Download citation
Download citation
link to html
The asymmetric unit of the title compound, [Cu2(C2N3)4(H2O)]n, contains two Cu atoms with CuN6 and CuN4O2 chromophores. The Cu atoms lie on inversion centres and the aqua ligands on a crystallographic twofold rotation axis. Two dicyanamide ligands link the metal ions into an infinite three-dimensional structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807015917/sa2040sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807015917/sa2040Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](N-C) = 0.002 Å
  • R factor = 0.017
  • wR factor = 0.047
  • Data-to-parameter ratio = 17.8

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 1 N4 -C3 -N2 -CU1 106.90 1.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 2 N6 -C5 -N4 -C3 171.00 0.80 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 3 N2 -C3 -N4 -C5 -172.40 0.90 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 4 N4 -C5 -N6 -CU12 76.90 1.00 1.555 1.555 1.555 3.445 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 5 N9 -C8 -N7 -CU1 93.40 1.30 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 6 N11 -C10 -N9 -C8 -177.90 1.20 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 7 N7 -C8 -N9 -C10 177.40 1.20 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 8 N9 -C10 -N11 -CU12 -81.90 1.30 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 9 C3 -N2 -CU1 -N2 -105.00 3.00 1.555 1.555 1.555 5.666 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 16 C8 -N7 -CU1 -N7 30.00 2.00 1.555 1.555 1.555 5.666 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 23 CU1 -O13 -CU1 -O13 47.00 8.00 2.655 1.555 1.555 5.666 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 24 C10 -N11 -CU12-N11 -88.00 14.00 1.555 1.555 1.555 7.655
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 12 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis CCD; data reduction: CrysAlis RED (Oxford Diffraction, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1998); software used to prepare material for publication: enCIFer (Allen et al., 2004).

Poly[aquadi-µ3-dicyanamido-di-µ2-dicyanamido-dicopper(II)] top
Crystal data top
[Cu2(C2N3)4(H2O)]F(000) = 800
Mr = 409.30Dx = 2.085 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 29546 reflections
a = 21.8718 (11) Åθ = 3.0–63.6°
b = 6.8726 (3) ŵ = 3.29 mm1
c = 8.8127 (4) ÅT = 100 K
β = 100.199 (4)°Plate, blue
V = 1303.76 (11) Å30.37 × 0.31 × 0.06 mm
Z = 4
Data collection top
Oxford Gemini R CCD area-detector
diffractometer
1989 independent reflections
Radiation source: fine-focus sealed tube1959 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.020
ω and φ scansθmax = 30.5°, θmin = 4.1°
Absorption correction: analytical
(Clark & Reid, 1995)
h = 3131
Tmin = 0.366, Tmax = 0.889k = 99
57505 measured reflectionsl = 1212
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.017Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.048All H-atom parameters refined
S = 1.19 w = 1/[σ2(Fo2) + (0.021P)2 + 1.966P]
where P = (Fo2 + 2Fc2)/3
1989 reflections(Δ/σ)max < 0.001
112 parametersΔρmax = 0.36 e Å3
0 restraintsΔρmin = 0.35 e Å3
Special details top

Experimental. face-indexed (CrysAlis RED; Oxford Diffraction, 2006)

