Tetra­kis(3,5-dimethyl-1H-pyrazole-κN2)(nitrato-κ2O,O′)cadmium(II) nitrate

Wang, S.-Q.; Jian, F.-F.

doi:10.1107/S160053680803626X

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 12| December 2008| Page m1532

doi:10.1107/S160053680803626X

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Tetrakis(3,5-dimethyl-1H-pyrazole-κN²)(nitrato-κ²O,O′)cadmium(II) nitrate

Su-Qing Wang ^a and Fang-Fang Jian ^b ^*

^aMicroscale Science Institute, Department of Chemistry and Chemical Engineering, Weifang University, Weifang 261061, People's Republic of China, and ^bMicroscale Science Institute, Weifang University, Weifang 261061, People's Republic of China
^*Correspondence e-mail: ffjian2008@163.com

(Received 30 October 2008; accepted 6 November 2008; online 13 November 2008)

The title compound, [Cd(NO₃)(C₅H₈N₂)₄]NO₃, was prepared by reaction of cadmium nitrate and 3,5-dimethylpyrazole in ethanol solution. The Cd atom adopts a distorted cis-CdO₂N₄ octahedral geometry involving four dimethylpyrazole molecules and one bidentate nitrate anion. The molecular structure and packing are stabilized by N—H⋯O and C—H⋯O inter- and intramolecular hydrogen-bonding interactions.

Related literature

For background on the coordination chemistry of Cd(II) in biological systems, see: Dressing et al. (1982 ). For related literature, see: Addison et al. (1984 ).

Experimental

Crystal data

[Cd(NO₃)(C₅H₈N₂)₄]NO₃
M_r = 620.97
Triclinic, $[P \overline 1]$
a = 9.1790 (18) Å
b = 11.353 (2) Å
c = 13.669 (3) Å
α = 94.79 (3)°
β = 105.61 (3)°
γ = 90.68 (3)°
V = 1366.2 (5) Å³
Z = 2
Mo Kα radiation
μ = 0.85 mm⁻¹
T = 293 (2) K
0.25 × 0.20 × 0.18 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: none
7482 measured reflections
5035 independent reflections
4677 reflections with I > 2σ(I)
R_int = 0.016

Refinement

R[F² > 2σ(F²)] = 0.046
wR(F²) = 0.137
S = 1.06
5035 reflections
319 parameters
1 restraint
H-atom parameters constrained
Δρ_max = 1.66 e Å⁻³
Δρ_min = −0.87 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N3—H4A⋯O1ⁱ	0.86	2.13	2.943 (8)	157
N3—H4A⋯O3ⁱ	0.86	2.50	3.289 (16)	152
N4—H5A⋯O1ⁱ	0.86	1.92	2.771 (8)	171
N6—H7A⋯O6ⁱⁱ	0.86	2.33	3.131 (6)	156
N9—H10A⋯O4	0.86	2.50	3.106 (5)	128
C5—H5B⋯O4	0.96	2.59	3.530 (7)	166
C10—H10B⋯O5	0.96	2.29	3.157 (7)	150
C13—H13A⋯O1ⁱⁱⁱ	0.93	2.49	3.375 (8)	159
Symmetry codes: (i) x-1, y, z; (ii) -x, -y+2, -z+1; (iii) -x+1, -y+1, -z+1.

Data collection: SMART (Bruker, 1997 ); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S160053680803626X/at2668sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S160053680803626X/at2668Isup2.hkl

checkCIF report

Comment top

It is also known that most of the Cd(II) in biological systems is not in the form of free Cd(II) ions, but is coordinated by the abundance of biological ligands (Dressing et al., 1982). Therefore the coordination chemistry of Cd(II) with ligands is of great interest. In this paper, we reported the synthesis and the crystal structure of tri(3,5-dimenthyl pyrazolyl)cadmium(II) nitrate (I).

In the molecule of (I) (Fig. 1), each Cd atoms is coordinated by four nitrogen atoms from four 3,5-dimethyl pyrazoles respectively and two oxygen atoms from nitrate anion. All the bond length and angle are in the normal range. Another nitrate anion exists in the crystal lattice.

