Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807053792/pv2040sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807053792/pv2040Isup2.hkl |
CCDC reference: 674046
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.004 Å
- R factor = 0.041
- wR factor = 0.064
- Data-to-parameter ratio = 16.2
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT230_ALERT_2_C Hirshfeld Test Diff for O1A - N1A .. 6.02 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cd1 - O1A .. 5.26 su PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N31B
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) 1.93
0 ALERT level A = In general: serious problem 0 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 0 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For geometric studies of the coordination mode of the nitrate anion, see: Kleywegt et al. (1985); Dowling et al. (1996).
1.8 g (1 mmol) of m-nitrobenzoylhydrazine was dissolved in 25 ml hot ethanol and mixed with 3 ml e thanolic solution of Cd(NO3)2 (3.1 g; 1 mmol). Colourless crystals were formed after 24 h, then filtered, washed with ethanol and dried on air.
All the hydrogen atoms were visible in the difference maps and were refined 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 were determined from the difference maps and were not refined [Uiso(H) = 1.5Ueq(N,O)].
Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis RED (Oxford Diffraction, 2006); data reduction: CrysAlis RED (Oxford Diffraction, 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 (Version 1.9.0_c; Westrip, 2007).
Fig. 1. Dimeric structure of the title compound with elipsoids drawn at the 50% probability level. [Symmetry code: (i) -x, -y + 2, -z.]. |
[Cd2(NO3)2(C7H7N3O3)2](NO3)2 | F(000) = 1192 |
Mr = 598.73 | Dx = 1.922 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 3275 reflections |
a = 7.9218 (16) Å | θ = 3.2–28.3° |
b = 7.6237 (15) Å | µ = 1.14 mm−1 |
c = 34.325 (7) Å | T = 293 K |
β = 93.67 (3)° | Plate, colourless |
V = 2068.7 (7) Å3 | 0.38 × 0.35 × 0.10 mm |
Z = 4 |
Kuma KM-4 with CCD area-detector diffractometer | 5111 independent reflections |
Radiation source: fine-focus sealed tube | 3275 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.060 |
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1 | θmax = 28.3°, θmin = 3.2° |
ω scans | h = −10→7 |
Absorption correction: numerical (CrysAlis; Oxford Diffraction, 2006) | k = −10→10 |
