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Acta Crystallogr Sect E Struct Rep Online. 2008 September 1; 64(Pt 9): m1148–m1149.
Published online 2008 August 9. doi:  10.1107/S1600536808023830
PMCID: PMC2960737

catena-Poly[[[μ-cyanido-1:2κ2 C:N-tricyanido-1κ3 C-bis(ethylenediamine)-2κ4 N,N′-copper(II)iron(II)]-μ-cyanido-κ2 C:N-[bis(ethylenediamine-κ2 N,N′)copper(II)]-μ-cyanido-κ2 N:C] 4.5-hy­drate]

Abstract

The asymmetric unit of the title compound, {[Cu2Fe(CN)6(C2H8N2)4]·4.5H2O}n, consists of two [Cu(C2H8N2)2]2+ cations, one [Fe(CN)6]4− anion, four water mol­ecules and a half water mol­ecule that lies on a twofold rotation axis. The FeII atom is coordinated by six C atoms from three terminal and three doubly bridging CN ligands. The bridging CN ligands connect the anion to a five-coordinate [Cu(C2H8N2)2]2+ cation and to two symmetry-related six-coordinate [Cu(C2H8N2)2]2+ cations, forming a one-dimensional polymer in the ab plane. Inter­molecular hydrogen bonds connect the polymer units into a three-dimensional network.

Related literature

For the corresponding complex catena-poly[bis­(cyanido-C)iron(II)]tetra(μ2-cyanido-C:N)bis­[bis­(ethyl­enediamine-N,N′)cadmium(II)], see: Fu & Wang (2005 [triangle]). For related literature, see: Fu et al. (2004 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-m1148-scheme1.jpg

Experimental

Crystal data

  • [Cu2Fe(CN)6(C2H8N2)4]·4.5H2O
  • M r = 660.56
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-m1148-efi1.jpg
  • a = 13.481 (7) Å
  • b = 13.497 (7) Å
  • c = 31.069 (15) Å
  • β = 93.547 (8)°
  • V = 5642 (5) Å3
  • Z = 8
  • Mo Kα radiation
  • μ = 2.05 mm−1
  • T = 298 (2) K
  • 0.25 × 0.15 × 0.09 mm

Data collection

  • Bruker SMART CCD area detector diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 1997 [triangle]) T min = 0.628, T max = 0.837
  • 14631 measured reflections
  • 4993 independent reflections
  • 2395 reflections with I > 2σ(I)
  • R int = 0.074

Refinement

  • R[F 2 > 2σ(F 2)] = 0.046
  • wR(F 2) = 0.070
  • S = 1.00
  • 4993 reflections
  • 348 parameters
  • 15 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.67 e Å−3
  • Δρmin = −0.47 e Å−3

Data collection: SMART (Bruker, 1997 [triangle]); cell refinement: SAINT (Bruker, 1997 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Table 1
Selected geometric parameters (Å, °)
Table 2
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808023830/sj2512sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808023830/sj2512Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

We are grateful for financial support from the National Natural Science Foundation of China (No. 20771021), and Shangdong Natural Science Foundation (No. Y2005B20).

supplementary crystallographic information

Comment

Hexacyanoferrate anions [Fe(CN)6]n- act as good building blocks to provide bimetallic assemblies exhibiting planar structures (Fu et al. 2005). In this paper we report the structure of the title compouund, (I), which forms linear polymer chains.

