In the title compound, [Cu2(CH3CO2)4(H2O)2]·2C11H6N2O, the dinuclear copper complex lies on a center of symmetry located midway between the two Cu atoms. The two Cu atoms are bridged by four acetate groups. The coordinated water molecules interact with the C11H6N2O molecules and bridging acetate ligands by hydrogen bonds, giving rise to a linear chain structure.
Supporting information
CCDC reference: 236019
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.006 Å
- R factor = 0.050
- wR factor = 0.114
- Data-to-parameter ratio = 16.5
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.89
PLAT127_ALERT_1_C Implicit Hall Symbol Inconsistent with Expl .... -P 2ya
PLAT128_ALERT_4_C Non-standard setting of Space group P21/c .... P21/a
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cu1 - O1W = 5.38 su
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat
O1W -H1W1 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat
O1W -H1# 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 2.01(3), Rep 2.010(10) ...... 3.00 su-Rat
H1# -N1 1.555 1.555
Alert level G
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: C30 H28 Cu2 N4 O12
Atom count from _chemical_formula_moiety:C30 H40 Cu2 N8 O14
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
10 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
2 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Tetra-µ-acetato-bis[aquacopper(II)]–4,5-diazafluoren-9-one (1/2)
top
Crystal data top
[Cu2(C2H3O2)4(H2O)2]·2C11H6N2O | F(000) = 780 |
Mr = 763.64 | Dx = 1.591 Mg m−3 |
Monoclinic, P21/a | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ya | Cell parameters from 8182 reflections |
a = 7.4661 (3) Å | θ = 2.5–27.7° |
b = 25.951 (1) Å | µ = 1.40 mm−1 |
c = 8.2342 (3) Å | T = 298 K |
β = 92.604 (1)° | Wedge, blue |
V = 1593.7 (1) Å3 | 0.32 × 0.24 × 0.21 mm |
Z = 2 | |
Data collection top
Bruker APEX area-detector diffractometer | 3753 independent reflections |
Radiation source: fine-focus sealed tube | 3120 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.044 |
φ and ω scans | θmax = 28.2°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −9→9 |
Tmin = 0.574, Tmax = 0.746 | k = −33→33 |
17996 measured reflections | l = −10→10 |
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)] = 0.050 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.114 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.12 | w = 1/[σ2(Fo2) + (0.0593P)2] where P = (Fo2 + 2Fc2)/3 |
3753 reflections | (Δ/σ)max = 0.001 |
227 parameters | Δρmax = 0.39 e Å−3 |
2 restraints | Δρmin = −0.60 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cu1 | 0.65362 (4) | 0.52446 (1) | 0.50035 (4) | 0.0292 (1) | |
