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
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (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
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-µ
3-dicyanamido-di-µ
2-dicyanamido-dicopper(II)]
top
Crystal data top
[Cu2(C2N3)4(H2O)] | F(000) = 800 |
Mr = 409.30 | Dx = 2.085 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 29546 reflections |
a = 21.8718 (11) Å | θ = 3.0–63.6° |
b = 6.8726 (3) Å | µ = 3.29 mm−1 |
c = 8.8127 (4) Å | T = 100 K |
β = 100.199 (4)° | Plate, blue |
V = 1303.76 (11) Å3 | 0.37 × 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 tube | 1959 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.020 |
ω and φ scans | θmax = 30.5°, θmin = 4.1° |
Absorption correction: analytical (Clark & Reid, 1995) | h = −31→31 |
Tmin = 0.366, Tmax = 0.889 | k = −9→9 |
57505 measured reflections | l = −12→12 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.017 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.048 | All 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 parameters | Δρmax = 0.36 e Å−3 |
0 restraints | Δρmin = −0.35 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
C3 | 0.44119 (5) | 0.12766 (18) | 0.33155 (13) | 0.0125 (2) | |
C5 | 0.37036 (5) | −0.05551 (17) | 0.16356 (14) | 0.0131 (2) | |
C8 | 0.63496 (5) | 0.41278 (17) | 0.45826 (13) | 0.01183 (19) | |
C10 | 0.70609 (5) | 0.34567 (17) | 0.30535 (13) | 0.01118 (19) | |
N2 | 0.46328 (5) | 0.25590 (15) | 0.40637 (12) | 0.01356 (19) | |
N4 | 0.42392 (5) | −0.02792 (17) | 0.25123 (15) | 0.0203 (2) | |
N6 | 0.32634 (5) | −0.10208 (16) | 0.07919 (13) | 0.01477 (19) | |
N7 | 0.58718 (5) | 0.40561 (16) | 0.49784 (12) | 0.01464 (19) | |
N9 | 0.69099 (5) | 0.43171 (16) | 0.42618 (12) | 0.01395 (19) | |
N11 | 0.72458 (5) | 0.27637 (16) | 0.20277 (12) | 0.01317 (18) | |
O13 | 0.5000 | 0.63494 (19) | 0.2500 | 0.0140 (2) | |
H13 | 0.5297 (11) | 0.720 (4) | 0.248 (3) | 0.049 (7)* | |
Cu1 | 0.5000 | 0.5000 | 0.5000 | 0.00942 (6) | |
Cu12 | 0.7500 | 0.2500 | 0.0000 | 0.00856 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C3 | 0.0105 (4) | 0.0137 (5) | 0.0132 (5) | −0.0002 (4) | 0.0022 (4) | 0.0000 (4) |
C5 | 0.0136 (5) | 0.0103 (5) | 0.0159 (5) | −0.0005 (4) | 0.0042 (4) | −0.0031 (4) |
C8 | 0.0136 (5) | 0.0111 (5) | 0.0105 (4) | −0.0008 (4) | 0.0012 (4) | −0.0026 (4) |
C10 | 0.0101 (4) | 0.0112 (5) | 0.0121 (5) | −0.0017 (4) | 0.0016 (4) | 0.0002 (4) |
N2 | 0.0119 (4) | 0.0146 (5) | 0.0144 (4) | −0.0025 (3) | 0.0030 (4) | −0.0034 (3) |
N4 | 0.0146 (5) | 0.0148 (5) | 0.0280 (6) | 0.0011 (4) | −0.0055 (4) | −0.0082 (4) |
N6 | 0.0116 (4) | 0.0150 (4) | 0.0180 (5) | −0.0015 (4) | 0.0033 (4) | −0.0055 (4) |
N7 | 0.0121 (4) | 0.0158 (5) | 0.0165 (4) | −0.0015 (4) | 0.0038 (3) | −0.0042 (4) |
N9 | 0.0115 (4) | 0.0176 (5) | 0.0137 (4) | −0.0031 (4) | 0.0048 (3) | −0.0054 (4) |
