Literature DB >> 21753980

(Acetato-κO)bis-(1,10-phenanthroline-κN,N')copper(II) acetate hepta-hydrate.

Buqin Jing, Lianzhi Li, Jianfang Dong, Tao Xu.   

Abstract

In the title complex, [Cu(CH(3)CO(2))(C(12)H(8)N(2))(2)](CH(3)CO(2))·7H(2)O, the central Cu(II) ion is five coordinate, being bound to four N atoms from two 1,10-phenanthroline ligands and one O atom from an acetate anion in a strongly distorted square-pyramidal configuration. Hydrogen-bonded water mol-ecules and an uncoordinated acetate anion form a two-dimensional polymeric structure parallel to (010). The cations are linked to this layer via O-H⋯O hydrogen bonds between one of the water mol-ecules and the coordinated acetate anion.

Entities:  

Year:  2011        PMID: 21753980      PMCID: PMC3099845          DOI: 10.1107/S1600536811009676

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


Related literature

For the structures of similar five-coordinate copper(II) complexes with 1,10-phenanthroline and carboxyl­ate anions, see: Tu et al. (2008 ▶); Xu et al. (2008 ▶).

Experimental

Crystal data

[Cu(C2H3O2)(C12H8N2)2](C2H3O2)·7H2O M = 668.15 Triclinic, a = 8.764 (4) Å b = 12.307 (5) Å c = 15.739 (7) Å α = 103.257 (7)° β = 102.243 (7)° γ = 97.606 (7)° V = 1585.2 (12) Å3 Z = 2 Mo Kα radiation μ = 0.75 mm−1 T = 298 K 0.42 × 0.38 × 0.32 mm

Data collection

Bruker SMART 1000 CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.728, T max = 0.795 8364 measured reflections 5570 independent reflections 3220 reflections with I > 2σ(I) R int = 0.040

