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The Cd atom in the title complex, [Cd(NO3)2(C15H13N5)]·H2O or [Cd(NO3)2(tpdaH2)]·H2O (tpdaH2 is tripyridyldiamine), has a pentagonal-bipyramidal coordination formed by the tridentate tpdaH2 ligand and two chelate nitrate groups. The tpdaH2 ligand is mer-coordinated, with the N atom of the central pyridine ring in the equatorial position [Cd-N = 2.3148 (17) Å] and the N atoms of the peripheral pyridine rings in the axial positions [Cd-N = 2.2345 (19) and 2.2351 (19) Å, and N-Cd-N = 169.39 (6)°]. The remaining four equatorial positions are occupied by the four O atoms of two nitrate groups, one of which has almost equal Cd-O bond lengths [2.431 (2) and 2.4644 (19) Å], whereas the other shows a significant difference between the Cd-O bond lengths [2.441 (2) and 2.603 (2) Å]. The H atoms of both NH groups of the tpdaH2 ligand are involved in hydrogen bonds with water O atoms as acceptors, whereas both water H atoms form hydrogen bonds with the O atoms of one of the nitrate groups. The hydrogen bonds link the molecules of the title complex and solvent molecules into an infinite three-dimensional network.
Supporting information
CCDC reference: 274671
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.004 Å
- R factor = 0.026
- wR factor = 0.060
- Data-to-parameter ratio = 15.6
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Cd1 - O2 .. 19.88 su
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Cd1 - O5 .. 21.99 su
PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O4
PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O5
Alert level C
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 1.02
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O1
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cd1
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N6
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N7
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1
C15 H13 Cd N7 O6
0 ALERT level A = In general: serious problem
4 ALERT level B = Potentially serious problem
7 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
9 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
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-Plus (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL-Plus.
[2,6-Bis(2-pyridylamino)pyridine]dinitratocadmium monohydrate
top
Crystal data top
[Cd(NO3)2(C15H13N5)]·H2O | F(000) = 1032 |
Mr = 517.74 | Dx = 1.815 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 6355 reflections |
