
![[kappa]](/logos/entities/kappa_rmgif.gif)
![[kappa]](/logos/entities/kappa_rmgif.gif)
![[mu]](/logos/entities/mu_rmgif.gif)
Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270113019999/wq3042sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S0108270113019999/wq3042Isup2.hkl |
CCDC reference: 964757
Recently, the design and synthesis of coordination polymers has attracted research interest for their intriguing structures and potentially useful properties (Dinca et al., 2006; Du et al., 2013; Férey et al., 2005; Pan et al., 2006; Seo et al., 2000). Many factors including the coordination modes of the metal ions, the metal–ligand ratios, the nature of the organic ligands, solvent effect, pH and temperature can impact on the resulting architectures of the complexes (Li & Du, 2011; Long et al., 2002; Pan et al., 2000; Tong et al., 2003). Among these factors, the selection of the organic ligand plays an important role in the design and prediction of the complexes. Notably, ligands containing different functional groups, including pyridine, triazole and carboxylic acid, are frequently chosen to regulate the structural assembly, to afford various coordination systems from discrete and to form infinite one-, two- and three-dimensional polymeric frameworks. To date, some multidentate ligands containing N-donor heterocyclic groups, such as 4,4'-bipyridine, 2,4'-bipyridine, 1,2-bis(pyridin-4-yl)ethane, 1,2-bis(pyridin-4-yl)ethyne, 1,3-bis(pyridin-4-yl)propane, 1,2,4-triazole and 4-amino-bis(pyridin-4-yl)-1,2,4-triazole have been used to assemble diverse coordination networks (Carlucci et al., 1999, 2003; Du et al., 2005; Steel, 2005; Tong et al., 1998). In addition, the synthetic pathways leading to the crystalline materials can also affect their structural and functional diversification. The hydrothermal method has proven to be a powerful method for the preparation of crystalline materials under high pressure and temperature (Li et al., 2011). Thus, in this work, 5-(pyridin-2-yl)-3,3'-bi(4H-1,2,4-triazole) (H2BPT) was used as the organic ligand to assemble with CdII under hydrothermal conditions (Wiley & Hart, 1953; Potts et al., 1960). As a multidentate ligand, H2BPT may display various coordination modes through different degrees of deprotonation to coordinate metal ions, and further, its aromatic rings can potentially provide multiple weak interaction sites to extend to higher-dimensional supramolecular networks.
A mixture of H2BPT (21.3 mg, 0.1 mmol) and Cd(NO3)2.4H2O (30.8 mg, 0.1 mmol) in water (10 ml) and methanol (5 ml) was sealed in a Teflon-lined stainless steel vessel (20 ml), which was heated to 413 K for 24 h and then gradually cooled to room temperature at a rate of 5 K h-1. Colourless block-shaped single crystals were obtained in 18% yield (7.5 mg). Analysis calculated for C10H10CdN8O4: C 28.69, H 2.41, N 26.77%; found: C 28.21, H 2.06, N 26.29%. IR (cm-1): 3422 (b), 1601 (vs), 1430 (m), 1406 (m), 1384 (s), 1332 (m), 1284 (s), 1197 (m), 1097 (m), 1023 (s), 993 (m), 961 (s), 891 (w), 796 (m), 750 (m), 719 (m), 699 (m), 450 (m).
Crystal data, data collection and structure refinement details are summarized in Table 1. All H atoms were initially located in a difference Fourier map, which were then constrained to an ideal geometry, and refined as riding atoms, with C—H = 0.93 Å (Csp2), C—H = 0.96 Å (Csp3), N—H = 0.86 Å (NH) and O—H = 0.85 Å (OH), and with Uiso(H) = 1.2Ueq(Csp2), Uiso(HH) = 1.5Ueq(Csp3), Uiso(H) = 1.2Ueq(N) and Uiso(H) = 1.5Ueq(O).
