Bis(tetra-phenyl-phospho-nium) tetra-chlorido-cobaltate(II).

The title compound, (C24H20P)2[CoCl4], was prepared under hydro-thermal conditions. In the crystal, the tetra-phenyl-phospho-nium cations are linked by pairs of weak C-H⋯π inter-actions into supra-molecular dimers; the Co(II) cations lie on twofold rotation axes and the tetra-hedral [CoCl4](2-) anions are linked with the tetra-phenyl-phospho-nium cations via weak C-H⋯Cl hydrogen bonds.

Related literature

For background and applications of compounds with supramolecular structures, see: Rowsell & Yaghi (2005 ▶); Dong et al. (2007 ▶); Wu & Lin (2007 ▶); Zhao et al. (2003 ▶); Neville et al. (2008 ▶); Huang et al. (2007 ▶). For applications of the tetra­phenyl­phospho­nium ion in supra­molecular chemistry and numerous coordination polymers, see: Zacharie et al. (1985 ▶); Schlueter & Geiser (2007 ▶).

Experimental

Crystal data

(C24H20P)2[CoCl4]

M = 879.46

Monoclinic,

a = 10.9154 (4) Å

b = 19.2514 (6) Å

c = 20.1826 (7) Å

β = 91.008 (2)°

V = 4240.4 (3) Å3

Z = 4

Mo Kα radiation

μ = 0.77 mm−1

T = 293 K

0.20 × 0.10 × 0.08 mm

Data collection

Bruker APEXII diffractometer

12226 measured reflections

3748 independent reflections

3180 reflections with I > 2σ(I)

R int = 0.028

Refinement

R[F 2 > 2σ(F 2)] = 0.030

wR(F 2) = 0.084

S = 1.04

3748 reflections

249 parameters

H-atom parameters constrained

Δρmax = 1.51 e Å−3

Δρmin = −0.22 e Å−3

Data collection: APEX2 (Bruker, 2006 ▶); cell refinement: SAINT (Bruker, 2006 ▶); data reduction: SAINT; program(s) used to solve structure: SIR2002 (Burla et al., 2003 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012 ▶); software used to prepare material for publication: WinGX (Farrugia, 2012 ▶), Mercury (Macrae et al., 2006 ▶) and POVRay (Persistence of Vision Team, 2004 ▶).

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536814011210/xu5791sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536814011210/xu5791Isup2.hkl

CCDC reference: 1003287

Additional supporting information: crystallographic information; 3D view; checkCIF report

(C24H20P)2[CoCl4]	F(000) = 1812
Mr = 879.46	Dx = 1.378 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 1536 reflections
a = 10.9154 (4) Å	θ = 3.2–25.1°
b = 19.2514 (6) Å	µ = 0.77 mm−1
c = 20.1826 (7) Å	T = 293 K
β = 91.008 (2)°	Prism, pink
V = 4240.4 (3) Å3	0.2 × 0.1 × 0.08 mm
Z = 4

Bruker APEXII diffractometer	3180 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.028
Graphite monochromator	θmax = 25.1°, θmin = 2.0°
φ scans	h = −12→12
12226 measured reflections	k = −22→22
3748 independent reflections	l = −24→22

Refinement on F2	0 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.030	w = 1/[σ2(Fo2) + (0.0401P)2 + 6.1572P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.084	(Δ/σ)max = 0.001
S = 1.04	Δρmax = 1.51 e Å−3
3748 reflections	Δρmin = −0.22 e Å−3
249 parameters

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

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
P1	0.41273 (5)	0.36748 (3)	0.07765 (3)	0.0200 (2)
C1	0.3837 (2)	0.29974 (11)	0.13639 (11)	0.0233 (7)
C2	0.3155 (2)	0.31597 (12)	0.19182 (11)	0.0308 (7)
C3	0.2894 (3)	0.26481 (13)	0.23755 (13)	0.0376 (8)
C4	0.3336 (2)	0.19823 (12)	0.22924 (12)	0.0355 (8)
C5	0.4026 (2)	0.18228 (12)	0.17495 (12)	0.0335 (8)
C6	0.4272 (2)	0.23227 (11)	0.12800 (12)	0.0290 (7)
C7	0.5226 (2)	0.33873 (11)	0.01785 (11)	0.0238 (7)
C8	0.6408 (2)	0.36542 (13)	0.01635 (12)	0.0291 (7)
C9	0.7214 (2)	0.34138 (14)	−0.03052 (13)	0.0375 (8)
C10	0.6855 (2)	0.29065 (13)	−0.07487 (12)	0.0370 (8)
C11	0.5686 (3)	0.26452 (12)	−0.07432 (12)	0.0363 (8)
C12	0.4866 (2)	0.28862 (12)	−0.02847 (12)	0.0314 (7)
C13	0.27533 (19)	0.39129 (10)	0.03328 (10)	0.0199 (6)
C14	0.2858 (2)	0.42599 (12)	−0.02717 (11)	0.0272 (7)
C15	0.1824 (2)	0.44748 (12)	−0.06129 (11)	0.0297 (7)
C16	0.0676 (2)	0.43485 (12)	−0.03560 (11)	0.0269 (7)
C17	0.0570 (2)	0.40171 (12)	0.02446 (11)	0.0271 (7)
C18	0.1604 (2)	0.38005 (11)	0.05921 (11)	0.0232 (7)
C19	0.47179 (19)	0.44088 (11)	0.12202 (10)	0.0205 (6)
C20	0.4177 (2)	0.50598 (11)	0.11488 (11)	0.0226 (6)
C21	0.4699 (2)	0.56215 (12)	0.14713 (11)	0.0289 (7)
C22	0.5746 (2)	0.55408 (13)	0.18543 (11)	0.0304 (7)
C23	0.6265 (2)	0.48956 (14)	0.19401 (11)	0.0315 (8)
C24	0.5750 (2)	0.43278 (13)	0.16272 (11)	0.0280 (7)
Co1	0.00000	0.45721 (2)	0.25000	0.0202 (1)
Cl1	0.10790 (5)	0.38813 (3)	0.32242 (3)	0.0338 (2)
Cl2	0.12506 (5)	0.52482 (3)	0.18779 (3)	0.0267 (2)
H2	0.28760	0.36110	0.19810	0.0370*
H3	0.24190	0.27530	0.27400	0.0450*
H4	0.31670	0.16410	0.26040	0.0430*
H5	0.43290	0.13750	0.16980	0.0400*
H6	0.47250	0.22100	0.09090	0.0350*
H8	0.66550	0.39920	0.04670	0.0350*
H9	0.80030	0.35960	−0.03210	0.0450*
H10	0.74100	0.27400	−0.10550	0.0440*
H11	0.54480	0.23060	−0.10480	0.0440*
H12	0.40700	0.27140	−0.02840	0.0380*
H14	0.36280	0.43460	−0.04440	0.0330*
H15	0.18950	0.47050	−0.10160	0.0360*
H16	−0.00230	0.44880	−0.05900	0.0320*
H17	−0.02010	0.39380	0.04180	0.0330*
H18	0.15280	0.35800	0.09990	0.0280*
H20	0.34740	0.51150	0.08870	0.0270*
H21	0.43410	0.60580	0.14300	0.0350*
H22	0.61050	0.59260	0.20570	0.0360*
H23	0.69600	0.48430	0.22080	0.0380*
H24	0.60930	0.38900	0.16880	0.0340*