The asymmetric unit of the title compound, [Cu2(C2H8N2)4Fe(CN)64.5H2O]n, consists of two [Cu(C2H8N2]2+ cations, one [Fe(CN)6]4- anion, four water molecules and a half water molecule that lies on a two-fold rotation axis (Fig. 1). The Fe1 atom is coordinated by six nitrile C atoms from three terminal CN- ligands and three doubly bridging CN- ligands. Cu1 is coordinated by five N atoms from two chelating ethylenediamine (en) ligands and a doubly bridging CN1- ligand while Cu2 binds to six N atoms from two chelated en ligands and two doubly bridging CN- ligands (Fig. 2). The average Fe—C distance of the bridging CN1- ligands of 1.909 (6) Å (Table 1) is slightly shorter than that of the terminal CN- ligands, 1.937 Å. The average Cu—N bond distance involving the en ligands is 2.009 Å considerably shorter than the average Cu—N(nitrile) distance of 2.472 Å. These are similar to the corresponding N—Cu bonds in the compound [Cu2(C4N2S2)2(C2H8N2)2]n (Fu, et al., 2004). The coordination geometries about the Fe1 and Cu2 centers are distorted octahedral with Cu1 dispaying a distorted square-pyramidal geometry. The bridging CN- ligands connect the anion to the five coordinate Cu1 cation and to the Cu2 and Cu2i (I = x+1/2, y-1/2, z) cations to form a one dimensional polymer. In the crystal structure, the water O atoms and N atoms from the en and CN- ligands participate in intermolecular hydrogen bonds (Table 2), which further connect the polymer chains into a three-dimensional network (Fig. 3).

Experimental

A solution (10 ml) of distilled water containing CuSO46H2O (1.0 mmol) was added slowly to aqueous mixture (20 ml)of K4[Fe(CN)6] (0.5 mmol) and NH3 (2 mmol). The mixture was stirred for 4 h and then filtered. crystals suitable for X-ray analysis were obtained by slow evaporation of a methanol/dichloromethane (1:2 v/v) solution over a period of three weeks. Elemental analysis found: C, 25.37%; H, 6.22%; N, 29.58%; calc. for C28 H82 Cu4 Fe2 N28O9: C, 25.45%; H, 6.26%; N, 29.69%.

Refinement

Water H atoms were found in difference maps and were refined freely with isotropic displacement parameters. All other H atoms were placed in idealized positions and constrained to ride on their parent atoms, with C—H = 0.97 Å and Uiso(H) = 1.2Ueq(C), N—H = 0.90 Å, and Uiso(H) = 1.2Ueq(N).

Figures

Fig. 1.
A view of the asymmetric unit of (I), with atom labels and 50% probability displacement ellipsoids.
Fig. 2.
The one-dimensional polymer chains of (I) with H bonds drawn as dashed lines.
Fig. 3.
Crystal packing of (I), showing the hydrogen-bonded interactions as dashed lines.

Crystal data

[Cu2Fe(CN)6(C2H8N2)4]·4.5H2OF(000) = 2744
Mr = 660.56Dx = 1.555 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 1697 reflections
a = 13.481 (7) Åθ = 2.3–20.2°
b = 13.497 (7) ŵ = 2.05 mm1
c = 31.069 (15) ÅT = 298 K
β = 93.547 (8)°Block, blue
V = 5642 (5) Å30.25 × 0.15 × 0.09 mm
Z = 8

Data collection

Bruker SMART CCD area detector diffractometer4993 independent reflections
Radiation source: fine-focus sealed tube2395 reflections with I > 2σ(I)
graphiteRint = 0.074
[var phi] and ω scansθmax = 25.0°, θmin = 1.3°
Absorption correction: multi-scan (SADABS; Bruker, 1997)h = −16→16
Tmin = 0.628, Tmax = 0.837k = −11→16
14631 measured reflectionsl = −32→36

