The title compound, (C
19H
18P)
2[ReCl
6], 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.
Supporting information
CCDC reference: 629827
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (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
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)
top
Crystal data top
(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) Å3 | 0.15 × 0.09 × 0.05 mm |
Z = 2 | |
Data collection top
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 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)] = 0.059 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.088 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0253P)2] where P = (Fo2 + 2Fc2)/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 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 | 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 (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
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) top
Re—Cl1i | 2.3233 (10) | C51—C61 | 1.376 (6) |
Re—Cl1 | 2.3233 (10) | C51—H51 | 0.9500 |
Re—Cl2Ai | 2.361 (5) | C61—H61 | 0.9500 |
Re—Cl2A | 2.361 (5) | C12—C22 | 1.392 (5) |
Re—Cl3i | 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—Cl2i | 2.3655 (12) | C32—C42 | 1.395 (5) |
Re—Cl3Ai | 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 |
| | | |
Cl1i—Re—Cl1 | 180.00 (5) | H121—C1—H131 | 109.5 |
Cl1i—Re—Cl2Ai | 82.4 (8) | C21—C11—C61 | 119.7 (3) |
Cl1—Re—Cl2Ai | 97.6 (8) | C21—C11—P | 121.9 (3) |
Cl1i—Re—Cl2A | 97.6 (8) | C61—C11—P | 118.4 (3) |
Cl1—Re—Cl2A | 82.4 (8) | C11—C21—C31 | 119.8 (4) |
Cl2Ai—Re—Cl2A | 180.000 (5) | C11—C21—H21 | 120.1 |
Cl1i—Re—Cl3i | 89.17 (5) | C31—C21—H21 | 120.1 |
Cl1—Re—Cl3i | 90.83 (5) | C41—C31—C21 | 120.2 (4) |
Cl2Ai—Re—Cl3i | 98.3 (6) | C41—C31—H31 | 119.9 |
Cl2A—Re—Cl3i | 81.7 (6) | C21—C31—H31 | 119.9 |
Cl1i—Re—Cl3 | 90.83 (5) | C31—C41—C51 | 120.4 (4) |
Cl1—Re—Cl3 | 89.17 (5) | C31—C41—H41 | 119.8 |
Cl2Ai—Re—Cl3 | 81.7 (6) | C51—C41—H41 | 119.8 |
Cl2A—Re—Cl3 | 98.3 (6) | C61—C51—C41 | 119.8 (4) |
Cl3i—Re—Cl3 | 180.0 | C61—C51—H51 | 120.1 |
Cl1i—Re—Cl2 | 90.26 (9) | C41—C51—H51 | 120.1 |
Cl1—Re—Cl2 | 89.74 (9) | C51—C61—C11 | 120.2 (4) |
Cl2Ai—Re—Cl2 | 168.6 (8) | C51—C61—H61 | 119.9 |
Cl2A—Re—Cl2 | 11.4 (8) | C11—C61—H61 | 119.9 |
Cl3i—Re—Cl2 | 90.28 (7) | C22—C12—C62 | 119.4 (3) |
Cl3—Re—Cl2 | 89.72 (7) | C22—C12—P | 120.8 (3) |
Cl1i—Re—Cl2i | 89.74 (9) | C62—C12—P | 119.7 (3) |
Cl1—Re—Cl2i | 90.26 (9) | C32—C22—C12 | 120.3 (3) |
Cl2Ai—Re—Cl2i | 11.4 (8) | C32—C22—H22 | 119.8 |
Cl2A—Re—Cl2i | 168.6 (8) | C12—C22—H22 | 119.8 |
Cl3i—Re—Cl2i | 89.72 (7) | C22—C32—C42 | 119.6 (3) |
Cl3—Re—Cl2i | 90.28 (7) | C22—C32—H32 | 120.2 |
Cl2—Re—Cl2i | 180.000 (1) | C42—C32—H32 | 120.2 |
Cl1i—Re—Cl3Ai | 89.1 (6) | C52—C42—C32 | 120.4 (4) |
Cl1—Re—Cl3Ai | 90.9 (6) | C52—C42—H42 | 119.8 |
Cl2Ai—Re—Cl3Ai | 89.1 (6) | C32—C42—H42 | 119.8 |
Cl2A—Re—Cl3Ai | 90.9 (6) | C42—C52—C62 | 120.1 (4) |
Cl3i—Re—Cl3Ai | 9.3 (7) | C42—C52—H52 | 119.9 |
Cl3—Re—Cl3Ai | 170.7 (7) | C62—C52—H52 | 119.9 |
Cl2—Re—Cl3Ai | 99.6 (7) | C52—C62—C12 | 120.1 (3) |
Cl2i—Re—Cl3Ai | 80.4 (7) | C52—C62—H62 | 120.0 |
Cl1i—Re—Cl3A | 90.9 (6) | C12—C62—H62 | 120.0 |
Cl1—Re—Cl3A | 89.1 (6) | C63—C13—C23 | 119.6 (3) |
Cl2Ai—Re—Cl3A | 90.9 (6) | C63—C13—P | 120.3 (3) |
Cl2A—Re—Cl3A | 89.1 (6) | C23—C13—P | 120.0 (3) |
Cl3i—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 |
Cl2i—Re—Cl3A | 99.6 (7) | C23—C33—C43 | 120.1 (4) |
Cl3Ai—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) top
D—H···A | D—H | H···A | D···A | D—H···A |
C22—H22···Cl2i | 0.95 | 2.76 | 3.535 (4) | 139 |
C62—H62···Cl2ii | 0.95 | 2.78 | 3.514 (4) | 135 |
C1—H131···Cl1iii | 0.98 | 2.67 | 3.538 (4) | 147 |
C63—H63···Cl1ii | 0.95 | 2.82 | 3.404 (4) | 121 |
C1—H121···Cl3 | 0.98 | 2.82 | 3.456 (6) | 123 |
C42—H42···Cl3iv | 0.95 | 2.83 | 3.695 (4) | 152 |
C23—H23···Cl3v | 0.95 | 2.73 | 3.582 (5) | 149 |
C42—H42···Cl3Aiv | 0.95 | 2.76 | 3.66 (1) | 158 |
C23—H23···Cl3Av | 0.95 | 2.60 | 3.40 (3) | 142 |
C22—H22···Cl2Ai | 0.95 | 2.71 | 3.56 (2) | 149 |
C62—H62···Cl2Aii | 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. |