a = 9.3371 (3) Å | θ = 2.1–27.5° |
b = 17.5155 (5) Å | µ = 1.21 mm−1 |
c = 11.6735 (3) Å | T = 295 K |
β = 96.964 (1)° | Irregular, yellow |
V = 1895.05 (9) Å3 | 0.25 × 0.25 × 0.20 mm |
Z = 4 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 4346 independent reflections |
Radiation source: fine-focus sealed tube | 3059 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
φ and ω scans | θmax = 27.5°, θmin = 2.1° |
Absorption correction: multi-scan (symmetry-related measurements; Blessing, 1995) | h = −12→12 |
Tmin = 0.687, Tmax = 0.773 | k = −22→22 |
16790 measured reflections | l = −15→13 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.026 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.060 | w = 1/[σ2(Fo2) + (0.03P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.01 | (Δ/σ)max = 0.003 |
4346 reflections | Δρmax = 0.37 e Å−3 |
278 parameters | Δρmin = −0.50 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00097 (18) |
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 | |
Cd1 | −0.22093 (2) | 0.580916 (9) | 0.241872 (16) | 0.05142 (8) | |
N1 | −0.4436 (2) | 0.56444 (9) | 0.15111 (16) | 0.0475 (5) | |
N2 | −0.4763 (2) | 0.44358 (10) | 0.23418 (17) | 0.0497 (5) | |
H2A | −0.5398 | 0.4230 | 0.2720 | 0.060* | |
N3 | −0.21821 (19) | 0.44965 (10) | 0.26503 (14) | 0.0407 (4) | |
N4 | 0.0387 (2) | 0.44884 (10) | 0.30035 (18) | 0.0547 (5) | |
H4A | 0.1069 | 0.4235 | 0.2745 | 0.066* | |
N5 | −0.0055 (2) | 0.57695 (10) | 0.34863 (16) | 0.0497 (5) | |
N6 | −0.0945 (2) | 0.64868 (13) | 0.0541 (2) | 0.0684 (6) | |
N7 | −0.3571 (2) | 0.67571 (13) | 0.4080 (2) | 0.0655 (6) | |
O1 | −0.0964 (2) | 0.57849 (10) | 0.06744 (17) | 0.0757 (5) | |
O2 | −0.1512 (2) | 0.68745 (10) | 0.1272 (2) | 0.0879 (6) | |
O3 | −0.0410 (3) | 0.67796 (14) | −0.0246 (2) | 0.1250 (10) | |
O4 | −0.3324 (2) | 0.60840 (12) | 0.43157 (18) | 0.0895 (7) | |
O5 | −0.3134 (3) | 0.69907 (10) | 0.31589 (19) | 0.0903 (7) | |
O6 | −0.4181 (2) | 0.71684 (13) | 0.4697 (2) | 0.1067 (8) | |
C1 | −0.5017 (3) | 0.62350 (13) | 0.0861 (2) | 0.0568 (6) | |
H1A | −0.4426 | 0.6644 | 0.0726 | 0.068* | |
C2 | −0.6429 (3) | 0.62553 (15) | 0.0395 (2) | 0.0611 (7) | |
H2B | −0.6797 | 0.6675 | −0.0031 | 0.073* | |
C3 | −0.7301 (3) | 0.56422 (15) | 0.0568 (2) | 0.0599 (7) | |
H3A | −0.8266 | 0.5641 | 0.0257 | 0.072* | |
C4 | −0.6729 (3) | 0.50356 (13) | 0.1201 (2) | 0.0532 (6) | |
H4B | −0.7301 | 0.4614 | 0.1316 | 0.064* | |