Tmin = 0.672, Tmax = 0.871 | l = −45→45 |
26291 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)] = 0.041 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.064 | H-atom parameters constrained |
S = 0.94 | w = 1/[σ2(Fo2) + (0.0233P)2] where P = (Fo2 + 2Fc2)/3 |
5111 reflections | (Δ/σ)max = 0.001 |
316 parameters | Δρmax = 0.63 e Å−3 |
0 restraints | Δρmin = −0.76 e Å−3 |
[Cd2(NO3)2(C7H7N3O3)2](NO3)2 | V = 2068.7 (7) Å3 |
Mr = 598.73 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 7.9218 (16) Å | µ = 1.14 mm−1 |
b = 7.6237 (15) Å | T = 293 K |
c = 34.325 (7) Å | 0.38 × 0.35 × 0.10 mm |
β = 93.67 (3)° |
Kuma KM-4 with CCD area-detector diffractometer | 5111 independent reflections |
Absorption correction: numerical (CrysAlis; Oxford Diffraction, 2006) | 3275 reflections with I > 2σ(I) |
Tmin = 0.672, Tmax = 0.871 | Rint = 0.060 |
26291 measured reflections |
R[F2 > 2σ(F2)] = 0.041 | 0 restraints |
wR(F2) = 0.064 | H-atom parameters constrained |
S = 0.94 | Δρmax = 0.63 e Å−3 |
5111 reflections | Δρmin = −0.76 e Å−3 |
316 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 | 0.21123 (3) | 0.91697 (3) | 0.065750 (7) | 0.03871 (9) | |
C1A | 0.3993 (3) | 1.3516 (4) | 0.14429 (8) | 0.0283 (7) | |
C11A | 0.3681 (4) | 1.2144 (4) | 0.11357 (8) | 0.0299 (7) | |
O11A | 0.2649 (3) | 1.0959 (3) | 0.11856 (6) | 0.0420 (5) | |
N11A | 0.4532 (3) | 1.2260 (3) | 0.08142 (7) | 0.0325 (6) | |
H11A | 0.5254 | 1.3101 | 0.0774 | 0.049* | |
N12A | 0.4232 (3) | 1.0998 (3) | 0.05130 (7) | 0.0348 (6) | |
H21A | 0.3816 | 1.1528 | 0.0296 | 0.052* | |
H22A | 0.5221 | 1.0456 | 0.0503 | 0.052* | |
C2A | 0.4693 (3) | 1.5141 (4) | 0.13664 (9) | 0.0305 (7) | |
H2A | 0.5050 | 1.5402 | 0.1120 | 0.037* | |
C3A | 0.4847 (4) | 1.6360 (4) | 0.16640 (9) | 0.0320 (7) | |
N31A | 0.5536 (4) | 1.8102 (4) | 0.15805 (9) | 0.0488 (7) | |
O31A | 0.5797 (4) | 1.8452 (3) | 0.12432 (8) | 0.0784 (9) | |
O32A | 0.5794 (4) | 1.9129 (3) | 0.18495 (8) | 0.0781 (8) | |
C4A | 0.4352 (4) | 1.6029 (4) | 0.20352 (9) | 0.0406 (8) | |
H4A | 0.4474 | 1.6873 | 0.2231 | 0.049* | |
C5A | 0.3668 (4) | 1.4395 (4) | 0.21075 (9) | 0.0431 (8) | |
H5A | 0.3332 | 1.4133 | 0.2356 | 0.052* | |
C6A | 0.3481 (3) | 1.3157 (4) | 0.18157 (8) | 0.0351 (8) | |
H6A | 0.3009 | 1.2072 | 0.1868 | 0.042* | |
C1B | −0.0259 (3) | 0.4933 (4) | 0.13333 (8) | 0.0280 (7) | |