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.047Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.070H atoms treated by a mixture of independent and constrained refinement
S = 1.00w = 1/[σ2(Fo2)] where P = (Fo2 + 2Fc2)/3
4993 reflections(Δ/σ)max = 0.001
348 parametersΔρmax = 0.67 e Å3
15 restraintsΔρmin = −0.47 e Å3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
Cu10.14883 (5)0.38885 (6)0.37321 (2)0.0446 (2)
Cu20.63210 (5)0.39053 (6)0.38794 (2)0.0494 (2)
Fe10.38981 (6)0.64597 (6)0.37999 (3)0.0328 (2)
N10.1742 (3)0.2994 (4)0.32332 (16)0.0728 (17)
H1A0.22530.25840.33050.087*
H1B0.12000.26240.31640.087*
N20.1342 (3)0.4945 (3)0.32725 (16)0.0562 (15)
H2A0.07910.53060.33070.067*
H2B0.18700.53540.32920.067*
N30.1608 (3)0.2829 (3)0.41874 (14)0.0465 (13)
H3A0.10940.24050.41530.056*
H3B0.21750.24860.41650.056*
N40.1050 (3)0.4741 (3)0.42098 (14)0.0552 (15)
H4A0.15310.51780.42890.066*
H4B0.05020.50820.41200.066*
N50.6854 (3)0.3574 (4)0.32995 (13)0.0538 (14)
H5A0.70420.41350.31700.065*
H5B0.73900.31800.33390.065*
N60.5073 (3)0.3308 (3)0.36175 (16)0.0625 (16)
H6A0.49700.27150.37390.075*
H6B0.45540.37020.36680.075*
N70.7606 (3)0.4297 (3)0.41861 (15)0.0624 (16)
H7C0.80850.38610.41280.075*
H7D0.77910.49010.40980.075*
N80.5739 (3)0.4383 (3)0.44283 (13)0.0483 (14)
H8A0.52450.48160.43640.058*
H8B0.54880.38670.45690.058*
N90.3237 (3)0.4320 (4)0.39355 (15)0.0531 (15)
N100.1843 (3)0.7038 (4)0.40890 (15)0.0539 (15)
N110.4716 (4)0.6769 (4)0.47419 (15)0.0568 (16)
N120.4435 (3)0.8605 (4)0.35978 (14)0.0488 (14)
N130.5947 (3)0.5724 (4)0.35587 (15)0.0535 (16)
N140.3119 (4)0.6286 (4)0.28505 (15)0.0665 (18)
O10.0188 (3)0.6836 (4)0.45869 (14)0.0775 (16)
O20.4258 (3)0.0620 (3)0.33942 (16)0.0716 (14)
O30.2555 (3)0.5748 (4)0.20204 (13)0.0963 (19)
O40.50000.7270 (5)0.25000.099 (2)
O50.3429 (3)0.1477 (5)0.41272 (18)0.1026 (18)
C10.1983 (5)0.3623 (6)0.2858 (2)0.091 (3)
H1C0.26610.38640.28930.109*
H1D0.19060.32480.25910.109*
C20.1274 (5)0.4455 (6)0.2852 (2)0.086 (3)
H2C0.14270.49230.26290.104*
H2D0.06040.42110.27890.104*
C30.1609 (4)0.3306 (5)0.46117 (18)0.064 (2)
H3C0.22570.35890.46890.076*
H3D0.14560.28240.48300.076*
C40.0834 (4)0.4102 (5)0.45824 (17)0.061 (2)
H4C0.01770.38130.45390.074*
H4D0.08600.44890.48460.074*
C50.6095 (5)0.3076 (6)0.3027 (2)0.106 (3)
H5C0.61120.33330.27360.127*
H5D0.62500.23750.30180.127*
C60.5141 (5)0.3190 (6)0.3164 (2)0.110 (3)
H6C0.47520.26150.30710.132*
H6D0.48400.37630.30200.132*
C70.7463 (5)0.4309 (5)0.46471 (19)0.072 (2)
H7A0.80210.46300.48020.087*
H7B0.74070.36390.47550.087*
C80.6534 (4)0.4868 (5)0.47051 (19)0.0606 (19)
H8C0.66100.55540.46200.073*
H8D0.63710.48510.50050.073*
C90.3514 (4)0.5131 (4)0.38950 (17)0.0385 (16)
C100.2612 (4)0.6829 (4)0.39777 (16)0.0361 (15)
