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The Re atom in the title compound, (C
12H
13N
2)
2[ReCl
6]·2H
2O, 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
CCDC reference: 242285
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (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
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]·2H2O | Z = 1 |
Mr = 805.43 | F(000) = 395 |
Triclinic, P1 | Dx = 1.874 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.991 (2) Å | Cell parameters from 2310 reflections |
b = 8.611 (2) Å | θ = 3.2–28.3° |
c = 11.007 (2) Å | µ = 4.85 mm−1 |
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 tube | 2378 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.073 |
ω scans | θmax = 28.3°, θmin = 3.2° |
Absorption correction: numerical | h = −9→10 |
Tmin = 0.870, Tmax = 0.987 | k = −11→11 |
5601 measured reflections | l = −14→14 |
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)] = 0.055 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.076 | H 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 parameters | Δρmax = 1.09 e Å−3 |
2 restraints | Δρmin = −1.23 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 | |
Re | 0.5000 | 0.5000 | 0.5000 | 0.01226 (14) | |
Cl1 | 0.3735 (2) | 0.2209 (2) | 0.40823 (16) | 0.0220 (5) | |
Cl2 | 0.2720 (2) | 0.5041 (2) | 0.61509 (16) | 0.0227 (5) | |
Cl3 | 0.6632 (2) | 0.4303 (2) | 0.66900 (16) | 0.0242 (5) | |
O | 0.4854 (6) | 0.2288 (6) | 0.1386 (4) | 0.0215 (12) | |
N1 | 0.7893 (7) | 0.0902 (7) | −0.0829 (5) | 0.0153 (14) | |
N2 | 0.6934 (8) | −0.0483 (7) | 0.1010 (6) | 0.0194 (15) | |
C1 | 0.8400 (9) | 0.1540 (9) | −0.1760 (7) | 0.0201 (18) | |
H1 | 0.7677 | 0.1137 | −0.2572 | 0.024* | |
C2 | 0.9919 (9) | 0.2761 (8) | −0.1640 (6) | 0.0166 (17) | |
H2 | 1.0216 | 0.3169 | −0.2347 | 0.020* | |
C3 | 1.0968 (9) | 0.3352 (8) | −0.0471 (6) | 0.0151 (16) | |
C4 | 1.0473 (9) | 0.2716 (8) | 0.0527 (6) | 0.0165 (17) | |
H4 | 1.1183 | 0.3092 | 0.1345 | 0.020* | |
C5 | 0.8934 (9) | 0.1526 (8) | 0.0314 (6) | 0.0124 (16) | |
C6 | 0.8287 (9) | 0.0817 (8) | 0.1347 (6) | 0.0128 (16) | |
C7 | 0.8913 (9) | 0.1466 (8) | 0.2611 (6) | 0.0199 (18) | |
H7 | 0.9861 | 0.2409 | 0.2870 | 0.024* | |
C8 | 0.8182 (9) | 0.0765 (8) | 0.3521 (7) | 0.0172 (17) | |
C9 | 0.6802 (9) | −0.0594 (8) | 0.3116 (6) | 0.0190 (17) | |