Refinement

R[F 2 > 2σ(F 2)] = 0.057 wR(F 2) = 0.130 S = 0.95 5570 reflections 399 parameters 52 restraints H-atom parameters constrained Δρmax = 0.42 e Å−3 Δρmin = −0.52 e Å−3 Data collection: SMART (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); 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 ▶) and DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536811009676/gk2351sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536811009676/gk2351Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cu(C2H3O2)(C12H8N2)2](C2H3O2)·7H2OZ = 2
Mr = 668.15F(000) = 698
Triclinic, P1Dx = 1.400 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.764 (4) ÅCell parameters from 1605 reflections
b = 12.307 (5) Åθ = 2.5–25.0°
c = 15.739 (7) ŵ = 0.75 mm1
α = 103.257 (7)°T = 298 K
β = 102.243 (7)°Block, blue
γ = 97.606 (7)°0.42 × 0.38 × 0.32 mm
V = 1585.2 (12) Å3
Bruker SMART 1000 CCD area-detector diffractometer5570 independent reflections
Radiation source: fine-focus sealed tube3220 reflections with I > 2σ(I)
graphiteRint = 0.040
φ and ω scansθmax = 25.1°, θmin = 1.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −10→10
Tmin = 0.728, Tmax = 0.795k = −13→14
8364 measured reflectionsl = −18→18
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.057Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.130H-atom parameters constrained
S = 0.95w = 1/[σ2(Fo2) + (0.0503P)2] where P = (Fo2 + 2Fc2)/3
5570 reflections(Δ/σ)max = 0.001
399 parametersΔρmax = 0.42 e Å3
52 restraintsΔρmin = −0.51 e Å3
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*/Ueq
Cu10.76867 (7)0.90326 (4)0.21867 (3)0.0411 (2)
N10.8381 (5)0.7950 (3)0.2885 (2)0.0428 (9)
N20.9810 (4)1.0118 (3)0.3166 (2)0.0410 (9)
N30.7103 (4)1.0131 (3)0.1481 (2)0.0363 (9)
N40.8395 (4)0.8328 (3)0.1056 (2)0.0416 (9)
O10.6008 (4)0.9292 (3)0.28563 (19)0.0505 (8)
O20.4739 (4)0.7876 (3)0.1694 (2)0.0558 (9)
O30.2159 (5)0.5069 (3)0.4746 (2)0.0872 (13)
O40.2102 (5)0.4656 (3)0.3301 (2)0.0790 (11)
O50.3093 (5)0.6651 (3)0.6385 (2)0.0866 (12)
H300.22140.65610.65320.104*
H290.26900.61670.58790.104*
O60.5986 (5)0.6653 (3)0.7512 (2)0.1047 (14)
H310.50880.66170.71600.126*
H320.65650.63120.72130.126*
O70.0874 (4)0.5649 (3)0.1938 (2)0.0842 (12)
H330.12810.52700.22860.101*
H340.14980.56610.15930.101*
O80.2819 (4)0.5844 (3)0.0791 (2)0.0719 (10)
H360.33550.64980.10920.086*
H350.27770.58160.02420.086*
O90.4959 (5)0.4446 (3)0.1306 (3)0.1239 (17)
H370.43550.48790.11280.149*
H380.49110.42270.17750.149*
O100.9190 (4)0.3319 (3)0.2593 (2)0.0804 (11)
H391.00880.37100.29100.096*
H400.89640.36890.22030.096*
O110.7928 (4)0.4387 (3)0.1067 (2)0.0795 (11)
H410.87930.48520.13450.095*
H420.70330.45350.11330.095*
C10.4791 (6)0.8554 (4)0.2423 (3)0.0450 (11)
C20.3383 (6)0.8525 (4)0.2816 (3)0.0719 (14)
H2A0.30630.92500.28950.108*
H2B0.36590.83580.33900.108*
H2C0.25230.79470.24170.108*
C30.7640 (6)0.6890 (4)0.2752 (3)0.0536 (13)
H30.67610.65880.22630.064*
C40.8123 (7)0.6213 (4)0.3313 (4)0.0638 (15)
H4A0.75740.54730.31980.077*
C50.9388 (8)0.6633 (4)0.4023 (4)0.0655 (16)
H50.97100.61850.44040.079*
C61.0229 (6)0.7751 (4)0.4193 (3)0.0484 (13)
C70.9670 (5)0.8385 (3)0.3599 (3)0.0383 (11)
C81.0420 (5)0.9535 (4)0.3748 (3)0.0398 (11)
C91.1722 (6)1.0032 (4)0.4485 (3)0.0531 (13)
C101.2401 (7)1.1171 (5)0.4607 (4)0.0696 (16)
H101.32701.15320.50890.084*
C111.1784 (7)1.1743 (4)0.4018 (4)0.0665 (15)
H111.22291.24980.40920.080*
C121.0484 (6)1.1193 (4)0.3305 (3)0.0528 (13)
H121.00681.15960.29070.063*
C131.1577 (7)0.8286 (5)0.4935 (3)0.0684 (17)
H131.19700.78690.53280.082*
C141.2290 (7)0.9368 (5)0.5082 (3)0.0670 (16)
H141.31590.96900.55730.080*
C150.6447 (5)1.1026 (3)0.1717 (3)0.0456 (12)
