[μ-2,2,4,4,6,6-Hexakis(3,5-dimethyl­pyrazol-1-yl)-2λ5,4λ5,6λ5-1,3,5,2,4,6-triaza­triphosphinine]bis­[bis­(nitrato- κ2O,O′)cadmium(II)]

Yun, S.Y.; Lee, S.W.

doi:10.1107/S160053680803585X

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 12| December 2008| Page m1513

doi:10.1107/S160053680803585X

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[μ-2,2,4,4,6,6-Hexakis(3,5-dimethylpyrazol-1-yl)-2λ⁵,4λ⁵,6λ⁵-1,3,5,2,4,6-triazatriphosphinine]bis[bis(nitrato- κ²O,O′)cadmium(II)]

Sung Yol Yun ^a and Soon W. Lee ^a ^*

^aDepartment of Chemistry (BK21), Sungkyunkwan University, Natural Science Campus, Suwon 440-746, South Korea
^*Correspondence e-mail: soonwlee@skku.edu

(Received 15 September 2008; accepted 1 November 2008; online 8 November 2008)

The complete title complex, [Cd₂(NO₃)₄(C₃₀H₄₂N₁₅P₃)], is generated by crystallographic twofold symmetry, with one P and one N atom of the cyclotriphosphazene ligand located on the rotation axis. The non-planar cyclotriphosphazene ring accommodates two Cd ions, and only four out of six exocylcic pyrazolyl ligands are bound to the Cd metal atoms. Each of these two symmetry-related Cd atoms is coordinated by two bidentate nitrato ligands, two exocylic pyrazolyl N atoms, and one cyclotriphosphazene N atom.

Related literature

For background, see: Allen (1991 ); Byun et al. (1996 ); Chandrasekhar & Nagendran (2001 ); Mark et al. (2005 ); Thomas et al. (1997 and references therein). For the synthesis of the ligand, see: Thomas et al. (1993 ). For related structures, see: Yun & Lee (2008 ).

Experimental

Crystal data

[Cd₂(NO₃)₄(C₃₀H₄₂N₁₅P₃)]
M_r = 1178.54
Orthorhombic, F d d 2
a = 28.2418 (5) Å
b = 36.2033 (6) Å
c = 10.3673 (2) Å
V = 10600.0 (3) Å³
Z = 8
Mo Kα radiation
μ = 0.96 mm⁻¹
T = 296 (2) K
0.30 × 0.14 × 0.10 mm

Data collection

Bruker SMART CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 1997 ) T_min = 0.851, T_max = 0.908
32426 measured reflections
6260 independent reflections
5122 reflections with I > 2σ(I)
R_int = 0.033

Refinement

R[F² > 2σ(F²)] = 0.044
wR(F²) = 0.112
S = 1.04
6260 reflections
299 parameters
1 restraint
H-atom parameters constrained
Δρ_max = 0.85 e Å⁻³
Δρ_min = −0.48 e Å⁻³
Absolute structure: Flack (1983 ), 2758 Friedel pairs
Flack parameter: −0.02 (2)

Table 1
Selected bond lengths (Å)

Cd1—N1	2.546 (3)
Cd1—N4	2.265 (3)
Cd1—N8	2.311 (4)
Cd1—O1	2.509 (5)
Cd1—O2	2.365 (6)
Cd1—O5	2.367 (8)
Cd1—O4	2.373 (9)

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

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S160053680803585X/hb2796sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S160053680803585X/hb2796Isup2.hkl