C11B | 0.0584 (3) | 0.6052 (4) | 0.10467 (8) | 0.0292 (7) | |
O11B | 0.1456 (3) | 0.7319 (3) | 0.11554 (6) | 0.0422 (6) | |
N11B | 0.0386 (3) | 0.5559 (3) | 0.06711 (7) | 0.0345 (6) | |
H11B | −0.0480 | 0.4930 | 0.0575 | 0.052* | |
N12B | 0.1088 (3) | 0.6642 (3) | 0.03862 (7) | 0.0342 (6) | |
H21B | 0.0277 | 0.6993 | 0.0207 | 0.051* | |
H22B | 0.1590 | 0.5965 | 0.0233 | 0.051* | |
C2B | −0.0491 (3) | 0.5612 (4) | 0.16999 (9) | 0.0345 (7) | |
H2B | −0.0152 | 0.6750 | 0.1764 | 0.041* | |
C3B | −0.1232 (4) | 0.4572 (4) | 0.19677 (9) | 0.0383 (8) | |
N31B | −0.1504 (4) | 0.5325 (5) | 0.23589 (9) | 0.0575 (9) | |
O31B | −0.1058 (4) | 0.6833 (5) | 0.24205 (8) | 0.0936 (10) | |
O32B | −0.2169 (4) | 0.4419 (4) | 0.25973 (8) | 0.0890 (10) | |
C4B | −0.1743 (4) | 0.2890 (5) | 0.18912 (10) | 0.0467 (9) | |
H4B | −0.2244 | 0.2222 | 0.2079 | 0.056* | |
C5B | −0.1495 (4) | 0.2211 (4) | 0.15282 (10) | 0.0461 (9) | |
H5B | −0.1831 | 0.1067 | 0.1469 | 0.055* | |
C6B | −0.0751 (4) | 0.3213 (4) | 0.12507 (9) | 0.0365 (8) | |
H6B | −0.0578 | 0.2735 | 0.1007 | 0.044* | |
N1A | −0.1265 (3) | 1.0524 (3) | 0.03837 (8) | 0.0355 (6) | |
O1A | 0.0176 (3) | 1.1213 (3) | 0.03396 (6) | 0.0446 (6) | |
O2A | −0.1387 (3) | 0.9443 (3) | 0.06509 (7) | 0.0578 (7) | |
O3A | −0.2493 (3) | 1.0939 (3) | 0.01617 (6) | 0.0458 (6) | |
N1B | 0.6356 (3) | 0.5968 (4) | 0.03179 (7) | 0.0369 (6) | |
O1B | 0.6860 (3) | 0.4722 (3) | 0.05402 (6) | 0.0470 (6) | |
O2B | 0.7298 (3) | 0.6450 (3) | 0.00571 (6) | 0.0483 (6) | |
O3B | 0.4979 (3) | 0.6670 (3) | 0.03588 (7) | 0.0605 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.04042 (14) | 0.03565 (13) | 0.03968 (14) | −0.01622 (13) | −0.00052 (10) | 0.00128 (13) |
C1A | 0.0280 (17) | 0.0297 (16) | 0.0271 (17) | −0.0040 (13) | 0.0012 (13) | 0.0007 (14) |
C11A | 0.0264 (17) | 0.0321 (17) | 0.0312 (17) | −0.0060 (14) | 0.0024 (14) | 0.0046 (15) |
O11A | 0.0475 (13) | 0.0426 (13) | 0.0373 (12) | −0.0235 (12) | 0.0136 (10) | −0.0040 (11) |
N11A | 0.0346 (14) | 0.0320 (14) | 0.0317 (14) | −0.0172 (12) | 0.0087 (12) | −0.0054 (12) |
N12A | 0.0315 (14) | 0.0403 (15) | 0.0331 (14) | −0.0098 (12) | 0.0048 (11) | −0.0078 (13) |
C2A | 0.0310 (17) | 0.0341 (17) | 0.0268 (17) | −0.0051 (14) | 0.0044 (13) | −0.0005 (14) |
C3A | 0.0350 (18) | 0.0246 (16) | 0.0360 (18) | −0.0058 (13) | 0.0010 (15) | 0.0018 (14) |
N31A | 0.064 (2) | 0.0316 (17) | 0.052 (2) | −0.0115 (15) | 0.0120 (16) | −0.0047 (16) |
