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At 173 K, the structure of the cyclic `triphosphenium' salt, bis­[1,1,3,3-tetra­phenyl-1,3,2-triphospho­lenylium] hexa­chloro­stannate(IV) dichloro­methane solvate, (C26H24P3)2[SnCl6]·2CH2Cl2, contains one cation, one solvent mol­ecule and half of a centrosymmetric hexa­chloro­stannate dianion in the asymmetric unit. There are no unusually short anion-cation distances and the structures of the component ions are comparable to those that have been reported previously.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806016345/lh2065sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806016345/lh2065Isup2.hkl
Contains datablock I

CCDC reference: 610839

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.008 Å
  • R factor = 0.054
  • wR factor = 0.112
  • Data-to-parameter ratio = 20.7

checkCIF/PLATON results

No syntax errors found



Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.612 0.807 Tmin(prime) and Tmax expected: 0.802 0.807 RR(prime) = 0.763 Please check that your absorption correction is appropriate. PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.76 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.08 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C323
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 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 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT-Plus (Bruker, 1997); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL, PLATON (Spek, 2003) and WinGX (Farrugia, 1999).

bis[1,1,3,3-tetraphenyl-1,3,2-triphospholenylium] hexachlorostannate dichloromethane solvate top
Crystal data top
(C26H24P3)2[SnCl6]·2CH2Cl2Z = 1
Mr = 1359.99F(000) = 686
Triclinic, P1Dx = 1.509 Mg m3
Hall symbol: -P 1Melting point: 230 K
a = 10.8589 (4) ÅMo Kα radiation, λ = 0.71073 Å
b = 11.5303 (5) ÅCell parameters from 9881 reflections
c = 13.0841 (5) Åθ = 2.4–27.5°
α = 68.777 (1)°µ = 1.07 mm1
β = 79.774 (1)°T = 173 K
γ = 81.332 (1)°Prism, colourless
V = 1496.16 (10) Å30.2 × 0.2 × 0.2 mm
Data collection top
Bruker APEX-CCD
diffractometer
6663 independent reflections
Radiation source: fine-focus sealed tube5978 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
φ and ω scansθmax = 27.5°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 1414
Tmin = 0.612, Tmax = 0.807k = 1414
13358 measured reflectionsl = 1616
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.054Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.112H-atom parameters constrained
S = 1.23 w = 1/[σ2(Fo2) + 2.7128P]
where P = (Fo2 + 2Fc2)/3
6663 reflections(Δ/σ)max < 0.001
322 parametersΔρmax = 0.99 e Å3
0 restraintsΔρmin = 1.30 e Å3
Special details top

Experimental. The data crystal was coated in mineral oil and placed rapidly in the cold nitrogen stream of the Kryoflex low-temperature device.

