Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807051914/pv2039sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807051914/pv2039Isup2.hkl |
CCDC reference: 669125
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.003 Å
- R factor = 0.026
- wR factor = 0.052
- Data-to-parameter ratio = 16.7
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Cd1 - O1A .. 10.46 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Cd1 - O2A .. 18.39 su
Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.02 PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.53 Ratio PLAT230_ALERT_2_C Hirshfeld Test Diff for O2A - N1A .. 5.56 su PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2A PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N1A PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N1B PLAT420_ALERT_2_C D-H Without Acceptor N12B - H21B ... ? PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 3
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 Cd1 (2) 2.31
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 8 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 8 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 2 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For the geometrical studies of the coordination mode of the nitrate anion, see: Kleywegt et al. (1985) and Dowling et al., (1996).
1.8 g (1 mmol) of p-nitrobenzoylhydrazine was dissolved in 50 ml hot ethanol and mixed with 3 ml e thanolic solution of Cd(NO3)2 (3.1 g; 1 mmol). Pale yellow crystals were formed after 24 h, then filtered, washed with ethanol and dried in the air.
All the hydrogen atoms were visible in the difference maps and were included in the refienements with isotropic displacement parameters correlated with the anisotropic displacement parameters of the atoms to which they were bonded [C—H 0.93 Å and Uiso(H) = 1.2Ueq(C)]. The positions of hydrogen atoms from hydrazine group and water molecules were determined from the difference maps and were not refined [Uiso(H) = 1.5Ueq(N, O)].
In the title compound, cadmium is coordinated by two p-nitrobenzoylhydrazine molecules, a water molecules and a bidentate chelating nitrate. These ligands create atypical seven coordination sphere around the Cd atom and the geometry around Cd can be described as a pentagonal bipyramid. The Cd—Onitrate bond lenghts difference, Co—O—N angles difference and Co—N—Oterminal are 0.18 Å, 7.9° and 173° respectively, and correlate well with the bidentate mode of the nitrate group (Kleywegt et al., 1985; Dowling et al., 1996). Noncoordinated and bidentate chelating nitrates create hydrogen bonding network in a and b directions, respectively. Interestingly, both oxygen atoms from the –NO2 groups do not participate in hydrogen bonding network. But two parallel-oriented organic ligands help to establish the packing.
