Methyl­triphenyl­phospho­nium hexa­chloro­rhenate(IV)

The title compound, (C₁₉H₁₈P)₂[ReCl₆], consists of alternating cationic and anionic layers. Unlike some related materials, the Re^IV cations (Re site symmetry ) of the hexa­chloro­rhenate(IV) anions do not order magnetically. Some of the Cl atoms of the anion are disordered over two positions related by rotation with respect to a Cl—Re—Cl axis, which can be correlated with C—H...Cl inter­actions.

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](C-C) = 0.006 Å
• Disorder in solvent or counterion
• R factor = 0.058
• wR factor = 0.088
• Data-to-parameter ratio = 37.2

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.52
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      36.00 Perc.

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   3 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: KM-4 CCD Software (Kuma Diffraction, 1999); cell refinement: KM-4 CCD Software; data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: SHELXL97.

Methyltriphenylphosphonium hexachlororhenate(IV)

Crystal data

(C19H18P)2[ReCl6]	F(000) = 942
Mr = 953.51	Dx = 1.670 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 16709 reflections
a = 9.144 (3) Å	θ = 3.5–35.0°
b = 16.343 (4) Å	µ = 3.74 mm^−1
c = 12.976 (4) Å	T = 100 K
β = 102.13 (3)°	Block, green
V = 1895.8 (10) Å^3	0.15 × 0.09 × 0.05 mm
Z = 2

Data collection

Kuma KM4 CCD area detector diffractometer	8322 independent reflections
Radiation source: fine-focus sealed tube	5603 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.060
ω scans	θmax = 35.0°, θmin = 4.5°
Absorption correction: part of the refinement model (ΔF) (Walker & Stuart, 1983)	h = −14→14
Tmin = 0.631, Tmax = 0.902	k = −26→18
31489 measured reflections	l = −20→20