checkCIF report

Comment top

Polyphosphazenes, linear or cyclic, are an important class of inorganic macromolecules (Mark et al., 2005), and various cyclotriphosphazene derivatives are frequently used as ligands for the preparation of their intriguing coordination and organometallic complexes (Allen, 1991; Chandrasekhar & Nagendran, 2001). Particular attention has been paid to the six-membered cyclotriphosphazene N₃P₃(3,5-Me₂pz)₆ (3,5-Me₂pz = 3,5-dimethylpyrazolyl), due to its several potential donor sites such as the exocyxlic pyrazolyl nitrogen atoms and the central cyclotriphosphazene ring nitrogen and phosphorus atoms. This ligand binds to transition metals via (1) two non-geminal pyrazolyl N atoms (non-geminal N₂ coordination), (2) two non-geminal pyrazolyl N atoms and one cyclotriphosphazene ring nitrogen (non-geminal N₃ coordination), (3) two geminal pyrazolyl N atoms (geminal N₂ coordination), or (4) two geminal pyrazolyl N atoms and one ring nitrogen (geminal N₃ coordination) (Thomas et al., 1997). We recently reported the structure of a C₃-symmetric tripalladium–cyclotriphosphazene complex, in which the cyclotriphosphazene exhibits the geminal N₂ coordination mode (Yun & Lee, 2008). In this paper, we describe the preparation and structure of the title compound, (I), a dicadmium–cyclotriphosphazene complex [Cd₂(NO₃)₄(N₃P₃(3,5-Me₂pz)₆)].

The molecular structure of (I) is given in Fig. 1, which demonstrates the non-geminal N₃ coordination mode of the cyclotriphosphazene ligand. This molecule possesses a crystallographic 2-fold axis passing through the P2 and N2 atoms, which explains the Z value of 8 instead of 16. The cyclotriphosphazene ring is severely distorted from planarity with an average atomic displacement of 0.146 Å. Each Cd(II) metal is seven-coordinate and bonded to four O atoms from two nitrates, two N atoms from two imidazole rings, and one nitrogen atom from the cyclotriphosphazene ring (Table 1). Four imidazole N atoms coordinate to the two Cd metals to form four 5-membered (PdPN₃) chelate rings. The fact that the cyclotriphosphazene ring accommodates only two rather than three Cd(NO₃)₂ units may be attributed to the steric bulk of the 7-coordinate Cd metals.

The Cd—N_pyz bond lengths [2.265 (3)–2.311 (4) Å] are significantly shorter than the Cd—N_ring bond length [2.546 (3) Å], indicating that the Cd ions interact more strongly with the imidazole N atoms than with the cyclotriphosphazene ring N atoms. Consistent with our expectation, the average P—N_ring bond length [1.583 (3) Å] is considerably shorter than the average P—N_pyz bond length [1.677 (3) Å]. The Cd···Cd separation is 7.0177 (6) Å, which is shorter than the corresponding separation (7.195 Å) observed in the chloro analogue [Cd₂Cl₄(N₃P₃(3,5-Me₂pz)₆)] (Byun et al., 1996).

Related literature top

For background, see: Allen (1991); Byun et al. (1996); Chandrasekhar & Nagendran (2001); Mark et al. (2005); Thomas et al. (1997 and references therein). For the synthesis of the ligand, see: Thomas et al. (1993). For related structures, see: Yun & Lee (2008).

Experimental top

The ligand was prepared by the literature method (Thomas et al., 1993). An acetone (30 ml) solution containing Cd(NO₃)₂.4H₂O (0.144 g, 0.75 mmol) and ligand N₃P₃(3,5-Me₂pz)₆ (0.176 g, 0.25 mmol) was stirred for 24 h at room temperature. The resulting white solution was filtered off, washed with diethyl ether (6 ml x 2) and then hexane (5 ml x 2) to give a white solid, which was crystallized from acetone/hexane (1:1 v/v) to yield colorless blocks of (I). IR (KBr, cm^-1): 2964 (s), 2362 (m), 1576 (m), 1383 (s), 1260 (s), 1095 (s), 1028 (s), 805 (s). mp: 411–413 K.

Computing details top

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

Figures top

Fig. 1. The molecular structure of (I) showing 50% probability displacement ellipsoids. H atoms are omitted for clarity. Atoms with the suffix A are generated by the symmetry operation (–x, –y, z).