N11 | 0.0143 (4) | 0.0149 (4) | 0.0110 (4) | −0.0020 (4) | 0.0043 (3) | −0.0016 (3) |
O13 | 0.0142 (5) | 0.0126 (5) | 0.0152 (5) | 0.000 | 0.0025 (4) | 0.000 |
Cu1 | 0.00780 (9) | 0.01024 (10) | 0.01047 (9) | −0.00232 (6) | 0.00226 (6) | −0.00301 (6) |
Cu12 | 0.00775 (9) | 0.01078 (10) | 0.00748 (9) | −0.00188 (6) | 0.00224 (6) | −0.00219 (6) |
Geometric parameters (Å, º) top
C3—N2 | 1.1543 (16) | N11—Cu12 | 1.9716 (10) |
C3—N4 | 1.3009 (16) | O13—Cu1 | 2.3904 (5) |
C5—N6 | 1.1527 (16) | O13—Cu1ii | 2.3904 (5) |
C5—N4 | 1.2979 (16) | O13—H13 | 0.88 (3) |
C8—N7 | 1.1599 (16) | Cu1—N2iii | 1.9762 (10) |
C8—N9 | 1.3119 (15) | Cu1—N7iii | 2.0174 (11) |
C10—N11 | 1.1563 (16) | Cu1—O13iii | 2.3904 (5) |
C10—N9 | 1.3104 (15) | Cu12—N11iv | 1.9716 (10) |
N2—Cu1 | 1.9762 (10) | Cu12—N6v | 1.9737 (10) |
N6—Cu12i | 1.9737 (10) | Cu12—N6vi | 1.9738 (10) |
N7—Cu1 | 2.0174 (11) | | |
| | | |
N2—C3—N4 | 172.01 (13) | N2—Cu1—N7 | 92.18 (4) |
N6—C5—N4 | 170.84 (13) | N7iii—Cu1—N7 | 180.0 |
N7—C8—N9 | 174.11 (12) | N2iii—Cu1—O13 | 89.38 (4) |
N11—C10—N9 | 174.00 (12) | N2—Cu1—O13 | 90.62 (4) |
C3—N2—Cu1 | 170.00 (10) | N7iii—Cu1—O13 | 92.19 (3) |
C5—N4—C3 | 126.04 (12) | N7—Cu1—O13 | 87.81 (3) |
C5—N6—Cu12i | 158.24 (11) | N2iii—Cu1—O13iii | 90.62 (4) |
C8—N7—Cu1 | 153.20 (10) | N2—Cu1—O13iii | 89.38 (4) |
C10—N9—C8 | 120.65 (10) | N7iii—Cu1—O13iii | 87.81 (3) |
C10—N11—Cu12 | 160.10 (10) | N7—Cu1—O13iii | 92.19 (3) |
Cu1—O13—Cu1ii | 134.34 (6) | O13—Cu1—O13iii | 180.0 |
Cu1—O13—H13 | 113.4 (18) | N11iv—Cu12—N11 | 179.999 (1) |
Cu1ii—O13—H13 | 96.9 (18) | N11iv—Cu12—N6v | 89.36 (4) |
N2iii—Cu1—N2 | 180.0 | N11—Cu12—N6v | 90.64 (4) |
N2iii—Cu1—N7iii | 92.18 (4) | N11iv—Cu12—N6vi | 90.64 (4) |
N2—Cu1—N7iii | 87.82 (4) | N11—Cu12—N6vi | 89.36 (4) |
N2iii—Cu1—N7 | 87.82 (4) | N6v—Cu12—N6vi | 180.0 |
| | | |
N4—C3—N2—Cu1 | 106.9 (10) | C8—N7—Cu1—N2iii | −64.0 (2) |
N6—C5—N4—C3 | 171.0 (8) | C8—N7—Cu1—N2 | 116.0 (2) |
N2—C3—N4—C5 | −172.4 (9) | C8—N7—Cu1—N7iii | 30 (2) |
N4—C5—N6—Cu12i | 76.9 (10) | C8—N7—Cu1—O13 | 25.5 (2) |
N9—C8—N7—Cu1 | 93.4 (13) | C8—N7—Cu1—O13iii | −154.5 (2) |
N11—C10—N9—C8 | −177.9 (12) | Cu1ii—O13—Cu1—N2iii | 156.42 (3) |
N7—C8—N9—C10 | 177.4 (12) | Cu1ii—O13—Cu1—N2 | −23.58 (3) |
N9—C10—N11—Cu12 | −81.9 (13) | Cu1ii—O13—Cu1—N7iii | −111.42 (3) |
C3—N2—Cu1—N2iii | −105 (3) | Cu1ii—O13—Cu1—N7 | 68.58 (3) |
C3—N2—Cu1—N7iii | 85.9 (6) | Cu1ii—O13—Cu1—O13iii | 47 (8) |
C3—N2—Cu1—N7 | −94.1 (6) | C10—N11—Cu12—N11iv | −88 (14) |
C3—N2—Cu1—O13 | −6.3 (6) | C10—N11—Cu12—N6v | −104.8 (3) |
C3—N2—Cu1—O13iii | 173.7 (6) | C10—N11—Cu12—N6vi | 75.2 (3) |
Symmetry codes: (i) x−1/2, y−1/2, 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···A | D—H | H···A | D···A | D—H···A |
O13—H13···N4vii | 0.88 (3) | 2.01 (3) | 2.8538 (15) | 162 (2) |
Symmetry code: (vii) −x+1, y+1, −z+1/2. |