.0936 (2)0.4883 (4)0.1947 (2)0.0394 (8)
N30.1944 (3)0.5620 (5)0.2995 (3)0.0595 (11)
O10.0783 (2)0.4823 (5)0.00000.0339 (8)
O20.009 (3)0.8525 (18)0.126 (2)0.097 (7)0.58 (10)
O30.0787 (17)1.020 (6)0.232 (3)0.110 (11)0.58 (10)
O2'0.047 (4)0.884 (6)0.151 (3)0.106 (13)0.42 (10)
O3'0.055 (3)1.093 (8)0.261 (3)0.109 (11)0.42 (10)
C10.1119 (3)0.5755 (6)0.2716 (3)0.0503 (11)
H10.07110.64020.30330.060*
C20.2285 (3)0.4627 (6)0.2355 (3)0.0546 (12)
H20.28630.42980.23460.066*
C30.1787 (3)0.3154 (5)0.0873 (3)0.0433 (10)
H3A0.13590.22600.08780.052*
H3B0.23570.26410.08530.052*
C40.1658 (3)0.4248 (7)0.00000.0352 (12)
C50.2277 (4)0.5736 (7)0.00000.0395 (13)
C60.3173 (4)0.5544 (9)0.00000.0640 (19)
C70.3745 (5)0.6848 (12)0.00000.079 (2)
H70.43390.66560.00000.095*
C80.3431 (5)0.8399 (11)0.00000.069 (2)
C90.2571 (5)0.8714 (9)0.00000.0640 (19)
H90.23690.98150.00000.077*
C100.1993 (4)0.7384 (7)0.00000.0448 (14)
H100.14020.76040.00000.054*
U11U22U33U12U13U23
Cu10.0307 (4)0.0620 (5)0.0232 (3)−0.0056 (3)0.0000.000
Cl10.0398 (9)0.0638 (12)0.132 (2)0.0021 (9)0.0000.000
F10.049 (3)0.078 (3)0.208 (7)0.022 (2)0.0000.000
F20.115 (4)0.105 (4)0.111 (4)−0.075 (3)0.0000.000
N10.0453 (19)0.0394 (18)0.0390 (18)−0.0007 (16)−0.0119 (15)0.0017 (16)
N20.0415 (18)0.049 (2)0.0276 (16)−0.0035 (16)−0.0047 (14)0.0001 (15)
N30.061 (2)0.064 (3)0.054 (2)−0.004 (2)−0.022 (2)−0.012 (2)
O10.0277 (18)0.047 (2)0.0268 (18)0.0006 (16)0.0000.000
O20.073 (13)0.066 (6)0.153 (12)−0.002 (6)0.008 (10)−0.014 (6)
O30.068 (8)0.101 (17)0.162 (17)0.005 (9)−0.027 (9)−0.003 (15)
O2'0.08 (2)0.087 (15)0.152 (17)0.024 (16)0.009 (16)−0.013 (13)
O3'0.078 (14)0.10 (2)0.151 (15)0.002 (14)−0.022 (11)−0.018 (13)
C10.054 (3)0.056 (3)0.041 (2)0.000 (2)−0.010 (2)−0.006 (2)
C20.049 (3)0.059 (3)0.056 (3)0.002 (2)−0.021 (2)−0.004 (2)
C30.051 (2)0.036 (2)0.042 (2)0.0042 (19)−0.007 (2)0.0003 (18)
C40.031 (3)0.033 (3)0.041 (3)0.000 (2)0.0000.000
C50.035 (3)0.039 (3)0.045 (3)0.001 (3)0.0000.000
C60.047 (4)0.059 (4)0.086 (5)0.000 (3)0.0000.000
C70.047 (4)0.089 (7)0.101 (7)−0.015 (4)0.0000.000
C80.068 (5)0.067 (5)0.071 (5)−0.036 (4)0.0000.000
C90.080 (5)0.045 (4)0.067 (5)−0.010 (4)0.0000.000
C100.048 (3)0.042 (3)0.045 (3)−0.002 (3)0.0000.000
Cu1—O1i1.927 (2)N3—C11.340 (6)
Cu1—O11.927 (2)O1—C41.427 (6)
Cu1—N21.933 (3)O1—Cu1i1.927 (2)
Cu1—N2ii1.933 (3)C1—H10.9300
Cu1—Cu1i2.9880 (13)C2—H20.9300
Cl1—O2'1.33 (2)C3—C41.531 (5)
Cl1—O2'iii1.33 (2)C3—H3A0.9700
Cl1—O3iii1.336 (12)C3—H3B0.9700
Cl1—O31.336 (12)C4—C51.522 (8)
Cl1—O3'1.47 (3)C4—C3iv1.531 (5)
Cl1—O3'iii1.47 (3)C5—C101.382 (8)
Cl1—O21.53 (2)C5—C61.392 (9)
Cl1—O2iii1.53 (2)C6—C71.364 (10)
F1—C61.368 (9)C7—C81.326 (12)
F2—C81.364 (8)C7—H70.9300
N1—C21.324 (5)C8—C91.352 (11)
N1—N21.358 (5)C9—C101.383 (9)
N1—C31.456 (5)C9—H90.9300
N2—C11.326 (5)C10—H100.9300
N3—C21.316 (6)
O1i—Cu1—O178.33 (16)C1—N2—Cu1132.8 (3)
O1i—Cu1—N2170.37 (12)N1—N2—Cu1121.3 (2)