C110.4408 (4)0.6643 (4)0.43898 (18)0.0357 (16)
C120.4243 (4)0.7784 (4)0.36780 (17)0.0343 (15)
C130.5186 (4)0.6004 (4)0.36404 (15)0.0350 (14)
C140.3402 (4)0.6327 (4)0.32031 (19)0.0421 (16)
H10.016 (4)0.718 (5)0.4802 (17)0.080*
H20.0778 (17)0.678 (4)0.4516 (17)0.080*
H30.372 (3)0.078 (3)0.3229 (15)0.080*
H40.4113 (17)−0.0018 (17)0.3443 (17)0.080*
H50.269 (4)0.598 (4)0.2280 (9)0.080*
H60.312 (2)0.575 (4)0.1913 (14)0.080*
H70.5503 (9)0.686 (2)0.249 (2)0.080*
H80.387 (3)0.173 (5)0.4315 (12)0.080*
H90.369 (4)0.145 (5)0.3890 (9)0.080*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Cu10.0491 (5)0.0375 (5)0.0478 (5)−0.0015 (4)0.0080 (4)−0.0004 (4)
Cu20.0362 (5)0.0676 (7)0.0450 (5)0.0023 (4)0.0059 (4)−0.0024 (4)
Fe10.0277 (4)0.0340 (5)0.0373 (5)−0.0017 (4)0.0067 (4)−0.0016 (4)
N10.072 (4)0.060 (4)0.089 (5)−0.014 (3)0.025 (3)−0.027 (3)
N20.042 (3)0.051 (4)0.075 (4)−0.011 (3)0.007 (3)0.023 (3)
N30.028 (3)0.044 (4)0.067 (4)−0.009 (2)0.005 (3)0.005 (3)
N40.049 (3)0.048 (4)0.070 (4)−0.008 (3)0.013 (3)−0.014 (3)
N50.051 (3)0.056 (4)0.056 (4)0.013 (3)0.017 (3)0.014 (3)
N60.039 (3)0.059 (4)0.090 (4)0.011 (3)0.006 (3)−0.012 (3)
N70.037 (3)0.055 (4)0.097 (5)0.000 (3)0.017 (3)−0.020 (3)
N80.043 (3)0.051 (4)0.052 (3)0.003 (3)0.003 (3)0.011 (3)
N90.043 (3)0.039 (4)0.079 (4)−0.004 (3)0.012 (3)0.002 (3)
N100.037 (3)0.054 (4)0.073 (4)0.009 (3)0.022 (3)0.001 (3)
N110.062 (4)0.076 (5)0.032 (3)−0.014 (3)0.006 (3)−0.001 (3)
N120.043 (3)0.046 (4)0.058 (4)0.004 (3)0.008 (2)0.005 (3)
N130.029 (3)0.067 (4)0.066 (4)0.007 (3)0.020 (3)−0.005 (3)
N140.063 (4)0.099 (5)0.036 (3)−0.018 (3)−0.006 (3)−0.007 (3)
O10.062 (3)0.103 (5)0.071 (4)−0.024 (3)0.033 (3)−0.032 (3)
O20.061 (3)0.064 (4)0.089 (4)−0.001 (3)−0.003 (3)0.015 (3)
O30.064 (3)0.175 (6)0.052 (3)−0.048 (4)0.023 (3)−0.038 (3)
O40.085 (5)0.102 (7)0.116 (6)0.0000.043 (6)0.000
O50.068 (4)0.124 (5)0.115 (4)−0.002 (4)0.001 (3)−0.029 (4)
C10.094 (6)0.114 (8)0.068 (6)−0.029 (6)0.039 (5)−0.012 (5)
C20.087 (6)0.129 (9)0.041 (5)−0.038 (6)−0.010 (5)0.023 (5)
C30.056 (5)0.095 (7)0.039 (5)−0.018 (4)−0.002 (4)0.003 (4)
C40.060 (5)0.080 (6)0.046 (4)−0.020 (4)0.019 (4)−0.010 (4)
C50.058 (5)0.186 (10)0.072 (6)0.008 (6)−0.012 (5)−0.059 (6)
C60.081 (6)0.181 (10)0.068 (6)−0.022 (6)0.007 (5)−0.053 (6)
C70.060 (5)0.099 (7)0.057 (5)0.002 (4)−0.012 (4)−0.022 (4)
C80.072 (5)0.059 (5)0.054 (5)−0.008 (4)0.024 (4)−0.007 (4)
C90.022 (3)0.044 (5)0.050 (4)0.011 (3)0.004 (3)−0.010 (3)
C100.045 (4)0.028 (4)0.035 (4)−0.008 (3)0.004 (3)0.002 (3)
C110.024 (3)0.035 (4)0.050 (4)−0.003 (3)0.015 (3)0.006 (3)
C120.025 (3)0.038 (4)0.041 (4)0.009 (3)0.005 (3)−0.004 (3)
C130.044 (4)0.031 (4)0.031 (3)−0.014 (3)0.007 (3)0.007 (3)
C140.027 (4)0.043 (4)0.058 (4)−0.007 (3)0.014 (3)0.004 (4)