The asymmetric unit of the title complex, [Cd(HBPT)(NO3)(CH3OH)]n, (I), is composed of one CdII centre, one nitrate anion, one HBPT- ligand and one coordinated methanol molecule. As shown in Fig. 1, each CdII ion adopts an octahedral geometry and is surrounded by four N atoms from two HBPT- ligands locating at the basal equatorial plane, and two axial O atoms from one monodentate nitrate anion and one methanol ligand, with an O1—Cd—O4 angle of 173.8 (1)°. The Cd—Npy bond length (py is pyridine) is 2.313 (2) Å (Cd—N1) and the Cd—Ntriazoyl bond lengths are in the range 2.268 (2)–2.393 (2) Å. The cis N—Cd—N angles fall in the range 72.4 (1)–110.4 (1)° and the trans N—Cd—N angles are 174.0 (1) and 175.5 (1) °. In addition, the O—Cd—N angles lie in the range 82.7 (1)–98.5 (1)°. In this structure, each HBPT- anion serves as a tetradentate bridging ligand, linking adjacent CdII centres to generate a one-dimensional polymeric motif (see Fig. 2), with a Cd···Cd distance of 6.600 (1) Å.
Furthermore, these adjacent one-dimensional coordination motifs are arranged in a parallel arrangement and are further connected via hydrogen-bonding interaction (O4—H4A···O3i; see Table 2 for details and symmetry code) between the coordinated methanol molecule and the nitrate anion, which consequently interlinks such one-dimensional arrays to afford the two-dimensional hydrogen-bonding network (see Fig. 3). In addition, this structure is also stabilized by an intramolecular N7—H7···N3ii hydrogen bond (Table 2) between the two triazole rings of the ligand. Further analysis indicates that these adjacent two-dimensional layers can be further connected to the resultant three-dimensional supramolecular network by π–π stacking interactions between the pyridine (atoms N1/C1—C5) and triazole (atoms C8/C9/N5–N7) rings, with a centre-to-centre distance of 3.847 (2) Å and a dihedral angle of 4.3 (2)°, as well as between two parallel pyridine rings with a centre-to-centre distance of 3.777 (2) Å (see Fig. 4). Notably, these adjacent two-dimensional layers are arranged in an interdigitated packing mode, and the aromatic stacking interactions are clearly shown in Fig. 5.
As reported previously (Dong, et al., 2012), another CdII coordination polymer {[Cd2(BPT)2(H2O)2].2H2O}n, (II) assembled from H2BPT has been investigated, which shows a three-dimensional (3,4)-connected network. The CdII centres in both complexes display the distorted octahedral coordination geometry. In the title complex, H2BPT is monodeprotonated and adopts a µ2-bridging mode, while in (II), two independent H2BPT ligands in different conformations are both fully deprotonated and display µ3-bridging modes. Besides BPT ligands, only a water molecule is involved in the coordination to the CdII atom of (II). Whereas for (I), both the additional nitrate and methanol ligands participate in the coordination with the metal centre. Such significant differences in the coordination environments result in the diverse extended networks.
In summary, assembly of Cd(NO3)2 with a multidentate organic ligand 5-(pyridin-2-yl)-3,3'-bi(4H-1,2,4-triazole) ligand affords the title complex under hydrothermal method. In this structure, the nitrate anion serves as a terminal ligand, whereas the HBPT- anion behaves as a bridge, generating a one-dimensional chain array. In addition, the resulting three-dimensional supramolecular network is extended via hydrogen bonding and aromatic stacking interactions.
Data collection: SMART (Bruker, 2001); cell refinement: SMART (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL (Bruker, 2001).
