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In the title compound, [Cu2(SO4)2(C20H36N8)(H2O)2]·6H2O, the dinuclear molecule lies across an inversion centre and contains square-pyramidal CuII ions separated by 7.5709 (18) Å. Symmetry-related molecules are linked together by hydrogen bonds between the coordinated water mol­ecules and the sulfate ligands. They are further linked by a framework of fused cyclic water tetra­meric and pseudo-hexa­gonal units in a three-dimensional hydrogen-bonded network involving both coordinated and uncoordinated water mol­ecules, as well as sulfate ligands. While the tetra­meric units are purely composed of water mol­ecules, the pseudo-hexa­gonal units involve O atoms from the sulfate. Further hydrogen bonding also involves the NH group from the imidazole in addition to the above-mentioned units.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805006896/wk6042sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805006896/wk6042Isup2.hkl
Contains datablock I

CCDC reference: 270562

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.061
  • wR factor = 0.148
  • Data-to-parameter ratio = 20.3

checkCIF/PLATON results

No syntax errors found




Alert level B PLAT480_ALERT_4_B Long H...A H-Bond Reported H4W .. O5 .. 2.98 Ang. PLAT480_ALERT_4_B Long H...A H-Bond Reported H2O .. O3W .. 3.00 Ang.
Alert level C PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.09 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.42 Ratio PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for S1 PLAT480_ALERT_4_C Long H...A H-Bond Reported H1O .. O2 .. 2.80 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H2W .. S1 .. 2.98 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H2W .. O3 .. 2.95 Ang. PLAT481_ALERT_4_C Long D...A H-Bond Reported O2W .. O5 .. 3.57 Ang.
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 7 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 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 6 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: XSCANS (Siemens, 1996); cell refinement: XSCANS; data reduction: XSCANS; 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: WinGX (Farrugia, 1999).

µ-[2,8-Dimethyl-5,11-bis(dimethylethyleneamine)-1,4,5,6,7,10,11,12- octahydroimidazo[4,5-h]imidazo[4,5-c][1,6]diazecine]bis[aquasulfatocopper(II)] hexahydrate top