	U11	U22	U33	U12	U13	U23
P1	0.0206 (3)	0.0189 (3)	0.0205 (3)	0.0001 (2)	0.0001 (2)	−0.0013 (2)
C1	0.0266 (12)	0.0210 (11)	0.0222 (11)	−0.0004 (9)	−0.0037 (9)	0.0011 (9)
C2	0.0441 (14)	0.0228 (12)	0.0255 (12)	0.0057 (11)	0.0025 (11)	0.0007 (9)
C3	0.0528 (16)	0.0346 (14)	0.0256 (13)	0.0020 (12)	0.0065 (12)	0.0037 (11)
C4	0.0484 (15)	0.0275 (13)	0.0303 (13)	−0.0040 (11)	−0.0064 (12)	0.0096 (10)
C5	0.0454 (15)	0.0187 (11)	0.0361 (14)	0.0038 (11)	−0.0070 (12)	0.0010 (10)
C6	0.0324 (13)	0.0255 (12)	0.0291 (12)	0.0037 (10)	−0.0013 (10)	−0.0025 (10)
C7	0.0272 (12)	0.0207 (11)	0.0235 (11)	0.0042 (9)	0.0018 (9)	0.0013 (9)
C8	0.0240 (12)	0.0355 (13)	0.0279 (12)	0.0022 (10)	−0.0009 (10)	0.0005 (10)
C9	0.0236 (12)	0.0548 (16)	0.0343 (14)	0.0069 (12)	0.0030 (11)	0.0031 (12)
C10	0.0404 (15)	0.0422 (15)	0.0286 (13)	0.0170 (12)	0.0101 (11)	0.0036 (11)
C11	0.0554 (17)	0.0254 (12)	0.0284 (13)	0.0060 (12)	0.0080 (12)	−0.0034 (10)
C12	0.0372 (13)	0.0252 (12)	0.0319 (13)	−0.0035 (10)	0.0056 (11)	−0.0036 (10)
C13	0.0212 (11)	0.0186 (10)	0.0199 (11)	−0.0011 (9)	−0.0018 (9)	−0.0027 (8)
C14	0.0239 (12)	0.0340 (13)	0.0237 (12)	−0.0033 (10)	0.0031 (9)	0.0040 (10)
C15	0.0342 (13)	0.0345 (13)	0.0203 (11)	−0.0004 (11)	0.0002 (10)	0.0061 (10)
C16	0.0260 (12)	0.0286 (12)	0.0258 (12)	0.0038 (10)	−0.0048 (10)	−0.0033 (10)
C17	0.0216 (11)	0.0317 (12)	0.0282 (12)	−0.0009 (10)	0.0035 (9)	−0.0010 (10)
C18	0.0256 (12)	0.0248 (11)	0.0192 (11)	−0.0028 (9)	0.0024 (9)	0.0018 (9)
C19	0.0200 (11)	0.0219 (11)	0.0198 (11)	−0.0015 (9)	0.0036 (9)	−0.0025 (9)
C20	0.0238 (11)	0.0233 (11)	0.0208 (11)	−0.0014 (9)	0.0035 (9)	0.0007 (9)
C21	0.0395 (14)	0.0207 (11)	0.0268 (12)	−0.0033 (10)	0.0079 (11)	−0.0002 (9)
C22	0.0354 (13)	0.0335 (13)	0.0225 (12)	−0.0165 (11)	0.0072 (10)	−0.0080 (10)
C23	0.0228 (12)	0.0483 (15)	0.0235 (12)	−0.0042 (11)	−0.0001 (10)	−0.0070 (11)
C24	0.0253 (12)	0.0324 (13)	0.0262 (12)	0.0054 (10)	−0.0016 (10)	−0.0036 (10)
Co1	0.0188 (2)	0.0189 (2)	0.0231 (2)	0.0000	0.0029 (2)	0.0000
Cl1	0.0315 (3)	0.0335 (3)	0.0367 (3)	0.0084 (3)	0.0074 (3)	0.0151 (3)
Cl2	0.0234 (3)	0.0296 (3)	0.0270 (3)	−0.0035 (2)	0.0015 (2)	0.0071 (2)

Co1—Cl2	2.2791 (6)	C19—C24	1.391 (3)
Co1—Cl1i	2.2873 (6)	C19—C20	1.392 (3)
Co1—Cl1	2.2873 (6)	C20—C21	1.380 (3)
Co1—Cl2i	2.2791 (6)	C21—C22	1.377 (3)
P1—C1	1.794 (2)	C22—C23	1.375 (4)
P1—C7	1.803 (2)	C23—C24	1.377 (3)
P1—C13	1.793 (2)	C2—H2	0.9301
P1—C19	1.787 (2)	C3—H3	0.9296
C1—C6	1.394 (3)	C4—H4	0.9302
C1—C2	1.390 (3)	C5—H5	0.9298
C2—C3	1.383 (3)	C6—H6	0.9302
C3—C4	1.381 (3)	C8—H8	0.9301
C4—C5	1.375 (3)	C9—H9	0.9310
C5—C6	1.380 (3)	C10—H10	0.9301
C7—C8	1.390 (3)	C11—H11	0.9310
C7—C12	1.395 (3)	C12—H12	0.9300
C8—C9	1.383 (3)	C14—H14	0.9301
C9—C10	1.377 (4)	C15—H15	0.9309
C10—C11	1.372 (4)	C16—H16	0.9299
C11—C12	1.379 (4)	C17—H17	0.9297
C13—C14	1.397 (3)	C18—H18	0.9295
C13—C18	1.385 (3)	C20—H20	0.9301
C14—C15	1.375 (3)	C21—H21	0.9299
C15—C16	1.386 (3)	C22—H22	0.9302
C16—C17	1.376 (3)	C23—H23	0.9293
C17—C18	1.383 (3)	C24—H24	0.9295
Cl1—Co1—Cl2	112.17 (2)	C22—C23—C24	119.7 (2)
Cl1—Co1—Cl1i	108.90 (3)	C19—C24—C23	120.1 (2)
Cl1—Co1—Cl2i	106.66 (2)	C3—C2—H2	120.17
Cl1i—Co1—Cl2	106.66 (2)	C1—C2—H2	120.06
Cl2—Co1—Cl2i	110.35 (3)	C2—C3—H3	119.85
Cl1i—Co1—Cl2i	112.17 (2)	C4—C3—H3	119.91
C13—P1—C19	109.84 (10)	C3—C4—H4	119.98
C1—P1—C19	108.05 (10)	C5—C4—H4	119.92
C1—P1—C7	110.27 (10)	C6—C5—H5	119.72
C1—P1—C13	111.10 (10)	C4—C5—H5	119.80
C7—P1—C13	107.73 (10)	C1—C6—H6	120.13
C7—P1—C19	109.86 (10)	C5—C6—H6	120.17
P1—C1—C6	122.16 (17)	C7—C8—H8	120.18
P1—C1—C2	118.14 (17)	C9—C8—H8	120.26
C2—C1—C6	119.7 (2)	C10—C9—H9	119.85
C1—C2—C3	119.8 (2)	C8—C9—H9	119.83
C2—C3—C4	120.2 (2)	C9—C10—H10	119.68
C3—C4—C5	120.1 (2)	C11—C10—H10	119.72
C4—C5—C6	120.5 (2)	C12—C11—H11	120.17
C1—C6—C5	119.7 (2)	C10—C11—H11	120.04
P1—C7—C8	121.99 (17)	C7—C12—H12	119.84
P1—C7—C12	118.55 (17)	C11—C12—H12	119.90
C8—C7—C12	119.5 (2)	C13—C14—H14	120.00
C7—C8—C9	119.6 (2)	C15—C14—H14	119.88
C8—C9—C10	120.3 (2)	C16—C15—H15	120.01
C9—C10—C11	120.6 (2)	C14—C15—H15	120.04
C10—C11—C12	119.8 (2)	C15—C16—H16	119.90
C7—C12—C11	120.3 (2)	C17—C16—H16	120.01
C14—C13—C18	119.55 (19)	C16—C17—H17	119.87
P1—C13—C18	121.79 (16)	C18—C17—H17	119.73
P1—C13—C14	118.54 (16)	C17—C18—H18	120.08
C13—C14—C15	120.1 (2)	C13—C18—H18	120.05
C14—C15—C16	120.0 (2)	C19—C20—H20	120.40
C15—C16—C17	120.1 (2)	C21—C20—H20	120.54
C16—C17—C18	120.4 (2)	C20—C21—H21	119.77
C13—C18—C17	119.9 (2)	C22—C21—H21	119.71
P1—C19—C24	119.24 (17)	C23—C22—H22	119.70
P1—C19—C20	120.76 (16)	C21—C22—H22	119.73
C20—C19—C24	120.0 (2)	C22—C23—H23	120.14
C19—C20—C21	119.1 (2)	C24—C23—H23	120.18
C20—C21—C22	120.5 (2)	C23—C24—H24	119.93
C21—C22—C23	120.6 (2)	C19—C24—H24	119.98

D—H···A	D—H	H···A	D···A	D—H···A
C3—H3···Cl1	0.93	2.80	3.552 (3)	138
C11—H11···Cl1ii	0.93	2.81	3.633 (2)	148
C23—H23···Cl2iii	0.93	2.77	3.644 (2)	156
C14—H14···Cg4iv	0.93	2.88	3.650 (2)	141
C21—H21···Cg2iv	0.93	2.79	3.446 (2)	129

Table 1

Selected bond lengths (Å)

Co1—Cl2	2.2791 (6)
Co1—Cl1	2.2873 (6)

Table 2

Hydrogen-bond geometry (Å, °)

Cg2 and Cg4 are the centroids of the C19–C24 and C7-C12 benzene rings, respectively.

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C3—H3⋯Cl1	0.93	2.80	3.552 (3)	138
C11—H11⋯Cl1i	0.93	2.81	3.633 (2)	148
C23—H23⋯Cl2ii	0.93	2.77	3.644 (2)	156
C14—H14⋯Cg4iii	0.93	2.88	3.650 (2)	141
C21—H21⋯Cg2iii	0.93	2.79	3.446 (2)	129

Symmetry codes: (i) ; (ii) ; (iii) .