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In the title polymeric compound, [Cu2(C8H3NO6)2(C10H8N2)(H2O)2]n, the unique Cu atom, the water molecule and the nitrogen heterocycle lie on mirror planes, and the disordered nitrophthalate dianion lies on a twofold axis. The Cu atom shows square-planar coordination as it is bonded to the O atoms of two carboxyl groups, to the N atom of a pyridyl ring and to a water molecule.
Supporting information
CCDC reference: 269401
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.007 Å
- R factor = 0.050
- wR factor = 0.137
- Data-to-parameter ratio = 12.6
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio
PLAT048_ALERT_1_C MoietyFormula Not Given ........................ ?
PLAT215_ALERT_3_C Disordered N2 has ADP max/min Ratio ....... 3.60
PLAT220_ALERT_2_C Large Non-Solvent N Ueq(max)/Ueq(min) ... 3.46 Ratio
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.31 Ratio
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C6
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C4
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.84
PLAT301_ALERT_3_C Main Residue Disorder ......................... 12.00 Perc.
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond C2 - C4 ... 1.36 Ang.
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond C4 - C4_e ... 1.38 Ang.
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
25 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
7 ALERT type 2 Indicator that the structure model may be wrong or deficient
3 ALERT type 3 Indicator that the structure quality may be low
12 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; 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.
catena-Poly[[µ-4,4'-bipyridine-bis[aquacopper(II)]]-di-µ-2-nitroterephthalato]
top
Crystal data top
[Cu2(C8H3NO6)2(C10H8N2)(H2O)2] | F(000) = 1488 |
Mr = 737.52 | Dx = 1.826 Mg m−3 |
Orthorhombic, Cmca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2 b c 2 | Cell parameters from 1365 reflections |
a = 21.662 (2) Å | θ = 2.4–23.2° |
b = 16.726 (2) Å | µ = 1.67 mm−1 |
c = 7.405 (1) Å | T = 295 K |
V = 2683.0 (5) Å3 | Block, blue |
Z = 4 | 0.29 × 0.15 × 0.12 mm |
Data collection top
Bruker SMART area-detector diffractometer | 1579 independent reflections |
Radiation source: fine-focus sealed tube | 980 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.082 |
φ and ω scans | θmax = 27.5°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −27→18 |
Tmin = 0.656, Tmax = 0.825 | k = −21→21 |
7488 measured reflections | l = −9→9 |
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) = 0.137 | H-atom parameters constrained |
S = 0.92 | w = 1/[σ2(Fo2) + (0.0768P)2] where P = (Fo2 + 2Fc2)/3 |
1579 reflections | (Δ/σ)max = 0.001 |
125 parameters | Δρmax = 0.64 e Å−3 |
15 restraints | Δρmin = −0.49 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Cu1 | 0.5000 | 0.65032 (5) | 0.8339 (1) | 0.0370 (3) | |
O1 | 0.4108 (1) | 0.6461 (2) | 0.8131 (5) | 0.051 (1) | |
O2 | 0.4018 (2) | 0.7729 (3) | 0.9007 (6) | 0.069 (1) | |
O3 | 0.3180 (5) | 0.5419 (7) | 0.964 (2) | 0.129 (4) | 0.50 |
O4 | 0.3030 (6) | 0.516 (1) | 0.676 (3) | 0.166 (6) | 0.50 |
O1w | 0.5000 | 0.7008 (4) | 0.5997 (6) | 0.051 (1) | |
N1 | 0.5000 | 0.5961 (3) | 1.0736 (7) | 0.037 (1) | |
N2 | 0.3011 (5) | 0.5542 (7) | 0.811 (2) | 0.131 (7) | 0.50 |
C1 | 0.3807 (2) | 0.7105 (4) | 0.8433 (6) | 0.046 (1) | |
C2 | 0.3127 (2) | 0.7075 (3) | 0.7958 (6) | 0.038 (1) | |
C3 | 0.2807 (2) | 0.7780 (3) | 0.7723 (6) | 0.040 (1) | |
C4 | 0.2809 (2) | 0.6380 (3) | 0.7717 (9) | 0.054 (1) | |
C5 | 0.5518 (2) | 0.5771 (4) | 1.1583 (8) | 0.064 (2) | |
C6 | 0.5534 (2) | 0.5389 (4) | 1.3219 (8) | 0.068 (2) | |
C7 | 0.5000 | 0.5194 (4) | 1.4090 (8) | 0.035 (1) | |
H1w | 0.5356 | 0.6964 | 0.5523 | 0.062* | |
H3 | 0.3012 | 0.8264 | 0.7868 | 0.048* | |
H4 | 0.3015 | 0.5895 | 0.7848 | 0.064* | 0.50 |
H5 | 0.5891 | 0.5904 | 1.1038 | 0.076* | |
H6 | 0.5912 | 0.5262 | 1.3741 | 0.081* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.0167 (4) | 0.0530 (6) | 0.0414 (5) | 0.000 | 0.000 | 0.0163 (4) |
O1 | 0.018 (2) | 0.074 (2) | 0.061 (2) | 0.002 (2) | 0.001 (1) | 0.030 (2) |
O2 | 0.032 (2) | 0.103 (3) | 0.073 (3) | −0.007 (2) | −0.0179 (18) | −0.027 (2) |
O3 | 0.093 (7) | 0.113 (7) | 0.180 (9) | −0.008 (6) | 0.016 (7) | 0.046 (7) |
O4 | 0.106 (8) | 0.17 (1) | 0.23 (1) | 0.026 (7) | −0.050 (8) | −0.044 (8) |
O1w | 0.019 (2) | 0.090 (4) | 0.045 (3) | 0.000 | 0.000 | 0.020 (3) |
N1 | 0.025 (3) | 0.049 (4) | 0.038 (3) | 0.000 | 0.000 | 0.009 (3) |
N2 | 0.026 (6) | 0.22 (2) | 0.14 (1) | −0.017 (8) | −0.023 (7) | −0.04 (2) |
C1 | 0.022 (2) | 0.086 (4) | 0.030 (2) | −0.002 (2) | −0.003 (2) | 0.008 (3) |
C2 | 0.021 (2) | 0.060 (3) | 0.033 (3) | 0.003 (2) | −0.002 (2) | 0.002 (2) |
C3 | 0.024 (2) | 0.055 (3) | 0.041 (3) | −0.006 (2) | −0.003 (2) | −0.004 (2) |
C4 | 0.033 (3) | 0.044 (3) | 0.084 (4) | 0.009 (2) | −0.005 (3) | 0.005 (3) |
C5 | 0.022 (2) | 0.111 (5) | 0.058 (3) | 0.001 (3) | 0.000 (2) | 0.041 (4) |
C6 | 0.026 (3) | 0.119 (5) | 0.057 (3) | 0.004 (3) | −0.003 (2) | 0.044 (4) |
C7 | 0.034 (3) | 0.037 (4) | 0.034 (3) | 0.000 | 0.000 | 0.008 (3) |
Geometric parameters (Å, º) top
Cu1—O1 | 1.939 (3) | C2—C3 | 1.379 (7) |
Cu1—O1i | 1.939 (3) | C3—C3ii | 1.372 (8) |
Cu1—O1w | 1.928 (5) | C4—C4ii | 1.38 (1) |
Cu1—N1 | 1.993 (5) | C5—C6 | 1.370 (7) |
O1—C1 | 1.278 (6) | C6—C7 | 1.363 (6) |
O2—C1 | 1.216 (7) | C7—C6i | 1.363 (6) |
O3—N2 | 1.212 (9) | C7—C7iii | 1.50 (1) |
O4—N2 | 1.19 (1) | O1w—H1w | 0.85 |
N1—C5i | 1.324 (5) | C3—H3 | 0.93 |
N1—C5 | 1.324 (5) | C4—H4 | 0.93 |
C1—C2 | 1.516 (6) | C5—H5 | 0.93 |
C2—C4 | 1.362 (7) | C6—H6 | 0.93 |
| | | |
O1—Cu1—O1i | 170.0 (2) | C3ii—C3—C2 | 121.2 (3) |
O1—Cu1—O1w | 86.8 (1) | C2—C4—C4ii | 121.4 (3) |
O1—Cu1—N1 | 93.1 (1) | N1—C5—C6 | 123.5 (5) |
O1i—Cu1—O1w | 86.8 (1) | C7—C6—C5 | 120.6 (5) |
O1i—Cu1—N1 | 93.1 (1) | C6i—C7—C6 | 116.0 (6) |
O1w—Cu1—N1 | 178.9 (2) | C6i—C7—C7iii | 122.0 (3) |
C1—O1—Cu1 | 117.7 (3) | C6—C7—C7iii | 122.0 (3) |
C5i—N1—C5 | 115.8 (6) | Cu1—O1w—H1w | 109.5 |
C5i—N1—Cu1 | 122.1 (3) | C3ii—C3—H3 | 119.4 |
C5—N1—Cu1 | 122.1 (3) | C2—C3—H3 | 119.4 |
O4—N2—O3 | 134 (2) | C2—C4—H4 | 119.3 |
O2—C1—O1 | 126.3 (4) | C4ii—C4—H4 | 119.3 |
O2—C1—C2 | 118.4 (5) | N1—C5—H5 | 118.2 |
O1—C1—C2 | 115.3 (5) | C6—C5—H5 | 118.2 |
C4—C2—C3 | 117.4 (4) | C7—C6—H6 | 119.7 |
C4—C2—C1 | 123.3 (5) | C5—C6—H6 | 119.7 |
C3—C2—C1 | 119.3 (4) | | |
| | | |
O1w—Cu1—O1—C1 | −77.9 (4) | O2—C1—C2—C3 | 17.1 (7) |
O1i—Cu1—O1—C1 | −129 (1) | O1—C1—C2—C3 | −161.0 (4) |
N1—Cu1—O1—C1 | 103.2 (4) | C4—C2—C3—C3ii | 0.5 (8) |
O1—Cu1—N1—C5i | −4.0 (5) | C1—C2—C3—C3ii | 179.4 (5) |
O1i—Cu1—N1—C5i | −176.2 (5) | C3—C2—C4—C4ii | −1 (1) |
O1—Cu1—N1—C5 | 176.2 (5) | C1—C2—C4—C4ii | −179.9 (7) |
O1i—Cu1—N1—C5 | 4.0 (5) | C5i—N1—C5—C6 | 1 (1) |
Cu1—O1—C1—O2 | −7.5 (7) | Cu1—N1—C5—C6 | −179.1 (5) |
Cu1—O1—C1—C2 | 170.4 (3) | N1—C5—C6—C7 | −1 (1) |
O2—C1—C2—C4 | −164.0 (5) | C5—C6—C7—C6i | 1 (1) |
O1—C1—C2—C4 | 17.9 (7) | C5—C6—C7—C7iii | −177.6 (7) |
Symmetry codes: (i) −x+1, y, z; (ii) −x+1/2, y, −z+3/2; (iii) −x+1, −y+1, −z+3. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w···O2iv | 0.85 | 1.83 | 2.625 (4) | 154 |
Symmetry code: (iv) −x+1, −y+3/2, z−1/2. |
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