[µ-2,2,4,4,6,6-Hexakis(3,5-dimethylpyrazol-1-yl)-2λ⁵,4λ⁵,6λ⁵- 1,3,5,2,4,6-triazatriphosphinine]bis[bis(nitrato- κ²O,O')cadmium(II)] top

Crystal data top

[Cd₂(NO₃)₄(C₃₀H₄₂N₁₅P₃)]	F(000) = 4736
M_r = 1178.54	D_x = 1.477 Mg m⁻³
Orthorhombic, Fdd2	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: F 2 -2d	Cell parameters from 9939 reflections
a = 28.2418 (5) Å	θ = 2.2–25.5°
b = 36.2033 (6) Å	µ = 0.96 mm⁻¹
c = 10.3673 (2) Å	T = 296 K
V = 10600.0 (3) Å³	BLOCK, colourless
Z = 8	0.30 × 0.14 × 0.10 mm

Data collection top

Bruker SMART CCD diffractometer	6260 independent reflections
Radiation source: sealed tube	5122 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.033
ω scans	θ_max = 28.4°, θ_min = 2.2°
Absorption correction: multi-scan (SADABS; Bruker, 1997)	h = −36→28
T_min = 0.851, T_max = 0.908	k = −48→40
32426 measured reflections	l = −13→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)] = 0.044	H-atom parameters constrained
wR(F²) = 0.112	w = 1/[σ²(F_o²) + (0.0676P)² + 6.1853P] where P = (F_o² + 2F_c²)/3
S = 1.04	(Δ/σ)_max = 0.001
6260 reflections	Δρ_max = 0.85 e Å⁻³
299 parameters	Δρ_min = −0.48 e Å⁻³
1 restraint	Absolute structure: Flack (1983), 2758 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.02 (2)

Crystal data top

[Cd₂(NO₃)₄(C₃₀H₄₂N₁₅P₃)]	V = 10600.0 (3) Å³
M_r = 1178.54	Z = 8
Orthorhombic, Fdd2	Mo Kα radiation
a = 28.2418 (5) Å	µ = 0.96 mm⁻¹
b = 36.2033 (6) Å	T = 296 K
c = 10.3673 (2) Å	0.30 × 0.14 × 0.10 mm

Data collection top

Bruker SMART CCD diffractometer	6260 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 1997)	5122 reflections with I > 2σ(I)
T_min = 0.851, T_max = 0.908	R_int = 0.033
32426 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.044	H-atom parameters constrained
wR(F²) = 0.112	Δρ_max = 0.85 e Å⁻³
S = 1.04	Δρ_min = −0.48 e Å⁻³
6260 reflections	Absolute structure: Flack (1983), 2758 Friedel pairs
299 parameters	Absolute structure parameter: −0.02 (2)
1 restraint