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
xyzUiso*/Ueq
C40.7732 (4)0.4236 (4)0.7364 (3)0.0325 (9)
H4A0.75810.40760.67050.039*
H4B0.69240.42370.78540.039*
C50.8280 (4)0.5493 (4)0.7019 (3)0.0341 (9)
H5A0.76410.61920.67260.041*
H5B0.90130.55450.64390.041*
C100.6085 (6)0.0732 (5)0.5760 (5)0.0682 (17)
H10A0.60890.07930.49850.082*
H10B0.59100.15860.57930.082*
C1110.7353 (4)0.5960 (4)0.9080 (4)0.0367 (9)
C1120.6409 (5)0.6846 (5)0.8590 (4)0.0487 (12)
H1120.64750.72280.78090.058*
C1130.5373 (5)0.7160 (5)0.9261 (5)0.0629 (16)
H1130.47140.77440.89370.076*
C1140.5298 (6)0.6626 (6)1.0395 (5)0.0667 (18)
H1140.46010.68711.08490.080*
C1150.6214 (6)0.5751 (6)1.0875 (5)0.0659 (17)
H1150.61400.53741.16570.079*
C1160.7248 (5)0.5413 (5)1.0224 (4)0.0495 (12)
H1160.78880.48071.05590.059*
C1210.9780 (4)0.6792 (4)0.7876 (3)0.0305 (8)
C1220.9378 (4)0.7916 (4)0.8055 (4)0.0386 (10)
H1220.85530.80490.84070.046*
C1231.0198 (5)0.8838 (4)0.7714 (4)0.0449 (11)
H1230.99300.96090.78320.054*
C1241.1400 (5)0.8647 (5)0.7205 (4)0.0494 (12)
H1241.19500.92900.69670.059*
C1251.1808 (5)0.7523 (5)0.7040 (4)0.0477 (12)
H1251.26400.73850.67020.057*
C1261.0994 (4)0.6605 (4)0.7373 (4)0.0392 (10)
H1261.12680.58350.72560.047*
C3110.9992 (4)0.2630 (4)0.7047 (3)0.0319 (9)
C3121.1275 (4)0.2647 (4)0.7027 (4)0.0417 (10)
H3121.15680.29050.75460.050*
C3131.2123 (4)0.2288 (4)0.6251 (4)0.0458 (11)
H3131.29990.22850.62470.055*
C3141.1705 (5)0.1935 (4)0.5488 (4)0.0471 (12)
H3141.22940.16850.49590.056*
C3151.0437 (5)0.1940 (4)0.5484 (4)0.0449 (11)
H3151.01530.17030.49470.054*
C3160.9578 (4)0.2289 (4)0.6257 (4)0.0396 (10)
H3160.87040.22960.62500.047*
C3210.8097 (4)0.1671 (4)0.8940 (4)0.0343 (9)
C3220.8324 (6)0.1071 (5)1.0018 (5)0.0678 (18)
H3220.88760.13861.03210.081*
C3230.7743 (8)0.0008 (6)1.0654 (6)0.094 (3)
H3230.79050.04081.13960.113*
C3240.6942 (6)0.0459 (5)1.0244 (5)0.0663 (16)
H3240.65500.11921.06970.080*
C3250.6706 (5)0.0129 (5)0.9179 (5)0.0543 (13)
H3250.61550.02000.88870.065*
C3260.7266 (4)0.1207 (4)0.8519 (4)0.0441 (11)
H3260.70840.16260.77830.053*
P10.87535 (10)0.55700 (10)0.82541 (8)0.0298 (2)
P20.97116 (12)0.37999 (11)0.90384 (10)0.0390 (3)
P30.88734 (10)0.30512 (10)0.80886 (9)0.0303 (2)
Cl10.72393 (10)0.45236 (12)0.46420 (9)0.0436 (3)
Cl20.49496 (11)0.32627 (11)0.67565 (9)0.0435 (3)
Cl30.46915 (10)0.36116 (11)0.40496 (9)0.0391 (2)
Cl40.75521 (15)0.00966 (15)0.61663 (14)0.0691 (4)
Cl50.48949 (17)0.01870 (19)0.66136 (16)0.0897 (6)
Sn10.50000.50000.50000.03227 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C40.032 (2)0.035 (2)0.031 (2)0.0001 (17)0.0094 (16)0.0106 (17)