Crystal data top
[Cu2(SO4)2(C20H36N8)(H2O)2]·6H2OZ = 1
Mr = 851.9F(000) = 446
Triclinic, P1Dx = 1.643 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.902 (2) ÅCell parameters from 51 reflections
b = 9.036 (2) Åθ = 5.0–22.6°
c = 15.164 (4) ŵ = 1.44 mm1
α = 103.60 (1)°T = 298 K
β = 93.36 (1)°Prism, green
γ = 108.75 (1)°0.25 × 0.1 × 0.1 mm
V = 861.1 (4) Å3
Data collection top
Siemens P4
diffractometer
θmax = 30°, θmin = 1.4°
Graphite monochromatorh = 19
2θ/ω scansk = 1211
6105 measured reflectionsl = 2121
4960 independent reflections3 standard reflections every 97 reflections
2931 reflections with I > 2σ(I) intensity decay: 6.3%
Rint = 0.050
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)] = 0.061Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.148H atoms treated by a mixture of independent and constrained refinement
S = 0.98 w = 1/[σ2(Fo2) + (0.0626P)2]
where P = (Fo2 + 2Fc2)/3
4960 reflections(Δ/σ)max < 0.001
244 parametersΔρmax = 0.66 e Å3
12 restraintsΔρmin = 0.57 e Å3
Special details top

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
Cu10.91530 (9)0.78851 (6)0.70690 (4)0.01848 (15)
C20.7129 (7)0.7272 (5)0.5026 (3)0.0222 (9)
C40.7944 (6)0.5371 (5)0.5427 (3)0.0176 (8)
C50.7452 (7)0.4852 (5)0.4500 (3)0.0205 (9)
C60.8753 (7)0.4720 (5)0.6138 (3)0.0199 (9)
H6A0.76970.43450.65090.024*
H6B0.91830.38230.58490.024*
C81.1243 (7)0.5762 (5)0.7575 (3)0.0237 (9)
H8A1.26890.64060.77920.028*
H8B1.10970.46250.74510.028*
C90.9963 (9)0.6158 (6)0.8295 (3)0.0320 (11)
H9A0.85860.53460.81410.038*
H9B1.05740.61260.8880.038*
C121.1806 (10)0.9094 (7)0.8826 (4)0.0501 (16)
H12A1.16681.01360.88850.075*
H12B1.28680.89980.84590.075*
H12C1.21690.89880.94240.075*
C110.8161 (12)0.7931 (8)0.8953 (4)0.0546 (18)
H11A0.85040.7780.9540.082*
H11B0.68650.71160.86520.082*
H11C0.80520.89860.90350.082*
C130.6654 (9)0.8767 (6)0.5040 (3)0.0325 (11)
H13A0.60370.90530.55760.049*
H13B0.5710.85780.45010.049*
H13C0.79080.96370.50520.049*
C141.2291 (7)0.6565 (5)0.6157 (3)0.0216 (9)
H14A1.20270.7280.58150.026*
H14B1.35770.71650.65710.026*
N10.6929 (6)0.6092 (4)0.4261 (2)0.0231 (8)
H10.65410.60990.37130.028*
N30.7759 (6)0.6867 (4)0.5751 (2)0.0219 (8)
N71.0562 (5)0.6110 (4)0.6716 (2)0.0177 (7)
N100.9812 (7)0.7795 (5)0.8380 (3)0.0312 (9)
O11.1668 (6)0.9836 (4)0.6799 (3)0.0367 (9)