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	−0.083094 (12)	−0.072056 (9)	0.52427 (3)	0.05498 (12)
P1	−0.04843 (3)	−0.00189 (2)	0.74616 (9)	0.0339 (2)
P2	0.0000	0.0000	0.51827 (12)	0.0311 (2)
O1	−0.0099 (2)	−0.0965 (2)	0.6318 (6)	0.1100 (19)
O2	−0.0638 (3)	−0.13446 (15)	0.5667 (8)	0.144 (3)
O3	−0.0064 (4)	−0.1554 (3)	0.6716 (11)	0.251 (7)
O4	−0.1372 (4)	−0.0530 (3)	0.3622 (15)	0.258 (8)
O5	−0.1455 (4)	−0.1014 (3)	0.4113 (10)	0.195 (5)
O6	−0.1902 (3)	−0.0824 (2)	0.2697 (10)	0.170 (4)
N1	−0.04555 (11)	−0.01150 (8)	0.5958 (3)	0.0357 (7)
N2	0.0000	0.0000	0.8214 (4)	0.0408 (10)
N3	−0.08391 (12)	−0.03495 (9)	0.8082 (3)	0.0429 (8)
N4	−0.10447 (12)	−0.06131 (10)	0.7314 (3)	0.0450 (8)
N5	−0.07821 (10)	0.03652 (9)	0.7738 (4)	0.0431 (7)
N6	−0.12225 (13)	0.03751 (11)	0.7149 (4)	0.0512 (9)
N7	0.01317 (12)	−0.03608 (9)	0.4208 (3)	0.0398 (7)
N8	−0.02456 (14)	−0.05705 (10)	0.3775 (4)	0.0490 (8)
N9	−0.0244 (3)	−0.1266 (3)	0.6295 (8)	0.114 (2)
N10	−0.1568 (2)	−0.07751 (19)	0.3548 (8)	0.0857 (18)
C1	−0.10083 (18)	−0.03802 (13)	0.9323 (4)	0.0536 (11)
C2	−0.1308 (2)	−0.06616 (15)	0.9360 (5)	0.0703 (15)
H2	−0.1472	−0.0748	1.0078	0.084*
C3	−0.13292 (19)	−0.08072 (14)	0.8077 (5)	0.0593 (12)
C4	−0.0847 (3)	−0.01309 (18)	1.0404 (5)	0.0837 (18)
H4A	−0.0628	0.0048	1.0073	0.126*
H4B	−0.0695	−0.0276	1.1059	0.126*
H4C	−0.1116	−0.0007	1.0768	0.126*
C5	−0.1598 (2)	−0.11282 (18)	0.7556 (7)	0.0834 (18)
H5A	−0.1533	−0.1154	0.6652	0.125*
H5B	−0.1931	−0.1088	0.7681	0.125*
H5C	−0.1504	−0.1349	0.8001	0.125*
C6	−0.07031 (19)	0.06865 (11)	0.8451 (4)	0.0486 (10)
C7	−0.11000 (19)	0.08900 (14)	0.8317 (5)	0.0606 (12)
H7	−0.1160	0.1119	0.8692	0.073*
C8	−0.14106 (18)	0.06886 (13)	0.7490 (5)	0.0607 (12)
C9	−0.02660 (19)	0.07712 (13)	0.9190 (5)	0.0615 (13)
H9A	−0.0046	0.0571	0.9103	0.092*
H9B	−0.0344	0.0804	1.0084	0.092*
H9C	−0.0126	0.0994	0.8862	0.092*
C10	−0.1886 (3)	0.0808 (2)	0.7004 (8)	0.097 (2)
H10A	−0.2016	0.0618	0.6464	0.146*
H10B	−0.1853	0.1031	0.6515	0.146*
H10C	−0.2094	0.0850	0.7722	0.146*
C11	0.05422 (16)	−0.04550 (12)	0.3580 (4)	0.0465 (10)
C12	0.0421 (2)	−0.07391 (11)	0.2775 (5)	0.0578 (12)
H12	0.0625	−0.0868	0.2233	0.069*
C13	−0.0061 (2)	−0.07985 (12)	0.2915 (4)	0.0569 (12)
C14	0.10103 (19)	−0.02914 (17)	0.3787 (5)	0.0659 (14)
H14A	0.0987	−0.0098	0.4416	0.099*
H14B	0.1126	−0.0191	0.2989	0.099*
H14C	0.1225	−0.0478	0.4091	0.099*
C15	−0.0358 (3)	−0.10831 (18)	0.2264 (6)	0.092 (2)
H15A	−0.0680	−0.1059	0.2546	0.138*