O31A | 0.136 (3) | 0.0435 (15) | 0.0596 (18) | −0.0336 (16) | 0.0397 (18) | −0.0036 (14) |
O32A | 0.124 (2) | 0.0463 (15) | 0.0645 (17) | −0.0368 (17) | 0.0137 (16) | −0.0237 (15) |
C4A | 0.047 (2) | 0.040 (2) | 0.0349 (18) | −0.0032 (17) | −0.0005 (15) | −0.0081 (17) |
C5A | 0.055 (2) | 0.047 (2) | 0.0272 (17) | −0.0048 (18) | 0.0063 (15) | −0.0014 (17) |
C6A | 0.0384 (19) | 0.0339 (18) | 0.0333 (18) | −0.0077 (14) | 0.0043 (15) | 0.0025 (15) |
C1B | 0.0251 (16) | 0.0306 (16) | 0.0280 (17) | −0.0036 (13) | 0.0000 (13) | −0.0003 (14) |
C11B | 0.0258 (16) | 0.0279 (17) | 0.0334 (17) | −0.0009 (14) | −0.0007 (13) | 0.0023 (15) |
O11B | 0.0552 (14) | 0.0336 (12) | 0.0365 (12) | −0.0221 (11) | −0.0070 (10) | 0.0011 (10) |
N11B | 0.0397 (15) | 0.0324 (15) | 0.0321 (14) | −0.0174 (12) | 0.0086 (12) | −0.0052 (12) |
N12B | 0.0394 (15) | 0.0357 (14) | 0.0284 (14) | −0.0065 (12) | 0.0096 (12) | −0.0019 (12) |
C2B | 0.0298 (17) | 0.0353 (18) | 0.0381 (18) | 0.0000 (15) | −0.0008 (14) | −0.0034 (16) |
C3B | 0.0340 (19) | 0.053 (2) | 0.0281 (17) | 0.0029 (16) | 0.0049 (14) | −0.0035 (16) |
N31B | 0.051 (2) | 0.077 (3) | 0.046 (2) | 0.0013 (18) | 0.0094 (16) | −0.0077 (19) |
O31B | 0.123 (3) | 0.098 (2) | 0.063 (2) | −0.031 (2) | 0.0344 (17) | −0.0359 (19) |
O32B | 0.112 (2) | 0.109 (3) | 0.0502 (17) | −0.011 (2) | 0.0390 (17) | 0.0055 (18) |
C4B | 0.047 (2) | 0.052 (2) | 0.042 (2) | −0.0091 (18) | 0.0073 (17) | 0.0115 (19) |
C5B | 0.055 (2) | 0.0328 (19) | 0.051 (2) | −0.0122 (17) | 0.0038 (18) | 0.0057 (18) |
C6B | 0.0411 (19) | 0.0340 (19) | 0.0347 (19) | −0.0056 (15) | 0.0046 (15) | −0.0031 (16) |
N1A | 0.0381 (17) | 0.0395 (17) | 0.0295 (15) | −0.0003 (13) | 0.0081 (13) | −0.0109 (14) |
O1A | 0.0268 (12) | 0.0586 (16) | 0.0487 (14) | −0.0106 (11) | 0.0053 (10) | −0.0038 (12) |
O2A | 0.0754 (18) | 0.0577 (17) | 0.0405 (14) | −0.0121 (14) | 0.0046 (12) | 0.0137 (13) |
O3A | 0.0289 (12) | 0.0581 (15) | 0.0502 (14) | 0.0012 (12) | 0.0011 (11) | 0.0049 (13) |
N1B | 0.0352 (16) | 0.0401 (17) | 0.0349 (15) | −0.0143 (14) | −0.0018 (13) | −0.0052 (14) |
O1B | 0.0386 (14) | 0.0502 (15) | 0.0520 (15) | −0.0163 (11) | 0.0007 (11) | 0.0178 (12) |
O2B | 0.0522 (15) | 0.0548 (15) | 0.0391 (13) | −0.0167 (12) | 0.0121 (11) | 0.0088 (11) |
O3B | 0.0341 (14) | 0.0755 (18) | 0.0716 (18) | 0.0063 (13) | 0.0002 (13) | −0.0077 (15) |