C50.035 (2)0.035 (2)0.030 (2)0.0018 (17)0.0093 (17)0.0092 (17)
C100.084 (5)0.055 (3)0.070 (4)0.004 (3)0.033 (3)0.020 (3)
C1110.038 (2)0.039 (2)0.035 (2)0.0116 (18)0.0014 (17)0.0149 (19)
C1120.041 (3)0.046 (3)0.050 (3)0.004 (2)0.000 (2)0.012 (2)
C1130.043 (3)0.056 (3)0.083 (4)0.000 (2)0.010 (3)0.025 (3)
C1140.065 (4)0.059 (4)0.072 (4)0.020 (3)0.034 (3)0.033 (3)
C1150.078 (4)0.068 (4)0.045 (3)0.009 (3)0.018 (3)0.024 (3)
C1160.054 (3)0.053 (3)0.039 (3)0.009 (2)0.003 (2)0.016 (2)
C1210.032 (2)0.031 (2)0.029 (2)0.0031 (16)0.0052 (16)0.0102 (16)
C1220.041 (3)0.032 (2)0.042 (2)0.0020 (18)0.0077 (19)0.0103 (19)
C1230.054 (3)0.030 (2)0.054 (3)0.005 (2)0.016 (2)0.013 (2)
C1240.047 (3)0.044 (3)0.054 (3)0.017 (2)0.008 (2)0.007 (2)
C1250.039 (3)0.045 (3)0.050 (3)0.010 (2)0.002 (2)0.008 (2)
C1260.040 (3)0.039 (2)0.038 (2)0.0019 (19)0.0001 (18)0.0164 (19)
C3110.036 (2)0.0252 (19)0.032 (2)0.0008 (16)0.0066 (16)0.0065 (16)
C3120.036 (2)0.041 (2)0.047 (3)0.0003 (19)0.0069 (19)0.014 (2)
C3130.034 (2)0.047 (3)0.050 (3)0.002 (2)0.001 (2)0.012 (2)
C3140.050 (3)0.038 (2)0.042 (3)0.001 (2)0.010 (2)0.009 (2)
C3150.054 (3)0.044 (3)0.037 (2)0.007 (2)0.004 (2)0.015 (2)
C3160.042 (3)0.039 (2)0.039 (2)0.0029 (19)0.0079 (19)0.015 (2)
C3210.032 (2)0.030 (2)0.041 (2)0.0039 (17)0.0016 (17)0.0124 (18)
C3220.092 (5)0.051 (3)0.053 (3)0.032 (3)0.036 (3)0.013 (3)
C3230.136 (7)0.069 (4)0.062 (4)0.049 (4)0.042 (4)0.024 (3)
C3240.072 (4)0.043 (3)0.073 (4)0.026 (3)0.003 (3)0.002 (3)
C3250.051 (3)0.053 (3)0.060 (3)0.024 (2)0.004 (2)0.020 (3)
C3260.044 (3)0.046 (3)0.044 (3)0.014 (2)0.009 (2)0.013 (2)
P10.0332 (6)0.0288 (5)0.0271 (5)0.0031 (4)0.0053 (4)0.0086 (4)
P20.0499 (7)0.0309 (6)0.0402 (6)0.0002 (5)0.0232 (5)0.0104 (5)
P30.0324 (6)0.0280 (5)0.0309 (5)0.0034 (4)0.0085 (4)0.0084 (4)
Cl10.0312 (5)0.0625 (7)0.0386 (6)0.0070 (5)0.0050 (4)0.0233 (5)
Cl20.0503 (7)0.0477 (6)0.0307 (5)0.0045 (5)0.0118 (5)0.0083 (5)
Cl30.0391 (6)0.0468 (6)0.0375 (5)0.0034 (5)0.0108 (4)0.0219 (5)
Cl40.0712 (10)0.0722 (10)0.0785 (10)0.0010 (8)0.0232 (8)0.0402 (8)
Cl50.0694 (11)0.1004 (14)0.0884 (13)0.0020 (10)0.0214 (9)0.0171 (11)
Sn10.0299 (2)0.0412 (2)0.0269 (2)0.00391 (16)0.00710 (15)0.01438 (17)
Geometric parameters (Å, º) top
C4—C51.533 (6)C126—H1260.9500
C4—P31.809 (4)C311—C3121.392 (6)
C4—H4A0.9900C311—C3161.392 (6)
C4—H4B0.9900C311—P31.812 (4)
C5—P11.815 (4)C312—C3131.380 (6)
C5—H5A0.9900C312—H3120.9500
C5—H5B0.9900C313—C3141.371 (7)
C10—Cl41.739 (6)C313—H3130.9500
C10—Cl51.756 (7)C314—C3151.378 (7)
C10—H10A0.9900C314—H3140.9500
C10—H10B0.9900C315—C3161.378 (6)
C111—C1161.390 (6)C315—H3150.9500
C111—C1121.395 (6)C316—H3160.9500
C111—P11.801 (4)C321—C3221.377 (6)
C112—C1131.386 (7)C321—C3261.392 (6)
C112—H1120.9500C321—P31.809 (4)
C113—C1141.378 (8)C322—C3231.379 (7)
C113—H1130.9500C322—H3220.9500
C114—C1151.364 (8)C323—C3241.360 (8)
C114—H1140.9500C323—H3230.9500
C115—C1161.381 (7)C324—C3251.363 (8)
C115—H1150.9500C324—H3240.9500
C116—H1160.9500C325—C3261.387 (6)
C121—C1261.388 (6)C325—H3250.9500
C121—C1221.392 (6)C326—H3260.9500
C121—P11.801 (4)P1—P22.1269 (15)
C122—C1231.387 (6)P2—P32.1290 (15)
C122—H1220.9500Cl1—Sn12.4110 (11)
C123—C1241.381 (7)Cl2—Sn12.4398 (11)
C123—H1230.9500Cl3—Sn12.4438 (10)
C124—C1251.385 (7)Sn1—Cl1i2.4110 (11)
C124—H1240.9500Sn1—Cl2i2.4398 (11)
C125—C1261.379 (6)Sn1—Cl3i2.4439 (10)
C125—H1250.9500
C5—C4—P3106.8 (3)C311—C312—H312120.0
C5—C4—H4A110.4C314—C313—C312120.3 (5)
P3—C4—H4A110.4C314—C313—H313119.9
C5—C4—H4B110.4C312—C313—H313119.9
P3—C4—H4B110.4C313—C314—C315120.4 (4)
H4A—C4—H4B108.6C313—C314—H314119.8
C4—C5—P1106.4 (3)C315—C314—H314119.8
C4—C5—H5A110.4C314—C315—C316120.1 (5)
P1—C5—H5A110.4C314—C315—H315120.0
C4—C5—H5B110.4C316—C315—H315120.0
P1—C5—H5B110.4C315—C316—C311120.1 (4)
H5A—C5—H5B108.6C315—C316—H316120.0
Cl4—C10—Cl5111.3 (3)C311—C316—H316120.0
Cl4—C10—H10A109.4C322—C321—C326119.4 (4)
Cl5—C10—H10A109.4C322—C321—P3119.8 (4)
Cl4—C10—H10B109.4C326—C321—P3120.8 (3)
Cl5—C10—H10B109.4C321—C322—C323119.3 (5)
H10A—C10—H10B108.0C321—C322—H322120.3
C116—C111—C112119.9 (4)C323—C322—H322120.3
C116—C111—P1119.0 (4)C324—C323—C322121.6 (6)
C112—C111—P1121.0 (3)C324—C323—H323119.2
C113—C112—C111119.1 (5)C322—C323—H323119.2
C113—C112—H112120.5C323—C324—C325119.6 (5)
C111—C112—H112120.5C323—C324—H324120.2
C114—C113—C112120.2 (6)C325—C324—H324120.2
C114—C113—H113119.9C324—C325—C326120.3 (5)
C112—C113—H113119.9C324—C325—H325119.9
C115—C114—C113120.8 (5)C326—C325—H325119.9
C115—C114—H114119.6C325—C326—C321119.8 (5)
C113—C114—H114119.6C325—C326—H326120.1
C114—C115—C116120.0 (5)C321—C326—H326120.1
C114—C115—H115120.0C111—P1—C121108.44 (19)
C116—C115—H115120.0C111—P1—C5107.4 (2)
C115—C116—C111120.0 (5)C121—P1—C5109.73 (19)
C115—C116—H116120.0C111—P1—P2114.07 (15)
C111—C116—H116120.0C121—P1—P2110.55 (14)
C126—C121—C122119.7 (4)C5—P1—P2106.54 (14)
C126—C121—P1118.5 (3)P1—P2—P388.56 (6)
C122—C121—P1121.8 (3)C4—P3—C321109.0 (2)
C123—C122—C121119.2 (4)C4—P3—C311106.83 (19)
C123—C122—H122120.4C321—P3—C311107.15 (19)
C121—C122—H122120.4C4—P3—P2108.29 (14)
C124—C123—C122120.6 (4)C321—P3—P2112.26 (15)
C124—C123—H123119.7C311—P3—P2113.09 (15)
C122—C123—H123119.7Cl1i—Sn1—Cl1180.0