The asymmetric unit and coordination environment of (I). Displacement
ellipsoids are drawn at the 30% probability level. [Symmetry code: (A)
x, -y+3/2, z-1/2.] [Please provide fully labelled
ellipsoid plot] A view of the one-dimensional coordination chain linked via the bridging HBPT- ligand. A view of the two-dimensional hydrogen-bonding layer linked via O4—H4A···O3 hydrogen-bonding interactions. The three-dimensional supramolecular network of (I) extended via aromatic stacking interactions. Adjacent layers are shown in different colors and the broken lines between them indicate the aromatic stacking interactions. A schematic diagram illustrating the aromatic stacking interactions. |
[Cd(C9H6N7)(NO3)(CH4O)] | F(000) = 824 |
Mr = 418.66 | Dx = 1.981 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 2997 reflections |
a = 8.0272 (13) Å | θ = 2.9–30.3° |
b = 17.482 (3) Å | µ = 1.59 mm−1 |
c = 11.4236 (13) Å | T = 296 K |
β = 118.899 (8)° | Block, colourless |
V = 1403.5 (4) Å3 | 0.28 × 0.22 × 0.20 mm |
Z = 4 |
Bruker SMART CCD area-detector diffractometer | 2483 independent reflections |
Radiation source: fine-focus sealed tube | 2142 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.022 |
phi and ω scans | θmax = 25.0°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −9→8 |
Tmin = 0.664, Tmax = 0.741 | k = −16→20 |
7110 measured reflections | l = −12→13 |
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) = 0.060 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0266P)2 + 0.9282P] where P = (Fo2 + 2Fc2)/3 |
2483 reflections | (Δ/σ)max = 0.001 |
209 parameters | Δρmax = 0.43 e Å−3 |
0 restraints | Δρmin = −0.38 e Å−3 |
[Cd(C9H6N7)(NO3)(CH4O)] | V = 1403.5 (4) Å3 |
Mr = 418.66 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 8.0272 (13) Å | µ = 1.59 mm−1 |
b = 17.482 (3) Å | T = 296 K |
c = 11.4236 (13) Å | 0.28 × 0.22 × 0.20 mm |
β = 118.899 (8)° |
Bruker SMART CCD area-detector diffractometer | 2483 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | 2142 reflections with I > 2σ(I) |
Tmin = 0.664, Tmax = 0.741 | Rint = 0.022 |
7110 measured reflections |
R[F2 > 2σ(F2)] = 0.024 | 0 restraints |
wR(F2) = 0.060 | H-atom parameters constrained |
S = 1.06 | Δρmax = 0.43 e Å−3 |
2483 reflections | Δρmin = −0.38 e Å−3 |
209 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 | 0.74109 (3) | 0.844581 (12) | 0.15250 (2) | 0.03064 (9) | |