Cd1—O11A | 2.287 (2) | C6A—H6A | 0.9300 |
Cd1—O11B | 2.301 (2) | C1B—C2B | 1.384 (4) |
Cd1—N12A | 2.262 (2) | C1B—C6B | 1.392 (4) |
Cd1—N12B | 2.268 (2) | C1B—C11B | 1.492 (4) |
Cd1—O1A | 2.399 (2) | C11B—O11B | 1.232 (3) |
Cd1—O2A | 2.778 (2) | C11B—N11B | 1.342 (3) |
Cd1—O3Ai | 2.848 (2) | N11B—N12B | 1.420 (3) |
Cd1—O3B | 3.184 (3) | N11B—H11B | 0.8831 |
C1A—C2A | 1.389 (4) | N12B—H21B | 0.9017 |
C1A—C6A | 1.394 (4) | N12B—H22B | 0.8532 |
C1A—C11A | 1.494 (4) | C2B—C3B | 1.374 (4) |
C11A—O11A | 1.238 (3) | C2B—H2B | 0.9300 |
C11A—N11A | 1.333 (3) | C3B—C4B | 1.365 (4) |
N11A—N12A | 1.421 (3) | C3B—N31B | 1.489 (4) |
N11A—H11A | 0.8760 | N31B—O32B | 1.216 (4) |
N12A—H21A | 0.8908 | N31B—O31B | 1.217 (4) |
N12A—H22A | 0.8890 | C4B—C5B | 1.375 (4) |
C2A—C3A | 1.381 (4) | C4B—H4B | 0.9300 |
C2A—H2A | 0.9300 | C5B—C6B | 1.382 (4) |
C3A—C4A | 1.380 (4) | C5B—H5B | 0.9300 |
C3A—N31A | 1.471 (4) | C6B—H6B | 0.9300 |
N31A—O32A | 1.218 (3) | N1A—O3A | 1.238 (3) |
N31A—O31A | 1.219 (3) | N1A—O2A | 1.241 (3) |
C4A—C5A | 1.387 (4) | N1A—O1A | 1.274 (3) |
C4A—H4A | 0.9300 | N1B—O3B | 1.232 (3) |
C5A—C6A | 1.377 (4) | N1B—O2B | 1.256 (3) |
C5A—H5A | 0.9300 | N1B—O1B | 1.267 (3) |
N12A—Cd1—N12B | 133.23 (9) | C1A—C6A—H6A | 119.7 |
N12A—Cd1—O11A | 72.73 (8) | C2B—C1B—C6B | 119.1 (3) |
N12A—Cd1—O11B | 138.33 (8) | C2B—C1B—C11B | 118.4 (3) |
N12A—Cd1—O1A | 87.82 (8) | C6B—C1B—C11B | 122.4 (3) |
N12B—Cd1—O11B | 72.07 (8) | O11B—C11B—N11B | 122.6 (3) |
N12B—Cd1—O11A | 151.16 (8) | O11B—C11B—C1B | 121.0 (3) |
N12B—Cd1—O1A | 99.40 (8) | N11B—C11B—C1B | 116.3 (3) |
O11A—Cd1—O11B | 79.41 (7) | C11B—O11B—Cd1 | 113.88 (18) |
O11A—Cd1—O1A | 93.12 (8) | C11B—N11B—N12B | 118.2 (2) |
O11B—Cd1—O1A | 124.58 (8) | C11B—N11B—H11B | 123.3 |
C2A—C1A—C6A | 119.5 (3) | N12B—N11B—H11B | 112.9 |
C2A—C1A—C11A | 122.7 (3) | N11B—N12B—Cd1 | 110.89 (16) |
C6A—C1A—C11A | 117.8 (3) | N11B—N12B—H21B | 110.5 |
O11A—C11A—N11A | 122.5 (3) | Cd1—N12B—H21B | 104.4 |
O11A—C11A—C1A | 119.6 (3) | N11B—N12B—H22B | 107.0 |
N11A—C11A—C1A | 117.9 (3) | Cd1—N12B—H22B | 126.8 |
C11A—O11A—Cd1 | 114.63 (18) | H21B—N12B—H22B | 95.6 |
C11A—N11A—N12A | 119.2 (2) | C3B—C2B—C1B | 118.6 (3) |
C11A—N11A—H11A | 123.3 | C3B—C2B—H2B | 120.7 |
N12A—N11A—H11A | 117.5 | C1B—C2B—H2B | 120.7 |
N11A—N12A—Cd1 | 110.48 (16) | C4B—C3B—C2B | 123.2 (3) |
N11A—N12A—H21A | 109.7 | C4B—C3B—N31B | 118.5 (3) |
Cd1—N12A—H21A | 102.8 | C2B—C3B—N31B | 118.2 (3) |