H150.62231.11930.22790.055*
C160.6083 (6)1.1721 (4)0.1156 (3)0.0523 (13)
H160.56151.23400.13430.063*
C170.6403 (6)1.1505 (4)0.0338 (3)0.0513 (13)
H170.61561.1970−0.00420.062*
C180.7112 (5)1.0573 (4)0.0067 (3)0.0425 (11)
C190.7425 (5)0.9900 (3)0.0663 (3)0.0355 (10)
C200.8106 (5)0.8918 (3)0.0430 (3)0.0375 (10)
C210.8427 (5)0.8604 (4)−0.0417 (3)0.0457 (12)
C220.9065 (6)0.7623 (4)−0.0606 (3)0.0626 (14)
H220.92820.7372−0.11640.075*
C230.9369 (6)0.7034 (4)0.0018 (4)0.0639 (15)
H230.98000.6382−0.01070.077*
C240.9030 (6)0.7413 (4)0.0850 (3)0.0532 (13)
H240.92580.70070.12770.064*
C250.7484 (6)1.0250 (4)−0.0786 (3)0.0571 (14)
H250.73021.0693−0.11890.068*
C260.8099 (6)0.9306 (5)−0.1011 (3)0.0595 (14)
H260.83160.9108−0.15740.071*
C270.2707 (7)0.5202 (4)0.4120 (4)0.0613 (14)
C280.4211 (7)0.6073 (5)0.4293 (4)0.091 (2)
H28A0.45250.64860.49190.136*
H28B0.40150.65910.39280.136*
H28C0.50440.56920.41430.136*
U11U22U33U12U13U23
Cu10.0453 (4)0.0407 (3)0.0410 (3)0.0129 (3)0.0110 (3)0.0155 (2)
N10.045 (3)0.038 (2)0.048 (2)0.0089 (18)0.013 (2)0.0147 (18)
N20.046 (3)0.041 (2)0.039 (2)0.0131 (18)0.0132 (19)0.0120 (18)
N30.037 (2)0.036 (2)0.037 (2)0.0099 (17)0.0103 (18)0.0087 (16)
N40.045 (3)0.038 (2)0.043 (2)0.0141 (18)0.0104 (19)0.0107 (18)
O10.050 (2)0.0593 (19)0.0417 (18)0.0101 (16)0.0143 (16)0.0107 (15)
O20.056 (2)0.060 (2)0.0471 (19)0.0071 (16)0.0128 (17)0.0082 (16)
O30.089 (3)0.111 (3)0.068 (3)0.011 (2)0.027 (2)0.034 (2)
O40.065 (3)0.104 (3)0.065 (3)0.014 (2)0.014 (2)0.018 (2)
O50.091 (3)0.095 (3)0.076 (3)0.024 (2)0.019 (2)0.028 (2)
O60.095 (4)0.137 (4)0.075 (3)0.049 (3)0.015 (3)0.005 (3)
O70.075 (3)0.104 (3)0.081 (3)0.006 (2)0.022 (2)0.042 (2)
O80.084 (3)0.063 (2)0.060 (2)0.001 (2)0.013 (2)0.0097 (18)
O90.092 (4)0.141 (4)0.186 (5)0.059 (3)0.056 (4)0.097 (4)
O100.072 (3)0.074 (2)0.091 (3)0.004 (2)0.005 (2)0.032 (2)
O110.057 (3)0.091 (3)0.078 (3)0.001 (2)0.012 (2)0.011 (2)
C10.044 (3)0.060 (3)0.041 (3)0.016 (2)0.016 (2)0.024 (2)
C20.062 (3)0.092 (3)0.065 (3)0.013 (3)0.028 (3)0.019 (3)
C30.057 (4)0.047 (3)0.063 (3)0.018 (3)0.018 (3)0.021 (3)
C40.081 (5)0.047 (3)0.082 (4)0.027 (3)0.034 (4)0.035 (3)
C50.096 (5)0.068 (4)0.064 (4)0.048 (4)0.040 (4)0.044 (3)
C60.056 (4)0.064 (3)0.041 (3)0.032 (3)0.022 (3)0.025 (3)
C70.042 (3)0.046 (3)0.033 (2)0.017 (2)0.014 (2)0.014 (2)
C80.031 (3)0.057 (3)0.033 (3)0.012 (2)0.013 (2)0.010 (2)
C90.046 (4)0.072 (4)0.040 (3)0.018 (3)0.015 (3)0.006 (3)
C100.052 (4)0.079 (4)0.057 (4)−0.005 (3)0.009 (3)−0.006 (3)
C110.064 (4)0.055 (3)0.068 (4)−0.010 (3)0.017 (3)0.003 (3)
C120.056 (4)0.048 (3)0.054 (3)0.002 (3)0.019 (3)0.012 (3)
C130.078 (5)0.103 (5)0.044 (3)0.054 (4)0.021 (3)0.033 (3)
C140.064 (4)0.096 (4)0.037 (3)0.035 (4)0.005 (3)0.006 (3)
C150.050 (3)0.037 (3)0.046 (3)0.007 (2)0.010 (2)0.006 (2)
C160.053 (4)0.038 (3)0.065 (3)0.014 (2)0.004 (3)0.017 (3)
C170.047 (3)0.046 (3)0.060 (3)0.004 (2)0.001 (3)0.026 (3)
C180.035 (3)0.048 (3)0.042 (3)−0.001 (2)0.004 (2)0.018 (2)
C190.028 (3)0.040 (3)0.036 (3)0.004 (2)0.005 (2)0.011 (2)
C200.025 (3)0.044 (3)0.037 (3)0.000 (2)0.004 (2)0.006 (2)
C210.038 (3)0.053 (3)0.040 (3)0.003 (2)0.010 (2)0.005 (2)
C220.053 (4)0.075 (4)0.055 (3)0.016 (3)0.018 (3)0.002 (3)
C230.056 (4)0.061 (3)0.072 (4)0.024 (3)0.022 (3)−0.001 (3)
C240.050 (3)0.048 (3)0.064 (3)0.018 (2)0.013 (3)0.014 (3)
C250.052 (4)0.076 (4)0.048 (3)0.006 (3)0.009 (3)0.032 (3)
C260.048 (4)0.091 (4)0.042 (3)0.011 (3)0.015 (3)0.022 (3)
C270.053 (4)0.067 (4)0.063 (4)0.019 (3)0.003 (3)0.021 (3)
C280.076 (5)0.088 (4)0.105 (5)−0.005 (4)0.024 (4)0.028 (4)
Cu1—N31.988 (3)C5—H50.9300
Cu1—N11.989 (3)C6—C71.402 (5)
Cu1—O12.001 (3)C6—C131.432 (7)
Cu1—N42.051 (3)C7—C81.423 (6)
Cu1—N22.191 (4)C8—C91.397 (6)