The molecular structure and packing are stabilized by the N—H···O and C—H···O inter and intraintermolecular hydrogen-bonding intercations.

Related literature top

For background on the coordination chemistry

of Cd(II) in biological systems, see: Dressing et al. (1982). For related literature, see: Addison et al. (1984).

Experimental top

Solid 3,5-dimethyl pyrazole 0.96 g (0.01 mol) and cadmium nitrate 0.77 g (0.0025 mol) were added in 50 ml anhydrous alcohol under stirring. The mixture was refluxed for 3.5 h. The colourless solution was filtered and the filtrate was left to stand undisturbed. Upon slow evaporation at room temperature, a colourless crystalline solid appeared three days later and was separated by filtration.

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

Fig. 1. The molecular structure and atom-labeling scheme for (I), with displacement ellipsoids drawn at the 30% probability level.

Tetrakis(3,5-dimethyl-1H-pyrazole-κN²)(nitrato-κ²O,O')cadmium(II) nitrate top

Crystal data top

[Cd(NO₃)(C₅H₈N₂)₄]NO₃	Z = 2
M_r = 620.97	F(000) = 636
Triclinic, P1	D_x = 1.509 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.1790 (18) Å	Cell parameters from 6067 reflections
b = 11.353 (2) Å	θ = 2.3–28.2°
c = 13.669 (3) Å	µ = 0.85 mm⁻¹
α = 94.79 (3)°	T = 293 K
β = 105.61 (3)°	Block, colourless
γ = 90.68 (3)°	0.25 × 0.20 × 0.18 mm
V = 1366.2 (5) Å³

Data collection top

Bruker SMART CCD area-detector diffractometer	4677 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.016
Graphite monochromator	θ_max = 25.5°, θ_min = 2.3°
ϕ and ω scans	h = −10→11
7482 measured reflections	k = −13→13
5035 independent reflections	l = −16→11

Refinement top

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)] = 0.047	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.137	H-atom parameters constrained
S = 1.06	w = 1/[σ²(F_o²) + (0.0885P)² + 1.8569P] where P = (F_o² + 2F_c²)/3
5035 reflections	(Δ/σ)_max < 0.001
319 parameters	Δρ_max = 1.66 e Å⁻³
1 restraint	Δρ_min = −0.87 e Å⁻³

Crystal data top

[Cd(NO₃)(C₅H₈N₂)₄]NO₃	γ = 90.68 (3)°
M_r = 620.97	V = 1366.2 (5) Å³
Triclinic, P1	Z = 2
a = 9.1790 (18) Å	Mo Kα radiation
b = 11.353 (2) Å	µ = 0.85 mm⁻¹
c = 13.669 (3) Å	T = 293 K
α = 94.79 (3)°	0.25 × 0.20 × 0.18 mm
β = 105.61 (3)°

Data collection top

Bruker SMART CCD area-detector diffractometer	4677 reflections with I > 2σ(I)
7482 measured reflections	R_int = 0.016
5035 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.047	1 restraint
wR(F²) = 0.137	H-atom parameters constrained
S = 1.06	Δρ_max = 1.66 e Å⁻³
5035 reflections	Δρ_min = −0.87 e Å⁻³
319 parameters

