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In the title controsymmetric dimeric copper(II) compound, [Cu
2(C
10H
7NO
4)
2(H
2O)
2], the Cu
II ion is five-coordinated in a square-pyramidal configuration, with one imine N atom, one phenolate O atom, one carboxylate O atom of the Schiff base and one O atom of a coordinated water molecule defining the basal plane, and the phenolate O atom of another Schiff base occupying the apical position. The Cu
II atoms are bridged by two phenolic O atoms, with a Cu
Cu distance of 3.250 (4) Å. In the crystal structure, the molecules are linked through intermolecular O—H
O hydrogen bonds, forming chains running along the
b axis.
Supporting information
CCDC reference: 620527
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.046
- wR factor = 0.125
- Data-to-parameter ratio = 13.7
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.97
PLAT150_ALERT_1_C Volume as Calculated Differs from that Given ... 1028.00 Ang-3
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.24
PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... O1A
CU1 O1A
Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
7 ALERT level C = Check and explain
2 ALERT level G = General alerts; check
7 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
0 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
Bis(µ
2-N-5-formysalicylideneglycinato-
κ4O,
N,
O':
O')bis[aquacopper(II)]
top
Crystal data top
[Cu2(C10H7NO4)2(H2O)2] | F(000) = 580 |
Mr = 573.44 | Dx = 1.853 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 793 reflections |
a = 9.281 (16) Å | θ = 2.8–27.1° |
b = 9.060 (15) Å | µ = 2.13 mm−1 |
c = 12.62 (2) Å | T = 293 K |
β = 104.495 (19)° | Block, green |
V = 1028 (3) Å3 | 0.30 × 0.20 × 0.20 mm |
Z = 2 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 2221 independent reflections |
Radiation source: fine-focus sealed tube | 1877 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.058 |
φ and ω scans | θmax = 27.0°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −11→11 |
Tmin = 0.567, Tmax = 0.675 | k = −9→11 |
4900 measured reflections | l = −13→16 |
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)] = 0.046 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.125 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0852P)2] where P = (Fo2 + 2Fc2)/3 |
2221 reflections | (Δ/σ)max = 0.002 |
162 parameters | Δρmax = 1.02 e Å−3 |
3 restraints | Δρmin = −0.84 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Cu1 | 0.60266 (4) | 1.11853 (4) | 0.45568 (3) | 0.02830 (17) | |