O1 | 0.4121 (3) | 0.87064 (14) | 0.0350 (3) | 0.0516 (6) | |
O2 | 0.3887 (4) | 0.74947 (16) | 0.0502 (3) | 0.0726 (9) | |
O3 | 0.1487 (4) | 0.81372 (19) | −0.0924 (3) | 0.0769 (9) | |
O4 | 1.0743 (3) | 0.83118 (15) | 0.2819 (2) | 0.0512 (6) | |
H4A | 1.0874 | 0.7879 | 0.3192 | 0.077* | |
N1 | 0.7561 (4) | 0.95130 (14) | 0.2769 (2) | 0.0320 (6) | |
N2 | 0.7475 (3) | 0.79871 (14) | 0.3438 (2) | 0.0277 (5) | |
N3 | 0.7483 (4) | 0.83071 (14) | 0.5339 (3) | 0.0362 (6) | |
N4 | 0.7474 (4) | 0.75356 (14) | 0.5249 (2) | 0.0351 (6) | |
N5 | 0.7548 (4) | 0.60146 (14) | 0.4648 (2) | 0.0339 (6) | |
N6 | 0.7508 (4) | 0.54615 (15) | 0.2860 (3) | 0.0459 (7) | |
N7 | 0.7455 (4) | 0.62351 (14) | 0.2743 (2) | 0.0348 (6) | |
H7 | 0.7408 | 0.6480 | 0.2075 | 0.042* | |
N8 | 0.3149 (4) | 0.81078 (19) | −0.0033 (3) | 0.0456 (7) | |
C1 | 0.7604 (5) | 1.02383 (19) | 0.2438 (3) | 0.0449 (9) | |
H1 | 0.7679 | 1.0342 | 0.1666 | 0.054* | |
C2 | 0.7544 (5) | 1.0841 (2) | 0.3183 (3) | 0.0501 (9) | |
H2 | 0.7570 | 1.1342 | 0.2919 | 0.060* | |
C3 | 0.7444 (6) | 1.0693 (2) | 0.4318 (3) | 0.0518 (10) | |
H3 | 0.7388 | 1.1095 | 0.4832 | 0.062* | |
C4 | 0.7427 (5) | 0.99541 (19) | 0.4701 (3) | 0.0432 (8) | |
H4 | 0.7378 | 0.9847 | 0.5482 | 0.052* | |
C5 | 0.7482 (4) | 0.93692 (17) | 0.3907 (3) | 0.0292 (7) | |
C6 | 0.7484 (4) | 0.85576 (16) | 0.4242 (3) | 0.0285 (7) | |
C7 | 0.7481 (4) | 0.73607 (16) | 0.4120 (3) | 0.0285 (7) | |
C8 | 0.7483 (4) | 0.65588 (16) | 0.3800 (3) | 0.0278 (6) | |
C9 | 0.7553 (5) | 0.53624 (19) | 0.4020 (3) | 0.0429 (8) | |
H9 | 0.7586 | 0.4881 | 0.4376 | 0.051* | |
C10 | 1.2111 (6) | 0.8400 (3) | 0.2421 (5) | 0.0775 (14) | |
H10A | 1.2094 | 0.7963 | 0.1907 | 0.116* | |
H10B | 1.3343 | 0.8445 | 0.3196 | 0.116* | |
H10C | 1.1845 | 0.8853 | 0.1885 | 0.116* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.04547 (16) | 0.03077 (14) | 0.02199 (13) | 0.00298 (10) | 0.02128 (11) | −0.00006 (9) |
O1 | 0.0472 (15) | 0.0414 (14) | 0.0593 (16) | −0.0043 (12) | 0.0203 (13) | −0.0028 (12) |
O2 | 0.080 (2) | 0.0429 (17) | 0.090 (2) | 0.0007 (15) | 0.0374 (18) | −0.0025 (16) |
O3 | 0.0449 (17) | 0.093 (2) | 0.070 (2) | −0.0092 (16) | 0.0097 (15) | −0.0044 (18) |
O4 | 0.0472 (14) | 0.0631 (17) | 0.0447 (14) | 0.0067 (12) | 0.0233 (12) | 0.0073 (12) |
N1 | 0.0467 (16) | 0.0281 (14) | 0.0252 (13) | 0.0005 (11) | 0.0205 (12) | 0.0011 (11) |