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	U_iso*/U_eq
Cd1	0.13316 (3)	0.80806 (2)	0.33031 (2)	0.03976 (14)
O4	0.3597 (4)	0.8966 (3)	0.4877 (3)	0.0559 (6)
O5	0.1497 (4)	0.9850 (3)	0.4459 (3)	0.0538 (6)
O6	0.3174 (5)	1.0465 (4)	0.5840 (3)	0.0679 (9)
N2	0.2219 (5)	0.6381 (3)	0.2677 (3)	0.0492 (7)
N3	0.1348 (5)	0.5493 (4)	0.2059 (4)	0.0600 (9)
H4A	0.0377	0.5444	0.1918	0.072*
N4	−0.2135 (4)	0.7666 (4)	0.1863 (3)	0.0497 (7)
H5A	−0.2040	0.6919	0.1909	0.060*
N5	−0.1073 (4)	0.8506 (3)	0.2393 (3)	0.0451 (6)
N6	−0.0798 (5)	0.7578 (3)	0.4743 (3)	0.0491 (7)
H7A	−0.1426	0.8045	0.4397	0.059*
N7	0.0527 (5)	0.7270 (3)	0.4544 (3)	0.0495 (6)
N8	0.2600 (4)	0.9168 (3)	0.2410 (3)	0.0461 (6)
N9	0.3644 (4)	1.0038 (3)	0.2868 (3)	0.0448 (7)
H10A	0.4081	1.0120	0.3512	0.054*
N10	0.2779 (4)	0.9758 (3)	0.5082 (3)	0.0464 (7)
C1	0.1461 (12)	0.3654 (6)	0.0977 (7)	0.112 (3)
H1A	0.2229	0.3187	0.0796	0.167*
H1B	0.0800	0.3925	0.0373	0.167*
H1C	0.0887	0.3183	0.1303	0.167*
C2	0.2191 (8)	0.4702 (5)	0.1697 (5)	0.0705 (13)
C3	0.3657 (8)	0.5085 (5)	0.2081 (5)	0.0731 (14)
H3A	0.4503	0.4715	0.1967	0.088*
C4	0.3647 (6)	0.6135 (4)	0.2678 (4)	0.0526 (9)
C5	0.4955 (6)	0.6919 (6)	0.3272 (5)	0.0731 (16)
H5B	0.4594	0.7572	0.3622	0.110*
H5C	0.5480	0.7210	0.2816	0.110*
H5D	0.5632	0.6478	0.3760	0.110*
C6	−0.4658 (7)	0.7409 (7)	0.0621 (6)	0.0848 (19)
H6A	−0.5406	0.7909	0.0249	0.127*
H6B	−0.5090	0.6967	0.1050	0.127*
H6C	−0.4327	0.6872	0.0151	0.127*
C7	−0.3346 (5)	0.8148 (5)	0.1261 (4)	0.0537 (9)
C8	−0.3053 (6)	0.9339 (5)	0.1395 (4)	0.0543 (9)
H8A	−0.3682	0.9912	0.1079	0.065*
C9	−0.1645 (5)	0.9538 (4)	0.2091 (3)	0.0464 (8)
C10	−0.0833 (7)	1.0697 (5)	0.2516 (5)	0.0689 (14)
H10B	0.0128	1.0559	0.2979	0.103*
H10C	−0.1429	1.1160	0.2873	0.103*
H10D	−0.0676	1.1116	0.1969	0.103*
C11	−0.2363 (8)	0.7287 (5)	0.5941 (5)	0.0694 (13)
H11A	−0.3011	0.7812	0.5520	0.104*
H11B	−0.2042	0.7641	0.6630	0.104*
H11C	−0.2906	0.6553	0.5920	0.104*
C12	−0.1004 (6)	0.7059 (4)	0.5551 (3)	0.0509 (8)
C13	0.0213 (7)	0.6372 (4)	0.5865 (4)	0.0572 (9)
H13A	0.0383	0.5892	0.6401	0.069*
C14	0.1155 (6)	0.6525 (4)	0.5233 (3)	0.0475 (7)
C15	0.2634 (6)	0.5992 (5)	0.5268 (5)	0.0657 (12)
H15A	0.3006	0.6251	0.4726	0.099*
H15B	0.2510	0.5145	0.5189	0.099*
H15C	0.3345	0.6234	0.5912	0.099*
C16	0.1073 (7)	0.8553 (6)	0.0647 (4)	0.0666 (14)
H16A	0.0727	0.7937	0.0979	0.100*
H16B	0.1547	0.8208	0.0150	0.100*
H16C	0.0228	0.8998	0.0314	0.100*
C17	0.2195 (5)	0.9358 (4)	0.1424 (3)	0.0462 (8)
C18	0.2983 (6)	1.0353 (4)	0.1273 (4)	0.0528 (9)
H18A	0.2891	1.0679	0.0658	0.063*
C19	0.3919 (5)	1.0756 (4)	0.2202 (4)	0.0459 (8)
C20	0.5065 (7)	1.1759 (5)	0.2532 (5)	0.0652 (13)
H20A	0.5515	1.1781	0.3254	0.098*
H20B	0.4578	1.2490	0.2373	0.098*
H20C	0.5835	1.1650	0.2180	0.098*