O20.7332 (5)0.9176 (4)0.7371 (2)0.0270 (7)
O1W0.2731 (6)0.3758 (5)0.8992 (3)0.0409 (9)
O30.9299 (6)1.1708 (4)0.7052 (3)0.0446 (10)
O2W0.6273 (8)0.3235 (7)0.9753 (3)0.0656 (15)
O40.8566 (7)1.1692 (5)0.8585 (3)0.0505 (11)
O3W0.4710 (6)0.3846 (4)0.7449 (2)0.0316 (8)
O50.5820 (6)1.1208 (5)0.7389 (4)0.0580 (13)
S10.77740 (19)1.09736 (14)0.76037 (9)0.0297 (3)
H1O1.121 (7)1.061 (6)0.689 (4)0.045*
H2O1.286 (6)1.024 (6)0.712 (4)0.045*
H1W0.284 (9)0.449 (5)0.941 (3)0.045*
H2W0.152 (4)0.315 (6)0.894 (4)0.045*
H5W0.409 (8)0.393 (7)0.792 (3)0.045*
H6W0.522 (8)0.315 (6)0.748 (4)0.045*
H3W0.521 (7)0.321 (7)0.945 (4)0.045*
H4W0.690 (7)0.282 (7)0.939 (4)0.045*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0230 (3)0.0169 (3)0.0167 (3)0.0102 (2)0.0025 (2)0.00214 (19)
C20.020 (2)0.023 (2)0.025 (2)0.0096 (18)0.0033 (18)0.0063 (18)
C40.0157 (19)0.0145 (19)0.022 (2)0.0058 (16)0.0041 (16)0.0016 (16)
C50.019 (2)0.021 (2)0.021 (2)0.0073 (17)0.0022 (17)0.0043 (17)
C60.021 (2)0.018 (2)0.020 (2)0.0057 (17)0.0039 (17)0.0040 (16)
C80.032 (3)0.025 (2)0.019 (2)0.017 (2)0.0000 (19)0.0062 (17)
C90.045 (3)0.033 (3)0.023 (2)0.020 (2)0.006 (2)0.008 (2)
C120.066 (4)0.043 (3)0.030 (3)0.014 (3)0.019 (3)0.002 (2)
C110.090 (5)0.068 (4)0.034 (3)0.056 (4)0.031 (3)0.021 (3)
C130.048 (3)0.031 (3)0.027 (2)0.025 (2)0.003 (2)0.010 (2)
C140.018 (2)0.021 (2)0.022 (2)0.0062 (17)0.0032 (17)0.0002 (17)
N10.026 (2)0.028 (2)0.0169 (18)0.0138 (17)0.0015 (15)0.0035 (15)
N30.027 (2)0.0219 (18)0.0185 (18)0.0135 (16)0.0046 (15)0.0016 (14)
N70.0215 (18)0.0153 (17)0.0158 (17)0.0082 (14)0.0013 (14)0.0009 (13)
N100.050 (3)0.027 (2)0.0204 (19)0.021 (2)0.0025 (19)0.0022 (16)
O10.0298 (19)0.0247 (18)0.056 (3)0.0089 (16)0.0089 (18)0.0117 (17)
O20.0306 (18)0.0176 (15)0.0333 (18)0.0117 (14)0.0064 (15)0.0024 (13)
O1W0.039 (2)0.047 (2)0.036 (2)0.0183 (19)0.0045 (18)0.0046 (18)
O30.048 (2)0.0287 (19)0.062 (3)0.0153 (18)0.013 (2)0.0175 (18)
O2W0.072 (3)0.082 (4)0.045 (3)0.054 (3)0.011 (2)0.014 (2)
O40.054 (3)0.039 (2)0.044 (2)0.014 (2)0.003 (2)0.0125 (18)
O3W0.038 (2)0.039 (2)0.0279 (18)0.0230 (17)0.0049 (15)0.0135 (16)
O50.033 (2)0.032 (2)0.110 (4)0.0215 (18)0.008 (2)0.009 (2)
S10.0252 (6)0.0201 (6)0.0416 (7)0.0133 (5)0.0018 (5)0.0020 (5)
Geometric parameters (Å, º) top
Cu1—O21.977 (3)C12—H12C0.96
Cu1—N32.027 (4)C11—N101.491 (7)
Cu1—N102.039 (4)C11—H11A0.96