N2 | 0.0378 (14) | 0.0272 (14) | 0.0228 (12) | 0.0001 (11) | 0.0184 (11) | 0.0015 (11) |
N3 | 0.0610 (18) | 0.0266 (14) | 0.0300 (14) | −0.0002 (12) | 0.0292 (13) | −0.0025 (11) |
N4 | 0.0592 (18) | 0.0295 (14) | 0.0262 (13) | −0.0013 (12) | 0.0283 (13) | 0.0005 (11) |
N5 | 0.0538 (17) | 0.0283 (14) | 0.0278 (13) | −0.0007 (12) | 0.0263 (12) | 0.0022 (11) |
N6 | 0.079 (2) | 0.0300 (16) | 0.0423 (16) | −0.0014 (14) | 0.0403 (16) | −0.0024 (13) |
N7 | 0.0588 (18) | 0.0285 (14) | 0.0274 (13) | −0.0023 (12) | 0.0290 (13) | −0.0003 (11) |
N8 | 0.0454 (18) | 0.052 (2) | 0.0426 (17) | −0.0038 (16) | 0.0240 (15) | −0.0059 (15) |
C1 | 0.067 (2) | 0.037 (2) | 0.0348 (18) | −0.0007 (17) | 0.0275 (17) | 0.0051 (15) |
C2 | 0.077 (3) | 0.0255 (18) | 0.046 (2) | −0.0005 (17) | 0.0279 (19) | 0.0020 (16) |
C3 | 0.082 (3) | 0.0310 (19) | 0.044 (2) | 0.0032 (18) | 0.032 (2) | −0.0080 (16) |
C4 | 0.068 (2) | 0.0375 (19) | 0.0314 (17) | 0.0028 (17) | 0.0302 (17) | −0.0008 (15) |
C5 | 0.0354 (17) | 0.0294 (16) | 0.0237 (14) | −0.0007 (13) | 0.0151 (13) | −0.0032 (13) |
C6 | 0.0362 (17) | 0.0283 (16) | 0.0227 (15) | −0.0001 (12) | 0.0156 (13) | −0.0015 (12) |
C7 | 0.0367 (17) | 0.0311 (17) | 0.0225 (14) | 0.0017 (13) | 0.0181 (13) | 0.0021 (13) |
C8 | 0.0381 (17) | 0.0302 (16) | 0.0212 (14) | −0.0018 (13) | 0.0191 (13) | −0.0004 (12) |
C9 | 0.073 (2) | 0.0255 (17) | 0.0420 (19) | −0.0011 (16) | 0.0368 (18) | 0.0019 (15) |
C10 | 0.064 (3) | 0.104 (4) | 0.080 (3) | 0.002 (3) | 0.047 (3) | 0.014 (3) |
Cd1—N4i | 2.268 (2) | N5—C9 | 1.348 (4) |
Cd1—N2 | 2.305 (2) | N5—Cd1ii | 2.393 (2) |
Cd1—N1 | 2.313 (2) | N6—C9 | 1.319 (4) |
Cd1—O1 | 2.357 (2) | N6—N7 | 1.358 (4) |
Cd1—O4 | 2.361 (2) | N7—C8 | 1.324 (4) |
Cd1—N5i | 2.393 (2) | N7—H7 | 0.8599 |
O1—N8 | 1.251 (4) | C1—C2 | 1.370 (5) |
O2—N8 | 1.234 (4) | C1—H1 | 0.9300 |
O3—N8 | 1.227 (4) | C2—C3 | 1.361 (5) |
O4—C10 | 1.385 (5) | C2—H2 | 0.9300 |
O4—H4A | 0.8502 | C3—C4 | 1.367 (5) |
N1—C1 | 1.329 (4) | C3—H3 | 0.9300 |
N1—C5 | 1.355 (4) | C4—C5 | 1.382 (4) |
N2—C7 | 1.343 (4) | C4—H4 | 0.9300 |
N2—C6 | 1.353 (4) | C5—C6 | 1.469 (4) |
N3—C6 | 1.329 (4) | C7—C8 | 1.449 (4) |
N3—N4 | 1.352 (3) | C9—H9 | 0.9300 |
N4—C7 | 1.328 (3) | C10—H10A | 0.9600 |
N4—Cd1ii | 2.268 (2) | C10—H10B | 0.9600 |
N5—C8 | 1.341 (4) | C10—H10C | 0.9600 |
N4i—Cd1—N2 | 110.43 (8) | O3—N8—O2 | 121.1 (3) |