N11A—N12A—H22A | 103.7 | O32B—N31B—O31B | 123.6 (4) |
Cd1—N12A—H22A | 113.0 | O32B—N31B—C3B | 118.8 (3) |
H21A—N12A—H22A | 117.3 | O31B—N31B—C3B | 117.7 (3) |
C3A—C2A—C1A | 118.5 (3) | C3B—C4B—C5B | 118.0 (3) |
C3A—C2A—H2A | 120.7 | C3B—C4B—H4B | 121.0 |
C1A—C2A—H2A | 120.7 | C5B—C4B—H4B | 121.0 |
C4A—C3A—C2A | 122.9 (3) | C4B—C5B—C6B | 120.6 (3) |
C4A—C3A—N31A | 118.4 (3) | C4B—C5B—H5B | 119.7 |
C2A—C3A—N31A | 118.7 (3) | C6B—C5B—H5B | 119.7 |
O32A—N31A—O31A | 123.3 (3) | C5B—C6B—C1B | 120.4 (3) |
O32A—N31A—C3A | 118.6 (3) | C5B—C6B—H6B | 119.8 |
O31A—N31A—C3A | 118.1 (3) | C1B—C6B—H6B | 119.8 |
C3A—C4A—C5A | 117.8 (3) | O3A—N1A—O2A | 122.0 (3) |
C3A—C4A—H4A | 121.1 | O3A—N1A—O1A | 119.8 (3) |
C5A—C4A—H4A | 121.1 | O2A—N1A—O1A | 118.3 (3) |
C6A—C5A—C4A | 120.7 (3) | N1A—O1A—Cd1 | 103.30 (18) |
C6A—C5A—H5A | 119.7 | O3B—N1B—O2B | 121.6 (3) |
C4A—C5A—H5A | 119.7 | O3B—N1B—O1B | 120.3 (3) |
C5A—C6A—C1A | 120.6 (3) | O2B—N1B—O1B | 118.0 (3) |
C5A—C6A—H6A | 119.7 | ||
C2A—C1A—C11A—O11A | −159.5 (3) | C6B—C1B—C11B—N11B | 20.1 (4) |
C6A—C1A—C11A—O11A | 17.5 (4) | N11B—C11B—O11B—Cd1 | 15.5 (3) |
C2A—C1A—C11A—N11A | 20.1 (4) | C1B—C11B—O11B—Cd1 | −167.0 (2) |
C6A—C1A—C11A—N11A | −162.9 (3) | N12A—Cd1—O11B—C11B | −149.64 (19) |
N11A—C11A—O11A—Cd1 | −6.3 (4) | N12B—Cd1—O11B—C11B | −13.7 (2) |
C1A—C11A—O11A—Cd1 | 173.26 (19) | O11A—Cd1—O11B—C11B | 162.0 (2) |
N12A—Cd1—O11A—C11A | 6.32 (19) | O1A—Cd1—O11B—C11B | 75.5 (2) |
N12B—Cd1—O11A—C11A | 163.6 (2) | O11B—C11B—N11B—N12B | −5.8 (4) |
O11B—Cd1—O11A—C11A | 155.0 (2) | C1B—C11B—N11B—N12B | 176.6 (2) |
O1A—Cd1—O11A—C11A | −80.4 (2) | C11B—N11B—N12B—Cd1 | −7.1 (3) |
O11A—C11A—N11A—N12A | 1.1 (4) | N12A—Cd1—N12B—N11B | 150.76 (16) |
C1A—C11A—N11A—N12A | −178.5 (2) | O11A—Cd1—N12B—N11B | 1.2 (3) |
C11A—N11A—N12A—Cd1 | 4.7 (3) | O11B—Cd1—N12B—N11B | 10.11 (16) |
N12B—Cd1—N12A—N11A | −170.52 (15) | O1A—Cd1—N12B—N11B | −113.34 (17) |
O11A—Cd1—N12A—N11A | −5.34 (16) | C6B—C1B—C2B—C3B | −1.3 (4) |
O11B—Cd1—N12A—N11A | −55.6 (2) | C11B—C1B—C2B—C3B | −178.6 (3) |
O1A—Cd1—N12A—N11A | 88.61 (17) | C1B—C2B—C3B—C4B | 0.5 (5) |
C6A—C1A—C2A—C3A | −0.5 (4) | C1B—C2B—C3B—N31B | −178.9 (2) |
C11A—C1A—C2A—C3A | 176.5 (3) | C4B—C3B—N31B—O32B | 0.1 (5) |
C1A—C2A—C3A—C4A | 0.7 (4) | C2B—C3B—N31B—O32B | 179.5 (3) |
C1A—C2A—C3A—N31A | −178.1 (3) | C4B—C3B—N31B—O31B | −179.2 (3) |
C4A—C3A—N31A—O32A | 6.8 (4) | C2B—C3B—N31B—O31B | 0.3 (5) |