C5 | −0.5282 (2) | 0.50510 (12) | 0.16760 (19) | 0.0429 (5) | |
C6 | −0.3413 (3) | 0.40808 (11) | 0.25235 (18) | 0.0413 (5) | |
C7 | −0.3422 (3) | 0.32918 (12) | 0.2591 (2) | 0.0492 (5) | |
H7A | −0.4289 | 0.3024 | 0.2514 | 0.059* | |
C8 | −0.2131 (3) | 0.29129 (13) | 0.2773 (2) | 0.0541 (6) | |
H8A | −0.2114 | 0.2383 | 0.2814 | 0.065* | |
C9 | −0.0865 (3) | 0.33173 (12) | 0.2896 (2) | 0.0510 (6) | |
H9A | 0.0020 | 0.3068 | 0.3011 | 0.061* | |
C10 | −0.0936 (2) | 0.41097 (11) | 0.28450 (19) | 0.0433 (5) | |
C11 | 0.0846 (2) | 0.51810 (12) | 0.34837 (19) | 0.0455 (5) | |
C12 | 0.2296 (3) | 0.52465 (14) | 0.3938 (2) | 0.0573 (6) | |
H12A | 0.2912 | 0.4829 | 0.3934 | 0.069* | |
C13 | 0.2801 (3) | 0.59257 (15) | 0.4388 (2) | 0.0644 (7) | |
H13A | 0.3766 | 0.5978 | 0.4684 | 0.077* | |
C14 | 0.1867 (3) | 0.65355 (15) | 0.4400 (2) | 0.0658 (7) | |
H14A | 0.2189 | 0.7005 | 0.4701 | 0.079* | |
C15 | 0.0468 (3) | 0.64329 (13) | 0.3960 (2) | 0.0605 (7) | |
H15A | −0.0165 | 0.6840 | 0.3986 | 0.073* | |
O7 | 0.2914 (2) | 0.34309 (11) | 0.29289 (18) | 0.0646 (5) | |
H7B | 0.277 (3) | 0.304 (2) | 0.248 (2) | 0.097* | |
H7C | 0.310 (4) | 0.3213 (19) | 0.351 (3) | 0.097* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.05242 (12) | 0.02919 (9) | 0.07100 (14) | −0.00053 (7) | 0.00080 (8) | 0.00281 (8) |
N1 | 0.0508 (12) | 0.0375 (10) | 0.0537 (12) | 0.0027 (8) | 0.0049 (9) | 0.0049 (8) |
N2 | 0.0423 (11) | 0.0419 (10) | 0.0658 (13) | −0.0018 (8) | 0.0106 (9) | 0.0119 (9) |
N3 | 0.0451 (10) | 0.0286 (8) | 0.0489 (11) | −0.0006 (8) | 0.0077 (8) | 0.0007 (7) |
N4 | 0.0424 (11) | 0.0374 (10) | 0.0857 (15) | 0.0013 (8) | 0.0139 (10) | −0.0086 (10) |
N5 | 0.0553 (12) | 0.0365 (10) | 0.0567 (12) | −0.0021 (9) | 0.0048 (9) | −0.0052 (9) |
N6 | 0.0652 (15) | 0.0551 (15) | 0.0853 (18) | −0.0095 (11) | 0.0105 (13) | 0.0103 (13) |
N7 | 0.0673 (15) | 0.0573 (14) | 0.0698 (17) | 0.0056 (11) | −0.0002 (12) | −0.0116 (12) |
O1 | 0.0928 (15) | 0.0498 (11) | 0.0878 (14) | −0.0128 (9) | 0.0247 (11) | −0.0028 (10) |
O2 | 0.0933 (16) | 0.0487 (11) | 0.1238 (19) | −0.0015 (10) | 0.0224 (14) | −0.0022 (12) |
O3 | 0.144 (2) | 0.1027 (18) | 0.139 (2) | −0.0056 (16) | 0.0598 (19) | 0.0548 (16) |
O4 | 0.1170 (18) | 0.0683 (13) | 0.0889 (15) | 0.0332 (12) | 0.0355 (13) | 0.0237 (11) |
O5 | 0.143 (2) | 0.0493 (11) | 0.0776 (15) | −0.0070 (12) | 0.0100 (14) | 0.0051 (10) |
O6 | 0.0984 (17) | 0.0939 (16) | 0.128 (2) | 0.0228 (13) | 0.0159 (14) | −0.0569 (15) |
C1 | 0.0674 (18) | 0.0404 (13) | 0.0620 (16) | 0.0060 (11) | 0.0056 (13) | 0.0110 (11) |