N1 | 0.7242 (2) | 0.9568 (3) | 0.43132 (18) | 0.0281 (5) | |
O1 | 0.6214 (2) | 1.0592 (2) | 0.60471 (16) | 0.0294 (5) | |
O2 | 1.1528 (3) | 0.7860 (3) | 0.97281 (18) | 0.0480 (6) | |
O3 | 0.5766 (3) | 1.1540 (3) | 0.29877 (17) | 0.0348 (5) | |
O4 | 0.5791 (3) | 1.0311 (2) | 0.14774 (16) | 0.0406 (6) | |
O5 | 0.4793 (2) | 1.2843 (2) | 0.47669 (17) | 0.0338 (5) | |
C1 | 0.8241 (4) | 0.8921 (3) | 0.5048 (3) | 0.0333 (7) | |
H1 | 0.8872 | 0.8259 | 0.4823 | 0.040* | |
C2 | 0.8447 (3) | 0.9158 (4) | 0.6205 (2) | 0.0301 (6) | |
C3 | 0.9708 (3) | 0.8548 (4) | 0.6918 (3) | 0.0332 (7) | |
H3 | 1.0397 | 0.8043 | 0.6631 | 0.040* | |
C4 | 0.9950 (3) | 0.8682 (3) | 0.8044 (3) | 0.0325 (7) | |
C5 | 0.8892 (3) | 0.9435 (4) | 0.8472 (2) | 0.0327 (7) | |
H5 | 0.9038 | 0.9515 | 0.9226 | 0.039* | |
C6 | 0.7661 (3) | 1.0046 (3) | 0.7797 (2) | 0.0319 (6) | |
H6 | 0.6981 | 1.0542 | 0.8099 | 0.038* | |
C7 | 0.7395 (3) | 0.9941 (3) | 0.6645 (2) | 0.0274 (6) | |
C8 | 1.1274 (3) | 0.8006 (4) | 0.8745 (3) | 0.0368 (7) | |
H8 | 1.1990 | 0.7656 | 0.8406 | 0.044* | |
C9 | 0.6961 (4) | 0.9192 (4) | 0.3162 (2) | 0.0341 (7) | |
H9A | 0.6386 | 0.8287 | 0.3016 | 0.041* | |
H9B | 0.7896 | 0.9037 | 0.2966 | 0.041* | |
C10 | 0.6109 (3) | 1.0443 (3) | 0.2492 (2) | 0.0304 (6) | |
H5B | 0.451 (4) | 1.349 (3) | 0.428 (2) | 0.042 (10)* | |
H5A | 0.485 (4) | 1.320 (4) | 0.5362 (16) | 0.048 (11)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.0321 (2) | 0.0299 (3) | 0.0185 (2) | 0.00479 (13) | −0.00185 (16) | 0.00197 (12) |
N1 | 0.0296 (11) | 0.0327 (14) | 0.0183 (11) | 0.0021 (10) | −0.0009 (9) | 0.0009 (9) |
O1 | 0.0250 (10) | 0.0384 (12) | 0.0205 (10) | 0.0054 (9) | −0.0022 (7) | 0.0037 (9) |
O2 | 0.0457 (13) | 0.0592 (17) | 0.0307 (13) | 0.0093 (12) | −0.0061 (10) | 0.0094 (11) |
O3 | 0.0458 (12) | 0.0324 (11) | 0.0209 (10) | 0.0012 (10) | −0.0012 (9) | 0.0027 (9) |
O4 | 0.0619 (15) | 0.0355 (13) | 0.0183 (10) | −0.0043 (11) | −0.0016 (9) | −0.0001 (9) |
O5 | 0.0429 (12) | 0.0302 (12) | 0.0228 (11) | 0.0051 (9) | −0.0022 (9) | 0.0009 (9) |
C1 | 0.0329 (15) | 0.0378 (18) | 0.0256 (15) | 0.0062 (12) | 0.0004 (12) | −0.0003 (12) |
C2 | 0.0263 (13) | 0.0370 (16) | 0.0221 (14) | 0.0022 (12) | −0.0031 (11) | 0.0002 (12) |
C3 | 0.0283 (14) | 0.0379 (17) | 0.0288 (15) | 0.0061 (12) | −0.0012 (12) | 0.0035 (12) |
C4 | 0.0285 (14) | 0.0361 (17) | 0.0264 (15) | 0.0002 (12) | −0.0055 (11) | 0.0042 (12) |