N4i—Cd1—N1 | 174.02 (9) | O3—N8—O1 | 120.0 (3) |
N2—Cd1—N1 | 74.17 (8) | O2—N8—O1 | 119.0 (3) |
N4i—Cd1—O1 | 98.46 (9) | N1—C1—C2 | 122.9 (3) |
N2—Cd1—O1 | 96.46 (9) | N1—C1—H1 | 118.5 |
N1—Cd1—O1 | 84.57 (9) | C2—C1—H1 | 118.6 |
N4i—Cd1—O4 | 87.54 (9) | C3—C2—C1 | 118.8 (3) |
N2—Cd1—O4 | 82.67 (8) | C3—C2—H2 | 120.6 |
N1—Cd1—O4 | 89.33 (9) | C1—C2—H2 | 120.6 |
O1—Cd1—O4 | 173.84 (8) | C2—C3—C4 | 119.9 (3) |
N4i—Cd1—N5i | 72.38 (8) | C2—C3—H3 | 120.0 |
N2—Cd1—N5i | 175.54 (8) | C4—C3—H3 | 120.0 |
N1—Cd1—N5i | 102.79 (8) | C3—C4—C5 | 118.7 (3) |
O1—Cd1—N5i | 86.42 (9) | C3—C4—H4 | 120.7 |
O4—Cd1—N5i | 94.10 (9) | C5—C4—H4 | 120.7 |
N8—O1—Cd1 | 112.0 (2) | N1—C5—C4 | 121.6 (3) |
C10—O4—Cd1 | 128.4 (2) | N1—C5—C6 | 115.7 (2) |
C10—O4—H4A | 109.7 | C4—C5—C6 | 122.7 (3) |
Cd1—O4—H4A | 103.3 | N3—C6—N2 | 113.3 (2) |
C1—N1—C5 | 118.0 (3) | N3—C6—C5 | 124.3 (3) |
C1—N1—Cd1 | 126.6 (2) | N2—C6—C5 | 122.4 (2) |
C5—N1—Cd1 | 115.28 (18) | N4—C7—N2 | 112.0 (3) |
C7—N2—C6 | 102.2 (2) | N4—C7—C8 | 118.0 (3) |
C7—N2—Cd1 | 145.69 (19) | N2—C7—C8 | 130.0 (3) |
C6—N2—Cd1 | 112.15 (18) | N7—C8—N5 | 109.5 (3) |
C6—N3—N4 | 105.0 (2) | N7—C8—C7 | 129.9 (3) |
C7—N4—N3 | 107.5 (2) | N5—C8—C7 | 120.6 (3) |
C7—N4—Cd1ii | 117.5 (2) | N6—C9—N5 | 114.7 (3) |
N3—N4—Cd1ii | 134.95 (19) | N6—C9—H9 | 122.6 |
C8—N5—C9 | 103.0 (2) | N5—C9—H9 | 122.6 |
C8—N5—Cd1ii | 111.41 (19) | O4—C10—H10A | 109.5 |
C9—N5—Cd1ii | 145.4 (2) | O4—C10—H10B | 109.5 |
C9—N6—N7 | 102.4 (3) | H10A—C10—H10B | 109.5 |
C8—N7—N6 | 110.5 (2) | O4—C10—H10C | 109.5 |
C8—N7—H7 | 124.8 | H10A—C10—H10C | 109.5 |
N6—N7—H7 | 124.8 | H10B—C10—H10C | 109.5 |
N4i—Cd1—O1—N8 | 39.3 (2) | C1—N1—C5—C6 | −178.6 (3) |
N2—Cd1—O1—N8 | −72.5 (2) | Cd1—N1—C5—C6 | 5.2 (3) |
N1—Cd1—O1—N8 | −145.9 (2) | C3—C4—C5—N1 | 0.3 (5) |
N5i—Cd1—O1—N8 | 110.9 (2) | C3—C4—C5—C6 | 179.5 (3) |
N4i—Cd1—O4—C10 | 62.0 (3) | N4—N3—C6—N2 | 0.0 (4) |
N2—Cd1—O4—C10 | 173.0 (3) | N4—N3—C6—C5 | 179.6 (3) |
N1—Cd1—O4—C10 | −112.9 (3) | C7—N2—C6—N3 | −0.4 (3) |
N5i—Cd1—O4—C10 | −10.1 (3) | Cd1—N2—C6—N3 | 178.8 (2) |
N2—Cd1—N1—C1 | 179.9 (3) | C7—N2—C6—C5 | 180.0 (3) |
O1—Cd1—N1—C1 | −81.8 (3) | Cd1—N2—C6—C5 | −0.8 (3) |
O4—Cd1—N1—C1 | 97.3 (3) | N1—C5—C6—N3 | 177.4 (3) |
N5i—Cd1—N1—C1 | 3.3 (3) | C4—C5—C6—N3 | −1.8 (5) |
N2—Cd1—N1—C5 | −4.3 (2) | N1—C5—C6—N2 | −3.0 (4) |
O1—Cd1—N1—C5 | 94.0 (2) | C4—C5—C6—N2 | 177.7 (3) |