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.059	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.088	H-atom parameters constrained
S = 1.09	w = 1/[σ^2(Fo^2) + (0.0253P)^2] where P = (Fo^2 + 2Fc^2)/3
8322 reflections	(Δ/σ)max = 0.001
224 parameters	Δρmax = 3.24 e Å^−3
2 restraints	Δρmin = −1.28 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Re	0.5000	0.5000	0.5000	0.01683 (6)
Cl1	0.60636 (11)	0.62970 (5)	0.51796 (8)	0.0267 (2)
Cl2	0.5588 (6)	0.48819 (11)	0.3316 (2)	0.0221 (7)	0.917 (18)
Cl3	0.2677 (2)	0.55976 (10)	0.4218 (4)	0.0217 (5)	0.917 (18)
Cl2A	0.607 (4)	0.4966 (16)	0.3494 (16)	0.022 (4)*	0.083 (18)
Cl3A	0.2804 (17)	0.5571 (14)	0.396 (2)	0.021 (5)*	0.083 (18)
P	−0.00703 (11)	0.71991 (5)	0.63491 (7)	0.01720 (19)
C1	0.0001 (5)	0.6342 (2)	0.5500 (3)	0.0273 (9)
H111	0.0614	0.5908	0.5896	0.041*
H121	0.0444	0.6512	0.4908	0.041*
H131	−0.1014	0.6136	0.5230	0.041*
C11	−0.1198 (4)	0.7995 (2)	0.5626 (3)	0.0178 (7)
C21	−0.2444 (4)	0.8304 (2)	0.5939 (3)	0.0244 (8)
H21	−0.2739	0.8089	0.6544	0.029*
C31	−0.3261 (5)	0.8930 (2)	0.5368 (4)	0.0320 (10)
H31	−0.4115	0.9144	0.5583	0.038*
C41	−0.2838 (5)	0.9242 (3)	0.4489 (3)	0.0353 (10)
H41	−0.3399	0.9673	0.4103	0.042*
C51	−0.1601 (5)	0.8931 (3)	0.4166 (3)	0.0373 (11)
H51	−0.1313	0.9148	0.3559	0.045*
C61	−0.0787 (5)	0.8308 (3)	0.4726 (3)	0.0300 (9)
H61	0.0056	0.8090	0.4500	0.036*
C12	0.1776 (4)	0.7608 (2)	0.6779 (3)	0.0181 (7)
C22	0.3032 (4)	0.7134 (2)	0.6753 (3)	0.0209 (8)
H22	0.2914	0.6594	0.6476	0.025*
C32	0.4452 (4)	0.7445 (2)	0.7127 (3)	0.0228 (8)
H32	0.5308	0.7119	0.7110	0.027*
C42	0.4620 (4)	0.8238 (2)	0.7531 (3)	0.0252 (9)
H42	0.5594	0.8453	0.7788	0.030*
C52	0.3382 (4)	0.8712 (2)	0.7560 (3)	0.0274 (9)
H52	0.3506	0.9252	0.7836	0.033*
C62	0.1961 (4)	0.8403 (2)	0.7188 (3)	0.0229 (8)
H62	0.1110	0.8731	0.7210	0.028*
C13	−0.0829 (4)	0.6887 (2)	0.7456 (3)	0.0196 (8)
C23	−0.1468 (4)	0.6115 (2)	0.7468 (3)	0.0248 (8)
H23	−0.1486	0.5750	0.6896	0.030*
C33	−0.2073 (4)	0.5879 (3)	0.8309 (3)	0.0318 (10)
H33	−0.2515	0.5354	0.8313	0.038*
C43	−0.2039 (5)	0.6408 (3)	0.9147 (4)	0.0344 (10)
H43	−0.2441	0.6242	0.9732	0.041*
C53	−0.1415 (5)	0.7179 (3)	0.9129 (3)	0.0353 (10)
H53	−0.1407	0.7546	0.9698	0.042*
C63	−0.0808 (5)	0.7417 (2)	0.8292 (3)	0.0262 (9)
H63	−0.0374	0.7945	0.8287	0.031*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Re	0.01748 (10)	0.01828 (10)	0.01595 (9)	0.00590 (10)	0.00632 (7)	0.00384 (10)
Cl1	0.0292 (5)	0.0224 (4)	0.0270 (5)	0.0009 (4)	0.0027 (4)	−0.0008 (4)
Cl2	0.0357 (16)	0.0162 (7)	0.0179 (7)	0.0006 (6)	0.0137 (8)	0.0000 (4)
Cl3	0.0173 (6)	0.0153 (6)	0.0307 (12)	0.0042 (4)	0.0006 (6)	−0.0008 (6)
P	0.0196 (5)	0.0182 (4)	0.0149 (4)	−0.0015 (4)	0.0061 (4)	−0.0045 (4)
C1	0.032 (2)	0.027 (2)	0.025 (2)	−0.0049 (18)	0.0123 (17)	−0.0130 (17)
C11	0.0130 (17)	0.0224 (18)	0.0169 (18)	−0.0023 (14)	0.0008 (14)	−0.0039 (14)
C21	0.021 (2)	0.029 (2)	0.025 (2)	−0.0039 (17)	0.0078 (17)	0.0014 (17)
C31	0.026 (2)	0.031 (2)	0.039 (3)	0.0052 (18)	0.0059 (19)	−0.001 (2)
C41	0.037 (3)	0.030 (2)	0.033 (3)	0.003 (2)	−0.006 (2)	0.0018 (19)
C51	0.047 (3)	0.045 (3)	0.021 (2)	−0.003 (2)	0.010 (2)	0.0073 (19)
C61	0.029 (2)	0.042 (2)	0.019 (2)	0.004 (2)	0.0065 (17)	0.0005 (18)
C12	0.0206 (19)	0.0202 (17)	0.0151 (17)	−0.0006 (15)	0.0075 (14)	−0.0021 (14)
C22	0.023 (2)	0.0214 (18)	0.0190 (19)	0.0045 (16)	0.0063 (15)	−0.0006 (15)
C32	0.0178 (19)	0.035 (2)	0.0162 (18)	0.0081 (16)	0.0041 (15)	0.0022 (16)
C42	0.021 (2)	0.038 (2)	0.0179 (19)	−0.0051 (18)	0.0067 (16)	−0.0022 (17)
C52	0.028 (2)	0.028 (2)	0.027 (2)	−0.0047 (18)	0.0059 (17)	−0.0095 (17)
C62	0.023 (2)	0.0222 (19)	0.024 (2)	0.0034 (16)	0.0065 (16)	−0.0038 (16)
C13	0.0197 (19)	0.0210 (18)	0.0175 (18)	−0.0005 (15)	0.0028 (15)	0.0006 (14)
C23	0.023 (2)	0.026 (2)	0.023 (2)	−0.0054 (17)	0.0005 (16)	0.0013 (16)
C33	0.024 (2)	0.038 (2)	0.030 (2)	−0.0056 (19)	−0.0014 (18)	0.0116 (19)
C43	0.026 (2)	0.047 (3)	0.031 (2)	−0.004 (2)	0.0059 (19)	0.014 (2)
C53	0.048 (3)	0.040 (2)	0.021 (2)	0.004 (2)	0.015 (2)	−0.0025 (19)
C63	0.038 (2)	0.0225 (19)	0.020 (2)	−0.0031 (18)	0.0101 (18)	−0.0002 (16)