C2A—C3A—N31A—O32A | −174.4 (3) | C2B—C3B—C4B—C5B | 0.2 (5) |
C4A—C3A—N31A—O31A | −172.1 (3) | N31B—C3B—C4B—C5B | 179.6 (3) |
C2A—C3A—N31A—O31A | 6.7 (4) | C3B—C4B—C5B—C6B | −0.1 (5) |
C2A—C3A—C4A—C5A | −0.2 (5) | C4B—C5B—C6B—C1B | −0.8 (5) |
N31A—C3A—C4A—C5A | 178.5 (3) | C2B—C1B—C6B—C5B | 1.4 (4) |
C3A—C4A—C5A—C6A | −0.5 (5) | C11B—C1B—C6B—C5B | 178.6 (3) |
C4A—C5A—C6A—C1A | 0.7 (5) | O3A—N1A—O1A—Cd1 | −158.5 (2) |
C2A—C1A—C6A—C5A | −0.2 (4) | O2A—N1A—O1A—Cd1 | 21.3 (3) |
C11A—C1A—C6A—C5A | −177.3 (3) | N12A—Cd1—O1A—N1A | −178.19 (17) |
C2B—C1B—C11B—O11B | 19.6 (4) | N12B—Cd1—O1A—N1A | 48.31 (17) |
C6B—C1B—C11B—O11B | −157.6 (3) | O11A—Cd1—O1A—N1A | −105.62 (16) |
C2B—C1B—C11B—N11B | −162.8 (3) | O11B—Cd1—O1A—N1A | −26.34 (19) |
Symmetry code: (i) −x, −y+2, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N11A—H11A···O1Bii | 0.88 | 1.98 | 2.833 (3) | 164.5 |
N12A—H21A···O2Biii | 0.89 | 2.12 | 2.963 (3) | 157.8 |
N12A—H22A···O3Aiv | 0.89 | 2.25 | 2.931 (3) | 133.3 |
N11B—H11B···O1Bv | 0.88 | 2.11 | 2.872 (3) | 144.3 |
N12B—H21B···O1Ai | 0.90 | 2.33 | 3.093 (3) | 142.2 |
N12B—H21B···O2Bv | 0.90 | 2.42 | 3.143 (3) | 137.5 |
N12B—H22B···O2Bvi | 0.85 | 2.30 | 3.124 (3) | 163.6 |
Symmetry codes: (i) −x, −y+2, −z; (ii) x, y+1, z; (iii) −x+1, −y+2, −z; (iv) x+1, y, z; (v) x−1, y, z; (vi) −x+1, −y+1, −z. |
Experimental details
Crystal data | |
Chemical formula | [Cd2(NO3)2(C7H7N3O3)2](NO3)2 |
Mr | 598.73 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 293 |
a, b, c (Å) | 7.9218 (16), 7.6237 (15), 34.325 (7) |
β (°) | 93.67 (3) |
V (Å3) | 2068.7 (7) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.14 |
Crystal size (mm) | 0.38 × 0.35 × 0.10 |
Data collection | |
Diffractometer | Kuma KM-4 with CCD area-detector diffractometer |
Absorption correction | Numerical (CrysAlis; Oxford Diffraction, 2006) |
Tmin, Tmax | 0.672, 0.871 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 26291, 5111, 3275 |
Rint | 0.060 |
(sin θ/λ)max (Å−1) | 0.667 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.041, 0.064, 0.94 |
No. of reflections | 5111 |
No. of parameters | 316 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.63, −0.76 |
Computer programs: CrysAlis CCD (Oxford Diffraction, 2006), CrysAlis RED (Oxford Diffraction, 2006), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 2005), publCIF (Version 1.9.0_c; Westrip, 2007).