For the geometrical studies of the coordination mode of the nitrate anion, see: Kleywegt et al. (1985) and Dowling et al., (1996).
Data collection: CrysAlis (Mayer, 2006); cell refinement: CrysAlis (Mayer, 2006); data reduction: CrysAlis (Mayer, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2005); software used to prepare material for publication: publCIF (Westrip, 2007).
Fig. 1. Molecular diagram of the title compound; displacement ellipsoids are drawn at 50% probability level. |
[Cd(NO3)(C7H7N3O3)2(H2O)]NO3 | Z = 2 |
Mr = 616.75 | F(000) = 616 |
Triclinic, P1 | Dx = 1.922 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 5.6112 (5) Å | Cell parameters from 4512 reflections |
b = 13.1253 (12) Å | θ = 3.8–28.7° |
c = 14.8985 (13) Å | µ = 1.11 mm−1 |
α = 101.314 (8)° | T = 293 K |
β = 96.944 (7)° | Prism, pale yellow |
γ = 92.410 (7)° | 0.52 × 0.38 × 0.27 mm |
V = 1065.60 (16) Å3 |
Kuma KM-4 with CCD area-detector diffractometer | 5431 independent reflections |
Radiation source: fine-focus sealed tube | 4512 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1 | θmax = 28.7°, θmin = 3.8° |
ω scans | h = −7→5 |
Absorption correction: numerical (CrysAlis; Mayer, 2006) | k = −17→17 |
Tmin = 0.732, Tmax = 0.871 | l = −20→19 |
15437 measured reflections |
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)] = 0.026 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.052 | H-atom parameters constrained |
S = 0.97 | w = 1/[σ2(Fo2) + (0.0267P)2] where P = (Fo2 + 2Fc2)/3 |
5431 reflections | (Δ/σ)max = 0.002 |
325 parameters | Δρmax = 0.97 e Å−3 |
0 restraints | Δρmin = −0.48 e Å−3 |
[Cd(NO3)(C7H7N3O3)2(H2O)]NO3 | γ = 92.410 (7)° |
Mr = 616.75 | V = 1065.60 (16) Å3 |
Triclinic, P1 | Z = 2 |
a = 5.6112 (5) Å | Mo Kα radiation |
b = 13.1253 (12) Å | µ = 1.11 mm−1 |
c = 14.8985 (13) Å | T = 293 K |
α = 101.314 (8)° | 0.52 × 0.38 × 0.27 mm |
β = 96.944 (7)° |
Kuma KM-4 with CCD area-detector diffractometer | 5431 independent reflections |
Absorption correction: numerical (CrysAlis; Mayer, 2006) | 4512 reflections with I > 2σ(I) |
Tmin = 0.732, Tmax = 0.871 | Rint = 0.027 |
15437 measured reflections |
R[F2 > 2σ(F2)] = 0.026 | 0 restraints |
wR(F2) = 0.052 | H-atom parameters constrained |
S = 0.97 | Δρmax = 0.97 e Å−3 |
5431 reflections | Δρmin = −0.48 e Å−3 |
325 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 | ||
Cd1 | 0.59006 (2) | 0.274165 (10) | 0.565944 (9) | 0.03011 (5) | |
C1A | 0.5103 (3) | 0.52629 (13) | 0.81049 (12) | 0.0261 (4) | |
C11A | 0.5625 (3) | 0.46464 (13) | 0.71999 (13) | 0.0290 (4) | |
O11A | 0.4313 (2) | 0.38598 (10) | 0.68154 (10) | 0.0407 (3) | |
N11A | 0.7531 (3) | 0.49594 (12) | 0.68482 (11) | 0.0348 (4) | |
H11A | 0.8437 | 0.5527 | 0.7047 | 0.052* | |