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C30.44119 (5)0.12766 (18)0.33155 (13)0.0125 (2)
C50.37036 (5)0.05551 (17)0.16356 (14)0.0131 (2)
C80.63496 (5)0.41278 (17)0.45826 (13)0.01183 (19)
C100.70609 (5)0.34567 (17)0.30535 (13)0.01118 (19)
N20.46328 (5)0.25590 (15)0.40637 (12)0.01356 (19)
N40.42392 (5)0.02792 (17)0.25123 (15)0.0203 (2)
N60.32634 (5)0.10208 (16)0.07919 (13)0.01477 (19)
N70.58718 (5)0.40561 (16)0.49784 (12)0.01464 (19)
N90.69099 (5)0.43171 (16)0.42618 (12)0.01395 (19)
N110.72458 (5)0.27637 (16)0.20277 (12)0.01317 (18)
O130.50000.63494 (19)0.25000.0140 (2)
H130.5297 (11)0.720 (4)0.248 (3)0.049 (7)*
Cu10.50000.50000.50000.00942 (6)
Cu120.75000.25000.00000.00856 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C30.0105 (4)0.0137 (5)0.0132 (5)0.0002 (4)0.0022 (4)0.0000 (4)
C50.0136 (5)0.0103 (5)0.0159 (5)0.0005 (4)0.0042 (4)0.0031 (4)
C80.0136 (5)0.0111 (5)0.0105 (4)0.0008 (4)0.0012 (4)0.0026 (4)
C100.0101 (4)0.0112 (5)0.0121 (5)0.0017 (4)0.0016 (4)0.0002 (4)
N20.0119 (4)0.0146 (5)0.0144 (4)0.0025 (3)0.0030 (4)0.0034 (3)
N40.0146 (5)0.0148 (5)0.0280 (6)0.0011 (4)0.0055 (4)0.0082 (4)
N60.0116 (4)0.0150 (4)0.0180 (5)0.0015 (4)0.0033 (4)0.0055 (4)
N70.0121 (4)0.0158 (5)0.0165 (4)0.0015 (4)0.0038 (3)0.0042 (4)
N90.0115 (4)0.0176 (5)0.0137 (4)0.0031 (4)0.0048 (3)0.0054 (4)
N110.0143 (4)0.0149 (4)0.0110 (4)0.0020 (4)0.0043 (3)0.0016 (3)
O130.0142 (5)0.0126 (5)0.0152 (5)0.0000.0025 (4)0.000
Cu10.00780 (9)0.01024 (10)0.01047 (9)0.00232 (6)0.00226 (6)0.00301 (6)
Cu120.00775 (9)0.01078 (10)0.00748 (9)0.00188 (6)0.00224 (6)0.00219 (6)
Geometric parameters (Å, º) top
C3—N21.1543 (16)N11—Cu121.9716 (10)
C3—N41.3009 (16)O13—Cu12.3904 (5)
C5—N61.1527 (16)O13—Cu1ii2.3904 (5)
C5—N41.2979 (16)O13—H130.88 (3)
C8—N71.1599 (16)Cu1—N2iii1.9762 (10)
C8—N91.3119 (15)Cu1—N7iii2.0174 (11)
C10—N111.1563 (16)Cu1—O13iii2.3904 (5)
C10—N91.3104 (15)Cu12—N11iv1.9716 (10)
N2—Cu11.9762 (10)Cu12—N6v1.9737 (10)
N6—Cu12i1.9737 (10)Cu12—N6vi1.9738 (10)
N7—Cu12.0174 (11)
N2—C3—N4172.01 (13)N2—Cu1—N792.18 (4)
N6—C5—N4170.84 (13)N7iii—Cu1—N7180.0
N7—C8—N9174.11 (12)N2iii—Cu1—O1389.38 (4)
N11—C10—N9174.00 (12)N2—Cu1—O1390.62 (4)
C3—N2—Cu1170.00 (10)N7iii—Cu1—O1392.19 (3)
C5—N4—C3126.04 (12)N7—Cu1—O1387.81 (3)
C5—N6—Cu12i158.24 (11)N2iii—Cu1—O13iii90.62 (4)
C8—N7—Cu1153.20 (10)N2—Cu1—O13iii89.38 (4)
C10—N9—C8120.65 (10)N7iii—Cu1—O13iii87.81 (3)
C10—N11—Cu12160.10 (10)N7—Cu1—O13iii92.19 (3)
Cu1—O13—Cu1ii134.34 (6)O13—Cu1—O13iii180.0
Cu1—O13—H13113.4 (18)N11iv—Cu12—N11179.999 (1)
Cu1ii—O13—H1396.9 (18)N11iv—Cu12—N6v89.36 (4)
N2iii—Cu1—N2180.0N11—Cu12—N6v90.64 (4)
N2iii—Cu1—N7iii92.18 (4)N11iv—Cu12—N6vi90.64 (4)
N2—Cu1—N7iii87.82 (4)N11—Cu12—N6vi89.36 (4)
N2iii—Cu1—N787.82 (4)N6v—Cu12—N6vi180.0
N4—C3—N2—Cu1106.9 (10)C8—N7—Cu1—N2iii64.0 (2)
N6—C5—N4—C3171.0 (8)C8—N7—Cu1—N2116.0 (2)
N2—C3—N4—C5172.4 (9)C8—N7—Cu1—N7iii30 (2)
N4—C5—N6—Cu12i76.9 (10)C8—N7—Cu1—O1325.5 (2)
N9—C8—N7—Cu193.4 (13)C8—N7—Cu1—O13iii154.5 (2)
N11—C10—N9—C8177.9 (12)Cu1ii—O13—Cu1—N2iii156.42 (3)
N7—C8—N9—C10177.4 (12)Cu1ii—O13—Cu1—N223.58 (3)
N9—C10—N11—Cu1281.9 (13)Cu1ii—O13—Cu1—N7iii111.42 (3)
C3—N2—Cu1—N2iii105 (3)Cu1ii—O13—Cu1—N768.58 (3)
C3—N2—Cu1—N7iii85.9 (6)Cu1ii—O13—Cu1—O13iii47 (8)
C3—N2—Cu1—N794.1 (6)C10—N11—Cu12—N11iv88 (14)
C3—N2—Cu1—O136.3 (6)C10—N11—Cu12—N6v104.8 (3)
C3—N2—Cu1—O13iii173.7 (6)C10—N11—Cu12—N6vi75.2 (3)
Symmetry codes: (i) x1/2, y1/2, z; (ii) x+1, y, z+1/2; (iii) x+1, y+1, z+1; (iv) x+3/2, y+1/2, z; (v) x+1, y, z; (vi) x+1/2, y+1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O13—H13···N4vii0.88 (3)2.01 (3)2.8538 (15)162 (2)
Symmetry code: (vii) x+1, y+1, 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