N1	0.7643 (6)	0.4506 (5)	0.1574 (5)	0.0806 (16)
O1	0.8224 (7)	0.5308 (6)	0.2225 (5)	0.1116 (18)*
O2	0.7028 (11)	0.3695 (9)	0.1665 (7)	0.164 (3)*
O3	0.7830 (17)	0.4749 (13)	0.0795 (12)	0.247 (6)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.0405 (2)	0.0371 (2)	0.0402 (2)	−0.00263 (12)	0.00835 (13)	0.00418 (12)
O4	0.0536 (12)	0.0644 (18)	0.0442 (11)	0.0005 (9)	0.0059 (9)	−0.0028 (10)
O5	0.0618 (15)	0.0429 (11)	0.0496 (14)	0.0006 (11)	0.0051 (9)	−0.0030 (9)
O6	0.079 (2)	0.068 (2)	0.0463 (17)	−0.0047 (17)	0.0045 (13)	−0.0119 (13)
N2	0.0505 (12)	0.0401 (10)	0.0565 (19)	−0.0024 (10)	0.0156 (13)	−0.0010 (10)
N3	0.0675 (15)	0.0397 (16)	0.070 (3)	−0.0119 (14)	0.0175 (19)	−0.0051 (14)
N4	0.0429 (13)	0.0510 (12)	0.051 (2)	−0.0062 (11)	0.0065 (11)	0.0048 (14)
N5	0.0432 (9)	0.0431 (12)	0.0471 (15)	−0.0030 (8)	0.0076 (8)	0.0091 (11)
N6	0.0595 (18)	0.0430 (19)	0.0497 (19)	0.0036 (14)	0.0214 (15)	0.0103 (13)
N7	0.0581 (15)	0.0460 (15)	0.0482 (16)	0.0079 (11)	0.0175 (12)	0.0144 (12)
N8	0.0434 (14)	0.0460 (14)	0.0456 (10)	−0.0075 (11)	0.0050 (10)	0.0097 (11)
N9	0.0458 (18)	0.0451 (18)	0.0430 (12)	−0.0069 (11)	0.0113 (12)	0.0045 (12)
N10	0.0557 (16)	0.0430 (17)	0.0392 (15)	−0.0088 (11)	0.0116 (10)	0.0023 (9)
C1	0.148 (6)	0.059 (4)	0.116 (6)	−0.019 (4)	0.031 (5)	−0.038 (3)
C2	0.093 (2)	0.044 (2)	0.072 (3)	−0.0035 (19)	0.022 (3)	−0.0101 (18)
C3	0.0842 (19)	0.053 (3)	0.088 (4)	0.004 (2)	0.040 (3)	−0.012 (2)
C4	0.0555 (13)	0.045 (2)	0.059 (3)	0.0029 (12)	0.0205 (19)	0.0004 (15)
C5	0.0479 (17)	0.077 (3)	0.086 (4)	0.002 (2)	0.010 (3)	−0.013 (3)
C6	0.054 (3)	0.100 (3)	0.082 (4)	−0.009 (2)	−0.010 (2)	−0.004 (3)
C7	0.0426 (17)	0.0707 (17)	0.045 (2)	0.0005 (13)	0.0080 (12)	0.0024 (18)
C8	0.0503 (19)	0.0663 (15)	0.045 (2)	0.0131 (14)	0.0091 (14)	0.0079 (18)
C9	0.0482 (17)	0.0466 (11)	0.045 (2)	0.0081 (10)	0.0124 (13)	0.0054 (15)
C10	0.071 (3)	0.0418 (14)	0.085 (4)	0.0075 (18)	0.006 (3)	0.005 (2)
C11	0.089 (3)	0.066 (3)	0.064 (3)	−0.009 (2)	0.043 (3)	0.000 (2)
C12	0.074 (2)	0.039 (2)	0.043 (2)	−0.0074 (16)	0.0224 (17)	−0.0003 (14)
C13	0.081 (3)	0.046 (2)	0.044 (2)	−0.0043 (18)	0.0141 (18)	0.0110 (15)
C14	0.0612 (19)	0.033 (2)	0.044 (2)	−0.0021 (14)	0.0061 (15)	0.0065 (13)
C15	0.061 (2)	0.051 (3)	0.078 (4)	0.0071 (19)	0.003 (2)	0.016 (2)
C16	0.067 (3)	0.080 (3)	0.0456 (19)	−0.015 (2)	0.0061 (19)	−0.002 (2)
C17	0.047 (2)	0.053 (2)	0.0399 (11)	−0.0012 (14)	0.0138 (13)	0.0033 (13)
C18	0.060 (3)	0.057 (2)	0.0459 (14)	−0.0009 (16)	0.0198 (16)	0.0114 (15)
C19	0.047 (2)	0.0426 (19)	0.0525 (16)	−0.0011 (13)	0.0213 (15)	0.0070 (14)
C20	0.071 (3)	0.055 (3)	0.076 (3)	−0.0182 (19)	0.032 (2)	0.003 (2)
N1	0.074 (3)	0.075 (3)	0.085 (4)	−0.042 (3)	0.008 (3)	0.012 (3)