N12A | 0.8041 (3) | 0.43772 (14) | 0.59929 (12) | 0.0460 (4) | |
H21A | 0.9605 | 0.4373 | 0.6088 | 0.069* | |
H22A | 0.7648 | 0.4700 | 0.5550 | 0.069* | |
C2A | 0.6575 (3) | 0.61149 (14) | 0.86218 (13) | 0.0330 (4) | |
H2A | 0.7939 | 0.6339 | 0.8398 | 0.040* | |
C3A | 0.6004 (3) | 0.66265 (14) | 0.94665 (13) | 0.0326 (4) | |
H3A | 0.6975 | 0.7193 | 0.9815 | 0.039* | |
C4A | 0.3976 (3) | 0.62799 (13) | 0.97783 (12) | 0.0268 (4) | |
N41A | 0.3394 (3) | 0.68027 (12) | 1.06882 (11) | 0.0333 (4) | |
O41A | 0.1525 (3) | 0.65143 (12) | 1.09355 (10) | 0.0501 (4) | |
O42A | 0.4805 (3) | 0.74886 (12) | 1.11520 (10) | 0.0508 (4) | |
C5A | 0.2474 (3) | 0.54486 (14) | 0.92790 (13) | 0.0323 (4) | |
H5A | 0.1096 | 0.5238 | 0.9502 | 0.039* | |
C6A | 0.3066 (3) | 0.49366 (14) | 0.84399 (13) | 0.0318 (4) | |
H6A | 0.2088 | 0.4369 | 0.8098 | 0.038* | |
C1B | 0.8042 (3) | 0.06198 (13) | 0.76333 (12) | 0.0260 (4) | |
C11B | 0.6867 (3) | 0.12651 (13) | 0.70058 (11) | 0.0249 (4) | |
O11B | 0.8056 (2) | 0.19365 (10) | 0.67342 (9) | 0.0330 (3) | |
N11B | 0.4503 (3) | 0.10695 (12) | 0.67616 (11) | 0.0299 (3) | |
H11B | 0.3780 | 0.0572 | 0.6923 | 0.045* | |
N12B | 0.3254 (3) | 0.15387 (12) | 0.60875 (11) | 0.0308 (3) | |
H21B | 0.2814 | 0.1053 | 0.5615 | 0.046* | |
H22B | 0.2058 | 0.1828 | 0.6323 | 0.046* | |
C2B | 1.0212 (3) | 0.10100 (14) | 0.81649 (13) | 0.0302 (4) | |
H2B | 1.0826 | 0.1678 | 0.8162 | 0.036* | |
C3B | 1.1467 (3) | 0.04045 (14) | 0.87002 (13) | 0.0332 (4) | |
H3B | 1.2942 | 0.0651 | 0.9047 | 0.040* | |
C4B | 1.0468 (3) | −0.05734 (14) | 0.87046 (12) | 0.0297 (4) | |
N41B | 1.1799 (3) | −0.12260 (13) | 0.92644 (11) | 0.0364 (4) | |
O41B | 1.0684 (3) | −0.19375 (12) | 0.94828 (11) | 0.0521 (4) | |
O42B | 1.3962 (3) | −0.10346 (13) | 0.94729 (13) | 0.0647 (5) | |
C5B | 0.8303 (3) | −0.09710 (15) | 0.82013 (14) | 0.0345 (4) | |
H5B | 0.7669 | −0.1630 | 0.8225 | 0.041* | |
C6B | 0.7087 (3) | −0.03661 (14) | 0.76572 (13) | 0.0337 (4) | |
H6B | 0.5623 | −0.0622 | 0.7306 | 0.040* | |
N1A | 0.8415 (3) | 0.12829 (13) | 0.44641 (11) | 0.0383 (4) | |
O1A | 0.9180 (2) | 0.22135 (10) | 0.48264 (9) | 0.0382 (3) | |
O2A | 0.6359 (3) | 0.09945 (13) | 0.45746 (11) | 0.0556 (4) | |
O3A | 0.9691 (3) | 0.06939 (14) | 0.40305 (15) | 0.0834 (7) | |
OW1 | 0.3449 (2) | 0.32151 (12) | 0.45157 (10) | 0.0459 (4) | |
HW1 | 0.2073 | 0.2912 | 0.4406 | 0.069* | |
HW2 | 0.4094 | 0.3029 | 0.4051 | 0.069* | |
N1B | 0.7706 (3) | 0.32891 (13) | 0.31690 (12) | 0.0374 (4) | |
O1B | 0.7783 (3) | 0.40791 (12) | 0.37923 (11) | 0.0529 (4) | |
O2B | 0.5936 (3) | 0.26465 (13) | 0.30181 (11) | 0.0552 (4) | |
O3B | 0.9381 (3) | 0.31474 (12) | 0.26942 (12) | 0.0562 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.03195 (8) | 0.02853 (8) | 0.03017 (8) | 0.00387 (5) | 0.00567 (5) | 0.00542 (5) |