C2 | 0.0729 (19) | 0.0557 (16) | 0.0533 (16) | 0.0216 (14) | 0.0016 (13) | 0.0062 (12) |
C3 | 0.0534 (15) | 0.0673 (17) | 0.0565 (16) | 0.0121 (12) | −0.0030 (12) | −0.0032 (13) |
C4 | 0.0501 (15) | 0.0530 (14) | 0.0552 (16) | −0.0028 (11) | 0.0010 (12) | −0.0001 (11) |
C5 | 0.0467 (14) | 0.0396 (11) | 0.0430 (13) | 0.0026 (9) | 0.0077 (10) | 0.0000 (10) |
C6 | 0.0482 (12) | 0.0362 (11) | 0.0400 (12) | −0.0023 (10) | 0.0072 (10) | 0.0035 (9) |
C7 | 0.0552 (14) | 0.0352 (11) | 0.0579 (15) | −0.0084 (11) | 0.0097 (11) | −0.0005 (10) |
C8 | 0.0697 (17) | 0.0289 (11) | 0.0656 (16) | 0.0005 (11) | 0.0163 (13) | 0.0019 (10) |
C9 | 0.0524 (14) | 0.0349 (11) | 0.0676 (16) | 0.0077 (10) | 0.0154 (12) | 0.0042 (11) |
C10 | 0.0487 (13) | 0.0353 (11) | 0.0469 (13) | 0.0006 (10) | 0.0097 (10) | −0.0002 (10) |
C11 | 0.0492 (15) | 0.0421 (12) | 0.0455 (14) | −0.0009 (10) | 0.0069 (11) | 0.0045 (10) |
C12 | 0.0531 (16) | 0.0584 (15) | 0.0596 (16) | 0.0005 (12) | 0.0030 (12) | 0.0033 (12) |
C13 | 0.0612 (17) | 0.0734 (19) | 0.0552 (16) | −0.0152 (14) | −0.0067 (13) | 0.0015 (13) |
C14 | 0.081 (2) | 0.0572 (16) | 0.0557 (17) | −0.0210 (14) | −0.0042 (14) | −0.0054 (13) |
C15 | 0.0744 (19) | 0.0429 (14) | 0.0625 (17) | −0.0022 (12) | 0.0016 (14) | −0.0078 (12) |
O7 | 0.0635 (12) | 0.0439 (10) | 0.0882 (15) | −0.0020 (8) | 0.0167 (11) | −0.0007 (10) |
Geometric parameters (Å, º) top
Cd1—N1 | 2.2345 (19) | C1—C2 | 1.365 (3) |
Cd1—N3 | 2.3148 (17) | C2—C3 | 1.377 (4) |
Cd1—N5 | 2.2351 (19) | C3—C4 | 1.365 (3) |
Cd1—O1 | 2.4644 (19) | C4—C5 | 1.397 (3) |
Cd1—O2 | 2.431 (2) | C6—C7 | 1.384 (3) |
Cd1—O4 | 2.603 (2) | C7—C8 | 1.370 (3) |
Cd1—O5 | 2.441 (2) | C8—C9 | 1.371 (3) |
N1—C1 | 1.357 (3) | C9—C10 | 1.391 (3) |
N1—C5 | 1.334 (3) | C11—C12 | 1.398 (3) |
N2—C5 | 1.381 (3) | C12—C13 | 1.361 (3) |
N2—C6 | 1.398 (3) | C13—C14 | 1.380 (4) |
N3—C6 | 1.354 (3) | C14—C15 | 1.356 (4) |
N3—C10 | 1.341 (3) | N2—H2A | 0.8602 |
N4—C10 | 1.395 (3) | N4—H4A | 0.8603 |
N4—C11 | 1.382 (3) | C1—H1A | 0.9293 |
N5—C11 | 1.331 (3) | C2—H2B | 0.9297 |
N5—C15 | 1.353 (3) | C3—H3A | 0.9297 |
N6—O1 | 1.240 (2) | C4—H4B | 0.9306 |
N6—O2 | 1.257 (3) | C7—H7A | 0.9305 |
N6—O3 | 1.211 (3) | C8—H8A | 0.9294 |
N7—O4 | 1.226 (3) | C9—H9A | 0.9299 |
N7—O5 | 1.263 (3) | C12—H12A | 0.9307 |
N7—O6 | 1.209 (3) | C13—H13A | 0.9296 |
O7—H7B | 0.86 (3) | C14—H14A | 0.9298 |
O7—H7C | 0.78 (3) | C15—H15A | 0.9290 |
| | | |
N1—Cd1—N3 | 85.62 (6) | N2—C5—C4 | 117.7 (2) |
