Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
The Re atom in the title compound, (C12H13N2)2[ReCl6]·2H2O, lies on a crystallographic centre of inversion. The structure consists of discrete anions, cations and solvent water mol­ecules. The solvent water mol­ecule and the pyridinium group form intermolecular O—H...Cl and N—H...O hydrogen bonds, respectively, giving a three-dimensional hydrogen-bonded structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804012255/lh6215sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804012255/lh6215Isup2.hkl
Contains datablock I

CCDC reference: 242285

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.010 Å
  • R factor = 0.055
  • wR factor = 0.075
  • Data-to-parameter ratio = 17.2

checkCIF/PLATON results

No syntax errors found



Alert level C ABSTY02_ALERT_1_C An _exptl_absorpt_correction_type has been given without a literature citation. This should be contained in the _exptl_absorpt_process_details field. Absorption correction given as numerical PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 10
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 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: KM-4-CCD Software (Oxford Diffraction, 1995-2004); cell refinement: KM-4-CCD Software; data reduction: KM-4-CCD Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

Bis(4,4'-dimethyl-2,2'-bipyridinium) hexachlororhenium(IV) dihydrate top
Crystal data top
(C12H13N2)2[ReCl6]·2H2OZ = 1
Mr = 805.43F(000) = 395
Triclinic, P1Dx = 1.874 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.991 (2) ÅCell parameters from 2310 reflections
b = 8.611 (2) Åθ = 3.2–28.3°
c = 11.007 (2) ŵ = 4.85 mm1
α = 100.50 (3)°T = 100 K
β = 98.46 (3)°Prism, yellow
γ = 102.37 (3)°0.08 × 0.05 × 0.05 mm
V = 713.6 (3) Å3
Data collection top
KM-4-CCD
diffractometer
3107 independent reflections
Radiation source: fine-focus sealed tube2378 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.073
ω scansθmax = 28.3°, θmin = 3.2°
Absorption correction: numericalh = 910
Tmin = 0.870, Tmax = 0.987k = 1111
5601 measured reflectionsl = 1414
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)] = 0.055Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.076H atoms treated by a mixture of independent and constrained refinement
S = 0.95 w = 1/[σ2(Fo2) + (0.0147P)2]
where P = (Fo2 + 2Fc2)/3
3107 reflections(Δ/σ)max < 0.001
181 parametersΔρmax = 1.09 e Å3
2 restraintsΔρmin = 1.23 e Å3
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
xyzUiso*/Ueq
Re0.50000.50000.50000.01226 (14)
Cl10.3735 (2)0.2209 (2)0.40823 (16)0.0220 (5)
Cl20.2720 (2)0.5041 (2)0.61509 (16)0.0227 (5)
Cl30.6632 (2)0.4303 (2)0.66900 (16)0.0242 (5)
O0.4854 (6)0.2288 (6)0.1386 (4)0.0215 (12)
N10.7893 (7)0.0902 (7)0.0829 (5)0.0153 (14)
N20.6934 (8)0.0483 (7)0.1010 (6)0.0194 (15)
C10.8400 (9)0.1540 (9)0.1760 (7)0.0201 (18)
H10.76770.11370.25720.024*
C20.9919 (9)0.2761 (8)0.1640 (6)0.0166 (17)
H21.02160.31690.23470.020*
C31.0968 (9)0.3352 (8)0.0471 (6)0.0151 (16)
C41.0473 (9)0.2716 (8)0.0527 (6)0.0165 (17)
H41.11830.30920.13450.020*
C50.8934 (9)0.1526 (8)0.0314 (6)0.0124 (16)
C60.8287 (9)0.0817 (8)0.1347 (6)0.0128 (16)
C70.8913 (9)0.1466 (8)0.2611 (6)0.0199 (18)
H70.98610.24090.28700.024*
C80.8182 (9)0.0765 (8)0.3521 (7)0.0172 (17)
C90.6802 (9)0.0594 (8)0.3116 (6)0.0190 (17)
H90.62810.11100.37090.023*
C100.6185 (9)0.1199 (8)0.1843 (7)0.0212 (18)
H100.52250.21280.15560.025*
C111.2625 (9)0.4667 (8)0.0269 (7)0.0246 (19)
H11A1.31180.45650.10360.037*