C1A | 0.0274 (9) | 0.0229 (8) | 0.0294 (9) | 0.0037 (7) | 0.0061 (7) | 0.0068 (7) |
C11A | 0.0313 (10) | 0.0229 (9) | 0.0334 (10) | 0.0017 (7) | 0.0068 (8) | 0.0056 (8) |
O11A | 0.0430 (8) | 0.0320 (7) | 0.0442 (8) | −0.0111 (6) | 0.0201 (7) | −0.0050 (6) |
N11A | 0.0383 (9) | 0.0304 (8) | 0.0340 (9) | −0.0082 (7) | 0.0136 (7) | −0.0006 (7) |
N12A | 0.0553 (11) | 0.0431 (10) | 0.0381 (10) | −0.0116 (8) | 0.0232 (9) | −0.0023 (8) |
C2A | 0.0301 (10) | 0.0301 (10) | 0.0394 (11) | −0.0027 (8) | 0.0119 (8) | 0.0052 (8) |
C3A | 0.0305 (10) | 0.0265 (9) | 0.0373 (10) | −0.0048 (8) | 0.0043 (8) | −0.0001 (8) |
C4A | 0.0286 (9) | 0.0250 (9) | 0.0275 (9) | 0.0049 (7) | 0.0051 (7) | 0.0052 (7) |
N41A | 0.0385 (9) | 0.0304 (8) | 0.0312 (8) | 0.0016 (7) | 0.0072 (7) | 0.0048 (7) |
O41A | 0.0526 (9) | 0.0513 (9) | 0.0458 (9) | −0.0077 (7) | 0.0255 (7) | −0.0005 (7) |
O42A | 0.0523 (9) | 0.0511 (9) | 0.0396 (8) | −0.0104 (8) | 0.0059 (7) | −0.0104 (7) |
C5A | 0.0291 (10) | 0.0336 (10) | 0.0346 (10) | −0.0044 (8) | 0.0096 (8) | 0.0061 (8) |
C6A | 0.0303 (10) | 0.0304 (9) | 0.0323 (10) | −0.0047 (8) | 0.0041 (8) | 0.0019 (8) |
C1B | 0.0275 (9) | 0.0263 (9) | 0.0238 (8) | 0.0026 (7) | 0.0041 (7) | 0.0038 (7) |
C11B | 0.0254 (9) | 0.0240 (8) | 0.0235 (8) | 0.0023 (7) | 0.0030 (7) | 0.0007 (7) |
O11B | 0.0265 (7) | 0.0380 (7) | 0.0370 (7) | −0.0032 (6) | 0.0007 (6) | 0.0168 (6) |
N11B | 0.0251 (8) | 0.0310 (8) | 0.0353 (8) | −0.0003 (6) | 0.0023 (7) | 0.0124 (7) |
N12B | 0.0247 (8) | 0.0309 (8) | 0.0351 (8) | 0.0037 (6) | −0.0012 (7) | 0.0055 (7) |
C2B | 0.0297 (10) | 0.0258 (9) | 0.0346 (10) | −0.0026 (7) | 0.0012 (8) | 0.0079 (8) |
C3B | 0.0294 (10) | 0.0326 (10) | 0.0348 (10) | −0.0035 (8) | −0.0050 (8) | 0.0071 (8) |
C4B | 0.0320 (10) | 0.0289 (9) | 0.0298 (9) | 0.0050 (8) | 0.0030 (8) | 0.0096 (8) |
N41B | 0.0368 (10) | 0.0339 (9) | 0.0380 (9) | 0.0034 (7) | −0.0030 (8) | 0.0106 (8) |
O41B | 0.0513 (10) | 0.0496 (9) | 0.0636 (10) | 0.0014 (7) | 0.0044 (8) | 0.0336 (8) |
O42B | 0.0421 (10) | 0.0599 (11) | 0.0930 (14) | −0.0023 (8) | −0.0207 (9) | 0.0366 (10) |
C5B | 0.0331 (10) | 0.0282 (10) | 0.0419 (11) | −0.0028 (8) | −0.0011 (9) | 0.0111 (9) |
C6B | 0.0289 (10) | 0.0308 (10) | 0.0387 (11) | −0.0051 (8) | −0.0034 (8) | 0.0070 (8) |
N1A | 0.0405 (10) | 0.0376 (9) | 0.0350 (9) | 0.0023 (8) | 0.0122 (8) | −0.0012 (8) |
O1A | 0.0403 (8) | 0.0327 (7) | 0.0396 (8) | −0.0032 (6) | 0.0084 (6) | 0.0014 (6) |
O2A | 0.0407 (9) | 0.0597 (10) | 0.0580 (10) | −0.0163 (7) | 0.0172 (8) | −0.0108 (8) |
O3A | 0.0816 (14) | 0.0546 (11) | 0.1101 (16) | 0.0039 (10) | 0.0610 (13) | −0.0220 (11) |
OW1 | 0.0313 (8) | 0.0685 (10) | 0.0401 (8) | 0.0015 (7) | 0.0009 (6) | 0.0193 (7) |
N1B | 0.0343 (9) | 0.0400 (10) | 0.0411 (10) | −0.0030 (8) | 0.0015 (8) | 0.0191 (8) |