H15B	−0.0242	−0.1325	0.2481	0.138*
H15C	−0.0342	−0.1049	0.1347	0.138*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.0606 (2)	0.05662 (19)	0.04776 (17)	−0.02047 (15)	0.00994 (15)	−0.01297 (14)
P1	0.0381 (5)	0.0323 (4)	0.0314 (4)	0.0014 (4)	0.0036 (4)	−0.0026 (3)
P2	0.0365 (6)	0.0296 (5)	0.0272 (5)	0.0004 (5)	0.000	0.000
O1	0.095 (4)	0.137 (5)	0.098 (4)	0.043 (4)	0.016 (3)	0.033 (4)
O2	0.189 (6)	0.068 (3)	0.176 (8)	−0.022 (4)	0.092 (6)	−0.016 (4)
O3	0.258 (10)	0.203 (8)	0.292 (12)	0.150 (8)	0.168 (9)	0.191 (9)
O4	0.165 (7)	0.185 (8)	0.422 (19)	−0.087 (7)	−0.175 (11)	0.126 (11)
O5	0.226 (9)	0.213 (10)	0.146 (7)	−0.137 (9)	−0.036 (7)	−0.002 (7)
O6	0.143 (6)	0.135 (5)	0.231 (9)	−0.028 (4)	−0.085 (7)	−0.035 (6)
N1	0.0366 (16)	0.0361 (15)	0.0343 (15)	−0.0021 (13)	0.0017 (12)	−0.0047 (12)
N2	0.046 (3)	0.045 (2)	0.031 (2)	0.000 (2)	0.000	0.000
N3	0.0471 (19)	0.0413 (18)	0.0403 (18)	−0.0063 (14)	0.0082 (14)	−0.0033 (14)
N4	0.0414 (18)	0.0480 (18)	0.0455 (18)	−0.0091 (16)	0.0084 (15)	−0.0042 (15)
N5	0.0419 (16)	0.0422 (16)	0.0452 (17)	0.0065 (13)	−0.0021 (16)	−0.0110 (15)
N6	0.0417 (19)	0.057 (2)	0.055 (2)	0.0120 (16)	−0.0053 (16)	−0.0146 (17)
N7	0.0434 (18)	0.0391 (17)	0.0368 (15)	0.0047 (14)	0.0064 (14)	−0.0042 (13)
N8	0.063 (2)	0.0416 (18)	0.0430 (18)	−0.0095 (17)	0.0077 (16)	−0.0141 (15)
N9	0.114 (6)	0.130 (7)	0.098 (5)	0.027 (6)	0.063 (4)	0.026 (5)
N10	0.072 (3)	0.069 (4)	0.116 (5)	−0.033 (3)	0.000 (3)	−0.008 (3)
C1	0.065 (3)	0.051 (2)	0.045 (2)	−0.009 (2)	0.017 (2)	−0.0054 (19)
C2	0.084 (4)	0.069 (3)	0.058 (3)	−0.013 (3)	0.033 (3)	0.006 (2)
C3	0.060 (3)	0.059 (3)	0.059 (3)	−0.018 (2)	0.016 (2)	0.002 (2)
C4	0.126 (5)	0.085 (4)	0.040 (3)	−0.028 (4)	0.021 (3)	−0.013 (3)
C5	0.084 (4)	0.087 (4)	0.080 (4)	−0.042 (3)	0.016 (3)	−0.003 (3)
C6	0.065 (3)	0.039 (2)	0.042 (2)	0.0061 (19)	0.002 (2)	−0.0057 (16)
C7	0.064 (3)	0.048 (3)	0.070 (3)	0.016 (2)	−0.008 (2)	−0.019 (2)
C8	0.059 (3)	0.065 (3)	0.058 (3)	0.026 (2)	0.003 (2)	−0.013 (2)
C9	0.067 (3)	0.051 (3)	0.066 (3)	−0.001 (2)	−0.004 (3)	−0.025 (2)
C10	0.078 (4)	0.099 (5)	0.114 (5)	0.039 (4)	−0.023 (4)	−0.028 (4)
C11	0.055 (3)	0.048 (2)	0.0358 (19)	0.0123 (19)	0.0070 (18)	0.0062 (17)
C12	0.079 (3)	0.053 (2)	0.042 (2)	0.013 (2)	0.012 (2)	−0.008 (2)
C13	0.086 (3)	0.044 (2)	0.040 (2)	−0.005 (2)	0.016 (2)	−0.0110 (19)
C14	0.049 (3)	0.097 (4)	0.052 (3)	0.013 (3)	0.010 (2)	−0.007 (3)
C15	0.136 (6)	0.072 (3)	0.069 (3)	−0.034 (4)	0.019 (4)	−0.036 (3)