Geometric parameters (Å, °)

Cu1—N41.996 (4)N8—C81.483 (6)
Cu1—N12.011 (5)N8—H8A0.9000
Cu1—N32.011 (4)N8—H8B0.9000
Cu1—N22.019 (4)N9—C91.166 (6)
Cu1—N92.472 (5)N10—C101.149 (5)
Cu2—N61.993 (4)N11—C111.158 (6)
Cu2—N71.996 (4)N12—C121.169 (6)
Cu2—N82.026 (4)N13—C131.137 (5)
Cu2—N52.030 (4)N14—C141.139 (6)
Cu2—N10i2.686 (5)O1—H10.81 (4)
Cu2—N132.686 (5)O1—H20.842 (14)
Fe1—C121.891 (6)O2—H30.888 (19)
Fe1—C91.895 (6)O2—H40.899 (18)
Fe1—C101.917 (5)O3—H50.873 (19)
Fe1—C111.933 (6)O3—H60.847 (19)
Fe1—C131.935 (6)O4—H70.879 (19)
Fe1—C141.940 (6)O5—H80.878 (19)
N1—C11.495 (7)O5—H90.839 (19)
N1—H1A0.9000C1—C21.474 (8)
N1—H1B0.9000C1—H1C0.9700
N2—C21.463 (7)C1—H1D0.9700
N2—H2A0.9000C2—H2C0.9700
N2—H2B0.9000C2—H2D0.9700
N3—C31.467 (6)C3—C41.497 (7)
N3—H3A0.9000C3—H3C0.9700
N3—H3B0.9000C3—H3D0.9700
N4—C41.487 (6)C4—H4C0.9700
N4—H4A0.9000C4—H4D0.9700
N4—H4B0.9000C5—C61.388 (7)
N5—C51.452 (7)C5—H5C0.9700
N5—H5A0.9000C5—H5D0.9700
N5—H5B0.9000C6—H6C0.9700
N6—C61.427 (7)C6—H6D0.9700
N6—H6A0.9000C7—C81.483 (7)
N6—H6B0.9000C7—H7A0.9700
N7—C71.457 (6)C7—H7B0.9700
N7—H7C0.9000C8—H8C0.9700
N7—H7D0.9000C8—H8D0.9700
N4—Cu1—N1172.59 (19)Cu2—N6—H6B109.6
N4—Cu1—N384.34 (19)H6A—N6—H6B108.1
N1—Cu1—N396.0 (2)C7—N7—Cu2107.9 (3)
N4—Cu1—N295.6 (2)C7—N7—H7C110.1
N1—Cu1—N283.9 (2)Cu2—N7—H7C110.1
N3—Cu1—N2178.96 (18)C7—N7—H7D110.1
N4—Cu1—N989.74 (17)Cu2—N7—H7D110.1
N1—Cu1—N997.67 (17)H7C—N7—H7D108.4
N3—Cu1—N987.37 (17)C8—N8—Cu2109.0 (3)
N2—Cu1—N993.67 (17)C8—N8—H8A109.9
N6—Cu2—N7171.0 (2)Cu2—N8—H8A109.9
N6—Cu2—N896.40 (19)C8—N8—H8B109.9
N7—Cu2—N883.32 (18)Cu2—N8—H8B109.9
N6—Cu2—N583.39 (19)H8A—N8—H8B108.3
N7—Cu2—N597.89 (18)C9—N9—Cu1120.0 (4)
N8—Cu2—N5173.55 (19)C13—N13—Cu2111.8 (4)
N6—Cu2—N10i85.50 (17)H1—O1—H2110 (4)
N7—Cu2—N10i85.77 (17)H3—O2—H498 (2)
N8—Cu2—N10i101.76 (16)H5—O3—H6103 (3)
N5—Cu2—N10i84.66 (16)H8—O5—H9107 (3)