O1B | 0.0530 (10) | 0.0456 (9) | 0.0582 (10) | −0.0054 (7) | 0.0150 (8) | 0.0026 (8) |
O2B | 0.0460 (9) | 0.0629 (10) | 0.0527 (10) | −0.0268 (8) | −0.0003 (8) | 0.0131 (8) |
O3B | 0.0514 (10) | 0.0489 (9) | 0.0706 (11) | −0.0043 (7) | 0.0279 (9) | 0.0072 (8) |
Cd1—OW1 | 2.2590 (14) | C1B—C2B | 1.389 (2) |
Cd1—O11A | 2.3242 (13) | C1B—C11B | 1.495 (2) |
Cd1—O11B | 2.3339 (12) | C11B—O11B | 1.241 (2) |
Cd1—N12A | 2.3489 (17) | C11B—N11B | 1.333 (2) |
Cd1—N12B | 2.3518 (16) | N11B—N12B | 1.410 (2) |
Cd1—O1A | 2.3934 (13) | N11B—H11B | 0.8442 |
Cd1—O2A | 2.5755 (15) | N12B—H21B | 0.8560 |
C1A—C6A | 1.386 (2) | N12B—H22B | 0.8629 |
C1A—C2A | 1.399 (3) | C2B—C3B | 1.387 (3) |
C1A—C11A | 1.499 (2) | C2B—H2B | 0.9300 |
C11A—O11A | 1.240 (2) | C3B—C4B | 1.380 (3) |
C11A—N11A | 1.331 (2) | C3B—H3B | 0.9300 |
N11A—N12A | 1.419 (2) | C4B—C5B | 1.372 (3) |
N11A—H11A | 0.8641 | C4B—N41B | 1.473 (2) |
N12A—H21A | 0.8728 | N41B—O42B | 1.219 (2) |
N12A—H22A | 0.8639 | N41B—O41B | 1.220 (2) |
C2A—C3A | 1.386 (3) | C5B—C6B | 1.385 (3) |
C2A—H2A | 0.9300 | C5B—H5B | 0.9300 |
C3A—C4A | 1.373 (2) | C6B—H6B | 0.9300 |
C3A—H3A | 0.9300 | N1A—O3A | 1.220 (2) |
C4A—C5A | 1.381 (3) | N1A—O2A | 1.239 (2) |
C4A—N41A | 1.475 (2) | N1A—O1A | 1.268 (2) |
N41A—O42A | 1.216 (2) | OW1—HW1 | 0.8358 |
N41A—O41A | 1.222 (2) | OW1—HW2 | 0.8199 |
C5A—C6A | 1.383 (3) | N1B—O3B | 1.242 (2) |
C5A—H5A | 0.9300 | N1B—O1B | 1.244 (2) |
C6A—H6A | 0.9300 | N1B—O2B | 1.245 (2) |
C1B—C6B | 1.388 (2) | ||
OW1—Cd1—O1A | 98.97 (5) | C4A—C5A—H5A | 120.7 |
OW1—Cd1—O2A | 89.50 (6) | C6A—C5A—H5A | 120.7 |
OW1—Cd1—O11A | 93.34 (5) | C5A—C6A—C1A | 120.53 (17) |
OW1—Cd1—O11B | 168.98 (5) | C5A—C6A—H6A | 119.7 |
OW1—Cd1—N12A | 90.92 (6) | C1A—C6A—H6A | 119.7 |
OW1—Cd1—N12B | 99.57 (5) | C6B—C1B—C2B | 120.07 (16) |
O11A—Cd1—O1A | 150.85 (5) | C6B—C1B—C11B | 121.82 (16) |
O11A—Cd1—O2A | 155.97 (5) | C2B—C1B—C11B | 118.03 (15) |
O11A—Cd1—O11B | 91.78 (5) | O11B—C11B—N11B | 122.99 (16) |
O11A—Cd1—N12A | 69.88 (5) | O11B—C11B—C1B | 121.07 (15) |
O11A—Cd1—N12B | 80.91 (5) | N11B—C11B—C1B | 115.94 (15) |
O11B—Cd1—O1A | 81.00 (5) | C11B—O11B—Cd1 | 114.86 (11) |
O11B—Cd1—O2A | 81.90 (5) | C11B—N11B—N12B | 120.89 (14) |
O11B—Cd1—N12A | 100.01 (6) | C11B—N11B—H11B | 120.1 |
O11B—Cd1—N12B | 71.62 (5) | N12B—N11B—H11B | 117.8 |
N12A—Cd1—O1A | 83.53 (5) | N11B—N12B—Cd1 | 109.29 (10) |
N12A—Cd1—O2A | 133.98 (5) | N11B—N12B—H21B | 106.6 |
N12A—Cd1—N12B | 149.50 (6) | Cd1—N12B—H21B | 108.0 |
N12B—Cd1—O1A | 122.36 (5) | N11B—N12B—H22B | 107.2 |
N12B—Cd1—O2A | 75.09 (5) | Cd1—N12B—H22B | 112.5 |
O1A—Cd1—O2A | 51.06 (4) | H21B—N12B—H22B | 113.0 |
C6A—C1A—C2A | 119.63 (16) | C3B—C2B—C1B | 120.11 (17) |
C6A—C1A—C11A | 116.70 (16) | C3B—C2B—H2B | 119.9 |
C2A—C1A—C11A | 123.66 (16) | C1B—C2B—H2B | 119.9 |
O11A—C11A—N11A | 122.42 (17) | C4B—C3B—C2B | 118.22 (17) |