O1 | 0.5214 (3) | 0.5801 (1) | 0.6030 (3) | 0.041 (1) | |
O2 | 0.2585 (3) | 0.5392 (1) | 0.6011 (3) | 0.039 (1) | |
O3 | 0.5618 (3) | 0.5494 (1) | 0.2866 (2) | 0.045 (1) | |
O4 | 0.3007 (3) | 0.5072 (1) | 0.2847 (2) | 0.042 (1) | |
O5 | 0.8710 (6) | 0.7722 (2) | −0.0983 (5) | 0.138 (2) | |
O1w | 0.9005 (3) | 0.5662 (1) | 0.5040 (3) | 0.044 (1) | |
N1 | 0.9394 (4) | 0.6184 (1) | 0.2056 (3) | 0.048 (1) | |
N2 | 1.0484 (4) | 0.7092 (1) | 0.4253 (4) | 0.055 (1) | |
C1 | 0.3567 (4) | 0.5781 (1) | 0.6279 (3) | 0.034 (1) | |
C2 | 0.2713 (4) | 0.6255 (1) | 0.6932 (4) | 0.045 (1) | |
C3 | 0.4127 (4) | 0.5365 (1) | 0.2228 (3) | 0.035 (1) | |
C4 | 0.3639 (5) | 0.5581 (1) | 0.0566 (4) | 0.050 (1) | |
C5 | 0.8870 (5) | 0.5857 (2) | 0.0857 (5) | 0.061 (1) | |
C6 | 0.8390 (6) | 0.6001 (2) | −0.0703 (6) | 0.077 (1) | |
C7 | 0.8394 (6) | 0.6510 (2) | −0.1102 (5) | 0.077 (1) | |
C8 | 0.8922 (5) | 0.6858 (2) | 0.0085 (4) | 0.056 (1) | |
C9 | 0.9074 (6) | 0.7433 (2) | 0.0133 (5) | 0.076 (1) | |
C10 | 0.9718 (5) | 0.7571 (1) | 0.1805 (5) | 0.058 (1) | |
C11 | 1.0104 (6) | 0.8035 (2) | 0.2568 (7) | 0.077 (1) | |
C12 | 1.0679 (6) | 0.8018 (2) | 0.4167 (7) | 0.079 (1) | |
C13 | 1.0858 (5) | 0.7552 (2) | 0.4941 (5) | 0.072 (1) | |
C14 | 0.9925 (4) | 0.7118 (1) | 0.2705 (4) | 0.042 (1) | |
C15 | 0.9419 (4) | 0.6675 (1) | 0.1633 (4) | 0.040 (1) | |
H1w1 | 0.915 (5) | 0.585 (1) | 0.423 (3) | 0.07 (1)* | |
H1w2 | 0.993 (3) | 0.549 (1) | 0.532 (4) | 0.04 (1)* | |
H2a | 0.3604 | 0.6458 | 0.7517 | 0.067* | |
H2b | 0.1794 | 0.6158 | 0.7651 | 0.067* | |
H2c | 0.2194 | 0.6454 | 0.6048 | 0.067* | |
H4a | 0.3101 | 0.5316 | −0.0106 | 0.074* | |
H4b | 0.4700 | 0.5706 | 0.0080 | 0.074* | |
H4c | 0.2804 | 0.5860 | 0.0665 | 0.074* | |
H5 | 0.8830 | 0.5508 | 0.1107 | 0.074* | |
H6 | 0.8066 | 0.5754 | −0.1480 | 0.093* | |
H7 | 0.8050 | 0.6619 | −0.2146 | 0.092* | |
H11 | 0.9977 | 0.8346 | 0.2015 | 0.093* | |
H12 | 1.0947 | 0.8321 | 0.4728 | 0.094* | |
H13 | 1.1270 | 0.7554 | 0.6024 | 0.087* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.0275 (2) | 0.0286 (2) | 0.0311 (2) | −0.0016 (1) | −0.0025 (1) | 0.0008 (1) |
O1 | 0.034 (1) | 0.031 (1) | 0.056 (1) | 0.000 (1) | 0.002 (1) | −0.008 (1) |
O2 | 0.033 (1) | 0.035 (1) | 0.049 (1) | 0.001 (1) | 0.002 (1) | −0.009 (1) |
O3 | 0.040 (1) | 0.055 (1) | 0.038 (1) | −0.005 (1) | −0.007 (1) | 0.016 (1) |
O4 | 0.044 (1) | 0.047 (1) | 0.034 (1) | −0.007 (1) | −0.008 (1) | 0.009 (1) |
O5 | 0.188 (5) | 0.112 (3) | 0.109 (3) | 0.017 (3) | −0.028 (3) | 0.069 (3) |
O1w | 0.033 (1) | 0.046 (1) | 0.052 (1) | −0.005 (1) | −0.005 (1) | 0.014 (1) |
N1 | 0.050 (2) | 0.043 (2) | 0.050 (2) | −0.007 (1) | 0.004 (1) | −0.001 (1) |