C123—C124—C125120.3 (4)Cl1i—Sn1—Cl290.39 (4)
C123—C124—H124119.9Cl1—Sn1—Cl289.61 (4)
C125—C124—H124119.9Cl1i—Sn1—Cl2i89.61 (4)
C126—C125—C124119.3 (5)Cl1—Sn1—Cl2i90.39 (4)
C126—C125—H125120.3Cl2—Sn1—Cl2i180.0
C124—C125—H125120.3Cl1i—Sn1—Cl390.95 (4)
C125—C126—C121120.9 (4)Cl1—Sn1—Cl389.05 (4)
C125—C126—H126119.6Cl2—Sn1—Cl390.70 (4)
C121—C126—H126119.6Cl2i—Sn1—Cl389.30 (4)
C312—C311—C316119.3 (4)Cl1i—Sn1—Cl3i89.05 (4)
C312—C311—P3120.3 (3)Cl1—Sn1—Cl3i90.95 (4)
C316—C311—P3120.4 (3)Cl2—Sn1—Cl3i89.30 (4)
C313—C312—C311119.9 (4)Cl2i—Sn1—Cl3i90.70 (4)
C313—C312—H312120.0Cl3—Sn1—Cl3i180.00 (3)
P3—C4—C5—P150.9 (3)C116—C111—P1—C5142.6 (4)
C116—C111—C112—C1130.4 (7)C112—C111—P1—C540.7 (4)
P1—C111—C112—C113177.0 (4)C116—C111—P1—P224.8 (4)
C111—C112—C113—C1141.7 (8)C112—C111—P1—P2158.5 (3)
C112—C113—C114—C1152.4 (9)C126—C121—P1—C111170.8 (3)
C113—C114—C115—C1161.7 (9)C122—C121—P1—C11110.4 (4)
C114—C115—C116—C1110.4 (9)C126—C121—P1—C572.2 (4)
C112—C111—C116—C1150.3 (7)C122—C121—P1—C5106.6 (4)
P1—C111—C116—C115176.4 (4)C126—C121—P1—P245.1 (4)
C126—C121—C122—C1230.8 (6)C122—C121—P1—P2136.2 (3)
P1—C121—C122—C123177.9 (3)C4—C5—P1—C11177.7 (3)
C121—C122—C123—C1240.2 (7)C4—C5—P1—C121164.6 (3)
C122—C123—C124—C1250.7 (8)C4—C5—P1—P244.9 (3)
C123—C124—C125—C1261.1 (8)C111—P1—P2—P3100.33 (16)
C124—C125—C126—C1210.5 (7)C121—P1—P2—P3137.16 (14)
C122—C121—C126—C1250.5 (7)C5—P1—P2—P317.98 (16)
P1—C121—C126—C125178.3 (4)C5—C4—P3—C321159.3 (3)
C316—C311—C312—C3132.1 (6)C5—C4—P3—C31185.2 (3)
P3—C311—C312—C313178.0 (3)C5—C4—P3—P236.9 (3)
C311—C312—C313—C3141.1 (7)C322—C321—P3—C4134.1 (4)
C312—C313—C314—C3150.3 (7)C326—C321—P3—C445.8 (4)
C313—C314—C315—C3160.7 (7)C322—C321—P3—C311110.6 (4)
C314—C315—C316—C3110.3 (7)C326—C321—P3—C31169.5 (4)
C312—C311—C316—C3151.7 (6)C322—C321—P3—P214.1 (5)
P3—C311—C316—C315178.4 (3)C326—C321—P3—P2165.8 (3)
C326—C321—C322—C3231.2 (9)C312—C311—P3—C4127.7 (3)
P3—C321—C322—C323178.9 (6)C316—C311—P3—C452.1 (4)
C321—C322—C323—C3240.4 (12)C312—C311—P3—C321115.5 (4)
C322—C323—C324—C3250.2 (12)C316—C311—P3—C32164.6 (4)
C323—C324—C325—C3260.7 (10)C312—C311—P3—P28.7 (4)
C324—C325—C326—C3211.5 (8)C316—C311—P3—P2171.2 (3)
C322—C321—C326—C3251.7 (8)P1—P2—P3—C47.71 (16)
P3—C321—C326—C325178.4 (4)P1—P2—P3—C321128.13 (15)
C116—C111—P1—C12198.8 (4)P1—P2—P3—C311110.48 (15)
C112—C111—P1—C12177.8 (4)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C4—H4A···Cl10.992.643.585 (4)159
C10—H10B···Cl20.992.673.583 (6)154
C313—H313···Cl2ii0.952.823.663 (5)148
Symmetry code: (ii) x+1, y, z.
 

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