O11A—C11A—C1A | 119.54 (16) | C4B—C3B—H3B | 120.9 |
N11A—C11A—C1A | 118.03 (16) | C2B—C3B—H3B | 120.9 |
C11A—O11A—Cd1 | 115.35 (12) | C5B—C4B—C3B | 122.94 (17) |
C11A—N11A—N12A | 118.33 (15) | C5B—C4B—N41B | 118.46 (16) |
C11A—N11A—H11A | 127.5 | C3B—C4B—N41B | 118.59 (16) |
N12A—N11A—H11A | 113.8 | O42B—N41B—O41B | 123.56 (17) |
N11A—N12A—Cd1 | 109.97 (11) | O42B—N41B—C4B | 118.14 (16) |
N11A—N12A—H21A | 101.8 | O41B—N41B—C4B | 118.29 (16) |
Cd1—N12A—H21A | 116.1 | C4B—C5B—C6B | 118.30 (17) |
N11A—N12A—H22A | 110.9 | C4B—C5B—H5B | 120.9 |
Cd1—N12A—H22A | 109.0 | C6B—C5B—H5B | 120.9 |
H21A—N12A—H22A | 108.9 | C5B—C6B—C1B | 120.33 (17) |
C3A—C2A—C1A | 120.16 (17) | C5B—C6B—H6B | 119.8 |
C3A—C2A—H2A | 119.9 | C1B—C6B—H6B | 119.8 |
C1A—C2A—H2A | 119.9 | O3A—N1A—O2A | 121.62 (18) |
C4A—C3A—C2A | 118.62 (17) | O3A—N1A—O1A | 120.49 (18) |
C4A—C3A—H3A | 120.7 | O2A—N1A—O1A | 117.88 (16) |
C2A—C3A—H3A | 120.7 | N1A—O1A—Cd1 | 99.38 (11) |
C3A—C4A—C5A | 122.53 (17) | N1A—O2A—Cd1 | 91.41 (11) |
C3A—C4A—N41A | 118.90 (16) | Cd1—OW1—HW1 | 114.8 |
C5A—C4A—N41A | 118.56 (16) | Cd1—OW1—HW2 | 104.6 |
O42A—N41A—O41A | 123.75 (17) | HW1—OW1—HW2 | 106.1 |
O42A—N41A—C4A | 118.31 (16) | O3B—N1B—O1B | 120.05 (17) |
O41A—N41A—C4A | 117.94 (16) | O3B—N1B—O2B | 120.16 (18) |
C4A—C5A—C6A | 118.51 (17) | O1B—N1B—O2B | 119.78 (18) |
C6A—C1A—C11A—O11A | −3.2 (3) | N12A—Cd1—O11B—C11B | 150.92 (12) |
C2A—C1A—C11A—O11A | 175.24 (18) | N12B—Cd1—O11B—C11B | 1.23 (12) |
C6A—C1A—C11A—N11A | 178.11 (17) | O1A—Cd1—O11B—C11B | −127.35 (13) |
C2A—C1A—C11A—N11A | −3.4 (3) | O2A—Cd1—O11B—C11B | −75.68 (12) |
N11A—C11A—O11A—Cd1 | 14.9 (2) | O11B—C11B—N11B—N12B | 7.5 (3) |
C1A—C11A—O11A—Cd1 | −163.67 (12) | C1B—C11B—N11B—N12B | −172.32 (14) |
OW1—Cd1—O11A—C11A | −106.43 (14) | C11B—N11B—N12B—Cd1 | −5.45 (18) |
O11B—Cd1—O11A—C11A | 83.33 (14) | OW1—Cd1—N12B—N11B | 175.23 (10) |
N12A—Cd1—O11A—C11A | −16.68 (14) | O11A—Cd1—N12B—N11B | −92.89 (11) |
N12B—Cd1—O11A—C11A | 154.41 (14) | O11B—Cd1—N12B—N11B | 2.05 (10) |
O1A—Cd1—O11A—C11A | 8.7 (2) | N12A—Cd1—N12B—N11B | −76.23 (16) |
O2A—Cd1—O11A—C11A | 157.28 (13) | O1A—Cd1—N12B—N11B | 68.13 (12) |
O11A—C11A—N11A—N12A | 1.2 (3) | O2A—Cd1—N12B—N11B | 88.32 (11) |
C1A—C11A—N11A—N12A | 179.79 (16) | C6B—C1B—C2B—C3B | 1.9 (3) |
C11A—N11A—N12A—Cd1 | −15.8 (2) | C11B—C1B—C2B—C3B | −174.74 (16) |
OW1—Cd1—N12A—N11A | 109.00 (13) | C1B—C2B—C3B—C4B | −1.6 (3) |
O11A—Cd1—N12A—N11A | 15.78 (12) | C2B—C3B—C4B—C5B | 0.3 (3) |
O11B—Cd1—N12A—N11A | −72.44 (13) | C2B—C3B—C4B—N41B | 179.43 (16) |
N12B—Cd1—N12A—N11A | −1.8 (2) | C5B—C4B—N41B—O42B | 157.60 (19) |
O1A—Cd1—N12A—N11A | −152.07 (14) | C3B—C4B—N41B—O42B | −21.6 (3) |
O2A—Cd1—N12A—N11A | −160.80 (11) | C5B—C4B—N41B—O41B | −21.4 (3) |
C6A—C1A—C2A—C3A | 0.3 (3) | C3B—C4B—N41B—O41B | 159.45 (18) |