Geometric parameters (Å, º) top

Cd1—N7	2.278 (4)	C6—C7	1.486 (7)
Cd1—N2	2.293 (4)	C6—H6A	0.9600
Cd1—N5	2.303 (4)	C6—H6B	0.9600
Cd1—N8	2.314 (4)	C6—H6C	0.9600
Cd1—O5	2.427 (3)	C7—C8	1.362 (7)
Cd1—O4	2.673 (3)	C8—C9	1.386 (7)
O4—N10	1.240 (5)	C8—H8A	0.9300
O5—N10	1.264 (5)	C9—C10	1.497 (7)
O6—N10	1.225 (5)	C10—H10B	0.9600
N2—C4	1.343 (6)	C10—H10C	0.9600
N2—N3	1.358 (6)	C10—H10D	0.9600
N3—C2	1.341 (8)	C11—C12	1.500 (7)
N3—H4A	0.8600	C11—H11A	0.9600
N4—C7	1.346 (6)	C11—H11B	0.9600
N4—N5	1.365 (5)	C11—H11C	0.9600
N4—H5A	0.8600	C12—C13	1.363 (8)
N5—C9	1.341 (6)	C13—C14	1.396 (7)
N6—C12	1.350 (6)	C13—H13A	0.9300
N6—N7	1.359 (6)	C14—C15	1.483 (7)
N6—H7A	0.8600	C15—H15A	0.9600
N7—C14	1.337 (6)	C15—H15B	0.9600
N8—C17	1.335 (6)	C15—H15C	0.9600
N8—N9	1.356 (5)	C16—C17	1.500 (7)
N9—C19	1.342 (6)	C16—H16A	0.9600
N9—H10A	0.8600	C16—H16B	0.9600
C1—C2	1.505 (8)	C16—H16C	0.9600
C1—H1A	0.9600	C17—C18	1.393 (7)
C1—H1B	0.9600	C18—C19	1.366 (7)
C1—H1C	0.9600	C18—H18A	0.9300
C2—C3	1.357 (9)	C19—C20	1.495 (7)
C3—C4	1.389 (7)	C20—H20A	0.9600
C3—H3A	0.9300	C20—H20B	0.9600
C4—C5	1.490 (7)	C20—H20C	0.9600
C5—H5B	0.9600	N1—O2	1.108 (10)
C5—H5C	0.9600	N1—O3	1.176 (15)
C5—H5D	0.9600	N1—O1	1.226 (8)