H11B1.34690.45560.04320.037*
H11C1.23690.57380.00710.037*
C120.8838 (10)0.1509 (9)0.4890 (6)0.0257 (19)
H12A0.81660.22870.51710.039*
H12B1.00750.20780.50280.039*
H12C0.87050.06520.53690.039*
H1A0.626 (10)0.099 (9)0.014 (7)0.05 (3)*
H2A0.571 (9)0.328 (6)0.176 (8)0.080*
H3A0.437 (10)0.168 (9)0.193 (6)0.080*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Re0.0142 (3)0.0123 (3)0.0094 (2)0.00004 (19)0.0036 (2)0.00312 (19)
Cl10.0271 (12)0.0166 (10)0.0183 (10)0.0035 (9)0.0071 (9)0.0022 (8)
Cl20.0175 (11)0.0271 (11)0.0193 (10)0.0030 (9)0.0061 (9)0.0024 (9)
Cl30.0268 (12)0.0274 (11)0.0185 (10)0.0071 (9)0.0004 (9)0.0077 (9)
O0.020 (3)0.031 (3)0.013 (3)0.001 (2)0.005 (2)0.010 (2)
N10.013 (3)0.022 (3)0.010 (3)0.002 (3)0.002 (3)0.007 (3)
N20.015 (4)0.027 (4)0.016 (4)0.002 (3)0.007 (3)0.008 (3)
C10.021 (5)0.027 (5)0.014 (4)0.008 (4)0.000 (3)0.009 (3)
C20.018 (4)0.021 (4)0.015 (4)0.007 (3)0.006 (3)0.007 (3)
C30.012 (4)0.018 (4)0.017 (4)0.004 (3)0.002 (3)0.006 (3)
C40.016 (4)0.018 (4)0.016 (4)0.006 (3)0.002 (3)0.005 (3)
C50.010 (4)0.013 (4)0.016 (4)0.005 (3)0.008 (3)0.000 (3)
C60.015 (4)0.010 (4)0.013 (4)0.004 (3)0.007 (3)0.002 (3)
C70.016 (4)0.021 (4)0.025 (4)0.002 (3)0.010 (4)0.008 (4)
C80.012 (4)0.025 (4)0.023 (4)0.011 (3)0.007 (3)0.014 (4)
C90.009 (4)0.026 (4)0.019 (4)0.000 (3)0.003 (3)0.004 (3)
C100.025 (5)0.017 (4)0.022 (4)0.004 (3)0.009 (4)0.004 (3)
C110.017 (5)0.028 (5)0.026 (5)0.002 (4)0.004 (4)0.006 (4)
C120.035 (5)0.025 (5)0.019 (4)0.002 (4)0.015 (4)0.007 (4)
Geometric parameters (Å, º) top
Re—Cl32.3556 (18)C3—C111.505 (8)
Re—Cl3i2.3556 (18)C4—C51.380 (8)
Re—Cl1i2.3647 (19)C4—H40.9500
Re—Cl12.3647 (19)C5—C61.492 (8)
Re—Cl22.3695 (18)C6—C71.375 (9)
Re—Cl2i2.3695 (18)C7—C81.397 (8)
O—H2A0.95 (7)C7—H70.9500
O—H3A0.94 (7)C8—C91.377 (8)
N1—C11.323 (8)C8—C121.492 (9)
N1—C51.348 (7)C9—C101.378 (9)
N2—C61.330 (8)C9—H90.9500
N2—C101.337 (8)C10—H100.9500
N2—H1A1.00 (7)C11—H11A0.9800
C1—C21.397 (9)C11—H11B0.9800
C1—H10.9500C11—H11C0.9800
C2—C31.370 (9)C12—H12A0.9800
C2—H20.9500C12—H12B0.9800
C3—C41.384 (8)C12—H12C0.9800
Cl3—Re—Cl3i180.0C3—C4—H4120.5
Cl3—Re—Cl1i89.60 (7)N1—C5—C4123.6 (6)
Cl3i—Re—Cl1i90.40 (7)N1—C5—C6114.2 (5)
Cl3—Re—Cl190.40 (7)C4—C5—C6122.1 (6)
Cl3i—Re—Cl189.60 (7)N2—C6—C7118.2 (6)
Cl1i—Re—Cl1180.0N2—C6—C5116.9 (6)
Cl3—Re—Cl288.99 (6)C7—C6—C5124.8 (6)
Cl3i—Re—Cl291.01 (6)C6—C7—C8121.2 (6)
Cl1i—Re—Cl290.26 (7)C6—C7—H7119.4
Cl1—Re—Cl289.74 (7)C8—C7—H7119.4
Cl3—Re—Cl2i91.01 (6)C9—C8—C7118.0 (7)
Cl3i—Re—Cl2i88.99 (6)C9—C8—C12121.2 (6)
Cl1i—Re—Cl2i89.74 (7)C7—C8—C12120.7 (6)
Cl1—Re—Cl2i90.26 (7)C10—C9—C8119.4 (7)
Cl2—Re—Cl2i180.0C10—C9—H9120.3
H2A—O—H3A118 (8)C8—C9—H9120.3
C1—N1—C5115.8 (6)N2—C10—C9120.2 (7)
C6—N2—C10123.0 (6)N2—C10—H10119.9
C6—N2—H1A126 (4)C9—C10—H10119.9
C10—N2—H1A110 (4)C3—C11—H11A109.5
N1—C1—C2124.9 (6)C3—C11—H11B109.5
N1—C1—H1117.5H11A—C11—H11B109.5
C2—C1—H1117.5C3—C11—H11C109.5
C3—C2—C1117.9 (6)H11A—C11—H11C109.5
C3—C2—H2121.0H11B—C11—H11C109.5
C1—C2—H2121.0C8—C12—H12A109.5
C2—C3—C4118.7 (6)C8—C12—H12B109.5
C2—C3—C11121.0 (6)H12A—C12—H12B109.5
C4—C3—C11120.4 (6)C8—C12—H12C109.5
C5—C4—C3119.0 (6)H12A—C12—H12C109.5
C5—C4—H4120.5H12B—C12—H12C109.5
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H1A···Oii1.00 (7)1.82 (8)2.808 (8)168 (6)
O—H2A···Cl2i0.95 (7)2.47 (8)3.266 (5)141 (5)
O—H3A···Cl10.94 (7)2.48 (7)3.231 (5)138 (6)
C9—H9···Cl1iii0.952.773.650 (7)155
C12—H12A···Cl30.982.793.733 (8)162
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y, z; (iii) x+1, y, z+1.
 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds