The one-dimensional coordination polymer poly[tetra­kis­[(4-chloro­phen­yl)methanaminium] [cadmate-μ-cyclo­hexa­phospho­rato]]

Abid, S.; Al-Deyab, S.S.; Rzaigui, M.

doi:10.1107/S160053681104133X

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 67| Part 11| November 2011| Pages m1549-m1550

doi:10.1107/S160053681104133X

Open

access

The one-dimensional coordination polymer poly[tetrakis[(4-chlorophenyl)methanaminium] [cadmate-μ-cyclohexaphosphorato]]

Sonia Abid,^a ^* S. Salem Al-Deyab ^b and Mohamed Rzaigui ^a

^aLaboratoire de Chimie des Matériaux, Faculté des Sciences de Bizerte, 7021 Zarzouna Bizerte, Tunisia, and ^bPetrochemical Research Chair, College of Science, King Saud University, Riyadh, Saudi Arabia
^*Correspondence e-mail: sonia.abid@fsb.rnu.tn

(Received 20 September 2011; accepted 7 October 2011; online 22 October 2011)

Cyclohexaphosphoric acid (P₆O₁₈H₆) reacts with cadmium carbonate and 4-chlorobenzylamine (CBA) to give the mononuclear title complex, (C₇H₉ClN)₄[Cd(P₆O₁₈)]_n, in which the Cd^II atom, lying on an inversion centre, has an octahedral coordination built of six O atoms of two centrosymmetric P₆O₁₈ rings. Each P₆O₁₈ ligand acts as a bridge, linking two Cd^II atoms and forming an anionic coordination polymer [Cd(P₆O₁₈)⁴⁻]_n extending along [010]. Adjacent polymeric chains are connected through N—H⋯O and C—H⋯O hydrogen bonds, generating a three-dimensional supramolecular network.

Related literature

For the crystal chemistry of condensed phosphates, see: Averbuch-Pouchot & Durif (1996 ); Durif (2005 ). For general background to supramolecular complexes, see: Kolotuchin et al. (1995 ); Tong et al. (1999 ). For Cl⋯Cl interactions, see: Hathwar et al. (2010 ) and for π–π interactions, see: Janiak et al. (2000 ). For the synthesis, see: Schülke & Kayser (1985 ). For related structures, see: Du et al. (2010 ); Hu et al. (2008 ); Kontturi et al. (2005 ); Man et al. (2006 ).

Experimental

Crystal data

(C₇H₉ClN)₄[Cd(P₆O₁₈)]
M_r = 1156.63
Triclinic, $[P \overline 1]$
a = 8.021 (4) Å
b = 8.1696 (16) Å
c = 17.919 (3) Å
α = 87.31 (5)°
β = 88.914 (19)°
γ = 70.100 (3)°
V = 1102.9 (6) Å³
Z = 1
Mo Kα radiation
μ = 1.03 mm⁻¹
T = 293 K
0.22 × 0.20 × 0.18 mm

Data collection

Enraf–Nonius TurboCAD-4 diffractometer
3873 measured reflections
3770 independent reflections
3506 reflections with I > 2σ(I)
R_int = 0.009
2 standard reflections every 120 min intensity decay: 1%

Refinement

R[F² > 2σ(F²)] = 0.027
wR(F²) = 0.074
S = 1.14
3770 reflections
277 parameters
H-atom parameters constrained
Δρ_max = 0.76 e Å⁻³
Δρ_min = −0.57 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯O1	0.89	1.91	2.785 (3)	167
N1—H1B⋯O6ⁱ	0.89	1.88	2.740 (3)	162
N1—H1C⋯O9ⁱⁱ	0.89	1.93	2.809 (4)	168
N2—H2A⋯O2	0.89	1.96	2.814 (4)	160
N2—H2B⋯O5ⁱⁱ	0.89	2.19	2.866 (3)	133
N2—H2C⋯O1ⁱⁱⁱ	0.89	1.95	2.824 (3)	169
C3—H3⋯O1^iv	0.93	2.56	3.339 (5)	142
C13—H13⋯O6ⁱⁱ	0.93	2.53	3.394 (4)	154
C14—H14B⋯O3^v	0.97	2.56	3.410 (4)	147
Symmetry codes: (i) x+1, y, z; (ii) -x+1, -y+1, -z+1; (iii) -x+2, -y, -z+1; (iv) x, y+1, z; (v) -x+1, -y, -z+1.

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994 ); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995 ); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997 ); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S160053681104133X/ff2028sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S160053681104133X/ff2028Isup2.hkl

checkCIF report

Comment top

The key to successful construction of supramolecular architecture is the control and manipulation of coordination bonds an non-covalent interactions by carefully selecting the coordination geometry of the metal atoms and the organic ligands containing appropriate functional groups (such as polyphosphoric acid and polyamine) (Kolotuchin et al., 1995). Up to now, a large number of supramolecular complexes with various dimensions and topologies have been achieved through judicious choice of linkers and metal ions (Tong et al., 1999). The approach to supramolecular framework employed in this work is to use the hexafunctional linker P₆O₁₈^6- that is of strong coordinating ability and suitable hydrogen bond acceptor. The 4-chlorobenzylamine (CBA) is used to create possibly π-π packing interactions between the aromatic rings and Cl—Cl interactions, which could facilitate the formation of ordered and non-interpenetrated open frameworks. In this contribution, we report the self-assembly of Cd^II with P₆O₁₈^6- in the presence of template (CBA) into a supramolecular open framework material [Cd(P₆O₁₈^6-)]_n.4n(CABH) (Scheme I). Single-crystal X-ray diffraction study of this compound shows that the asymmetric unit contains half of cadmium atom, half of a cycle P₆O₁₈ and two crystallographically independent 4-chlorobenzylammonium (CBAH) cations (Fig. 1). The Cd atom locates on an inversion centre and is coordinated by six O atoms. The CdO₆ octahedron, sharing six vertex oxygen atoms with two adjacent P₆O₁₈ rings, is slightly distorted compared to other cases (Du et al., 2010; Kontturi et al., 2005; Man et al., 2006; Hu et al., 2008). Bond distances Cd—O range from 2.230 (2) to 2.353 (7)Å and angles O—Cd—O range from 83.53 (8) to 88.19 (7) °. The P₆O₁₈ units display average P–O distances of 1.540 A and P–P distances of 2.967 Å, values usually found in other condensed anions (Averbuch-Pouchot & Durif, 1996). The values of the P—P—P angles, varying from 87.13 (1) to 128.55 (1)°, are in the range of values observed with other cyclohexaphosphates (Durif, 2005). As shown in Fig. 2, the Cd^II atoms are bridged by P₆O₁₈ rings to form infinite 1-D coordination polymers [Cd(P₆O₁₈)]n parallel to the b axis. Fig. 3 shows the supramolecular open framework structure built of the infinite zigzag chains linked by hydrogen bonds of types N(C)—H···O ranging from 2.714 (3) to 3.410 (4) Å, established by the protonated amine (CBAH). The phenyl rings of these organic molecules are planar, with a mean plane deviation of 0.0043 Å and are parallel with a dihedral angle of 4.94°. The orientations of the –CH₂—NH₃⁺ substituent in the two cations (CBAH) are distinct, as seen from the following torsion angles: N1—C7—C1—C2 = 13.1 (3) and N2—C14—C8—C9 = 118.3 (17)°. The supramolecular framework structure is further stabilized by electrostatic strengths, Cl–Cl interactions [4.051 Å] (Hathwar et al., 2010). The inter-planar distance between nearby phenyl rings is in the vicinity of 4.165 Å, which is longer than 3.80 Å, value required for the formation of π–π interactions (Janiak et al., 2000).

Related literature top

For the crystal chemistry of condensed phosphates, see: Averbuch-Pouchot & Durif (1996); Durif (2005). For general supramolecular complexes, see: Kolotuchin et al. (1995); Tong et al. (1999). For Cl···Cl interactions, see: Hathwar et al. (2010) and for π–π interactions, see: Janiak et al. (2000). For the synthesis, see: Schülke & Kayser (1985). For related structures, see: Du et al. (2010); Hu et al. (2008); Kontturi et al. (2005); Man et al. (2006).

Experimental top

The chemicals used to prepare the title compounds include CdCO₃, 4-chlorobenzylamine (CBA) and H₆P₆O₁₈. Both first reagents were commercially available (Accros), the third one was produced from Li₆P₆O₁₈.6H₂O, which is prepared by the process of Schülke (Schülke & Kayser, 1985) and protonated with an ion-exchange resin (Amberlite IR 120) in its H-state. An aqueous solution of H₆P₆O₁₈ (5 mmol, 15 ml) was added dropwise to a stirred mixture of CdCO₃ (0.86 g, 5 mmol), 4-chlorobenzylamine (2.45 ml, 20 mmol)and C₂H₅OH (50 ml). The obtained solution was allowed to stand in air at room temperature until formation of single crystals of the title complex.

Computing details top

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994); cell refinement: CAD-4 EXPRESS (Enraf–Nonius, 1994); data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999).

Figures top

	Fig. 1. ORTEP-3 (Farrugia,(1999)) view of (I) with atom numbering scheme. Displacement ellipsoids for non-H atoms are drawn at the 30% probability level.
	Fig. 2. Perspective view showing the 1-D coordination polymers [Cd(P₆O₁₈)^4-]_n developed along the b axis.
	Fig. 3. Perspective view of [Cd(P₆O₁₈)].4(CBAH) showing the the supramolecular open framework structure.

poly[tetrakis[(4-chlorophenyl)methanaminium] [cadmate-µ-cyclohexaphosphorato]] top

Crystal data top

(C₇H₉ClN)₄[Cd(P₆O₁₈)]	Z = 1
M_r = 1156.63	F(000) = 582
Triclinic, P1	D_x = 1.741 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.021 (4) Å	Cell parameters from 25 reflections
b = 8.1696 (16) Å	θ = 9.1–10.8°
c = 17.919 (3) Å	µ = 1.03 mm⁻¹
α = 87.31 (5)°	T = 293 K
β = 88.914 (19)°	Prism, colourless
γ = 70.100 (3)°	0.22 × 0.20 × 0.18 mm
V = 1102.9 (6) Å³

Data collection top

Enraf–Nonius TurboCAD-4 diffractometer	R_int = 0.009
Radiation source: Enraf Nonius FR590	θ_max = 28.0°, θ_min = 2.3°
Graphite monochromator	h = −9→10
non–profiled ω scans	k = 0→10
3873 measured reflections	l = −5→23
3770 independent reflections	2 standard reflections every 120 min
3506 reflections with I > 2σ(I)	intensity decay: 1%

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)] = 0.027	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.074	H-atom parameters constrained
S = 1.14	w = 1/[σ²(F_o²) + (0.0373P)² + 0.863P] where P = (F_o² + 2F_c²)/3
3770 reflections	(Δ/σ)_max = 0.022
277 parameters	Δρ_max = 0.76 e Å⁻³
0 restraints	Δρ_min = −0.57 e Å⁻³

Crystal data top

(C₇H₉ClN)₄[Cd(P₆O₁₈)]	γ = 70.100 (3)°
M_r = 1156.63	V = 1102.9 (6) Å³
Triclinic, P1	Z = 1
a = 8.021 (4) Å	Mo Kα radiation
b = 8.1696 (16) Å	µ = 1.03 mm⁻¹
c = 17.919 (3) Å	T = 293 K
α = 87.31 (5)°	0.22 × 0.20 × 0.18 mm
β = 88.914 (19)°

Data collection top

Enraf–Nonius TurboCAD-4 diffractometer	R_int = 0.009
3873 measured reflections	2 standard reflections every 120 min
3770 independent reflections	intensity decay: 1%
3506 reflections with I > 2σ(I)

Refinement top

R[F² > 2σ(F²)] = 0.027	0 restraints
wR(F²) = 0.074	H-atom parameters constrained
S = 1.14	Δρ_max = 0.76 e Å⁻³
3770 reflections	Δρ_min = −0.57 e Å⁻³
277 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
P1	0.67291 (7)	0.07788 (7)	0.58321 (4)	0.02160 (17)
P2	0.31753 (7)	0.30435 (7)	0.62408 (4)	0.02213 (17)
P3	0.21259 (7)	0.28764 (8)	0.46566 (4)	0.02360 (18)
O1	0.8257 (2)	0.0489 (2)	0.63383 (12)	0.0306 (5)
O2	0.6552 (2)	0.1994 (2)	0.51710 (12)	0.0278 (5)
O3	0.4957 (2)	0.1402 (2)	0.63318 (13)	0.0332 (5)
O4	0.6588 (2)	−0.1001 (2)	0.55819 (13)	0.0321 (6)
O5	0.3676 (2)	0.4624 (2)	0.60678 (11)	0.0265 (5)
O6	0.2085 (2)	0.3003 (2)	0.69060 (12)	0.0316 (5)
O7	0.2237 (3)	0.2579 (3)	0.55466 (12)	0.0354 (6)
O8	0.0311 (2)	0.3219 (2)	0.44049 (13)	0.0390 (6)
O9	0.3052 (2)	0.4116 (2)	0.43979 (12)	0.0295 (5)
Cd	0.5000	0.5000	0.5000	0.02314 (9)
N1	0.8521 (3)	0.3592 (3)	0.68090 (16)	0.0336 (6)
H1A	0.8605	0.2565	0.6633	0.050*
H1B	0.9603	0.3617	0.6892	0.050*
H1C	0.7969	0.4438	0.6476	0.050*
C1	0.7286 (4)	0.5549 (4)	0.7877 (2)	0.0373 (9)
C2	0.7656 (4)	0.6922 (4)	0.7522 (2)	0.0452 (10)
H2	0.8130	0.6803	0.7042	0.054*
C3	0.7325 (5)	0.8486 (5)	0.7875 (2)	0.0500 (10)
H3	0.7541	0.9424	0.7631	0.060*
C4	0.6673 (5)	0.8608 (5)	0.8592 (2)	0.0564 (12)
C5	0.6306 (6)	0.7272 (6)	0.8958 (3)	0.0661 (13)
H5	0.5852	0.7391	0.9442	0.079*
C6	0.6619 (5)	0.5735 (5)	0.8598 (2)	0.0522 (11)
H6	0.6377	0.4813	0.8844	0.063*
C7	0.7503 (5)	0.3849 (4)	0.7516 (2)	0.0502 (11)
H7A	0.8092	0.2893	0.7867	0.060*
H7B	0.6336	0.3799	0.7420	0.060*
Cl1	0.6261 (2)	1.05722 (18)	0.90321 (8)	0.1103 (6)
N2	0.8179 (3)	0.1736 (3)	0.37553 (14)	0.0286 (6)
H2A	0.7756	0.1534	0.4200	0.043*
H2B	0.8255	0.2800	0.3734	0.043*
H2C	0.9251	0.0952	0.3689	0.043*
C8	0.7590 (4)	0.1923 (4)	0.24011 (19)	0.0358 (8)
C9	0.8004 (5)	0.0633 (5)	0.1879 (2)	0.0564 (12)
H9	0.7943	−0.0456	0.2019	0.068*
C10	0.8495 (7)	0.0933 (6)	0.1169 (3)	0.0694 (15)
H10	0.8750	0.0059	0.0826	0.083*
C11	0.8614 (6)	0.2538 (6)	0.0958 (2)	0.0589 (12)
C12	0.8237 (5)	0.3838 (5)	0.1459 (2)	0.0558 (11)
H12	0.8325	0.4915	0.1317	0.067*
C13	0.7730 (4)	0.3532 (4)	0.2169 (2)	0.0453 (10)
H13	0.7472	0.4416	0.2507	0.054*
C14	0.6978 (4)	0.1610 (4)	0.3163 (2)	0.0401 (9)
H14A	0.5808	0.2454	0.3244	0.048*
H14B	0.6877	0.0460	0.3198	0.048*
Cl2	0.9233 (3)	0.2940 (2)	0.00535 (8)	0.1069 (6)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
P1	0.0171 (2)	0.0128 (2)	0.0337 (4)	−0.0031 (2)	0.0003 (3)	−0.0040 (3)
P2	0.0190 (2)	0.0152 (3)	0.0315 (4)	−0.0047 (2)	0.0032 (3)	−0.0051 (3)
P3	0.0204 (2)	0.0144 (3)	0.0364 (4)	−0.0057 (2)	−0.0049 (3)	−0.0045 (4)
O1	0.0246 (8)	0.0235 (8)	0.0421 (13)	−0.0050 (7)	−0.0056 (8)	−0.0079 (10)
O2	0.0262 (8)	0.0182 (8)	0.0356 (13)	−0.0035 (6)	0.0047 (8)	−0.0001 (10)
O3	0.0249 (8)	0.0201 (8)	0.0471 (15)	0.0005 (7)	0.0114 (9)	0.0041 (11)
O4	0.0235 (7)	0.0152 (7)	0.0566 (16)	−0.0043 (6)	−0.0065 (9)	−0.0078 (11)
O5	0.0288 (8)	0.0161 (7)	0.0355 (12)	−0.0084 (6)	0.0038 (8)	−0.0060 (10)
O6	0.0268 (8)	0.0288 (9)	0.0387 (13)	−0.0085 (7)	0.0084 (8)	−0.0065 (11)
O7	0.0427 (10)	0.0386 (11)	0.0354 (14)	−0.0273 (9)	−0.0031 (9)	−0.0022 (12)
O8	0.0230 (8)	0.0293 (9)	0.0635 (17)	−0.0050 (7)	−0.0104 (9)	−0.0154 (12)
O9	0.0334 (8)	0.0195 (8)	0.0392 (13)	−0.0133 (7)	−0.0079 (9)	−0.0007 (10)
Cd	0.02384 (11)	0.01532 (11)	0.03217 (18)	−0.00887 (9)	−0.00109 (10)	−0.00258 (13)
N1	0.0303 (10)	0.0249 (10)	0.0464 (17)	−0.0101 (9)	−0.0057 (11)	−0.0041 (13)
C1	0.0316 (12)	0.0382 (15)	0.043 (2)	−0.0126 (12)	−0.0013 (13)	−0.0018 (19)
C2	0.0535 (17)	0.0464 (18)	0.042 (2)	−0.0242 (15)	0.0066 (16)	−0.012 (2)
C3	0.068 (2)	0.0419 (17)	0.047 (3)	−0.0273 (17)	0.0068 (18)	−0.006 (2)
C4	0.074 (2)	0.050 (2)	0.049 (3)	−0.0237 (19)	0.009 (2)	−0.015 (2)
C5	0.091 (3)	0.070 (3)	0.042 (3)	−0.032 (2)	0.017 (2)	−0.012 (3)
C6	0.066 (2)	0.049 (2)	0.044 (3)	−0.0245 (18)	0.006 (2)	0.008 (2)
C7	0.0545 (18)	0.0404 (17)	0.062 (3)	−0.0249 (15)	0.0130 (18)	−0.008 (2)
Cl1	0.1789 (15)	0.0753 (8)	0.0887 (11)	−0.0554 (9)	0.0468 (10)	−0.0485 (9)
N2	0.0239 (9)	0.0246 (10)	0.0353 (15)	−0.0048 (8)	0.0001 (9)	−0.0065 (12)
C8	0.0382 (13)	0.0338 (14)	0.0370 (19)	−0.0138 (12)	−0.0073 (13)	−0.0016 (17)
C9	0.081 (2)	0.0355 (17)	0.053 (3)	−0.0185 (17)	−0.008 (2)	−0.010 (2)
C10	0.112 (3)	0.048 (2)	0.045 (3)	−0.022 (2)	0.002 (2)	−0.015 (3)
C11	0.082 (3)	0.064 (2)	0.030 (2)	−0.025 (2)	0.0006 (19)	0.003 (3)
C12	0.072 (2)	0.0465 (19)	0.054 (3)	−0.0269 (18)	−0.006 (2)	0.000 (2)
C13	0.0578 (18)	0.0387 (17)	0.045 (2)	−0.0227 (15)	0.0010 (16)	−0.009 (2)
C14	0.0350 (13)	0.0433 (16)	0.048 (2)	−0.0211 (12)	−0.0060 (14)	−0.0035 (19)
Cl2	0.1687 (16)	0.1080 (12)	0.0444 (8)	−0.0486 (12)	0.0145 (9)	−0.0017 (10)

Geometric parameters (Å, º) top

P1—O1	1.4846 (19)	C3—C4	1.372 (6)
P1—O2	1.486 (2)	C3—H3	0.9300
P1—O4	1.5822 (16)	C4—C5	1.362 (6)
P1—O3	1.607 (2)	C4—Cl1	1.748 (3)
P2—O6	1.471 (2)	C5—C6	1.383 (5)
P2—O5	1.4947 (18)	C5—H5	0.9300
P2—O7	1.5909 (19)	C6—H6	0.9300
P2—O3	1.5975 (18)	C7—H7A	0.9700
P3—O8	1.4614 (18)	C7—H7B	0.9700
P3—O9	1.499 (2)	N2—C14	1.478 (3)
P3—O4ⁱ	1.6009 (16)	N2—H2A	0.8900
P3—O7	1.601 (2)	N2—H2B	0.8900
O2—Cd	2.3534 (18)	N2—H2C	0.8900
O4—P3ⁱ	1.6009 (16)	C8—C9	1.392 (4)
O5—Cd	2.230 (2)	C8—C13	1.401 (5)
O9—Cd	2.2432 (17)	C8—C14	1.482 (5)
Cd—O5ⁱⁱ	2.230 (2)	C9—C10	1.361 (6)
Cd—O9ⁱⁱ	2.2432 (17)	C9—H9	0.9300
Cd—O2ⁱⁱ	2.3534 (18)	C10—C11	1.382 (7)
N1—C7	1.478 (4)	C10—H10	0.9300
N1—H1A	0.8900	C11—C12	1.374 (5)
N1—H1B	0.8900	C11—Cl2	1.735 (5)
N1—H1C	0.8900	C12—C13	1.365 (5)
C1—C2	1.380 (5)	C12—H12	0.9300
C1—C6	1.383 (5)	C13—H13	0.9300
C1—C7	1.515 (4)	C14—H14A	0.9700
C2—C3	1.393 (4)	C14—H14B	0.9700
C2—H2	0.9300

O1—P1—O2	117.93 (12)	C3—C2—H2	119.7
O1—P1—O4	111.66 (10)	C4—C3—C2	118.4 (4)
O2—P1—O4	109.88 (11)	C4—C3—H3	120.8
O1—P1—O3	107.43 (12)	C2—C3—H3	120.8
O2—P1—O3	109.96 (11)	C5—C4—C3	122.2 (3)
O4—P1—O3	98.11 (10)	C5—C4—Cl1	119.5 (3)
O6—P2—O5	118.97 (11)	C3—C4—Cl1	118.2 (3)
O6—P2—O7	107.58 (11)	C4—C5—C6	118.8 (4)
O5—P2—O7	111.28 (13)	C4—C5—H5	120.6
O6—P2—O3	106.68 (13)	C6—C5—H5	120.6
O5—P2—O3	108.08 (11)	C5—C6—C1	121.0 (4)
O7—P2—O3	102.99 (12)	C5—C6—H6	119.5
O8—P3—O9	118.36 (13)	C1—C6—H6	119.5
O8—P3—O4ⁱ	111.32 (9)	N1—C7—C1	114.6 (3)
O9—P3—O4ⁱ	104.99 (10)	N1—C7—H7A	108.6
O8—P3—O7	110.18 (13)	C1—C7—H7A	108.6
O9—P3—O7	110.64 (11)	N1—C7—H7B	108.6
O4ⁱ—P3—O7	99.62 (12)	C1—C7—H7B	108.6
P1—O2—Cd	131.47 (10)	H7A—C7—H7B	107.6
P2—O3—P1	131.59 (16)	C14—N2—H2A	109.5
P1—O4—P3ⁱ	138.76 (11)	C14—N2—H2B	109.5
P2—O5—Cd	122.36 (10)	H2A—N2—H2B	109.5
P2—O7—P3	139.86 (14)	C14—N2—H2C	109.5
P3—O9—Cd	129.75 (13)	H2A—N2—H2C	109.5
O5—Cd—O5ⁱⁱ	180.0	H2B—N2—H2C	109.5
O5—Cd—O9	88.19 (7)	C9—C8—C13	117.2 (4)
O5ⁱⁱ—Cd—O9	91.81 (7)	C9—C8—C14	121.0 (3)
O5—Cd—O9ⁱⁱ	91.81 (7)	C13—C8—C14	121.8 (3)
O5ⁱⁱ—Cd—O9ⁱⁱ	88.19 (7)	C10—C9—C8	121.4 (4)
O9—Cd—O9ⁱⁱ	180.00 (10)	C10—C9—H9	119.3
O5—Cd—O2	83.53 (8)	C8—C9—H9	119.3
O5ⁱⁱ—Cd—O2	96.47 (8)	C9—C10—C11	119.8 (3)
O9—Cd—O2	83.70 (7)	C9—C10—H10	120.1
O9ⁱⁱ—Cd—O2	96.30 (7)	C11—C10—H10	120.1
O5—Cd—O2ⁱⁱ	96.47 (8)	C12—C11—C10	120.5 (4)
O5ⁱⁱ—Cd—O2ⁱⁱ	83.53 (8)	C12—C11—Cl2	119.2 (4)
O9—Cd—O2ⁱⁱ	96.30 (7)	C10—C11—Cl2	120.3 (3)
O9ⁱⁱ—Cd—O2ⁱⁱ	83.70 (7)	C13—C12—C11	119.3 (4)
O2—Cd—O2ⁱⁱ	180.000 (1)	C13—C12—H12	120.3
C7—N1—H1A	109.5	C11—C12—H12	120.3
C7—N1—H1B	109.5	C12—C13—C8	121.7 (3)
H1A—N1—H1B	109.5	C12—C13—H13	119.2
C7—N1—H1C	109.5	C8—C13—H13	119.2
H1A—N1—H1C	109.5	N2—C14—C8	113.1 (2)
H1B—N1—H1C	109.5	N2—C14—H14A	109.0
C2—C1—C6	118.9 (3)	C8—C14—H14A	109.0
C2—C1—C7	123.9 (3)	N2—C14—H14B	109.0
C6—C1—C7	117.2 (3)	C8—C14—H14B	109.0
C1—C2—C3	120.7 (3)	H14A—C14—H14B	107.8
C1—C2—H2	119.7

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···O1	0.89	1.91	2.785 (3)	167
N1—H1B···O6ⁱⁱⁱ	0.89	1.88	2.740 (3)	162
N1—H1C···O9ⁱⁱ	0.89	1.93	2.809 (4)	168
N2—H2A···O2	0.89	1.96	2.814 (4)	160
N2—H2B···O5ⁱⁱ	0.89	2.19	2.866 (3)	133
N2—H2C···O1^iv	0.89	1.95	2.824 (3)	169
C3—H3···O1^v	0.93	2.56	3.339 (5)	142
C13—H13···O6ⁱⁱ	0.93	2.53	3.394 (4)	154
C14—H14B···O3ⁱ	0.97	2.56	3.410 (4)	147

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

Experimental details

Crystal data
Chemical formula	(C₇H₉ClN)₄[Cd(P₆O₁₈)]
M_r	1156.63
Crystal system, space group	Triclinic, P1
Temperature (K)	293
a, b, c (Å)	8.021 (4), 8.1696 (16), 17.919 (3)
α, β, γ (°)	87.31 (5), 88.914 (19), 70.100 (3)
V (Å³)	1102.9 (6)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	1.03
Crystal size (mm)	0.22 × 0.20 × 0.18

Data collection
Diffractometer	Enraf–Nonius TurboCAD-4 diffractometer
Absorption correction	–
No. of measured, independent and observed [I > 2σ(I)] reflections	3873, 3770, 3506
R_int	0.009
(sin θ/λ)_max (Å⁻¹)	0.660

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.027, 0.074, 1.14
No. of reflections	3770
No. of parameters	277
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.76, −0.57

Computer programs: CAD-4 EXPRESS (Enraf–Nonius, 1994), XCAD4 (Harms & Wocadlo, 1995), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 (Farrugia, 1997), WinGX publication routines (Farrugia, 1999).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···O1	0.89	1.91	2.785 (3)	167
N1—H1B···O6ⁱ	0.89	1.88	2.740 (3)	162
N1—H1C···O9ⁱⁱ	0.89	1.93	2.809 (4)	168
N2—H2A···O2	0.89	1.96	2.814 (4)	160
N2—H2B···O5ⁱⁱ	0.89	2.19	2.866 (3)	133
N2—H2C···O1ⁱⁱⁱ	0.89	1.95	2.824 (3)	169
C3—H3···O1^iv	0.93	2.56	3.339 (5)	142
C13—H13···O6ⁱⁱ	0.93	2.53	3.394 (4)	154
C14—H14B···O3^v	0.97	2.56	3.410 (4)	147

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

References

Averbuch-Pouchot, M. T. & Durif, A. (1996). In Topics in Phosphate Chemistry. Singapore: World Scientific. Google Scholar
Du, Z. Y., Sun, Y. H., Xie, Y. R., Lin, J. & Wen, H. R. (2010). Inorg. Chem. Commun. 13, 77–80. Web of Science CSD CrossRef CAS Google Scholar
Durif, A. (2005). Solid State Sci. 7, 760–766. Web of Science CrossRef CAS Google Scholar
Enraf–Nonius (1994). CAD-4 EXPRESS. Enraf–Nonius, Delft, The Netherlands. Google Scholar
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. CrossRef IUCr Journals Google Scholar
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838. CrossRef CAS IUCr Journals Google Scholar
Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany. Google Scholar
Hathwar, V. R., Roopan, S. M., Subashini, R., Khan, F. N. & Row, T. N. G. (2010). J. Chem. Sci. 122, 677–685. CSD CrossRef CAS Google Scholar
Hu, J.-Y., Zhao, J.-A., Hou, H.-W. & Fan, Y.-T. (2008). Inorg. Chem. Commun. 11, 1110–1112. Web of Science CSD CrossRef CAS Google Scholar
Janiak, C. (2000). J. Chem. Soc. Dalton Trans. pp. 3885–3896. Web of Science CrossRef Google Scholar
Kolotuchin, S. V., Fenlon, E. E., Wilson, S. R., Loweth, C. J. & Zimmerman, S. C. (1995). Angew. Chem. Int. Ed. 34, 2654–2657. CrossRef CAS Google Scholar
Kontturi, M., Laurila, E., Mattsson, R., Peraniemi, S., Vepsalainen, J. J. & Ahlgren, M. (2005). Inorg. Chem. 44, 2400–2406. Web of Science CSD CrossRef PubMed CAS Google Scholar
Man, S. P., Motevalli, M., Gardiner, S., Sullivan, A. & Wilson, J. (2006). Polyhedron, 25, 1017–1032. Web of Science CSD CrossRef CAS Google Scholar
Schülke, U. & Kayser, R. (1985). Z. Anorg. Allg. Chem. 531, 167–175. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Tong, M. L., Lee, H. K., Chen, X. M., Huang, R. B. & Mak, T. C. M. (1999). J. Chem. Soc. Dalton Trans. pp. 3657–3659. Web of Science CSD CrossRef Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 67| Part 11| November 2011| Pages m1549-m1550

doi:10.1107/S160053681104133X

Open

access

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text

Search IUCr Journals		doi		Advanced search
Author		volume	page

metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

The one-dimensional coordination polymer poly[tetra­kis­[(4-chloro­phen­yl)methanaminium] [cadmate-μ-cyclo­hexa­phospho­rato]]

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

References

metal-organic compounds

The one-dimensional coordination polymer poly[tetrakis[(4-chlorophenyl)methanaminium] [cadmate-μ-cyclohexaphosphorato]]