Cu1—N72.113 (3)C11—H11B0.96
Cu1—O12.179 (4)C11—H11C0.96
C2—N31.329 (6)C13—H13A0.96
C2—N11.343 (5)C13—H13B0.96
C2—C131.485 (6)C13—H13C0.96
C4—C51.358 (6)C14—C5i1.493 (6)
C4—N31.375 (5)C14—N71.511 (6)
C4—C61.503 (6)C14—H14A0.97
C5—N11.396 (6)C14—H14B0.97
C5—C14i1.493 (6)N1—H10.86
C6—N71.501 (5)O1—H1O0.84 (4)
C6—H6A0.97O1—H2O0.85 (4)
C6—H6B0.97O2—S11.502 (3)
C8—N71.494 (5)O1W—H1W0.78 (4)
C8—C91.494 (6)O1W—H2W0.83 (2)
C8—H8A0.97O3—S11.471 (4)
C8—H8B0.97O2W—H3W0.83 (4)
C9—N101.493 (6)O2W—H4W0.81 (4)
C9—H9A0.97O4—S11.469 (4)
C9—H9B0.97O3W—H5W0.85 (4)
C12—N101.486 (7)O3W—H6W0.82 (4)
C12—H12A0.96O5—S11.461 (4)
C12—H12B0.96
O2—Cu1—N393.79 (14)N10—C11—H11C109.5
O2—Cu1—N1095.13 (15)H11A—C11—H11C109.5
N3—Cu1—N10152.59 (17)H11B—C11—H11C109.5
O2—Cu1—N7168.72 (13)C2—C13—H13A109.5
N3—Cu1—N781.75 (14)C2—C13—H13B109.5
N10—Cu1—N784.53 (15)H13A—C13—H13B109.5
O2—Cu1—O195.41 (14)C2—C13—H13C109.5
N3—Cu1—O196.43 (15)H13A—C13—H13C109.5
N10—Cu1—O1108.43 (17)H13B—C13—H13C109.5
N7—Cu1—O195.38 (14)C5i—C14—N7113.9 (4)
N3—C2—N1109.5 (4)C5i—C14—H14A108.8
N3—C2—C13126.2 (4)N7—C14—H14A108.8
N1—C2—C13124.2 (4)C5i—C14—H14B108.8
C5—C4—N3110.4 (4)N7—C14—H14B108.8
C5—C4—C6134.0 (4)H14A—C14—H14B107.7
N3—C4—C6115.4 (3)C2—N1—C5109.0 (4)
C4—C5—N1104.3 (4)C2—N1—H1125.5
C4—C5—C14i129.4 (4)C5—N1—H1125.5
N1—C5—C14i125.7 (4)C2—N3—C4106.7 (3)
N7—C6—C4105.7 (3)C2—N3—Cu1140.7 (3)
N7—C6—H6A110.6C4—N3—Cu1110.3 (3)
C4—C6—H6A110.6C8—N7—C6111.8 (3)
N7—C6—H6B110.6C8—N7—C14112.8 (3)
C4—C6—H6B110.6C6—N7—C14110.2 (3)
H6A—C6—H6B108.7C8—N7—Cu1108.4 (2)
N7—C8—C9109.9 (4)C6—N7—Cu199.8 (2)
N7—C8—H8A109.7C14—N7—Cu1113.2 (3)
C9—C8—H8A109.7C12—N10—C11109.6 (5)
N7—C8—H8B109.7C12—N10—C9110.8 (4)
C9—C8—H8B109.7C11—N10—C9107.4 (4)
H8A—C8—H8B108.2C12—N10—Cu1109.8 (3)
N10—C9—C8111.5 (4)C11—N10—Cu1113.7 (3)
N10—C9—H9A109.3C9—N10—Cu1105.5 (3)
C8—C9—H9A109.3Cu1—O1—H1O103 (4)
N10—C9—H9B109.3Cu1—O1—H2O123 (4)
C8—C9—H9B109.3H1O—O1—H2O104 (4)
H9A—C9—H9B108S1—O2—Cu1131.3 (2)
N10—C12—H12A109.5H1W—O1W—H2W104 (5)
N10—C12—H12B109.5H3W—O2W—H4W107 (4)
H12A—C12—H12B109.5H5W—O3W—H6W104 (4)
N10—C12—H12C109.5O5—S1—O4110.0 (3)
H12A—C12—H12C109.5O5—S1—O3110.3 (3)
H12B—C12—H12C109.5O4—S1—O3110.2 (3)
N10—C11—H11A109.5O5—S1—O2107.0 (2)
N10—C11—H11B109.5O4—S1—O2109.5 (2)
H11A—C11—H11B109.5O3—S1—O2109.8 (2)
N3—C4—C5—N10.6 (5)C5i—C14—N7—Cu1149.0 (3)
C6—C4—C5—N1176.0 (4)O2—Cu1—N7—C888.7 (7)