H9 | 0.6281 | −0.1110 | 0.3709 | 0.023* | |
C10 | 0.6185 (9) | −0.1199 (8) | 0.1843 (7) | 0.0212 (18) | |
H10 | 0.5225 | −0.2128 | 0.1556 | 0.025* | |
C11 | 1.2625 (9) | 0.4667 (8) | −0.0269 (7) | 0.0246 (19) | |
H11A | 1.3118 | 0.4565 | −0.1036 | 0.037* | |
H11B | 1.3469 | 0.4556 | 0.0432 | 0.037* | |
H11C | 1.2369 | 0.5738 | −0.0071 | 0.037* | |
C12 | 0.8838 (10) | 0.1509 (9) | 0.4890 (6) | 0.0257 (19) | |
H12A | 0.8166 | 0.2287 | 0.5171 | 0.039* | |
H12B | 1.0075 | 0.2078 | 0.5028 | 0.039* | |
H12C | 0.8705 | 0.0652 | 0.5369 | 0.039* | |
H1A | 0.626 (10) | −0.099 (9) | 0.014 (7) | 0.05 (3)* | |
H2A | 0.571 (9) | 0.328 (6) | 0.176 (8) | 0.080* | |
H3A | 0.437 (10) | 0.168 (9) | 0.193 (6) | 0.080* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Re | 0.0142 (3) | 0.0123 (3) | 0.0094 (2) | 0.00004 (19) | 0.0036 (2) | 0.00312 (19) |
Cl1 | 0.0271 (12) | 0.0166 (10) | 0.0183 (10) | −0.0035 (9) | 0.0071 (9) | 0.0022 (8) |
Cl2 | 0.0175 (11) | 0.0271 (11) | 0.0193 (10) | −0.0030 (9) | 0.0061 (9) | 0.0024 (9) |
Cl3 | 0.0268 (12) | 0.0274 (11) | 0.0185 (10) | 0.0071 (9) | 0.0004 (9) | 0.0077 (9) |
O | 0.020 (3) | 0.031 (3) | 0.013 (3) | −0.001 (2) | 0.005 (2) | 0.010 (2) |
N1 | 0.013 (3) | 0.022 (3) | 0.010 (3) | 0.002 (3) | −0.002 (3) | 0.007 (3) |
N2 | 0.015 (4) | 0.027 (4) | 0.016 (4) | −0.002 (3) | 0.007 (3) | 0.008 (3) |
C1 | 0.021 (5) | 0.027 (5) | 0.014 (4) | 0.008 (4) | 0.000 (3) | 0.009 (3) |
C2 | 0.018 (4) | 0.021 (4) | 0.015 (4) | 0.007 (3) | 0.006 (3) | 0.007 (3) |
C3 | 0.012 (4) | 0.018 (4) | 0.017 (4) | 0.004 (3) | 0.002 (3) | 0.006 (3) |
C4 | 0.016 (4) | 0.018 (4) | 0.016 (4) | 0.006 (3) | −0.002 (3) | 0.005 (3) |
C5 | 0.010 (4) | 0.013 (4) | 0.016 (4) | 0.005 (3) | 0.008 (3) | 0.000 (3) |
C6 | 0.015 (4) | 0.010 (4) | 0.013 (4) | 0.004 (3) | 0.007 (3) | −0.002 (3) |
C7 | 0.016 (4) | 0.021 (4) | 0.025 (4) | 0.002 (3) | 0.010 (4) | 0.008 (4) |
C8 | 0.012 (4) | 0.025 (4) | 0.023 (4) | 0.011 (3) | 0.007 (3) | 0.014 (4) |
C9 | 0.009 (4) | 0.026 (4) | 0.019 (4) | 0.000 (3) | 0.003 (3) | 0.004 (3) |
C10 | 0.025 (5) | 0.017 (4) | 0.022 (4) | 0.004 (3) | 0.009 (4) | 0.004 (3) |
C11 | 0.017 (5) | 0.028 (5) | 0.026 (5) | −0.002 (4) | 0.004 (4) | 0.006 (4) |
C12 | 0.035 (5) | 0.025 (5) | 0.019 (4) | 0.002 (4) | 0.015 (4) | 0.007 (4) |
Geometric parameters (Å, º) top
Re—Cl3 | 2.3556 (18) | C3—C11 | 1.505 (8) |