C5 | 0.0319 (14) | 0.0412 (18) | 0.0190 (13) | −0.0028 (13) | −0.0047 (11) | 0.0009 (12) |
C6 | 0.0323 (14) | 0.0364 (17) | 0.0242 (14) | 0.0038 (12) | 0.0019 (11) | −0.0008 (12) |
C7 | 0.0244 (12) | 0.0305 (15) | 0.0219 (13) | −0.0018 (11) | −0.0041 (10) | 0.0037 (11) |
C8 | 0.0315 (15) | 0.0404 (18) | 0.0314 (16) | 0.0026 (13) | −0.0056 (12) | 0.0026 (13) |
C9 | 0.0412 (16) | 0.0360 (16) | 0.0208 (14) | 0.0019 (13) | −0.0001 (12) | −0.0042 (12) |
C10 | 0.0336 (14) | 0.0308 (16) | 0.0228 (14) | −0.0072 (12) | −0.0005 (11) | 0.0019 (11) |
Geometric parameters (Å, º) top
Cu1—N1 | 1.920 (3) | C2—C3 | 1.399 (4) |
Cu1—O1 | 1.922 (4) | C2—C7 | 1.427 (4) |
Cu1—O1A | 2.589 (4) | C3—C4 | 1.388 (5) |
Cu1—O3 | 1.961 (4) | C3—H3 | 0.9300 |
Cu1—O5 | 1.946 (3) | C4—C5 | 1.410 (5) |
N1—C1 | 1.279 (4) | C4—C8 | 1.457 (4) |
N1—C9 | 1.451 (4) | C5—C6 | 1.360 (4) |
O1—C7 | 1.306 (3) | C5—H5 | 0.9300 |
O2—C8 | 1.212 (4) | C6—C7 | 1.416 (5) |
O3—C10 | 1.257 (4) | C6—H6 | 0.9300 |
O4—C10 | 1.246 (4) | C8—H8 | 0.9300 |
O5—H5B | 0.842 (18) | C9—C10 | 1.513 (4) |
O5—H5A | 0.808 (18) | C9—H9A | 0.9700 |
C1—C2 | 1.441 (5) | C9—H9B | 0.9700 |
C1—H1 | 0.9300 | | |
| | | |
N1—Cu1—O1 | 91.75 (11) | C3—C4—C8 | 118.8 (3) |
N1—Cu1—O5 | 178.55 (9) | C5—C4—C8 | 122.2 (3) |
O1—Cu1—O5 | 89.69 (11) | C6—C5—C4 | 120.9 (3) |
N1—Cu1—O3 | 83.81 (11) | C6—C5—H5 | 119.5 |
O1—Cu1—O3 | 172.98 (9) | C4—C5—H5 | 119.5 |
O5—Cu1—O3 | 94.77 (10) | C5—C6—C7 | 121.3 (3) |
C1—N1—C9 | 122.3 (3) | C5—C6—H6 | 119.4 |
C1—N1—Cu1 | 125.6 (2) | C7—C6—H6 | 119.4 |
C9—N1—Cu1 | 111.98 (18) | O1—C7—C6 | 118.0 (3) |
C7—O1—Cu1 | 123.33 (19) | O1—C7—C2 | 123.8 (3) |
C10—O3—Cu1 | 113.0 (2) | C6—C7—C2 | 118.2 (2) |
Cu1—O5—H5B | 122 (2) | O2—C8—C4 | 125.9 (3) |
Cu1—O5—H5A | 122 (3) | O2—C8—H8 | 117.1 |
H5B—O5—H5A | 110 (3) | C4—C8—H8 | 117.1 |
N1—C1—C2 | 123.7 (3) | N1—C9—C10 | 108.7 (3) |
N1—C1—H1 | 118.1 | N1—C9—H9A | 109.9 |
C2—C1—H1 | 118.1 | C10—C9—H9A | 109.9 |
C3—C2—C7 | 119.3 (3) | N1—C9—H9B | 109.9 |
C3—C2—C1 | 118.0 (3) | C10—C9—H9B | 109.9 |
C7—C2—C1 | 122.6 (3) | H9A—C9—H9B | 108.3 |
C4—C3—C2 | 121.3 (3) | O4—C10—O3 | 124.3 (3) |
C4—C3—H3 | 119.4 | O4—C10—C9 | 117.3 (3) |
C2—C3—H3 | 119.4 | O3—C10—C9 | 118.4 (3) |
C3—C4—C5 | 119.0 (3) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5A···O4i | 0.81 (2) | 1.99 (3) | 2.705 (4) | 148 (4) |
O5—H5B···O4ii | 0.84 (2) | 1.89 (2) | 2.708 (4) | 163 (3) |
Symmetry codes: (i) x, −y+5/2, z+1/2; (ii) −x+1, y+1/2, −z+1/2. |
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