N2 | 0.058 (2) | 0.051 (2) | 0.056 (2) | −0.003 (1) | −0.006 (1) | −0.006 (1) |
C1 | 0.040 (2) | 0.031 (1) | 0.031 (1) | 0.006 (1) | −0.005 (1) | 0.001 (1) |
C2 | 0.051 (2) | 0.036 (2) | 0.048 (2) | 0.010 (1) | 0.002 (2) | −0.006 (1) |
C3 | 0.042 (2) | 0.034 (2) | 0.030 (1) | 0.007 (1) | −0.001 (1) | 0.000 (1) |
C4 | 0.050 (2) | 0.062 (2) | 0.036 (2) | 0.001 (2) | −0.007 (1) | 0.014 (2) |
C5 | 0.056 (2) | 0.059 (2) | 0.070 (3) | −0.015 (2) | 0.014 (2) | −0.015 (2) |
C6 | 0.059 (3) | 0.110 (4) | 0.065 (3) | −0.024 (2) | 0.012 (2) | −0.034 (3) |
C7 | 0.060 (2) | 0.132 (4) | 0.038 (2) | −0.005 (3) | −0.003 (2) | −0.002 (2) |
C8 | 0.046 (2) | 0.075 (3) | 0.048 (2) | 0.006 (2) | 0.001 (2) | 0.014 (2) |
C9 | 0.074 (3) | 0.078 (3) | 0.074 (3) | 0.014 (2) | 0.001 (2) | 0.039 (3) |
C10 | 0.049 (2) | 0.045 (2) | 0.078 (3) | 0.008 (2) | 0.008 (2) | 0.018 (2) |
C11 | 0.067 (3) | 0.040 (2) | 0.127 (4) | 0.011 (2) | 0.024 (3) | 0.017 (2) |
C12 | 0.061 (3) | 0.053 (2) | 0.122 (4) | −0.007 (2) | 0.021 (3) | −0.027 (3) |
C13 | 0.063 (2) | 0.078 (3) | 0.076 (3) | −0.012 (2) | 0.002 (2) | −0.025 (2) |
C14 | 0.035 (2) | 0.039 (2) | 0.054 (2) | 0.001 (1) | 0.004 (1) | 0.007 (1) |
C15 | 0.032 (2) | 0.047 (2) | 0.040 (2) | −0.002 (1) | 0.003 (1) | 0.005 (1) |
Geometric parameters (Å, º) top
Cu1—O1 | 1.963 (2) | C8—C9 | 1.497 (6) |
Cu1—O2i | 1.976 (2) | C9—C10 | 1.481 (6) |
Cu1—O3 | 1.969 (2) | C10—C11 | 1.383 (6) |
Cu1—O4i | 1.967 (2) | C10—C14 | 1.395 (4) |
Cu1—O1w | 2.137 (2) | C11—C12 | 1.367 (6) |
Cu1—Cu1i | 2.6214 (6) | C12—C13 | 1.371 (6) |
O1—C1 | 1.257 (3) | C14—C15 | 1.488 (4) |
O2—C1 | 1.262 (3) | O1W—H1w1 | 0.84 (1) |
O3—C3 | 1.255 (4) | O1W—H1w2 | 0.84 (1) |
O4—C3 | 1.256 (4) | C2—H2a | 0.96 |
O5—C9 | 1.207 (4) | C2—H2b | 0.96 |
N1—C15 | 1.320 (4) | C2—H2c | 0.96 |
N1—C5 | 1.346 (4) | C4—H4a | 0.96 |
N2—C14 | 1.324 (4) | C4—H4b | 0.96 |
N2—C13 | 1.344 (4) | C4—H4c | 0.96 |
C1—C2 | 1.497 (4) | C5—H5 | 0.93 |
C3—C4 | 1.508 (4) | C6—H6 | 0.93 |
C5—C6 | 1.369 (6) | C7—H7 | 0.93 |
C6—C7 | 1.362 (6) | C11—H11 | 0.93 |
C7—C8 | 1.375 (6) | C12—H12 | 0.93 |
C8—C15 | 1.395 (4) | C13—H13 | 0.93 |
| | | |
O1—Cu1—O2i | 168.6 (1) | C11—C12—C13 | 119.8 (4) |
O1—Cu1—O3 | 88.9 (1) | N2—C13—C12 | 124.9 (4) |
O1—Cu1—O4i | 89.4 (1) | N2—C14—C10 | 125.2 (3) |
O1—Cu1—O1w | 94.1 (1) | N2—C14—C15 | 126.4 (3) |
O2i—Cu1—O3 | 90.3 (1) | C10—C14—C15 | 108.4 (3) |
O2i—Cu1—O4i | 89.1 (1) | N1—C15—C8 | 124.3 (3) |
O2i—Cu1—O1w | 97.3 (1) | N1—C15—C14 | 126.5 (3) |
O3—Cu1—O4i | 168.7 (1) | C8—C15—C14 | 109.2 (3) |
O3—Cu1—O1w | 96.4 (1) | Cu1—O1w—H1w1 | 115 (3) |
O4i—Cu1—O1w | 94.9 (1) | Cu1—O1w—H1w2 | 116 (2) |
C1—O1—Cu1 | 123.7 (2) | H1w1—O1w—H1w2 | 113 (4) |