O4—Cd1—N1—C5 | −86.8 (2) | N3—N4—C7—N2 | −0.7 (4) |
N5i—Cd1—N1—C5 | 179.1 (2) | Cd1ii—N4—C7—N2 | 178.56 (18) |
N4i—Cd1—N2—C7 | −2.9 (4) | N3—N4—C7—C8 | 179.7 (3) |
N1—Cd1—N2—C7 | −178.9 (4) | Cd1ii—N4—C7—C8 | −1.1 (4) |
O1—Cd1—N2—C7 | 98.7 (4) | C6—N2—C7—N4 | 0.7 (3) |
O4—Cd1—N2—C7 | −87.5 (4) | Cd1—N2—C7—N4 | −178.0 (2) |
N4i—Cd1—N2—C6 | 178.54 (19) | C6—N2—C7—C8 | −179.8 (3) |
N1—Cd1—N2—C6 | 2.55 (19) | Cd1—N2—C7—C8 | 1.6 (6) |
O1—Cd1—N2—C6 | −79.9 (2) | N6—N7—C8—N5 | −0.3 (4) |
O4—Cd1—N2—C6 | 93.9 (2) | N6—N7—C8—C7 | 178.8 (3) |
C6—N3—N4—C7 | 0.4 (3) | C9—N5—C8—N7 | 0.0 (4) |
C6—N3—N4—Cd1ii | −178.7 (2) | Cd1ii—N5—C8—N7 | −176.5 (2) |
C9—N6—N7—C8 | 0.5 (4) | C9—N5—C8—C7 | −179.2 (3) |
Cd1—O1—N8—O3 | −161.8 (3) | Cd1ii—N5—C8—C7 | 4.3 (4) |
Cd1—O1—N8—O2 | 18.6 (4) | N4—C7—C8—N7 | 178.6 (3) |
C5—N1—C1—C2 | −1.0 (5) | N2—C7—C8—N7 | −1.0 (6) |
Cd1—N1—C1—C2 | 174.7 (3) | N4—C7—C8—N5 | −2.4 (4) |
N1—C1—C2—C3 | 0.3 (6) | N2—C7—C8—N5 | 178.0 (3) |
C1—C2—C3—C4 | 0.7 (6) | N7—N6—C9—N5 | −0.5 (4) |
C2—C3—C4—C5 | −1.0 (6) | C8—N5—C9—N6 | 0.4 (4) |
C1—N1—C5—C4 | 0.7 (5) | Cd1ii—N5—C9—N6 | 174.6 (3) |
Cd1—N1—C5—C4 | −175.5 (2) |
Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) x, −y+3/2, z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H4A···O3iii | 0.85 | 1.98 | 2.830 (4) | 173 |
N7—H7···N3i | 0.86 | 2.05 | 2.870 (4) | 160 |
Symmetry codes: (i) x, −y+3/2, z−1/2; (iii) x+1, −y+3/2, z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Cd(C9H6N7)(NO3)(CH4O)] |
Mr | 418.66 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 296 |
a, b, c (Å) | 8.0272 (13), 17.482 (3), 11.4236 (13) |
β (°) | 118.899 (8) |
V (Å3) | 1403.5 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.59 |
Crystal size (mm) | 0.28 × 0.22 × 0.20 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2001) |
Tmin, Tmax | 0.664, 0.741 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7110, 2483, 2142 |
Rint | 0.022 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.024, 0.060, 1.06 |
No. of reflections | 2483 |
No. of parameters | 209 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.43, −0.38 |
Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Bruker, 2001).
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H4A···O3i | 0.85 | 1.98 | 2.830 (4) | 173.1 |
N7—H7···N3ii | 0.86 | 2.05 | 2.870 (4) | 160.2 |
Symmetry codes: (i) x+1, −y+3/2, z+1/2; (ii) x, −y+3/2, z−1/2. |