Literature DB >> 21201309

Aqua-bis(2-chloro-acetato-κO)(1,10-phenanthroline-κN,N')copper(II).

Rongdong Yang1, Yanfei Li, Junshan Sun, Jikun Li, Changqing Chu.   

Abstract

In the title complex, [Cu(C(2)H(2)ClO(2))(2)(C(12)H(8)N(2))(H(2)O)], the Cu(II) ion is five-coordinated by two N atoms [Cu-N = 2.005 (2) and 2.029 (2) Å] from the 1,10-phenanthroline ligand, two O atoms [Cu-O = 1.943 (2)-1.966 (2) Å] from two 2-chloro-acetate ligands and one water mol-ecule [Cu-O = 2.253 (2) Å] in a distorted square-pyramidal geometry. The crystal structure exhibits inter-molecular O-H⋯O hydrogen bonds, short Cl⋯Cl contacts [3.334 (1) Å] and π-π inter-actions [centroid-centroid distance 3.621 (11) Å].

Entities:  

Year:  2008        PMID： 21201309      PMCID： PMC2960263          DOI： 10.1107/S1600536808000044

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


Related literature

For related crystal structures, see: Sieroń (2007 ▶); Czylkowska et al. (2004 ▶); Chen et al. (1996 ▶); Overgaard et al. (2003 ▶).

Experimental

Crystal data

[Cu(C2H2ClO2)2(C12H8N2)(H2O)] M = 448.73 Triclinic, a = 8.7730 (6) Å b = 9.2382 (7) Å c = 11.4492 (8) Å α = 96.2180 (10)° β = 106.6760 (10)° γ = 97.9190 (10)° V = 869.66 (11) Å3 Z = 2 Mo Kα radiation μ = 1.59 mm−1 T = 273 (2) K 0.38 × 0.25 × 0.19 mm

Data collection

Bruker SMART CCD area detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.583, T max = 0.752 4610 measured reflections 3057 independent reflections 2837 reflections with I > 2σ(I) R int = 0.015