N3—C4—C5—C14i170.4 (4)N3—Cu1—N7—C8156.1 (3)
C6—C4—C5—C14i4.9 (8)N10—Cu1—N7—C80.1 (3)
C5—C4—C6—N7129.9 (5)O1—Cu1—N7—C8108.2 (3)
N3—C4—C6—N745.2 (5)O2—Cu1—N7—C628.3 (8)
N7—C8—C9—N1048.3 (5)N3—Cu1—N7—C639.1 (2)
N3—C2—N1—C50.1 (5)N10—Cu1—N7—C6117.1 (3)
C13—C2—N1—C5178.4 (4)O1—Cu1—N7—C6134.8 (2)
C4—C5—N1—C20.3 (5)O2—Cu1—N7—C14145.4 (6)
C14i—C5—N1—C2171.2 (4)N3—Cu1—N7—C1478.0 (3)
N1—C2—N3—C40.4 (5)N10—Cu1—N7—C14125.8 (3)
C13—C2—N3—C4178.0 (4)O1—Cu1—N7—C1417.7 (3)
N1—C2—N3—Cu1159.5 (4)C8—C9—N10—C1272.4 (5)
C13—C2—N3—Cu122.1 (8)C8—C9—N10—C11167.8 (4)
C5—C4—N3—C20.7 (5)C8—C9—N10—Cu146.3 (5)
C6—C4—N3—C2177.0 (4)O2—Cu1—N10—C1296.3 (4)
C5—C4—N3—Cu1165.9 (3)N3—Cu1—N10—C12155.2 (4)
C6—C4—N3—Cu110.4 (4)N7—Cu1—N10—C1295.0 (4)
O2—Cu1—N3—C248.2 (5)O1—Cu1—N10—C121.2 (4)
N10—Cu1—N3—C2157.0 (5)O2—Cu1—N10—C1126.9 (4)
N7—Cu1—N3—C2142.2 (5)N3—Cu1—N10—C1181.6 (5)
O1—Cu1—N3—C247.7 (5)N7—Cu1—N10—C11141.8 (4)
O2—Cu1—N3—C4152.4 (3)O1—Cu1—N10—C11124.3 (4)
N10—Cu1—N3—C443.5 (5)O2—Cu1—N10—C9144.3 (3)
N7—Cu1—N3—C417.2 (3)N3—Cu1—N10—C935.8 (5)
O1—Cu1—N3—C4111.8 (3)N7—Cu1—N10—C924.4 (3)
C9—C8—N7—C684.2 (4)O1—Cu1—N10—C9118.3 (3)
C9—C8—N7—C14151.0 (4)N3—Cu1—O2—S1112.5 (3)
C9—C8—N7—Cu124.8 (4)N10—Cu1—O2—S193.5 (3)
C4—C6—N7—C8167.4 (3)N7—Cu1—O2—S1178.8 (6)
C4—C6—N7—C1466.4 (4)O1—Cu1—O2—S115.7 (3)
C4—C6—N7—Cu152.9 (3)Cu1—O2—S1—O5156.7 (3)
C5i—C14—N7—C887.4 (4)Cu1—O2—S1—O484.0 (3)
C5i—C14—N7—C638.2 (5)Cu1—O2—S1—O337.0 (3)
Symmetry code: (i) x+2, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1O···O20.84 (4)2.80 (5)3.077 (5)102 (4)
O1—H1O···O30.84 (4)1.89 (4)2.688 (5)159 (5)
O1—H1O···S10.84 (4)2.75 (5)3.368 (4)132 (5)
O2W—H3W···O1W0.83 (4)2.06 (4)2.864 (6)163 (5)
O3W—H5W···O1W0.85 (4)1.94 (4)2.783 (5)170 (5)
O2W—H4W···O4ii0.81 (4)2.05 (4)2.859 (6)174 (6)
O2W—H4W···O5ii0.81 (4)2.98 (5)3.566 (7)131 (4)
O3W—H6W···O5ii0.82 (4)1.91 (4)2.713 (5)167 (6)
O1—H2O···O5iii0.85 (4)1.92 (4)2.728 (5)158 (6)
O1W—H1W···O2Wiv0.78 (4)2.02 (4)2.773 (6)162 (6)
N1—H1···O3Wv0.861.932.788 (5)171
O1—H2O···O3Wvi0.85 (4)3.00 (5)3.420 (5)113 (4)
O1W—H2W···S1vii0.83 (2)2.98 (4)3.688 (4)145 (5)
O1W—H2W···O3vii0.83 (2)2.95 (5)3.391 (6)116 (5)
O1W—H2W···O4vii0.83 (2)2.00 (2)2.815 (6)170 (6)
Symmetry codes: (ii) x, y1, z; (iii) x+1, y, z; (iv) x+1, y+1, z+2; (v) x+1, y+1, z+1; (vi) x+1, y+1, z; (vii) x1, y1, z.
 

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