Download citation
Download citation
link to html
The title mol­ecule, [Cu2(H2N2O2)4(H2O)2], possesses a center of symmetry and contains two almost planar eight-membered central rings which are nearly normal to each other. Molecules are linked by O—H...O hydrogen bonds to form a three-dimensional network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803013217/lh6072sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803013217/lh6072Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](N-N) = 0.007 Å
  • R factor = 0.051
  • wR factor = 0.110
  • Data-to-parameter ratio = 16.2

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 28.29 From the CIF: _reflns_number_total 1624 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 1736 Completeness (_total/calc) 93.55% Alert C: < 95% complete PLAT_420 Alert C D-H Without Acceptor N2 - H20 ... ? PLAT_420 Alert C D-H Without Acceptor N2 - H21 ... ? PLAT_420 Alert C D-H Without Acceptor N4 - H40 ... ? PLAT_420 Alert C D-H Without Acceptor N4 - H41 ... ?
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
5 Alert Level C = Please check

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens,1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: PARST (Nardelli, 1995) and WinGX publication routines (Farrugia, 1999).

Tetra-µ-nitroamine-bis[aquacopper(II)] top
Crystal data top
[Cu2(H2N2O2)4(H2O)2]F(000) = 824
Mr = 409.26Dx = 1.952 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 2792 reflections
a = 13.1677 (18) Åθ = 5.8–56.5°
b = 8.5716 (12) ŵ = 3.12 mm1
c = 13.8499 (19) ÅT = 293 K
β = 117.024 (2)°Slab, blue
V = 1392.5 (3) Å30.36 × 0.28 × 0.22 mm
Z = 4
Data collection top
Siemens SMART CCD area-detector
diffractometer
1624 independent reflections
Radiation source: fine-focus sealed tube1391 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.030
Detector resolution: 8.33 pixels mm-1θmax = 28.3°, θmin = 3.0°
ω scansh = 1717
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 1111
Tmin = 0.368, Tmax = 0.504l = 1418
3874 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.051H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.110 w = 1/[σ2(Fo2) + (0.0377P)2 + 5.3609P]
where P = (Fo2 + 2Fc2)/3
S = 1.29(Δ/σ)max < 0.001
1624 reflectionsΔρmax = 0.55 e Å3
100 parametersΔρmin = 0.63 e Å3
0 restraintsExtinction correction: SHELXL97, FC*=KFC[1+0.001XFC2Λ3/SIN(2Θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0022 (5)
Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Refinement. Refinement on F2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating -R-factor-obs 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu10.04995 (4)0.58403 (6)0.45508 (4)0.0158 (2)
O10.0954 (3)0.3795 (4)0.4257 (3)0.0275 (10)
O20.0080 (3)0.7644 (4)0.4998 (3)0.0297 (10)