N6—Cu2—N1394.80 (17)C2—C1—N1105.7 (5)
N7—Cu2—N1394.15 (17)C2—C1—H1C110.6
N8—Cu2—N1387.01 (16)N1—C1—H1C110.6
N5—Cu2—N1386.58 (16)C2—C1—H1D110.6
N10i—Cu2—N13171.15 (13)N1—C1—H1D110.6
C12—Fe1—C9177.1 (2)H1C—C1—H1D108.7
C12—Fe1—C1092.9 (2)N2—C2—C1109.2 (6)
C9—Fe1—C1086.6 (2)N2—C2—H2C109.8
C12—Fe1—C1189.5 (2)C1—C2—H2C109.8
C9—Fe1—C1193.3 (2)N2—C2—H2D109.8
C10—Fe1—C1188.2 (2)C1—C2—H2D109.8
C12—Fe1—C1390.8 (2)H2C—C2—H2D108.3
C9—Fe1—C1389.8 (2)N3—C3—C4107.4 (5)
C10—Fe1—C13176.2 (2)N3—C3—H3C110.2
C11—Fe1—C1390.6 (2)C4—C3—H3C110.2
C12—Fe1—C1488.3 (2)N3—C3—H3D110.2
C9—Fe1—C1488.9 (2)C4—C3—H3D110.2
C10—Fe1—C1492.0 (2)H3C—C3—H3D108.5
C11—Fe1—C14177.8 (2)N4—C4—C3107.1 (5)
C13—Fe1—C1489.3 (2)N4—C4—H4C110.3
C1—N1—Cu1108.4 (4)C3—C4—H4C110.3
C1—N1—H1A110.0N4—C4—H4D110.3
Cu1—N1—H1A110.0C3—C4—H4D110.3
C1—N1—H1B110.0H4C—C4—H4D108.5
Cu1—N1—H1B110.0C6—C5—N5113.8 (6)
H1A—N1—H1B108.4C6—C5—H5C108.8
C2—N2—Cu1108.1 (4)N5—C5—H5C108.8
C2—N2—H2A110.1C6—C5—H5D108.8
Cu1—N2—H2A110.1N5—C5—H5D108.8
C2—N2—H2B110.1H5C—C5—H5D107.7
Cu1—N2—H2B110.1C5—C6—N6115.6 (6)
H2A—N2—H2B108.4C5—C6—H6C108.4
C3—N3—Cu1108.4 (4)N6—C6—H6C108.4
C3—N3—H3A110.0C5—C6—H6D108.4
Cu1—N3—H3A110.0N6—C6—H6D108.4
C3—N3—H3B110.0H6C—C6—H6D107.4
Cu1—N3—H3B110.0N7—C7—C8106.9 (5)
H3A—N3—H3B108.4N7—C7—H7A110.4
C4—N4—Cu1109.0 (4)C8—C7—H7A110.4
C4—N4—H4A109.9N7—C7—H7B110.4
Cu1—N4—H4A109.9C8—C7—H7B110.4
C4—N4—H4B109.9H7A—C7—H7B108.6
Cu1—N4—H4B109.9C7—C8—N8106.9 (5)
H4A—N4—H4B108.3C7—C8—H8C110.4
C5—N5—Cu2110.1 (4)N8—C8—H8C110.4
C5—N5—H5A109.6C7—C8—H8D110.4
Cu2—N5—H5A109.6N8—C8—H8D110.4
C5—N5—H5B109.6H8C—C8—H8D108.6
Cu2—N5—H5B109.6N9—C9—Fe1176.3 (6)
H5A—N5—H5B108.2N10—C10—Fe1178.9 (5)
C6—N6—Cu2110.2 (4)N11—C11—Fe1178.9 (5)
C6—N6—H6A109.6N12—C12—Fe1178.4 (5)
Cu2—N6—H6A109.6N13—C13—Fe1178.0 (5)
C6—N6—H6B109.6N14—C14—Fe1177.4 (6)
N4—Cu1—N1—C1103.2 (16)N1—C1—C2—N254.8 (7)