Refinement

R[F 2 > 2σ(F 2)] = 0.026 wR(F 2) = 0.074 S = 1.00 3057 reflections 235 parameters 3 restraints H-atom parameters constrained Δρmax = 0.30 e Å−3 Δρmin = −0.29 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, 1997 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808000044/cv2370sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808000044/cv2370Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cu(C2H2ClO2)2(C12H8N2)(H2O)]Z = 2
Mr = 448.73F000 = 454
Triclinic, P1Dx = 1.714 Mg m−3
a = 8.7730 (6) ÅMo Kα radiation λ = 0.71073 Å
b = 9.2382 (7) ÅCell parameters from 3430 reflections
c = 11.4492 (8) Åθ = 2.5–28.2º
α = 96.2180 (10)ºµ = 1.59 mm−1
β = 106.6760 (10)ºT = 273 (2) K
γ = 97.9190 (10)ºBlock, blue
V = 869.66 (11) Å30.38 × 0.25 × 0.19 mm
Bruker SMART CCD area detector diffractometer3057 independent reflections
Radiation source: fine-focus sealed tube2837 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.015
T = 273(2) Kθmax = 25.1º
phi and ω scansθmin = 1.9º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)h = −10→10
Tmin = 0.583, Tmax = 0.752k = −8→10
4610 measured reflectionsl = −13→13
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.026H-atom parameters constrained
wR(F2) = 0.074  w = 1/[σ2(Fo2) + (0.043P)2 + 0.4807P] where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max = 0.001
3057 reflectionsΔρmax = 0.30 e Å−3
235 parametersΔρmin = −0.29 e Å−3
3 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods
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
Cu10.23816 (3)0.68495 (3)0.71095 (2)0.03304 (10)
Cl1−0.22927 (8)0.98116 (9)0.83337 (8)0.0671 (2)
Cl20.40479 (7)0.93989 (7)0.62804 (6)0.04661 (16)
O10.14841 (19)0.84228 (17)0.77963 (15)0.0421 (4)
O2−0.1084 (2)0.7271 (2)0.7366 (2)0.0635 (5)
O30.11593 (19)0.68927 (16)0.53849 (14)0.0408 (4)
O40.0053 (2)0.7855 (2)0.37496 (17)0.0622 (5)
O50.06637 (19)0.50494 (17)0.74928 (15)0.0430 (4)
H150.03120.41800.70910.052*
H16−0.01230.55170.73850.052*
N10.4251 (2)0.70913 (19)0.86886 (16)0.0328 (4)
N20.3550 (2)0.53104 (19)0.65745 (16)0.0334 (4)
C10.0003 (3)0.8353 (2)0.77567 (19)0.0365 (5)
C2−0.0300 (3)0.9841 (3)0.8242 (2)0.0400 (5)
H2A−0.00991.05430.77080.048*
H2B0.04641.01890.90570.048*
C30.1023 (3)0.7947 (2)0.4784 (2)0.0366 (5)
C40.2075 (3)0.9464 (3)0.5315 (2)0.0488 (6)
H4A0.15391.00310.57880.059*
H4B0.21710.99810.46390.059*
C50.4552 (3)0.7987 (3)0.9743 (2)0.0404 (5)
H5A0.38510.86400.98050.049*
C60.5887 (3)0.7988 (3)1.0767 (2)0.0486 (6)
H60.60710.86421.14900.058*
C70.6915 (3)0.7028 (3)1.0699 (2)0.0469 (6)
H70.77970.70141.13800.056*
C80.6639 (3)0.6057 (3)0.9596 (2)0.0388 (5)
C90.7622 (3)0.4983 (3)0.9421 (2)0.0479 (6)
H90.85210.49111.00670.057*
C100.7268 (3)0.4079 (3)0.8339 (3)0.0477 (6)
H100.79340.34010.82490.057*
C110.5883 (3)0.4140 (2)0.7322 (2)0.0387 (5)
C120.5395 (3)0.3200 (3)0.6177 (2)0.0453 (6)
H120.60110.25000.60280.054*
C130.4019 (3)0.3317 (3)0.5290 (2)0.0460 (6)