N7—Cd1—N2	96.81 (14)	C7—C6—H6B	109.5
N7—Cd1—N5	93.80 (14)	H6A—C6—H6B	109.5
N2—Cd1—N5	113.69 (15)	C7—C6—H6C	109.5
N7—Cd1—N8	164.83 (15)	H6A—C6—H6C	109.5
N2—Cd1—N8	89.43 (14)	H6B—C6—H6C	109.5
N5—Cd1—N8	96.33 (13)	N4—C7—C8	105.9 (4)
N7—Cd1—O5	81.49 (13)	N4—C7—C6	121.7 (5)
N2—Cd1—O5	154.81 (14)	C8—C7—C6	132.3 (5)
N5—Cd1—O5	91.50 (13)	C7—C8—C9	107.4 (4)
N8—Cd1—O5	86.98 (13)	C7—C8—H8A	126.3
N7—Cd1—O4	83.20 (13)	C9—C8—H8A	126.3
N2—Cd1—O4	105.38 (13)	N5—C9—C8	109.8 (4)
N5—Cd1—O4	140.88 (12)	N5—C9—C10	122.0 (4)
N8—Cd1—O4	81.82 (12)	C8—C9—C10	128.2 (4)
O5—Cd1—O4	49.43 (12)	C9—C10—H10B	109.5
N10—O4—Cd1	90.4 (2)	C9—C10—H10C	109.5
N10—O5—Cd1	101.7 (3)	H10B—C10—H10C	109.5
C4—N2—N3	105.2 (4)	C9—C10—H10D	109.5
C4—N2—Cd1	128.6 (3)	H10B—C10—H10D	109.5
N3—N2—Cd1	125.3 (3)	H10C—C10—H10D	109.5
C2—N3—N2	111.5 (5)	C12—C11—H11A	109.5
C2—N3—H4A	124.2	C12—C11—H11B	109.5
N2—N3—H4A	124.2	H11A—C11—H11B	109.5
C7—N4—N5	112.0 (4)	C12—C11—H11C	109.5
C7—N4—H5A	124.0	H11A—C11—H11C	109.5
N5—N4—H5A	124.0	H11B—C11—H11C	109.5
C9—N5—N4	104.9 (4)	N6—C12—C13	106.1 (4)
C9—N5—Cd1	130.1 (3)	N6—C12—C11	121.7 (5)
N4—N5—Cd1	123.7 (3)	C13—C12—C11	132.2 (5)
C12—N6—N7	111.5 (4)	C12—C13—C14	107.2 (4)
C12—N6—H7A	124.2	C12—C13—H13A	126.4
N7—N6—H7A	124.2	C14—C13—H13A	126.4
C14—N7—N6	105.9 (4)	N7—C14—C13	109.2 (4)
C14—N7—Cd1	132.7 (3)	N7—C14—C15	122.2 (5)
N6—N7—Cd1	121.3 (3)	C13—C14—C15	128.6 (5)
C17—N8—N9	105.2 (4)	C14—C15—H15A	109.5
C17—N8—Cd1	129.0 (3)	C14—C15—H15B	109.5
N9—N8—Cd1	122.8 (3)	H15A—C15—H15B	109.5
C19—N9—N8	112.3 (4)	C14—C15—H15C	109.5
C19—N9—H10A	123.9	H15A—C15—H15C	109.5
N8—N9—H10A	123.9	H15B—C15—H15C	109.5
O6—N10—O4	123.0 (4)	C17—C16—H16A	109.5
O6—N10—O5	119.2 (4)	C17—C16—H16B	109.5
O4—N10—O5	117.8 (4)	H16A—C16—H16B	109.5
C2—C1—H1A	109.5	C17—C16—H16C	109.5
C2—C1—H1B	109.5	H16A—C16—H16C	109.5
H1A—C1—H1B	109.5	H16B—C16—H16C	109.5
C2—C1—H1C	109.5	N8—C17—C18	109.8 (4)
H1A—C1—H1C	109.5	N8—C17—C16	121.7 (4)
H1B—C1—H1C	109.5	C18—C17—C16	128.5 (4)
N3—C2—C3	106.9 (5)	C19—C18—C17	106.8 (4)
N3—C2—C1	120.8 (6)	C19—C18—H18A	126.6
C3—C2—C1	132.3 (6)	C17—C18—H18A	126.6
C2—C3—C4	106.6 (5)	N9—C19—C18	105.9 (4)
C2—C3—H3A	126.7	N9—C19—C20	121.6 (5)
C4—C3—H3A	126.7	C18—C19—C20	132.5 (5)
N2—C4—C3	109.8 (5)	C19—C20—H20A	109.5
N2—C4—C5	121.6 (4)	C19—C20—H20B	109.5
C3—C4—C5	128.7 (5)	H20A—C20—H20B	109.5
C4—C5—H5B	109.5	C19—C20—H20C	109.5
C4—C5—H5C	109.5	H20A—C20—H20C	109.5
H5B—C5—H5C	109.5	H20B—C20—H20C	109.5
C4—C5—H5D	109.5	O2—N1—O3	124.1 (11)
H5B—C5—H5D	109.5	O2—N1—O1	128.2 (8)
H5C—C5—H5D	109.5	O3—N1—O1	107.6 (9)
C7—C6—H6A	109.5