Cd1—O11A | 2.287 (2) | Cd1—O1A | 2.399 (2) |
Cd1—O11B | 2.301 (2) | Cd1—O2A | 2.778 (2) |
Cd1—N12A | 2.262 (2) | Cd1—O3Ai | 2.848 (2) |
Cd1—N12B | 2.268 (2) | Cd1—O3B | 3.184 (3) |
N12A—Cd1—N12B | 133.23 (9) | N12B—Cd1—O11A | 151.16 (8) |
N12A—Cd1—O11A | 72.73 (8) | N12B—Cd1—O1A | 99.40 (8) |
N12A—Cd1—O11B | 138.33 (8) | O11A—Cd1—O11B | 79.41 (7) |
N12A—Cd1—O1A | 87.82 (8) | O11A—Cd1—O1A | 93.12 (8) |
N12B—Cd1—O11B | 72.07 (8) | O11B—Cd1—O1A | 124.58 (8) |
Symmetry code: (i) −x, −y+2, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N11A—H11A···O1Bii | 0.88 | 1.98 | 2.833 (3) | 164.5 |
N12A—H21A···O2Biii | 0.89 | 2.12 | 2.963 (3) | 157.8 |
N12A—H22A···O3Aiv | 0.89 | 2.25 | 2.931 (3) | 133.3 |
N11B—H11B···O1Bv | 0.88 | 2.11 | 2.872 (3) | 144.3 |
N12B—H21B···O1Ai | 0.90 | 2.33 | 3.093 (3) | 142.2 |
N12B—H21B···O2Bv | 0.90 | 2.42 | 3.143 (3) | 137.5 |
N12B—H22B···O2Bvi | 0.85 | 2.30 | 3.124 (3) | 163.6 |
Symmetry codes: (i) −x, −y+2, −z; (ii) x, y+1, z; (iii) −x+1, −y+2, −z; (iv) x+1, y, z; (v) x−1, y, z; (vi) −x+1, −y+1, −z. |
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In the dimeric structure of bis((µ2-nitrato-O,O',O'')-cis-bis(m-nitrobenzoylhydrazino-N,O)cadmium(II)) bis(nitrate), two cis coordinated organic ligands and two bridging nitrate anions form atypical seven coordinated arrangement around the Cd-atom. Because the dimer lies on the inversion centre the asymmetric unit contains only half of the dimer. Therefore, two cadmium(II) ions and their coordination spheres are symmetrically dependent. By the same reason two bridging nitrate anions are also symmetrically dependent. Although bridging coordination mode of nitrate anion is clearly seen, it is worth noticing that this anion donates three oxygen atoms to the cadmium(II) and monodentate and bidentate coordination can be specified. In the former mode, the Cd—Onitrate bond lenghts difference, Co—O—N angles difference and Co—N—Oterminal angle for one nitrate are 0.38 Å, 17.3° and 160.4° respectively and correlate well with the anisobidentate coordination mode (Kleywegt et al., 1985; Dowling et al., 1996). In the latter mode, respective parameters distinctly indicates monodentate coordination (0.93 Å, 45.9° and 139.3°).
Intriguingly, the Cd-atom is displaced from the centre of the coordination polyhedron (augmented trigonal prism) in the direction of one face (0.54 Å). However, it seems that this displacement is caused by free NO3- anion. In spite of the Cd···ONO2 distance (3.184 Å) which is too long for a bond, indeed it is worth considering as a weak interaction. The position of the free nitrate anion is stabillized by several hydrogen bonding interactions both NH and NH2 groups from organic ligand.