C11A—C1A—C2A—C3A | −178.11 (17) | C3B—C4B—C5B—C6B | 0.8 (3) |
C1A—C2A—C3A—C4A | −0.1 (3) | N41B—C4B—C5B—C6B | −178.35 (16) |
C2A—C3A—C4A—C5A | −0.6 (3) | C4B—C5B—C6B—C1B | −0.5 (3) |
C2A—C3A—C4A—N41A | 178.35 (16) | C2B—C1B—C6B—C5B | −0.8 (3) |
C3A—C4A—N41A—O42A | −3.8 (3) | C11B—C1B—C6B—C5B | 175.71 (17) |
C5A—C4A—N41A—O42A | 175.18 (17) | O3A—N1A—O1A—Cd1 | −173.76 (18) |
C3A—C4A—N41A—O41A | 176.75 (17) | O2A—N1A—O1A—Cd1 | 5.45 (19) |
C5A—C4A—N41A—O41A | −4.3 (2) | OW1—Cd1—O1A—N1A | −85.00 (12) |
C3A—C4A—C5A—C6A | 1.1 (3) | O11A—Cd1—O1A—N1A | 161.17 (11) |
N41A—C4A—C5A—C6A | −177.84 (16) | O11B—Cd1—O1A—N1A | 83.85 (11) |
C4A—C5A—C6A—C1A | −0.9 (3) | N12A—Cd1—O1A—N1A | −174.90 (12) |
C2A—C1A—C6A—C5A | 0.2 (3) | N12B—Cd1—O1A—N1A | 22.41 (13) |
C11A—C1A—C6A—C5A | 178.74 (17) | O2A—Cd1—O1A—N1A | −2.98 (11) |
C6B—C1B—C11B—O11B | −153.76 (18) | O3A—N1A—O2A—Cd1 | 174.2 (2) |
C2B—C1B—C11B—O11B | 22.8 (2) | O1A—N1A—O2A—Cd1 | −5.00 (18) |
C6B—C1B—C11B—N11B | 26.0 (2) | OW1—Cd1—O2A—N1A | 104.98 (12) |
C2B—C1B—C11B—N11B | −157.42 (16) | O11A—Cd1—O2A—N1A | −157.92 (12) |
N11B—C11B—O11B—Cd1 | −4.9 (2) | O11B—Cd1—O2A—N1A | −81.93 (12) |
C1B—C11B—O11B—Cd1 | 174.84 (11) | N12A—Cd1—O2A—N1A | 14.19 (16) |
OW1—Cd1—O11B—C11B | −36.6 (3) | N12B—Cd1—O2A—N1A | −154.98 (13) |
O11A—Cd1—O11B—C11B | 81.04 (12) | O1A—Cd1—O2A—N1A | 3.01 (11) |
D—H···A | D—H | H···A | D···A | D—H···A |
N11A—H11A···O3Bi | 0.86 | 2.03 | 2.886 (2) | 171.2 |
N12A—H21A···O1Bi | 0.87 | 2.42 | 2.977 (2) | 122.2 |
N12A—H22A···O1B | 0.86 | 2.60 | 3.209 (2) | 128.8 |
N11B—H11B···O3Aii | 0.84 | 2.59 | 3.176 (2) | 127.6 |
N12B—H22B···O11Biii | 0.86 | 2.40 | 3.212 (2) | 156.9 |
OW1—HW1···O1Aiii | 0.84 | 2.05 | 2.815 (2) | 151.2 |
OW1—HW2···O2B | 0.82 | 1.95 | 2.769 (2) | 174.2 |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+1, −y, −z+1; (iii) x−1, y, z. |
Experimental details
Crystal data | |
Chemical formula | [Cd(NO3)(C7H7N3O3)2(H2O)]NO3 |
Mr | 616.75 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 5.6112 (5), 13.1253 (12), 14.8985 (13) |
α, β, γ (°) | 101.314 (8), 96.944 (7), 92.410 (7) |
V (Å3) | 1065.60 (16) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.11 |
Crystal size (mm) | 0.52 × 0.38 × 0.27 |
Data collection | |
Diffractometer | Kuma KM-4 with CCD area-detector |
Absorption correction | Numerical (CrysAlis; Mayer, 2006) |
Tmin, Tmax | 0.732, 0.871 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 15437, 5431, 4512 |
Rint | 0.027 |
(sin θ/λ)max (Å−1) | 0.676 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.026, 0.052, 0.97 |
No. of reflections | 5431 |
No. of parameters | 325 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.97, −0.48 |
Computer programs: CrysAlis (Mayer, 2006), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 2005), publCIF (Westrip, 2007).