H130.36880.26900.45370.055*
C140.3111 (3)0.4378 (2)0.5512 (2)0.0390 (5)
H140.21680.44390.49010.047*
C150.4909 (2)0.5181 (2)0.74641 (19)0.0319 (4)
C160.5289 (2)0.6148 (2)0.86151 (19)0.0317 (4)
U11U22U33U12U13U23
Cu10.03296 (16)0.03095 (16)0.03298 (16)0.00803 (11)0.00661 (11)0.00203 (10)
Cl10.0439 (4)0.0748 (5)0.0858 (5)0.0241 (3)0.0227 (3)0.0012 (4)
Cl20.0413 (3)0.0447 (3)0.0484 (3)−0.0015 (2)0.0122 (3)−0.0006 (3)
O10.0360 (8)0.0378 (8)0.0516 (9)0.0094 (7)0.0135 (7)−0.0010 (7)
O20.0409 (10)0.0442 (10)0.0972 (16)0.0042 (8)0.0163 (10)−0.0071 (10)
O30.0474 (9)0.0287 (8)0.0373 (8)0.0040 (7)−0.0002 (7)0.0058 (6)
O40.0747 (13)0.0462 (10)0.0453 (10)0.0019 (9)−0.0113 (9)0.0129 (8)
O50.0435 (9)0.0342 (8)0.0493 (9)0.0040 (7)0.0130 (7)0.0051 (7)
N10.0344 (9)0.0302 (9)0.0328 (9)0.0031 (7)0.0105 (7)0.0032 (7)
N20.0359 (9)0.0312 (9)0.0328 (9)0.0052 (7)0.0109 (8)0.0037 (7)
C10.0357 (12)0.0380 (12)0.0352 (11)0.0099 (10)0.0078 (9)0.0069 (9)
C20.0376 (12)0.0416 (12)0.0415 (12)0.0122 (10)0.0117 (10)0.0041 (10)
C30.0399 (12)0.0330 (11)0.0340 (11)0.0085 (9)0.0069 (9)0.0025 (9)
C40.0540 (15)0.0334 (12)0.0501 (14)0.0061 (11)0.0024 (12)0.0077 (10)
C50.0457 (13)0.0362 (12)0.0372 (12)0.0049 (10)0.0129 (10)−0.0011 (9)
C60.0548 (15)0.0482 (14)0.0327 (12)−0.0027 (12)0.0063 (11)−0.0022 (10)
C70.0418 (13)0.0490 (14)0.0390 (12)−0.0038 (11)−0.0005 (10)0.0114 (11)
C80.0344 (11)0.0398 (12)0.0409 (12)0.0010 (9)0.0090 (9)0.0142 (10)
C90.0337 (12)0.0546 (15)0.0570 (15)0.0110 (11)0.0099 (11)0.0230 (12)
C100.0400 (13)0.0467 (14)0.0657 (16)0.0188 (11)0.0217 (12)0.0192 (12)
C110.0396 (12)0.0326 (11)0.0516 (13)0.0075 (9)0.0231 (10)0.0129 (10)
C120.0530 (15)0.0319 (12)0.0609 (15)0.0109 (10)0.0316 (13)0.0060 (10)
C130.0582 (15)0.0329 (12)0.0474 (14)0.0002 (11)0.0247 (12)−0.0048 (10)
C140.0436 (12)0.0339 (11)0.0363 (11)0.0008 (9)0.0121 (10)0.0005 (9)
C150.0326 (11)0.0288 (10)0.0370 (11)0.0040 (8)0.0145 (9)0.0080 (8)
C160.0302 (10)0.0313 (10)0.0341 (11)0.0024 (8)0.0107 (9)0.0091 (8)
Cu1—O11.9427 (15)C4—H4A0.9700
Cu1—O31.9657 (15)C4—H4B0.9700
Cu1—N22.0052 (18)C5—C61.399 (3)
Cu1—N12.0294 (18)C5—H5A0.9300
Cu1—O52.2531 (16)C6—C71.361 (4)
Cl1—C21.778 (2)C6—H60.9300
Cl1—Cl2i3.3340 (10)C7—C81.406 (3)
Cl2—C41.779 (3)C7—H70.9300
O1—C11.279 (3)C8—C161.398 (3)
O2—C11.226 (3)C8—C91.435 (3)
O3—C31.251 (3)C9—C101.346 (4)
O4—C31.231 (3)C9—H90.9300
O5—H150.8498C10—C111.434 (3)
O5—H160.8498C10—H100.9300
N1—C51.324 (3)C11—C151.398 (3)
N1—C161.357 (3)C11—C121.408 (3)
N2—C141.336 (3)C12—C131.363 (4)
N2—C151.357 (3)C12—H120.9300
C1—C21.514 (3)C13—C141.392 (3)
C2—H2A0.9700C13—H130.9300
C2—H2B0.9700C14—H140.9300
C3—C41.524 (3)C15—C161.434 (3)
Cl1···Cl2i3.334 (1)Cg1···Cg2ii3.621 (11)
O1—Cu1—O394.93 (7)H4A—C4—H4B107.7
O1—Cu1—N2173.08 (7)N1—C5—C6122.4 (2)
O3—Cu1—N291.04 (7)N1—C5—H5A118.8
O1—Cu1—N191.67 (7)C6—C5—H5A118.8
O3—Cu1—N1160.92 (7)C7—C6—C5119.7 (2)
N2—Cu1—N181.58 (7)C7—C6—H6120.2