Geometric parameters (Å, º) top

Cd1—N1	2.546 (3)	C1—C4	1.509 (7)
Cd1—N4	2.265 (3)	C2—C3	1.432 (8)
Cd1—N8	2.311 (4)	C2—H2	0.9300
Cd1—O1	2.509 (5)	C3—C5	1.490 (8)
Cd1—O2	2.365 (6)	C4—H4A	0.9600
Cd1—O5	2.367 (8)	C4—H4B	0.9600
Cd1—O4	2.373 (9)	C4—H4C	0.9600
P1—N2	1.576 (2)	C5—H5A	0.9600
P1—N1	1.599 (3)	C5—H5B	0.9600
P1—N5	1.650 (3)	C5—H5C	0.9600
P1—N3	1.688 (3)	C6—C7	1.349 (7)
P2—N1	1.573 (3)	C6—C9	1.485 (7)
P2—N1ⁱ	1.573 (3)	C7—C8	1.427 (7)
P2—N7ⁱ	1.693 (3)	C7—H7	0.9300
P2—N7	1.693 (3)	C8—C10	1.498 (8)
O1—N9	1.165 (11)	C9—H9A	0.9600
O2—N9	1.323 (11)	C9—H9B	0.9600
O3—N9	1.239 (10)	C9—H9C	0.9600
O4—N10	1.049 (9)	C10—H10A	0.9600
O5—N10	1.094 (12)	C10—H10B	0.9600
O6—N10	1.302 (10)	C10—H10C	0.9600
N2—P1ⁱ	1.576 (2)	C11—C12	1.368 (6)
N3—N4	1.372 (5)	C11—C14	1.464 (8)
N3—C1	1.376 (6)	C12—C13	1.386 (8)
N4—C3	1.328 (6)	C12—H12	0.9300
N5—N6	1.386 (5)	C13—C15	1.489 (7)
N5—C6	1.396 (5)	C14—H14A	0.9600
N6—C8	1.302 (5)	C14—H14B	0.9600
N7—C11	1.373 (5)	C14—H14C	0.9600
N7—N8	1.383 (5)	C15—H15A	0.9600
N8—C13	1.323 (6)	C15—H15B	0.9600
C1—C2	1.325 (7)	C15—H15C	0.9600

N4—Cd1—N8	140.76 (12)	C2—C1—N3	108.1 (4)
N4—Cd1—O2	92.8 (2)	C2—C1—C4	129.1 (5)
N8—Cd1—O2	100.51 (19)	N3—C1—C4	122.7 (4)
N4—Cd1—O5	110.4 (3)	C1—C2—C3	106.4 (4)
N8—Cd1—O5	108.2 (3)	C1—C2—H2	126.8
O2—Cd1—O5	80.4 (5)	C3—C2—H2	126.8
N4—Cd1—O4	116.7 (4)	N4—C3—C2	109.5 (4)
N8—Cd1—O4	85.8 (4)	N4—C3—C5	120.3 (5)
O2—Cd1—O4	123.8 (4)	C2—C3—C5	130.2 (5)
O5—Cd1—O4	45.7 (4)	C1—C4—H4A	109.5
N4—Cd1—O1	81.87 (16)	C1—C4—H4B	109.5
N8—Cd1—O1	77.65 (18)	H4A—C4—H4B	109.5
O2—Cd1—O1	52.5 (3)	C1—C4—H4C	109.5
O5—Cd1—O1	132.4 (4)	H4A—C4—H4C	109.5
O4—Cd1—O1	161.3 (4)	H4B—C4—H4C	109.5
N4—Cd1—N1	71.75 (11)	C3—C5—H5A	109.5
N8—Cd1—N1	72.03 (11)	C3—C5—H5B	109.5
O2—Cd1—N1	132.3 (3)	H5A—C5—H5B	109.5
O5—Cd1—N1	147.2 (4)	C3—C5—H5C	109.5
O4—Cd1—N1	103.0 (3)	H5A—C5—H5C	109.5
O1—Cd1—N1	80.3 (2)	H5B—C5—H5C	109.5
N2—P1—N1	116.61 (18)	C7—C6—N5	105.6 (4)
N2—P1—N5	108.63 (13)	C7—C6—C9	129.1 (4)
N1—P1—N5	112.25 (18)	N5—C6—C9	125.3 (4)
N2—P1—N3	110.93 (16)	C6—C7—C8	107.1 (4)
N1—P1—N3	104.34 (17)	C6—C7—H7	126.5
N5—P1—N3	103.21 (17)	C8—C7—H7	126.5
N1—P2—N1ⁱ	118.5 (2)	N6—C8—C7	111.0 (4)
N1—P2—N7ⁱ	109.24 (16)	N6—C8—C10	121.7 (5)
N1ⁱ—P2—N7ⁱ	106.30 (16)	C7—C8—C10	127.3 (4)
N1—P2—N7	106.30 (16)	C6—C9—H9A	109.5
N1ⁱ—P2—N7	109.24 (16)	C6—C9—H9B	109.5
N7ⁱ—P2—N7	106.7 (2)	H9A—C9—H9B	109.5
N9—O1—Cd1	91.9 (6)	C6—C9—H9C	109.5
N9—O2—Cd1	94.6 (5)	H9A—C9—H9C	109.5
N10—O4—Cd1	98.5 (7)	H9B—C9—H9C	109.5
N10—O5—Cd1	97.3 (6)	C8—C10—H10A	109.5
P2—N1—P1	118.8 (2)	C8—C10—H10B	109.5
P2—N1—Cd1	114.81 (15)	H10A—C10—H10B	109.5
P1—N1—Cd1	116.75 (16)	C8—C10—H10C	109.5
P1—N2—P1ⁱ	120.7 (3)	H10A—C10—H10C	109.5
N4—N3—C1	109.8 (3)	H10B—C10—H10C	109.5
N4—N3—P1	121.5 (3)	C12—C11—N7	105.4 (4)
C1—N3—P1	128.3 (3)	C12—C11—C14	128.2 (4)
C3—N4—N3	106.2 (4)	N7—C11—C14	126.3 (4)
C3—N4—Cd1	129.4 (3)	C11—C12—C13	107.3 (4)
N3—N4—Cd1	123.9 (2)	C11—C12—H12	126.3
N6—N5—C6	110.8 (3)	C13—C12—H12	126.3
N6—N5—P1	113.7 (3)	N8—C13—C12	111.2 (4)
C6—N5—P1	135.5 (3)	N8—C13—C15	121.0 (5)
C8—N6—N5	105.6 (4)	C12—C13—C15	127.8 (5)
C11—N7—N8	111.1 (3)	C11—C14—H14A	109.5
C11—N7—P2	131.3 (3)	C11—C14—H14B	109.5
N8—N7—P2	116.6 (2)	H14A—C14—H14B	109.5
C13—N8—N7	104.9 (4)	C11—C14—H14C	109.5
C13—N8—Cd1	125.4 (3)	H14A—C14—H14C	109.5
N7—N8—Cd1	117.8 (2)	H14B—C14—H14C	109.5
O1—N9—O3	129.7 (12)	C13—C15—H15A	109.5
O1—N9—O2	120.5 (9)	C13—C15—H15B	109.5
O3—N9—O2	109.7 (12)	H15A—C15—H15B	109.5
O4—N10—O5	118.3 (10)	C13—C15—H15C	109.5
O4—N10—O6	123.1 (10)	H15A—C15—H15C	109.5
O5—N10—O6	117.9 (8)	H15B—C15—H15C	109.5