N1—C31.328 (5)C9—C101.401 (6)
N1—C71.360 (5)C9—C141.435 (6)
N2—C121.325 (5)C10—C111.354 (7)
N2—C81.355 (5)C10—H100.9300
N3—C151.324 (5)C11—C121.386 (7)
N3—C191.352 (5)C11—H110.9300
N4—C241.326 (5)C12—H120.9300
N4—C201.354 (5)C13—C141.339 (7)
O1—C11.257 (5)C13—H130.9300
O2—C11.242 (5)C14—H140.9300
O3—C271.218 (6)C15—C161.383 (5)
O4—C271.270 (6)C15—H150.9300
O5—H300.8500C16—C171.351 (6)
O5—H290.8500C16—H160.9300
O6—H310.8501C17—C181.400 (6)
O6—H320.8500C17—H170.9300
O7—H330.8500C18—C191.396 (5)
O7—H340.8500C18—C251.429 (6)
O8—H360.8500C19—C201.425 (5)
O8—H350.8501C20—C211.399 (5)
O9—H370.8500C21—C221.394 (6)
O9—H380.8499C21—C261.424 (6)
O10—H390.8501C22—C231.352 (6)
O10—H400.8499C22—H220.9300
O11—H410.8500C23—C241.393 (6)
O11—H420.8500C23—H230.9300
C1—C21.493 (6)C24—H240.9300
C2—H2A0.9600C25—C261.350 (6)
C2—H2B0.9600C25—H250.9300
C2—H2C0.9600C26—H260.9300
C3—C41.387 (6)C27—C281.516 (7)
C3—H30.9300C28—H28A0.9600
C4—C51.343 (7)C28—H28B0.9600
C4—H4A0.9300C28—H28C0.9600
C5—C61.410 (7)
N3—Cu1—N1177.12 (15)C11—C10—C9119.7 (5)
N3—Cu1—O192.58 (13)C11—C10—H10120.2
N1—Cu1—O189.98 (13)C9—C10—H10120.2
N3—Cu1—N481.55 (13)C10—C11—C12119.4 (5)
N1—Cu1—N496.80 (13)C10—C11—H11120.3
O1—Cu1—N4151.73 (14)C12—C11—H11120.3
N3—Cu1—N298.35 (13)N2—C12—C11122.8 (5)
N1—Cu1—N279.82 (14)N2—C12—H12118.6
O1—Cu1—N2101.51 (13)C11—C12—H12118.6
N4—Cu1—N2106.69 (14)C14—C13—C6122.1 (5)
C3—N1—C7118.4 (4)C14—C13—H13119.0
C3—N1—Cu1125.9 (3)C6—C13—H13119.0
C7—N1—Cu1115.5 (3)C13—C14—C9120.4 (5)
C12—N2—C8118.3 (4)C13—C14—H14119.8
C12—N2—Cu1132.5 (3)C9—C14—H14119.8
C8—N2—Cu1109.0 (3)N3—C15—C16122.3 (4)
C15—N3—C19118.2 (3)N3—C15—H15118.9
C15—N3—Cu1128.0 (3)C16—C15—H15118.9
C19—N3—Cu1113.8 (3)C17—C16—C15120.2 (4)
C24—N4—C20117.6 (4)C17—C16—H16119.9
C24—N4—Cu1131.1 (3)C15—C16—H16119.9
C20—N4—Cu1111.3 (3)C16—C17—C18119.2 (4)
C1—O1—Cu1106.7 (3)C16—C17—H17120.4
H30—O5—H2991.1C18—C17—H17120.4
H31—O6—H32109.2C19—C18—C17117.4 (4)
H33—O7—H34102.8C19—C18—C25118.3 (4)
H36—O8—H35105.8C17—C18—C25124.3 (4)
H37—O9—H38121.0N3—C19—C18122.7 (4)
H39—O10—H40101.1N3—C19—C20116.4 (3)
H41—O11—H42121.7C18—C19—C20121.0 (4)
O2—C1—O1122.1 (4)N4—C20—C21123.4 (4)
O2—C1—C2120.6 (5)N4—C20—C19116.9 (4)
O1—C1—C2117.2 (4)C21—C20—C19119.7 (4)
C1—C2—H2A109.5C22—C21—C20116.6 (4)
C1—C2—H2B109.5C22—C21—C26125.1 (4)
H2A—C2—H2B109.5C20—C21—C26118.2 (4)
C1—C2—H2C109.5C23—C22—C21120.3 (5)
H2A—C2—H2C109.5C23—C22—H22119.9
H2B—C2—H2C109.5C21—C22—H22119.9
N1—C3—C4122.7 (5)C22—C23—C24119.4 (5)
N1—C3—H3118.7C22—C23—H23120.3
C4—C3—H3118.7C24—C23—H23120.3
C5—C4—C3119.6 (5)N4—C24—C23122.6 (4)
C5—C4—H4A120.2N4—C24—H24118.7
C3—C4—H4A120.2C23—C24—H24118.7
C4—C5—C6120.2 (4)C26—C25—C18120.5 (4)
C4—C5—H5119.9C26—C25—H25119.7
C6—C5—H5119.9C18—C25—H25119.7
C7—C6—C5117.0 (5)C25—C26—C21122.3 (4)
C7—C6—C13118.3 (5)C25—C26—H26118.9
C5—C6—C13124.8 (5)C21—C26—H26118.9
N1—C7—C6122.1 (4)O3—C27—O4124.5 (6)
N1—C7—C8117.7 (4)O3—C27—C28120.0 (6)
C6—C7—C8120.1 (4)O4—C27—C28115.6 (5)
N2—C8—C9122.2 (4)C27—C28—H28A109.5
N2—C8—C7117.8 (4)C27—C28—H28B109.5
C9—C8—C7120.0 (4)H28A—C28—H28B109.5
C8—C9—C10117.6 (5)C27—C28—H28C109.5
C8—C9—C14119.2 (5)H28A—C28—H28C109.5
C10—C9—C14123.3 (5)H28B—C28—H28C109.5
C3—C4—C5—C6−0.6 (8)
D—H···AD—HH···AD···AD—H···A
O5—H29···O30.851.902.738 (5)170
O6—H31···O50.851.922.768 (5)176
O7—H33···O40.851.962.797 (5)167
O7—H34···O80.851.912.760 (5)173
O8—H36···O20.851.862.710 (4)173
O9—H37···O80.851.982.826 (5)174
O10—H40···O110.852.233.070 (5)168
O11—H42···O90.851.892.714 (5)164
O5—H30···O10i0.852.032.819 (5)155
O6—H32···O4i0.851.942.778 (5)169
O9—H38···O6i0.851.942.737 (6)156
O10—H39···O4ii0.851.872.702 (5)164
O11—H41···O7ii0.851.882.724 (5)170
O8—H35···O11iii0.851.972.796 (5)165
Table 1