N3—Cu1—N1—C1−164.2 (4)Cu1—N3—C3—C442.0 (5)
N2—Cu1—N1—C116.8 (4)Cu1—N4—C4—C339.0 (5)
N9—Cu1—N1—C1−76.1 (4)N3—C3—C4—N4−53.4 (6)
N4—Cu1—N2—C2−160.1 (4)Cu2—N5—C5—C617.3 (9)
N1—Cu1—N2—C212.5 (4)N5—C5—C6—N6−29.8 (11)
N3—Cu1—N2—C2−72 (11)Cu2—N6—C6—C527.0 (9)
N9—Cu1—N2—C2109.8 (4)Cu2—N7—C7—C8−47.8 (5)
N4—Cu1—N3—C3−16.3 (4)N7—C7—C8—N855.1 (6)
N1—Cu1—N3—C3171.1 (3)Cu2—N8—C8—C7−35.9 (6)
N2—Cu1—N3—C3−105 (11)Cu1—N9—C9—Fe1−27 (8)
N9—Cu1—N3—C373.7 (3)C12—Fe1—C9—N9−15 (11)
N1—Cu1—N4—C480.4 (17)C10—Fe1—C9—N964 (8)
N3—Cu1—N4—C4−12.9 (4)C11—Fe1—C9—N9152 (8)
N2—Cu1—N4—C4166.0 (4)C13—Fe1—C9—N9−118 (8)
N9—Cu1—N4—C4−100.3 (4)C14—Fe1—C9—N9−28 (8)
N6—Cu2—N5—C5−2.0 (5)C12—Fe1—C10—N10−146 (33)
N7—Cu2—N5—C5169.1 (5)C9—Fe1—C10—N1037 (33)
N8—Cu2—N5—C5−90.5 (17)C11—Fe1—C10—N10−57 (33)
N13—Cu2—N5—C5−97.2 (5)C13—Fe1—C10—N1016 (36)
N7—Cu2—N6—C6−111.6 (13)C14—Fe1—C10—N10126 (33)
N8—Cu2—N6—C6160.7 (5)C12—Fe1—C11—N117(26)
N5—Cu2—N6—C6−12.8 (5)C9—Fe1—C11—N11−173 (100)
N13—Cu2—N6—C673.2 (5)C10—Fe1—C11—N11−86 (26)
N6—Cu2—N7—C7−66.9 (13)C13—Fe1—C11—N1197 (26)
N8—Cu2—N7—C721.9 (4)C14—Fe1—C11—N119(30)
N5—Cu2—N7—C7−164.5 (4)C9—Fe1—C12—N1234 (23)
N13—Cu2—N7—C7108.4 (4)C10—Fe1—C12—N12−45 (20)
N6—Cu2—N8—C8179.1 (4)C11—Fe1—C12—N12−133 (20)
N7—Cu2—N8—C88.1 (4)C13—Fe1—C12—N12136 (20)
N5—Cu2—N8—C8−93.1 (17)C14—Fe1—C12—N1247 (20)
N13—Cu2—N8—C8−86.4 (4)Cu2—N13—C13—Fe141 (15)
N4—Cu1—N9—C9−66.4 (5)C12—Fe1—C13—N13122 (15)
N1—Cu1—N9—C9113.6 (5)C9—Fe1—C13—N13−61 (15)
N3—Cu1—N9—C9−150.7 (5)C10—Fe1—C13—N13−40 (17)
N2—Cu1—N9—C929.3 (5)C11—Fe1—C13—N1332 (15)
N6—Cu2—N13—C1353.0 (5)C14—Fe1—C13—N13−150 (15)
N7—Cu2—N13—C13−126.3 (5)C12—Fe1—C14—N14−3(12)
N8—Cu2—N13—C13−43.2 (5)C9—Fe1—C14—N14176 (100)
N5—Cu2—N13—C13136.1 (5)C10—Fe1—C14—N1490 (12)
Cu1—N1—C1—C2−42.4 (6)C11—Fe1—C14—N14−6(17)
Cu1—N2—C2—C1−40.4 (6)C13—Fe1—C14—N14−94 (12)