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N3—H4A···O1ⁱ	0.86	2.13	2.943 (8)	157
N3—H4A···O3ⁱ	0.86	2.50	3.289 (16)	152
N4—H5A···O1ⁱ	0.86	1.92	2.771 (8)	171
N6—H7A···O6ⁱⁱ	0.86	2.33	3.131 (6)	156
N9—H10A···O4	0.86	2.50	3.106 (5)	128
C5—H5B···O4	0.96	2.59	3.530 (7)	166
C10—H10B···O5	0.96	2.29	3.157 (7)	150
C13—H13A···O1ⁱⁱⁱ	0.93	2.49	3.375 (8)	159

Symmetry codes: (i) x−1, y, z; (ii) −x, −y+2, −z+1; (iii) −x+1, −y+1, −z+1.

Experimental details

Crystal data
Chemical formula	[Cd(NO₃)(C₅H₈N₂)₄]NO₃
M_r	620.97
Crystal system, space group	Triclinic, P1
Temperature (K)	293
a, b, c (Å)	9.1790 (18), 11.353 (2), 13.669 (3)
α, β, γ (°)	94.79 (3), 105.61 (3), 90.68 (3)
V (Å³)	1366.2 (5)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	0.85
Crystal size (mm)	0.25 × 0.20 × 0.18

Data collection
Diffractometer	Bruker SMART CCD area-detector diffractometer
Absorption correction	–
No. of measured, independent and observed [I > 2σ(I)] reflections	7482, 5035, 4677
R_int	0.016
(sin θ/λ)_max (Å⁻¹)	0.606

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.047, 0.137, 1.06
No. of reflections	5035
No. of parameters	319
No. of restraints	1
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.66, −0.87

Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1997), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N3—H4A···O1ⁱ	0.86	2.13	2.943 (8)	156.6
N3—H4A···O3ⁱ	0.86	2.50	3.289 (16)	152.2
N4—H5A···O1ⁱ	0.86	1.92	2.771 (8)	171.4
N6—H7A···O6ⁱⁱ	0.86	2.33	3.131 (6)	155.7
N9—H10A···O4	0.86	2.50	3.106 (5)	128.4
C5—H5B···O4	0.96	2.59	3.530 (7)	166.1
C10—H10B···O5	0.96	2.29	3.157 (7)	149.7
C13—H13A···O1ⁱⁱⁱ	0.93	2.49	3.375 (8)	159.4

Symmetry codes: (i) x−1, y, z; (ii) −x, −y+2, −z+1; (iii) −x+1, −y+1, −z+1.

References

Addison, A. W., Rao, T. N., Reedijk, J., Vanrijn, J. & Verschoor, G. C. (1984). J. Chem. Soc. Dalton Trans. pp. 1349–1356. CSD CrossRef Web of Science Google Scholar
Bruker (1997). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Dressing, S. A., Mass, R. P. & Weiss, C. M. (1982). Bull. Environ. Contam. Toxicol. 28, 172–180. CrossRef CAS PubMed Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar

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Volume 64| Part 12| December 2008| Page m1532

doi:10.1107/S160053680803626X

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