Selected bond lengths (Å)

Cu1—N31.988 (3)
Cu1—N11.989 (3)
Cu1—O12.001 (3)
Cu1—N42.051 (3)
Cu1—N22.191 (4)
Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
O5—H29⋯O30.851.902.738 (5)170
O6—H31⋯O50.851.922.768 (5)176
O7—H33⋯O40.851.962.797 (5)167
O7—H34⋯O80.851.912.760 (5)173
O8—H36⋯O20.851.862.710 (4)173
O9—H37⋯O80.851.982.826 (5)174
O10—H40⋯O110.852.233.070 (5)168
O11—H42⋯O90.851.892.714 (5)164
O5—H30⋯O10i0.852.032.819 (5)155
O6—H32⋯O4i0.851.942.778 (5)169
O9—H38⋯O6i0.851.942.737 (6)156
O10—H39⋯O4ii0.851.872.702 (5)164
O11—H41⋯O7ii0.851.882.724 (5)170
O8—H35⋯O11iii0.851.972.796 (5)165

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

  3 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.  Bis(1,10-phenanthroline-κN,N')(phenyl-acetato-κO)copper(II) phenyl-acetate hexa-hydrate.

Authors:  Bing-Tian Tu; Hong-Zhen Xie; Ying-Tao Ren; Jing-Zhong Chen
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2008-10-31

3.  (Formato-κO)bis-(1,10-phenanthroline-κN,N')copper(II) formate hexa-hydrate.

Authors:  Wei Xu; Jian-Li Lin; Hong-Zhen Xie; Ming Zhang
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2008-11-08
  3 in total
  1 in total

1.  Crystal structure of aqua-bis-(hepta-fluoro-butano-ato-κO)(1,10'-phenanthroline-κ(2) N,N')copper(II).

Authors:  Ibrahim Kani
Journal:  Acta Crystallogr E Crystallogr Commun       Date:  2016-01-01
  1 in total

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