N1—Cd1—N5 | 169.39 (6) | N3—C6—C7 | 122.8 (2) |
N1—Cd1—O1 | 96.37 (7) | N3—C6—N2 | 121.02 (18) |
N1—Cd1—O2 | 97.71 (7) | N3—C10—C9 | 123.2 (2) |
N1—Cd1—O4 | 88.99 (7) | N3—C10—N4 | 121.22 (18) |
N1—Cd1—O5 | 85.90 (7) | N4—C11—C12 | 117.6 (2) |
N3—Cd1—O1 | 94.57 (6) | N5—C11—N4 | 121.1 (2) |
N3—Cd1—O2 | 145.78 (7) | N5—C11—C12 | 121.3 (2) |
N3—Cd1—O4 | 94.83 (6) | N5—C15—C14 | 123.5 (2) |
N3—Cd1—O5 | 143.15 (6) | N5—C15—H15A | 118.24 |
N5—Cd1—O1 | 88.70 (7) | C1—C2—C3 | 118.7 (2) |
N5—Cd1—O2 | 92.73 (7) | C1—C2—H2B | 120.70 |
N5—Cd1—O4 | 87.53 (7) | C2—C1—H1A | 118.51 |
N5—Cd1—O5 | 99.33 (7) | C2—C3—H3A | 120.44 |
N5—Cd1—N3 | 84.70 (6) | C3—C2—H2B | 120.55 |
O1—Cd1—O4 | 169.50 (7) | C3—C4—C5 | 119.7 (2) |
O1—N6—O2 | 115.9 (2) | C3—C4—H4B | 120.12 |
O2—Cd1—O1 | 51.22 (6) | C4—C3—C2 | 119.2 (2) |
O2—Cd1—O4 | 119.20 (7) | C4—C3—H3A | 120.43 |
O2—Cd1—O5 | 70.97 (7) | C5—N2—H2A | 113.52 |
O3—N6—O1 | 121.9 (3) | C5—C4—H4B | 120.16 |
O3—N6—O2 | 122.2 (3) | C6—N2—H2A | 113.61 |
O4—N7—O5 | 115.5 (2) | C6—C7—H7A | 120.60 |
O5—Cd1—O1 | 121.99 (6) | C7—C6—N2 | 116.2 (2) |
O5—Cd1—O4 | 49.23 (6) | C7—C8—C9 | 119.8 (2) |
O6—N7—O4 | 121.9 (3) | C7—C8—H8A | 120.07 |
O6—N7—O5 | 122.6 (3) | C8—C7—C6 | 118.8 (2) |
N6—O1—Cd1 | 95.86 (16) | C8—C7—H7A | 120.64 |
N6—O2—Cd1 | 97.01 (15) | C8—C9—C10 | 118.4 (2) |
N7—O4—Cd1 | 94.06 (16) | C8—C9—H9A | 120.83 |
N7—O5—Cd1 | 101.03 (15) | C9—C8—H8A | 120.10 |
C1—N1—Cd1 | 116.92 (15) | C9—C10—N4 | 115.6 (2) |
C5—N1—C1 | 118.1 (2) | C10—N4—H4A | 112.92 |
C5—N1—Cd1 | 124.44 (15) | C10—C9—H9A | 120.79 |
C5—N2—C6 | 132.87 (18) | C11—N4—H4A | 112.87 |
C6—N3—Cd1 | 121.62 (14) | C11—C12—H12A | 120.29 |
C10—N3—C6 | 117.02 (18) | C12—C13—C14 | 119.4 (3) |
C10—N3—Cd1 | 121.23 (14) | C12—C13—H13A | 120.28 |
C11—N4—C10 | 134.18 (19) | C13—C12—C11 | 119.5 (2) |
C11—N5—C15 | 118.0 (2) | C13—C12—H12A | 120.21 |
C11—N5—Cd1 | 123.31 (15) | C13—C14—H14A | 120.84 |
C15—N5—Cd1 | 117.23 (16) | C14—C13—H13A | 120.34 |
N1—C1—C2 | 123.0 (2) | C14—C15—H15A | 118.24 |
N1—C1—H1A | 118.51 | C15—C14—C13 | 118.3 (2) |
N1—C5—N2 | 121.0 (2) | C15—C14—H14A | 120.85 |
N1—C5—C4 | 121.3 (2) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2A···O7i | 0.86 | 2.14 | 2.938 (3) | 153 |
N4—H4A···O7 | 0.86 | 2.22 | 3.009 (3) | 153 |
O7—H7B···O5ii | 0.86 (3) | 2.03 (3) | 2.843 (2) | 158 |
O7—H7C···O6iii | 0.78 (3) | 2.31 (3) | 3.063 (2) | 163 |
Symmetry codes: (i) x−1, y, z; (ii) −x, y−1/2, −z+1/2; (iii) −x, −y+1, −z+1. |
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