C1—O2—Cu1i | 122.8 (2) | C1—C2—H2a | 109.5 |
C3—O3—Cu1 | 123.5 (2) | C1—C2—H2b | 109.5 |
C3—O4—Cu1i | 121.8 (2) | H2a—C2—H2b | 109.5 |
C15—N1—C5 | 114.9 (3) | C1—C2—H2c | 109.5 |
C14—N2—C13 | 114.4 (3) | H2a—C2—H2c | 109.5 |
O1—C1—O2 | 124.7 (3) | H2b—C2—H2c | 109.5 |
O1—C1—C2 | 117.4 (3) | C3—C4—H4a | 109.5 |
O2—C1—C2 | 117.9 (3) | C3—C4—H4b | 109.5 |
O3—C3—O4 | 125.9 (3) | H4a—C4—H4b | 109.5 |
O3—C3—C4 | 117.0 (3) | C3—C4—H4c | 109.5 |
O4—C3—C4 | 117.1 (3) | H4a—C4—H4c | 109.5 |
N1—C5—C6 | 124.8 (4) | H4b—C4—H4c | 109.5 |
C7—C6—C5 | 119.1 (4) | N1—C5—H5 | 117.6 |
C6—C7—C8 | 118.0 (4) | C6—C5—H5 | 117.6 |
C7—C8—C15 | 118.8 (4) | C7—C6—H6 | 120.4 |
C7—C8—C9 | 133.8 (4) | C5—C6—H6 | 120.4 |
C15—C8—C9 | 107.4 (3) | C6—C7—H7 | 121.0 |
O5—C9—C10 | 127.6 (5) | C8—C7—H7 | 121.0 |
O5—C9—C8 | 125.8 (5) | C12—C11—H11 | 121.3 |
C10—C9—C8 | 106.6 (3) | C10—C11—H11 | 121.3 |
C11—C10—C14 | 118.5 (4) | C11—C12—H12 | 120.1 |
C11—C10—C9 | 133.2 (4) | C13—C12—H12 | 120.1 |
C14—C10—C9 | 108.3 (3) | N2—C13—H13 | 117.5 |
C12—C11—C10 | 117.3 (4) | C12—C13—H13 | 117.5 |
| | | |
O4i—Cu1—O1—C1 | −88.0 (2) | C15—C8—C9—C10 | 0.9 (4) |
O3—Cu1—O1—C1 | 80.8 (2) | O5—C9—C10—C11 | −0.9 (8) |
O2i—Cu1—O1—C1 | −5.5 (6) | C8—C9—C10—C11 | −179.9 (4) |
O1w—Cu1—O1—C1 | 177.1 (2) | O5—C9—C10—C14 | 178.5 (5) |
Cu1i—Cu1—O1—C1 | −2.8 (2) | C8—C9—C10—C14 | −0.5 (4) |
O1—Cu1—O3—C3 | −85.4 (2) | C14—C10—C11—C12 | 0.4 (6) |
O4i—Cu1—O3—C3 | −3.8 (6) | C9—C10—C11—C12 | 179.7 (4) |
O2i—Cu1—O3—C3 | 83.2 (2) | C10—C11—C12—C13 | 0.3 (6) |
O1w—Cu1—O3—C3 | −179.4 (2) | C14—N2—C13—C12 | 0.8 (6) |
Cu1i—Cu1—O3—C3 | −1.0 (2) | C11—C12—C13—N2 | −1.0 (7) |
Cu1—O1—C1—O2 | 5.1 (4) | C13—N2—C14—C10 | 0.0 (5) |
Cu1—O1—C1—C2 | −174.5 (2) | C13—N2—C14—C15 | 179.9 (3) |
Cu1i—O2—C1—O1 | −4.3 (4) | C11—C10—C14—N2 | −0.6 (5) |
Cu1i—O2—C1—C2 | 175.2 (2) | C9—C10—C14—N2 | 179.9 (3) |
Cu1—O3—C3—O4 | 1.2 (4) | C11—C10—C14—C15 | 179.5 (3) |
Cu1—O3—C3—C4 | −178.7 (2) | C9—C10—C14—C15 | 0.0 (4) |
Cu1i—O4—C3—O3 | −0.5 (4) | C5—N1—C15—C8 | 1.0 (5) |
Cu1i—O4—C3—C4 | 179.4 (2) | C5—N1—C15—C14 | 179.5 (3) |
C15—N1—C5—C6 | 0.3 (5) | C7—C8—C15—N1 | −1.0 (5) |
N1—C5—C6—C7 | −1.5 (6) | C9—C8—C15—N1 | 177.9 (3) |
C5—C6—C7—C8 | 1.4 (6) | C7—C8—C15—C14 | −179.7 (3) |
C6—C7—C8—C15 | −0.3 (6) | C9—C8—C15—C14 | −0.9 (4) |
C6—C7—C8—C9 | −178.8 (4) | N2—C14—C15—N1 | 2.0 (5) |
C7—C8—C9—O5 | 0.4 (8) | C10—C14—C15—N1 | −178.1 (3) |
C15—C8—C9—O5 | −178.2 (5) | N2—C14—C15—C8 | −179.3 (3) |
C7—C8—C9—C10 | 179.5 (4) | C10—C14—C15—C8 | 0.5 (4) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···N1 | 0.84 (1) | 2.01 (1) | 2.834 (3) | 170 (4) |
O1w—H1w2···O2ii | 0.84 (1) | 2.06 (2) | 2.843 (3) | 156 (3) |
Symmetry code: (ii) x+1, y, z. |