O1—Cu1—N292.30 (13)C2—N3—C1102.9 (4)
O1i—Cu1—N2ii92.30 (13)C4—O1—Cu1i128.15 (10)
O1—Cu1—N2ii170.37 (12)C4—O1—Cu1128.15 (10)
N2—Cu1—N2ii97.2 (2)Cu1i—O1—Cu1101.67 (16)
O1i—Cu1—Cu1i39.16 (8)N2—C1—N3113.9 (4)
O1—Cu1—Cu1i39.16 (8)N2—C1—H1123.0
N2—Cu1—Cu1i131.42 (10)N3—C1—H1123.0
N2ii—Cu1—Cu1i131.42 (10)N3—C2—N1111.7 (4)
O2'—Cl1—O2'iii124 (3)N3—C2—H2124.2
O2'—Cl1—O3iii127 (2)N1—C2—H2124.2
O2'iii—Cl1—O3iii76.9 (12)N1—C3—C4110.8 (3)
O2'—Cl1—O376.9 (12)N1—C3—H3A109.5
O2'iii—Cl1—O3127 (2)C4—C3—H3A109.5
O3iii—Cl1—O3133 (4)N1—C3—H3B109.5
O2'—Cl1—O3'110.0 (11)C4—C3—H3B109.5
O2'iii—Cl1—O3'105.2 (13)H3A—C3—H3B108.1
O3iii—Cl1—O3'109 (3)O1—C4—C5110.2 (4)
O3—Cl1—O3'33.1 (6)O1—C4—C3iv107.8 (3)
O2'—Cl1—O3'iii105.2 (13)C5—C4—C3iv111.1 (3)
O2'iii—Cl1—O3'iii110.0 (11)O1—C4—C3107.8 (3)
O3iii—Cl1—O3'iii33.1 (6)C5—C4—C3111.1 (3)
O3—Cl1—O3'iii109 (3)C3iv—C4—C3108.6 (4)
O3'—Cl1—O3'iii100 (2)C10—C5—C6114.8 (6)
O2'—Cl1—O228 (2)C10—C5—C4122.6 (5)
O2'iii—Cl1—O2106.2 (16)C6—C5—C4122.6 (6)
O3iii—Cl1—O2104.1 (11)C7—C6—F1118.0 (7)
O3—Cl1—O2105.3 (11)C7—C6—C5124.1 (7)
O3'—Cl1—O2138.4 (14)F1—C6—C5117.8 (6)
O3'iii—Cl1—O294.2 (13)C8—C7—C6118.0 (7)
O2'—Cl1—O2iii106.2 (16)C8—C7—H7121.0
O2'iii—Cl1—O2iii28 (2)C6—C7—H7121.0
O3iii—Cl1—O2iii105.3 (11)C7—C8—C9122.2 (7)
O3—Cl1—O2iii104.1 (11)C7—C8—F2118.8 (8)
O3'—Cl1—O2iii94.2 (13)C9—C8—F2119.0 (8)
O3'iii—Cl1—O2iii138.4 (14)C8—C9—C10119.5 (7)
O2—Cl1—O2iii101 (2)C8—C9—H9120.2
C2—N1—N2108.2 (3)C10—C9—H9120.2
C2—N1—C3131.3 (4)C5—C10—C9121.4 (6)
N2—N1—C3120.3 (3)C5—C10—H10119.3
C1—N2—N1103.3 (3)C9—C10—H10119.3
C2—N1—N2—C1−0.3 (4)Cu1—O1—C4—C5−99.6 (3)
C3—N1—N2—C1−176.2 (4)Cu1i—O1—C4—C3iv−21.8 (5)
C2—N1—N2—Cu1163.9 (3)Cu1—O1—C4—C3iv138.9 (3)
C3—N1—N2—Cu1−12.0 (5)Cu1i—O1—C4—C3−138.9 (3)
O1i—Cu1—N2—C1121.8 (9)Cu1—O1—C4—C321.8 (5)
O1—Cu1—N2—C1135.0 (4)N1—C3—C4—O1−65.7 (4)
N2ii—Cu1—N2—C1−46.9 (4)N1—C3—C4—C555.2 (5)
Cu1i—Cu1—N2—C1133.1 (4)N1—C3—C4—C3iv177.8 (2)
O1i—Cu1—N2—N1−37.0 (10)O1—C4—C5—C100.0
O1—Cu1—N2—N1−23.8 (3)C3iv—C4—C5—C10119.5 (3)
N2ii—Cu1—N2—N1154.3 (3)C3—C4—C5—C10−119.5 (3)
Cu1i—Cu1—N2—N1−25.7 (3)O1—C4—C5—C6180.0
O1i—Cu1—O1—C4−164.6 (5)C3iv—C4—C5—C6−60.5 (3)
N2—Cu1—O1—C417.6 (4)C3—C4—C5—C660.5 (3)
N2ii—Cu1—O1—C4−151.2 (8)C10—C5—C6—C70.0
Cu1i—Cu1—O1—C4−164.6 (5)C4—C5—C6—C7180.0
O1i—Cu1—O1—Cu1i0.0C10—C5—C6—F1180.0
N2—Cu1—O1—Cu1i−177.77 (17)C4—C5—C6—F10.0
N2ii—Cu1—O1—Cu1i13.5 (10)F1—C6—C7—C8180.0
N1—N2—C1—N3−0.3 (5)C5—C6—C7—C80.0
Cu1—N2—C1—N3−161.8 (3)C6—C7—C8—C90.0
C2—N3—C1—N20.8 (6)C6—C7—C8—F2180.0
C1—N3—C2—N1−0.9 (6)C7—C8—C9—C100.0
N2—N1—C2—N30.8 (5)F2—C8—C9—C10180.0
C3—N1—C2—N3176.1 (4)C6—C5—C10—C90.0
C2—N1—C3—C4−110.2 (5)C4—C5—C10—C9180.0
N2—N1—C3—C464.5 (5)C8—C9—C10—C50.0
Cu1i—O1—C4—C599.6 (3)
  4 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.  Crystal structure, magnetic properties, and 57Fe Mössbauer spectroscopy of the two-dimensional coordination polymers [M(1,2-bis(1,2,4-triazol-4-yl)ethane)2(NCS)2] (MII = Fe, Co).