Geometric parameters (Å, º)

Re—Cl1^i	2.3233 (10)	C51—C61	1.376 (6)
Re—Cl1	2.3233 (10)	C51—H51	0.9500
Re—Cl2A^i	2.361 (5)	C61—H61	0.9500
Re—Cl2A	2.361 (5)	C12—C22	1.392 (5)
Re—Cl3^i	2.3641 (12)	C12—C62	1.401 (5)
Re—Cl3	2.3641 (12)	C22—C32	1.384 (5)
Re—Cl2	2.3655 (12)	C22—H22	0.9500
Re—Cl2^i	2.3655 (12)	C32—C42	1.395 (5)
Re—Cl3A^i	2.366 (5)	C32—H32	0.9500
Re—Cl3A	2.366 (5)	C42—C52	1.379 (5)
P—C12	1.793 (4)	C42—H42	0.9500
P—C1	1.793 (4)	C52—C62	1.383 (5)
P—C13	1.795 (4)	C52—H52	0.9500
P—C11	1.797 (4)	C62—H62	0.9500
C1—H111	0.9800	C13—C63	1.385 (5)
C1—H121	0.9800	C13—C23	1.392 (5)
C1—H131	0.9800	C23—C33	1.377 (5)
C11—C21	1.383 (5)	C23—H23	0.9500
C11—C61	1.396 (5)	C33—C43	1.384 (6)
C21—C31	1.386 (5)	C33—H33	0.9500
C21—H21	0.9500	C43—C53	1.386 (6)
C31—C41	1.377 (6)	C43—H43	0.9500
C31—H31	0.9500	C53—C63	1.376 (5)
C41—C51	1.383 (6)	C53—H53	0.9500
C41—H41	0.9500	C63—H63	0.9500
Cl1^i—Re—Cl1	180.00 (5)	H121—C1—H131	109.5
Cl1^i—Re—Cl2A^i	82.4 (8)	C21—C11—C61	119.7 (3)
Cl1—Re—Cl2A^i	97.6 (8)	C21—C11—P	121.9 (3)
Cl1^i—Re—Cl2A	97.6 (8)	C61—C11—P	118.4 (3)
Cl1—Re—Cl2A	82.4 (8)	C11—C21—C31	119.8 (4)
Cl2A^i—Re—Cl2A	180.000 (5)	C11—C21—H21	120.1
Cl1^i—Re—Cl3^i	89.17 (5)	C31—C21—H21	120.1
Cl1—Re—Cl3^i	90.83 (5)	C41—C31—C21	120.2 (4)
Cl2A^i—Re—Cl3^i	98.3 (6)	C41—C31—H31	119.9
Cl2A—Re—Cl3^i	81.7 (6)	C21—C31—H31	119.9
Cl1^i—Re—Cl3	90.83 (5)	C31—C41—C51	120.4 (4)
Cl1—Re—Cl3	89.17 (5)	C31—C41—H41	119.8
Cl2A^i—Re—Cl3	81.7 (6)	C51—C41—H41	119.8
Cl2A—Re—Cl3	98.3 (6)	C61—C51—C41	119.8 (4)
Cl3^i—Re—Cl3	180.0	C61—C51—H51	120.1
Cl1^i—Re—Cl2	90.26 (9)	C41—C51—H51	120.1
Cl1—Re—Cl2	89.74 (9)	C51—C61—C11	120.2 (4)
Cl2A^i—Re—Cl2	168.6 (8)	C51—C61—H61	119.9
Cl2A—Re—Cl2	11.4 (8)	C11—C61—H61	119.9
Cl3^i—Re—Cl2	90.28 (7)	C22—C12—C62	119.4 (3)
Cl3—Re—Cl2	89.72 (7)	C22—C12—P	120.8 (3)
Cl1^i—Re—Cl2^i	89.74 (9)	C62—C12—P	119.7 (3)
Cl1—Re—Cl2^i	90.26 (9)	C32—C22—C12	120.3 (3)
Cl2A^i—Re—Cl2^i	11.4 (8)	C32—C22—H22	119.8
Cl2A—Re—Cl2^i	168.6 (8)	C12—C22—H22	119.8