Symmetry code: (i) −x, −y, z.

Experimental details

Crystal data
Chemical formula	[Cd₂(NO₃)₄(C₃₀H₄₂N₁₅P₃)]
M_r	1178.54
Crystal system, space group	Orthorhombic, Fdd2
Temperature (K)	296
a, b, c (Å)	28.2418 (5), 36.2033 (6), 10.3673 (2)
V (Å³)	10600.0 (3)
Z	8
Radiation type	Mo Kα
µ (mm⁻¹)	0.96
Crystal size (mm)	0.30 × 0.14 × 0.10

Data collection
Diffractometer	Bruker SMART CCD diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 1997)
T_min, T_max	0.851, 0.908
No. of measured, independent and observed [I > 2σ(I)] reflections	32426, 6260, 5122
R_int	0.033
(sin θ/λ)_max (Å⁻¹)	0.669

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.044, 0.112, 1.04
No. of reflections	6260
No. of parameters	299
No. of restraints	1
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.85, −0.48
Absolute structure	Flack (1983), 2758 Friedel pairs
Absolute structure parameter	−0.02 (2)

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

Selected bond lengths (Å) top

Cd1—N1	2.546 (3)	Cd1—O2	2.365 (6)
Cd1—N4	2.265 (3)	Cd1—O5	2.367 (8)
Cd1—N8	2.311 (4)	Cd1—O4	2.373 (9)
Cd1—O1	2.509 (5)

Acknowledgements

This paper was supported by Samsung Research Fund, Sungkyumkwan University, 2008.

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