Authors:  Yann Garcia; Georges Bravic; Christine Gieck; Daniel Chasseau; Wolfgang Tremel; Philipp Gütlich
Journal:  Inorg Chem       Date:  2005-12-26       Impact factor: 5.165

3.  Different oxidation states of copper(I, I/II, II) thiocyanate complexes containing 1,2,4-triazole as a bridging ligand: syntheses, crystal structures, and magnetic properties of 2-D polymer Cu I(admtrz)SCN, linear trinuclear [CuI2CuII(admtrz)6(SCN)2](ClO4)2, and triangular trinuclear [CuII3(admtrz)4(SCN)3(mu3-OH)(H2O)](ClO4)2.H2O (admtrz = 4-amino-3,5-dimethyl-1,2,4-triazole).

Authors:  Jia-Cheng Liu; Guo-Cong Guo; Jin-Shun Huang; Xiao-Zeng You
Journal:  Inorg Chem       Date:  2003-01-13       Impact factor: 5.165

4.  Novel triazole-bridged cadmium coordination polymers varying from zero- to three-dimensionality.

Authors:  Long Yi; Bin Ding; Bin Zhao; Peng Cheng; Dai-Zheng Liao; Shi-Ping Yan; Zong-Hui Jiang
Journal:  Inorg Chem       Date:  2004-01-12       Impact factor: 5.165
  4 in total

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