Symmetry codes: (i) x+1/2, y−1/2, z.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
N1—H1B···O4ii0.902.593.316 (5)139.
N2—H2A···O2iii0.902.142.999 (6)159.
N2—H2B···N140.902.573.335 (6)144.
N3—H3B···O50.902.183.074 (7)172.
N4—H4A···N100.902.633.308 (7)133.
N5—H5A···O3iv0.902.333.214 (7)167.
N6—H6B···N90.902.173.044 (6)163.
N7—H7C···N12i0.902.553.293 (6)140.
N7—H7D···O5v0.902.293.153 (8)160.
N8—H8B···N11vi0.902.343.104 (6)143.
O1—H1···N11vii0.81 (4)2.01 (5)2.807 (6)167 (6)
O1—H2···N100.84 (1)2.04 (3)2.806 (6)150 (6)
O2—H3···O3viii0.89 (2)1.84 (3)2.697 (6)161 (4)
O2—H4···N12ix0.90 (2)1.96 (2)2.799 (7)155 (2)
O3—H5···N140.87 (2)1.88 (2)2.741 (6)170 (6)
O3—H6···N13iv0.85 (2)1.99 (2)2.787 (6)156 (5)
O4—H7···N14iv0.88 (2)2.33 (3)3.118 (6)149 (5)
O5—H8···O1i0.88 (2)1.92 (3)2.734 (7)153 (5)
O5—H9···O20.84 (2)2.09 (4)2.844 (7)150 (6)

Symmetry codes: (ii) x−1/2, y−1/2, z; (iii) x−1/2, y+1/2, z; (iv) −x+1, y, −z+1/2; (i) x+1/2, y−1/2, z; (v) x+1/2, y+1/2, z; (vi) −x+1, −y+1, −z+1; (vii) −x+1/2, −y+3/2, −z+1; (viii) −x+1/2, y−1/2, −z+1/2; (ix) x, y−1, z.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SJ2512).

References

  • Bruker (1997). SMART, SAINT and SADABS Bruker AXS Inc., Madison, Wisconsin, USA.
  • Fu, A.-Y. & Wang, D.-Q. (2005). Z. Kristallogr. New Cryst. Struct Volume? 220.
  • Fu, A.-Y., Wang, D.-Q. & Sun, D.-Z. (2004). Acta Cryst. E60, m1869–m1871.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]

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