Cl3^i—Re—Cl2^i	89.72 (7)	C22—C32—C42	119.6 (3)
Cl3—Re—Cl2^i	90.28 (7)	C22—C32—H32	120.2
Cl2—Re—Cl2^i	180.000 (1)	C42—C32—H32	120.2
Cl1^i—Re—Cl3A^i	89.1 (6)	C52—C42—C32	120.4 (4)
Cl1—Re—Cl3A^i	90.9 (6)	C52—C42—H42	119.8
Cl2A^i—Re—Cl3A^i	89.1 (6)	C32—C42—H42	119.8
Cl2A—Re—Cl3A^i	90.9 (6)	C42—C52—C62	120.1 (4)
Cl3^i—Re—Cl3A^i	9.3 (7)	C42—C52—H52	119.9
Cl3—Re—Cl3A^i	170.7 (7)	C62—C52—H52	119.9
Cl2—Re—Cl3A^i	99.6 (7)	C52—C62—C12	120.1 (3)
Cl2^i—Re—Cl3A^i	80.4 (7)	C52—C62—H62	120.0
Cl1^i—Re—Cl3A	90.9 (6)	C12—C62—H62	120.0
Cl1—Re—Cl3A	89.1 (6)	C63—C13—C23	119.6 (3)
Cl2A^i—Re—Cl3A	90.9 (6)	C63—C13—P	120.3 (3)
Cl2A—Re—Cl3A	89.1 (6)	C23—C13—P	120.0 (3)
Cl3^i—Re—Cl3A	170.7 (7)	C33—C23—C13	120.2 (4)
Cl3—Re—Cl3A	9.3 (7)	C33—C23—H23	119.9
Cl2—Re—Cl3A	80.4 (7)	C13—C23—H23	119.9
Cl2^i—Re—Cl3A	99.6 (7)	C23—C33—C43	120.1 (4)
Cl3A^i—Re—Cl3A	179.999 (3)	C23—C33—H33	120.0
C12—P—C1	109.21 (18)	C43—C33—H33	120.0
C12—P—C13	110.73 (17)	C33—C43—C53	119.7 (4)
C1—P—C13	109.89 (18)	C33—C43—H43	120.1
C12—P—C11	107.01 (16)	C53—C43—H43	120.1
C1—P—C11	109.62 (19)	C63—C53—C43	120.4 (4)
C13—P—C11	110.33 (17)	C63—C53—H53	119.8
P—C1—H111	109.5	C43—C53—H53	119.8
P—C1—H121	109.5	C53—C63—C13	120.0 (4)
H111—C1—H121	109.5	C53—C63—H63	120.0
P—C1—H131	109.5	C13—C63—H63	120.0
H111—C1—H131	109.5

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C22—H22···Cl2^i	0.95	2.76	3.535 (4)	139
C62—H62···Cl2^ii	0.95	2.78	3.514 (4)	135
C1—H131···Cl1^iii	0.98	2.67	3.538 (4)	147
C63—H63···Cl1^ii	0.95	2.82	3.404 (4)	121
C1—H121···Cl3	0.98	2.82	3.456 (6)	123
C42—H42···Cl3^iv	0.95	2.83	3.695 (4)	152
C23—H23···Cl3^v	0.95	2.73	3.582 (5)	149
C42—H42···Cl3A^iv	0.95	2.76	3.66 (1)	158
C23—H23···Cl3A^v	0.95	2.60	3.40 (3)	142
C22—H22···Cl2A^i	0.95	2.71	3.56 (2)	149
C62—H62···Cl2A^ii	0.95	2.71	3.35 (2)	125

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x−1/2, −y+3/2, z+1/2; (iii) x−1, y, z; (iv) x+1/2, −y+3/2, z+1/2; (v) −x, −y+1, −z+1.