O1—Cu1—O593.30 (6)C5—C6—H6120.2
O3—Cu1—O598.18 (6)C6—C7—C8119.7 (2)
N2—Cu1—O589.32 (7)C6—C7—H7120.1
N1—Cu1—O599.28 (7)C8—C7—H7120.1
C1—O1—Cu1125.47 (14)C16—C8—C7116.6 (2)
C3—O3—Cu1130.63 (14)C16—C8—C9118.6 (2)
Cu1—O5—H15127.2C7—C8—C9124.8 (2)
Cu1—O5—H1695.7C10—C9—C8121.3 (2)
H15—O5—H16108.2C10—C9—H9119.3
C5—N1—C16117.97 (19)C8—C9—H9119.3
C5—N1—Cu1129.49 (16)C9—C10—C11121.2 (2)
C16—N1—Cu1112.52 (13)C9—C10—H10119.4
C14—N2—C15118.05 (19)C11—C10—H10119.4
C14—N2—Cu1128.50 (16)C15—C11—C12116.5 (2)
C15—N2—Cu1113.32 (13)C15—C11—C10118.7 (2)
O2—C1—O1127.3 (2)C12—C11—C10124.8 (2)
O2—C1—C2121.8 (2)C13—C12—C11119.9 (2)
O1—C1—C2110.88 (19)C13—C12—H12120.0
C1—C2—Cl1113.88 (16)C11—C12—H12120.0
C1—C2—H2A108.8C12—C13—C14119.9 (2)
Cl1—C2—H2A108.8C12—C13—H13120.0
C1—C2—H2B108.8C14—C13—H13120.0
Cl1—C2—H2B108.8N2—C14—C13122.0 (2)
H2A—C2—H2B107.7N2—C14—H14119.0
O4—C3—O3123.8 (2)C13—C14—H14119.0
O4—C3—C4115.3 (2)N2—C15—C11123.6 (2)
O3—C3—C4120.9 (2)N2—C15—C16116.28 (18)
C3—C4—Cl2113.92 (17)C11—C15—C16120.1 (2)
C3—C4—H4A108.8N1—C16—C8123.6 (2)
Cl2—C4—H4A108.8N1—C16—C15116.28 (18)
C3—C4—H4B108.8C8—C16—C15120.1 (2)
Cl2—C4—H4B108.8
O3—Cu1—O1—C165.71 (18)C5—C6—C7—C80.8 (4)
N2—Cu1—O1—C1−144.9 (5)C6—C7—C8—C160.0 (3)
N1—Cu1—O1—C1−132.21 (18)C6—C7—C8—C9−179.0 (2)
O5—Cu1—O1—C1−32.81 (18)C16—C8—C9—C100.2 (3)
O1—Cu1—O3—C352.0 (2)C7—C8—C9—C10179.2 (2)
N2—Cu1—O3—C3−124.4 (2)C8—C9—C10—C11−0.7 (4)
N1—Cu1—O3—C3−57.7 (3)C9—C10—C11—C151.0 (3)
O5—Cu1—O3—C3146.1 (2)C9—C10—C11—C12−177.6 (2)
O1—Cu1—N1—C52.6 (2)C15—C11—C12—C13−1.2 (3)
O3—Cu1—N1—C5112.9 (2)C10—C11—C12—C13177.4 (2)
N2—Cu1—N1—C5−178.9 (2)C11—C12—C13—C140.7 (4)
O5—Cu1—N1—C5−91.01 (19)C15—N2—C14—C13−1.5 (3)
O1—Cu1—N1—C16−179.12 (14)Cu1—N2—C14—C13−177.15 (17)
O3—Cu1—N1—C16−68.8 (3)C12—C13—C14—N20.7 (4)
N2—Cu1—N1—C16−0.65 (14)C14—N2—C15—C110.9 (3)
O5—Cu1—N1—C1687.26 (14)Cu1—N2—C15—C11177.24 (16)
O1—Cu1—N2—C14−170.8 (5)C14—N2—C15—C16−176.64 (18)
O3—Cu1—N2—C14−21.29 (19)Cu1—N2—C15—C16−0.3 (2)
N1—Cu1—N2—C14176.37 (19)C12—C11—C15—N20.4 (3)
O5—Cu1—N2—C1476.88 (19)C10—C11—C15—N2−178.3 (2)
O1—Cu1—N2—C1513.4 (6)C12—C11—C15—C16177.90 (19)
O3—Cu1—N2—C15162.87 (14)C10—C11—C15—C16−0.8 (3)
N1—Cu1—N2—C150.53 (14)C5—N1—C16—C81.0 (3)
O5—Cu1—N2—C15−98.96 (14)Cu1—N1—C16—C8−177.50 (16)
Cu1—O1—C1—O25.6 (3)C5—N1—C16—C15179.16 (18)
Cu1—O1—C1—C2−172.99 (14)Cu1—N1—C16—C150.7 (2)
O2—C1—C2—Cl16.1 (3)C7—C8—C16—N1−1.0 (3)
O1—C1—C2—Cl1−175.31 (16)C9—C8—C16—N1178.1 (2)
Cu1—O3—C3—O4−170.39 (19)C7—C8—C16—C15−179.08 (19)
Cu1—O3—C3—C49.1 (3)C9—C8—C16—C150.0 (3)
O4—C3—C4—Cl2−147.4 (2)N2—C15—C16—N1−0.2 (3)
O3—C3—C4—Cl233.1 (3)C11—C15—C16—N1−177.89 (18)
C16—N1—C5—C6−0.1 (3)N2—C15—C16—C8178.01 (18)
Cu1—N1—C5—C6178.14 (17)C11—C15—C16—C80.3 (3)
N1—C5—C6—C7−0.8 (4)
D—H···AD—HH···AD···AD—H···A
O5—H15···O4iii0.851.962.796 (2)169
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O5—H15⋯O4i0.851.962.796 (2)169

Symmetry code: (i) .

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