Cd1—OW1 | 2.2590 (14) | Cd1—N12B | 2.3518 (16) |
Cd1—O11A | 2.3242 (13) | Cd1—O1A | 2.3934 (13) |
Cd1—O11B | 2.3339 (12) | Cd1—O2A | 2.5755 (15) |
Cd1—N12A | 2.3489 (17) | ||
OW1—Cd1—O1A | 98.97 (5) | O11B—Cd1—O1A | 81.00 (5) |
OW1—Cd1—O2A | 89.50 (6) | O11B—Cd1—O2A | 81.90 (5) |
OW1—Cd1—O11A | 93.34 (5) | O11B—Cd1—N12A | 100.01 (6) |
OW1—Cd1—O11B | 168.98 (5) | O11B—Cd1—N12B | 71.62 (5) |
OW1—Cd1—N12A | 90.92 (6) | N12A—Cd1—O1A | 83.53 (5) |
OW1—Cd1—N12B | 99.57 (5) | N12A—Cd1—O2A | 133.98 (5) |
O11A—Cd1—O1A | 150.85 (5) | N12A—Cd1—N12B | 149.50 (6) |
O11A—Cd1—O2A | 155.97 (5) | N12B—Cd1—O1A | 122.36 (5) |
O11A—Cd1—O11B | 91.78 (5) | N12B—Cd1—O2A | 75.09 (5) |
O11A—Cd1—N12A | 69.88 (5) | O1A—Cd1—O2A | 51.06 (4) |
O11A—Cd1—N12B | 80.91 (5) |
D—H···A | D—H | H···A | D···A | D—H···A |
N11A—H11A···O3Bi | 0.86 | 2.03 | 2.886 (2) | 171.2 |
N12A—H21A···O1Bi | 0.87 | 2.42 | 2.977 (2) | 122.2 |
N12A—H22A···O1B | 0.86 | 2.60 | 3.209 (2) | 128.8 |
N11B—H11B···O3Aii | 0.84 | 2.59 | 3.176 (2) | 127.6 |
N12B—H22B···O11Biii | 0.86 | 2.40 | 3.212 (2) | 156.9 |
OW1—HW1···O1Aiii | 0.84 | 2.05 | 2.815 (2) | 151.2 |
OW1—HW2···O2B | 0.82 | 1.95 | 2.769 (2) | 174.2 |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+1, −y, −z+1; (iii) x−1, y, z. |
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In the title compound, cadmium is coordinated by two p-nitrobenzoylhydrazine molecules, a water molecules and a bidentate chelating nitrate. These ligands create atypical seven coordination sphere around the Cd atom and the geometry around Cd can be described as a pentagonal bipyramid. The Cd—Onitrate bond lenghts difference, Co—O—N angles difference and Co—N—Oterminal are 0.18 Å, 7.9° and 173° respectively, and correlate well with the bidentate mode of the nitrate group (Kleywegt et al., 1985; Dowling et al., 1996). Noncoordinated and bidentate chelating nitrates create hydrogen bonding network in a and b directions, respectively. Interestingly, both oxygen atoms from the –NO2 groups do not participate in hydrogen bonding network. But two parallel-oriented organic ligands help to establish the packing.