O30.1837 (2)0.5889 (4)0.6004 (2)0.0252 (8)
O40.1004 (2)0.5600 (4)0.3244 (2)0.0249 (9)
O50.1246 (3)0.7082 (5)0.3673 (3)0.0335 (11)
N10.0670 (3)0.2525 (6)0.4494 (3)0.0350 (14)
N20.1035 (4)0.1046 (6)0.4155 (4)0.0487 (17)
N30.1828 (3)0.5214 (5)0.6807 (3)0.0293 (11)
N40.2837 (4)0.5355 (7)0.7875 (4)0.0517 (16)
H200.143200.109100.380500.0590*
H210.084700.015600.431200.0590*
H400.341600.589200.794000.0620*
H410.284400.490100.843200.0620*
H500.179 (5)0.762 (8)0.381 (5)0.041 (17)*
H510.109 (4)0.676 (7)0.314 (4)0.022 (14)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0122 (2)0.0191 (3)0.0157 (3)0.0014 (2)0.0059 (2)0.0004 (2)
O10.0274 (15)0.0230 (17)0.0369 (18)0.0002 (12)0.0187 (14)0.0054 (13)
O20.0306 (16)0.0233 (17)0.0387 (17)0.0036 (13)0.0188 (15)0.0044 (14)
O30.0187 (13)0.0344 (16)0.0215 (14)0.0020 (13)0.0083 (11)0.0016 (13)
O40.0167 (13)0.0323 (18)0.0205 (14)0.0061 (12)0.0038 (11)0.0031 (12)
O50.040 (2)0.042 (2)0.0277 (18)0.0204 (17)0.0235 (16)0.0115 (16)
N10.0223 (19)0.043 (3)0.038 (2)0.0016 (17)0.0122 (17)0.0062 (19)
N20.053 (3)0.038 (3)0.061 (3)0.006 (2)0.031 (3)0.017 (2)
N30.0239 (18)0.032 (2)0.030 (2)0.0026 (16)0.0106 (16)0.0009 (17)
N40.037 (2)0.070 (4)0.036 (2)0.018 (2)0.006 (2)0.005 (2)
Geometric parameters (Å, º) top
Cu1—O11.954 (4)O5—H510.72 (5)
Cu1—O21.946 (4)O5—H500.80 (7)
Cu1—O31.983 (3)N1—N21.505 (7)
Cu1—O41.995 (3)N3—N41.477 (6)
Cu1—O52.159 (4)N2—H200.8602
O1—N11.243 (6)N2—H210.8599
O2—N1i1.271 (6)N4—H400.8596
O3—N31.258 (5)N4—H410.8603
O4—N3i1.265 (5)
O1—Cu1—O2168.72 (17)Cu1—O5—H50138 (4)
O1—Cu1—O390.88 (15)Cu1—O5—H51113 (5)
O1—Cu1—O489.43 (15)O2i—N1—N2116.0 (4)
O1—Cu1—O593.68 (17)O1—N1—O2i125.4 (5)
O2—Cu1—O387.48 (15)O1—N1—N2118.6 (4)
O2—Cu1—O489.99 (15)O3—N3—O4i123.8 (4)
O2—Cu1—O597.60 (16)O4i—N3—N4117.4 (4)
O3—Cu1—O4168.61 (12)O3—N3—N4118.8 (4)
O3—Cu1—O598.02 (14)N1—N2—H20120.01
O4—Cu1—O593.33 (14)N1—N2—H21119.94
Cu1—O1—N1125.0 (4)H20—N2—H21120.05
Cu1—O2—N1i120.8 (3)N3—N4—H40120.01
Cu1—O3—N3121.8 (3)N3—N4—H41119.95
Cu1—O4—N3i125.5 (2)H40—N4—H41120.04
H50—O5—H51106 (6)
O3—Cu1—O1—N188.4 (4)O5—Cu1—O4—N3i172.0 (4)
O4—Cu1—O1—N180.2 (4)Cu1—O1—N1—N2176.5 (3)
O5—Cu1—O1—N1173.5 (4)Cu1—O1—N1—Cu1i2.0 (3)
O3—Cu1—O2—N1i86.5 (4)Cu1—O1—N1—O2i3.0 (6)
O4—Cu1—O2—N1i82.4 (4)Cu1—O2—N1i—N2i177.9 (3)
O5—Cu1—O2—N1i175.8 (3)Cu1—O2—N1i—O1i1.7 (6)
O1—Cu1—O3—N382.6 (3)Cu1—O3—N3—N4177.4 (3)
O2—Cu1—O3—N386.3 (3)Cu1—O3—N3—Cu1i0.0 (3)
O5—Cu1—O3—N3176.4 (3)Cu1—O3—N3—O4i3.2 (6)
O1—Cu1—O4—N3i78.3 (4)Cu1—O4—N3i—O3i5.9 (6)
O2—Cu1—O4—N3i90.4 (4)Cu1—O4—N3i—N4i174.8 (3)
Symmetry code: (i) x, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H50···O3ii0.80 (7)2.13 (7)2.928 (5)174 (6)
O5—H51···O4iii0.72 (5)2.12 (5)2.828 (5)167 (6)
Symmetry codes: (ii) x+1/2, y+3/2, z+1; (iii) x, y, z+1/2.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds