Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807037154/dn2223sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807037154/dn2223Isup2.hkl |
CCDC reference: 660052
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.003 Å
- R factor = 0.023
- wR factor = 0.064
- Data-to-parameter ratio = 12.5
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O3
Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 1.01 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O5 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N3
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 PLAT794_ALERT_5_G Check Predicted Bond Valency for Cu1 (2) 2.08
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 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 1 ALERT type 5 Informative message, check
Cu(NO3)2.3H2O (0.0242 g, 0.1 mmol) was dissolved in a small test tube (5 ml e thanol),then 1,10-phenanthroline (0.0199 g, 1 mmol) was added, NaOH (0.006 g, 0.15 mmol) was then added to the above solution. The whole mixture was sealed in a close vessel with 30 ml e ther. 4 days later, blue crystals of (I) were obtained.
All H were fixed geometrically and treated as riding on their parent atoms with C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C).
Each CuIIion is five-coordinated and possess a slightly distorted square-pyramidal coordination geometry, defined by two N atoms from one 1,10-phenanthroline ligand, two O atoms of two different bridging nitrate acid anion, and one O atom of a symetry related mono-dentate nitrate anion (Fig. 1). The compound forms a one-dimensional chain using nitrate anion as an end-to-end bridging ligand. The Cu—N bond lengths is almost equal, with Cu1—N1 being 1.998 (2) Å and Cu1—N2 being 2.004 (2) Å, respectively. The bond length between Cu1 and O atoms which set at the peak of the square-pyramidal are longer than between the O atoms which locates at the plane of square-pyramidal, the shorter bond lengths of Cu1—O1 and Cu1—O6 being 1.9556 (17) Å and 1.9979 (18) Å, the longer Cu—O bond length is 2.3410 (18) Å for Cu1—O4.
The packing is further stabilized by π_π stacking interactions involving the phenanthroline ring systems, the distance between the closest centroids being 3.66\%A with an interplanar distance of 3.60\%A.
For related literature, see: McFadden & McPhail (1975).
Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
[Cu(NO3)3(C10H8N2)] | Z = 4 |
Mr = 367.77 | F(000) = 740.0 |
Monoclinic, P21/n | Dx = 1.815 Mg m−3 |
Hall symbol: -P 2yn | Mo Kα radiation, λ = 0.71073 Å |
a = 8.7832 (15) Å | µ = 1.66 mm−1 |
b = 9.1136 (16) Å | T = 293 K |
c = 17.173 (3) Å | Block, blue |
β = 101.686 (2)° | 0.40 × 0.25 × 0.20 mm |
V = 1346.2 (4) Å3 |
Bruker SMART CCD area-detector diffractometer | 2595 independent reflections |
Radiation source: fine-focus sealed tube | 2071 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
φ and ω scans | θmax = 26.0°, θmin = 2.4° |
Absorption correction: ψ scan (North et al., 1968) | h = −10→10 |
Tmin = 0.607, Tmax = 0.707 | k = −11→11 |
8361 measured reflections | l = −21→21 |
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)] = 0.024 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.064 | H-atom parameters constrained |
S = 1.06 | w = 1[σ2(Fo2) + (0.0308P)2 + 0.6118P] where P = (Fo2 + 2Fc2)3 |
2595 reflections | (Δ/σ)max = 0.002 |
208 parameters | Δρmax = 0.27 e Å−3 |
0 restraints | Δρmin = −0.27 e Å−3 |
[Cu(NO3)3(C10H8N2)] | V = 1346.2 (4) Å3 |
Mr = 367.77 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 8.7832 (15) Å | µ = 1.66 mm−1 |
b = 9.1136 (16) Å | T = 293 K |
c = 17.173 (3) Å | 0.40 × 0.25 × 0.20 mm |
β = 101.686 (2)° |
Bruker SMART CCD area-detector diffractometer | 2595 independent reflections |
Absorption correction: ψ scan (North et al., 1968) | 2071 reflections with I > 2σ(I) |
Tmin = 0.607, Tmax = 0.707 | Rint = 0.025 |
8361 measured reflections |
R[F2 > 2σ(F2)] = 0.024 | 0 restraints |
wR(F2) = 0.064 | H-atom parameters constrained |
S = 1.06 | Δρmax = 0.27 e Å−3 |
2595 reflections | Δρmin = −0.27 e Å−3 |
208 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Cu1 | 0.83503 (3) | 0.42791 (3) | 0.696821 (13) | 0.03409 (9) | |
N1 | 0.70510 (18) | 0.36714 (18) | 0.59243 (9) | 0.0336 (3) | |
N2 | 0.89172 (19) | 0.59365 (17) | 0.63144 (10) | 0.0348 (4) | |
N3 | 1.0982 (2) | 0.4773 (2) | 0.81600 (10) | 0.0411 (4) | |
N4 | 0.88410 (19) | 0.12873 (19) | 0.72182 (10) | 0.0375 (4) | |
O1 | 0.95129 (17) | 0.50491 (18) | 0.79780 (8) | 0.0459 (4) | |
O2 | 1.1715 (2) | 0.5285 (2) | 0.87827 (10) | 0.0624 (5) | |
O3 | 1.1543 (2) | 0.4000 (3) | 0.77103 (11) | 0.0764 (6) | |
O4 | 0.87904 (17) | 0.00535 (16) | 0.75191 (9) | 0.0459 (4) | |
O5 | 0.9548 (2) | 0.15217 (19) | 0.66849 (11) | 0.0620 (5) | |
O6 | 0.81196 (16) | 0.23479 (15) | 0.74821 (8) | 0.0387 (3) | |
C1 | 0.6044 (2) | 0.2574 (2) | 0.57589 (12) | 0.0409 (5) | |
H1 | 0.5843 | 0.1996 | 0.6173 | 0.049* | |
C2 | 0.5276 (3) | 0.2260 (2) | 0.49841 (13) | 0.0447 (5) | |
H2 | 0.4563 | 0.1494 | 0.4889 | 0.054* | |
C3 | 0.5575 (2) | 0.3078 (2) | 0.43656 (12) | 0.0415 (5) | |
H3 | 0.5078 | 0.2863 | 0.3847 | 0.050* | |
C4 | 0.6639 (2) | 0.4248 (2) | 0.45183 (11) | 0.0356 (4) | |
C5 | 0.7326 (2) | 0.4513 (2) | 0.53139 (11) | 0.0308 (4) | |
C6 | 0.7046 (3) | 0.5186 (3) | 0.39209 (12) | 0.0439 (5) | |
H6 | 0.6634 | 0.5001 | 0.3387 | 0.053* | |
C7 | 0.8020 (3) | 0.6335 (3) | 0.41217 (12) | 0.0443 (5) | |
H7 | 0.8270 | 0.6923 | 0.3723 | 0.053* | |
C8 | 0.8675 (2) | 0.6664 (2) | 0.49334 (12) | 0.0372 (4) | |
C9 | 0.8347 (2) | 0.5732 (2) | 0.55247 (11) | 0.0316 (4) | |
C10 | 0.9630 (3) | 0.7881 (2) | 0.51904 (14) | 0.0469 (5) | |
H10 | 0.9897 | 0.8527 | 0.4821 | 0.056* | |
C11 | 1.0165 (3) | 0.8110 (2) | 0.59846 (14) | 0.0492 (5) | |
H11 | 1.0774 | 0.8926 | 0.6159 | 0.059* | |
C12 | 0.9792 (2) | 0.7110 (2) | 0.65335 (13) | 0.0430 (5) | |
H12 | 1.0171 | 0.7274 | 0.7072 | 0.052* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.04125 (15) | 0.03153 (14) | 0.02821 (13) | −0.00254 (10) | 0.00398 (10) | −0.00099 (9) |
N1 | 0.0400 (9) | 0.0289 (8) | 0.0312 (8) | −0.0026 (7) | 0.0059 (7) | 0.0014 (7) |
N2 | 0.0376 (8) | 0.0304 (8) | 0.0365 (8) | −0.0013 (7) | 0.0075 (7) | −0.0034 (7) |
N3 | 0.0447 (10) | 0.0394 (9) | 0.0374 (9) | 0.0016 (8) | 0.0040 (8) | 0.0007 (8) |
N4 | 0.0375 (9) | 0.0358 (9) | 0.0382 (9) | −0.0020 (8) | 0.0052 (7) | 0.0025 (8) |
O1 | 0.0427 (8) | 0.0510 (9) | 0.0400 (8) | 0.0055 (7) | −0.0014 (6) | −0.0121 (7) |
O2 | 0.0539 (10) | 0.0664 (11) | 0.0564 (10) | 0.0050 (9) | −0.0136 (8) | −0.0195 (9) |
O3 | 0.0592 (11) | 0.1147 (17) | 0.0551 (11) | 0.0235 (11) | 0.0110 (9) | −0.0262 (11) |
O4 | 0.0466 (8) | 0.0337 (8) | 0.0578 (9) | 0.0045 (7) | 0.0120 (7) | 0.0140 (7) |
O5 | 0.0791 (12) | 0.0495 (10) | 0.0710 (11) | 0.0040 (9) | 0.0474 (10) | 0.0071 (9) |
O6 | 0.0498 (8) | 0.0342 (7) | 0.0333 (7) | 0.0056 (6) | 0.0110 (6) | 0.0023 (6) |
C1 | 0.0478 (11) | 0.0329 (10) | 0.0406 (11) | −0.0070 (9) | 0.0059 (9) | 0.0033 (9) |
C2 | 0.0480 (12) | 0.0345 (11) | 0.0478 (12) | −0.0085 (9) | 0.0006 (10) | −0.0035 (10) |
C3 | 0.0483 (12) | 0.0398 (11) | 0.0336 (10) | 0.0003 (10) | 0.0016 (9) | −0.0060 (9) |
C4 | 0.0406 (10) | 0.0344 (10) | 0.0320 (9) | 0.0036 (9) | 0.0078 (8) | −0.0020 (8) |
C5 | 0.0345 (9) | 0.0275 (9) | 0.0311 (9) | 0.0027 (8) | 0.0085 (8) | 0.0003 (7) |
C6 | 0.0508 (12) | 0.0518 (13) | 0.0296 (10) | 0.0008 (11) | 0.0097 (9) | 0.0013 (9) |
C7 | 0.0515 (12) | 0.0473 (12) | 0.0374 (11) | 0.0019 (11) | 0.0168 (10) | 0.0093 (10) |
C8 | 0.0380 (10) | 0.0352 (10) | 0.0416 (10) | 0.0028 (9) | 0.0153 (9) | 0.0033 (9) |
C9 | 0.0333 (9) | 0.0285 (9) | 0.0342 (9) | 0.0028 (8) | 0.0097 (8) | −0.0014 (8) |
C10 | 0.0501 (12) | 0.0370 (12) | 0.0572 (13) | −0.0063 (10) | 0.0197 (11) | 0.0067 (10) |
C11 | 0.0481 (12) | 0.0358 (12) | 0.0638 (14) | −0.0119 (10) | 0.0117 (11) | −0.0036 (11) |
C12 | 0.0463 (11) | 0.0367 (11) | 0.0439 (11) | −0.0051 (9) | 0.0042 (9) | −0.0064 (9) |
Cu1—O1 | 1.9558 (14) | C2—C3 | 1.366 (3) |
Cu1—O6 | 1.9975 (14) | C2—H2 | 0.9300 |
Cu1—N1 | 1.9985 (16) | C3—C4 | 1.407 (3) |
Cu1—N2 | 2.0042 (17) | C3—H3 | 0.9300 |
Cu1—O4i | 2.3407 (15) | C4—C5 | 1.398 (3) |
N1—C1 | 1.327 (3) | C4—C6 | 1.435 (3) |
N1—C5 | 1.360 (2) | C5—C9 | 1.428 (3) |
N2—C12 | 1.326 (3) | C6—C7 | 1.352 (3) |
N2—C9 | 1.360 (2) | C6—H6 | 0.9300 |
N3—O3 | 1.221 (2) | C7—C8 | 1.428 (3) |
N3—O2 | 1.224 (2) | C7—H7 | 0.9300 |
N3—O1 | 1.289 (2) | C8—C9 | 1.398 (3) |
N4—O5 | 1.225 (2) | C8—C10 | 1.407 (3) |
N4—O4 | 1.242 (2) | C10—C11 | 1.366 (3) |
N4—O6 | 1.287 (2) | C10—H10 | 0.9300 |
O4—Cu1ii | 2.3407 (15) | C11—C12 | 1.397 (3) |
C1—C2 | 1.394 (3) | C11—H11 | 0.9300 |
C1—H1 | 0.9300 | C12—H12 | 0.9300 |
O1—Cu1—O6 | 90.34 (6) | C2—C3—C4 | 119.57 (18) |
O1—Cu1—N1 | 174.57 (6) | C2—C3—H3 | 120.2 |
O6—Cu1—N1 | 93.53 (6) | C4—C3—H3 | 120.2 |
O1—Cu1—N2 | 94.70 (7) | C5—C4—C3 | 116.87 (18) |
O6—Cu1—N2 | 166.06 (6) | C5—C4—C6 | 118.35 (18) |
N1—Cu1—N2 | 82.41 (7) | C3—C4—C6 | 124.78 (19) |
O1—Cu1—O4i | 82.72 (6) | N1—C5—C4 | 123.17 (17) |
O6—Cu1—O4i | 86.47 (6) | N1—C5—C9 | 116.37 (17) |
N1—Cu1—O4i | 93.71 (6) | C4—C5—C9 | 120.45 (17) |
N2—Cu1—O4i | 107.04 (6) | C7—C6—C4 | 121.03 (19) |
C1—N1—C5 | 118.36 (17) | C7—C6—H6 | 119.5 |
C1—N1—Cu1 | 129.46 (14) | C4—C6—H6 | 119.5 |
C5—N1—Cu1 | 112.15 (12) | C6—C7—C8 | 121.37 (19) |
C12—N2—C9 | 117.93 (17) | C6—C7—H7 | 119.3 |
C12—N2—Cu1 | 130.12 (14) | C8—C7—H7 | 119.3 |
C9—N2—Cu1 | 111.86 (12) | C9—C8—C10 | 116.66 (19) |
O3—N3—O2 | 124.37 (19) | C9—C8—C7 | 118.70 (19) |
O3—N3—O1 | 118.15 (18) | C10—C8—C7 | 124.64 (19) |
O2—N3—O1 | 117.47 (18) | N2—C9—C8 | 123.56 (18) |
O5—N4—O4 | 122.36 (18) | N2—C9—C5 | 116.42 (17) |
O5—N4—O6 | 119.50 (17) | C8—C9—C5 | 119.99 (18) |
O4—N4—O6 | 118.14 (16) | C11—C10—C8 | 119.8 (2) |
N3—O1—Cu1 | 117.52 (12) | C11—C10—H10 | 120.1 |
N4—O4—Cu1ii | 121.92 (12) | C8—C10—H10 | 120.1 |
N4—O6—Cu1 | 113.88 (11) | C10—C11—C12 | 119.6 (2) |
N1—C1—C2 | 122.10 (19) | C10—C11—H11 | 120.2 |
N1—C1—H1 | 119.0 | C12—C11—H11 | 120.2 |
C2—C1—H1 | 119.0 | N2—C12—C11 | 122.4 (2) |
C3—C2—C1 | 119.9 (2) | N2—C12—H12 | 118.8 |
C3—C2—H2 | 120.1 | C11—C12—H12 | 118.8 |
C1—C2—H2 | 120.1 |
Symmetry codes: (i) −x+3/2, y+1/2, −z+3/2; (ii) −x+3/2, y−1/2, −z+3/2. |
Experimental details
Crystal data | |
Chemical formula | [Cu(NO3)3(C10H8N2)] |
Mr | 367.77 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 8.7832 (15), 9.1136 (16), 17.173 (3) |
β (°) | 101.686 (2) |
V (Å3) | 1346.2 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.66 |
Crystal size (mm) | 0.40 × 0.25 × 0.20 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector |
Absorption correction | ψ scan (North et al., 1968) |
Tmin, Tmax | 0.607, 0.707 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8361, 2595, 2071 |
Rint | 0.025 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.024, 0.064, 1.06 |
No. of reflections | 2595 |
No. of parameters | 208 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.27, −0.27 |
Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1997), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 1997), SHELXL97.
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Each CuIIion is five-coordinated and possess a slightly distorted square-pyramidal coordination geometry, defined by two N atoms from one 1,10-phenanthroline ligand, two O atoms of two different bridging nitrate acid anion, and one O atom of a symetry related mono-dentate nitrate anion (Fig. 1). The compound forms a one-dimensional chain using nitrate anion as an end-to-end bridging ligand. The Cu—N bond lengths is almost equal, with Cu1—N1 being 1.998 (2) Å and Cu1—N2 being 2.004 (2) Å, respectively. The bond length between Cu1 and O atoms which set at the peak of the square-pyramidal are longer than between the O atoms which locates at the plane of square-pyramidal, the shorter bond lengths of Cu1—O1 and Cu1—O6 being 1.9556 (17) Å and 1.9979 (18) Å, the longer Cu—O bond length is 2.3410 (18) Å for Cu1—O4.
The packing is further stabilized by π_π stacking interactions involving the phenanthroline ring systems, the distance between the closest centroids being 3.66\%A with an interplanar distance of 3.60\%A.