Re—Cl3i | 2.3556 (18) | C4—C5 | 1.380 (8) |
Re—Cl1i | 2.3647 (19) | C4—H4 | 0.9500 |
Re—Cl1 | 2.3647 (19) | C5—C6 | 1.492 (8) |
Re—Cl2 | 2.3695 (18) | C6—C7 | 1.375 (9) |
Re—Cl2i | 2.3695 (18) | C7—C8 | 1.397 (8) |
O—H2A | 0.95 (7) | C7—H7 | 0.9500 |
O—H3A | 0.94 (7) | C8—C9 | 1.377 (8) |
N1—C1 | 1.323 (8) | C8—C12 | 1.492 (9) |
N1—C5 | 1.348 (7) | C9—C10 | 1.378 (9) |
N2—C6 | 1.330 (8) | C9—H9 | 0.9500 |
N2—C10 | 1.337 (8) | C10—H10 | 0.9500 |
N2—H1A | 1.00 (7) | C11—H11A | 0.9800 |
C1—C2 | 1.397 (9) | C11—H11B | 0.9800 |
C1—H1 | 0.9500 | C11—H11C | 0.9800 |
C2—C3 | 1.370 (9) | C12—H12A | 0.9800 |
C2—H2 | 0.9500 | C12—H12B | 0.9800 |
C3—C4 | 1.384 (8) | C12—H12C | 0.9800 |
| | | |
Cl3—Re—Cl3i | 180.0 | C3—C4—H4 | 120.5 |
Cl3—Re—Cl1i | 89.60 (7) | N1—C5—C4 | 123.6 (6) |
Cl3i—Re—Cl1i | 90.40 (7) | N1—C5—C6 | 114.2 (5) |
Cl3—Re—Cl1 | 90.40 (7) | C4—C5—C6 | 122.1 (6) |
Cl3i—Re—Cl1 | 89.60 (7) | N2—C6—C7 | 118.2 (6) |
Cl1i—Re—Cl1 | 180.0 | N2—C6—C5 | 116.9 (6) |
Cl3—Re—Cl2 | 88.99 (6) | C7—C6—C5 | 124.8 (6) |
Cl3i—Re—Cl2 | 91.01 (6) | C6—C7—C8 | 121.2 (6) |
Cl1i—Re—Cl2 | 90.26 (7) | C6—C7—H7 | 119.4 |
Cl1—Re—Cl2 | 89.74 (7) | C8—C7—H7 | 119.4 |
Cl3—Re—Cl2i | 91.01 (6) | C9—C8—C7 | 118.0 (7) |
Cl3i—Re—Cl2i | 88.99 (6) | C9—C8—C12 | 121.2 (6) |
Cl1i—Re—Cl2i | 89.74 (7) | C7—C8—C12 | 120.7 (6) |
Cl1—Re—Cl2i | 90.26 (7) | C10—C9—C8 | 119.4 (7) |
Cl2—Re—Cl2i | 180.0 | C10—C9—H9 | 120.3 |
H2A—O—H3A | 118 (8) | C8—C9—H9 | 120.3 |
C1—N1—C5 | 115.8 (6) | N2—C10—C9 | 120.2 (7) |
C6—N2—C10 | 123.0 (6) | N2—C10—H10 | 119.9 |
C6—N2—H1A | 126 (4) | C9—C10—H10 | 119.9 |
C10—N2—H1A | 110 (4) | C3—C11—H11A | 109.5 |
N1—C1—C2 | 124.9 (6) | C3—C11—H11B | 109.5 |
N1—C1—H1 | 117.5 | H11A—C11—H11B | 109.5 |
C2—C1—H1 | 117.5 | C3—C11—H11C | 109.5 |
C3—C2—C1 | 117.9 (6) | H11A—C11—H11C | 109.5 |
C3—C2—H2 | 121.0 | H11B—C11—H11C | 109.5 |
C1—C2—H2 | 121.0 | C8—C12—H12A | 109.5 |
C2—C3—C4 | 118.7 (6) | C8—C12—H12B | 109.5 |
C2—C3—C11 | 121.0 (6) | H12A—C12—H12B | 109.5 |
C4—C3—C11 | 120.4 (6) | C8—C12—H12C | 109.5 |
C5—C4—C3 | 119.0 (6) | H12A—C12—H12C | 109.5 |
C5—C4—H4 | 120.5 | H12B—C12—H12C | 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 |
N2—H1A···Oii | 1.00 (7) | 1.82 (8) | 2.808 (8) | 168 (6) |
O—H2A···Cl2i | 0.95 (7) | 2.47 (8) | 3.266 (5) | 141 (5) |
O—H3A···Cl1 | 0.94 (7) | 2.48 (7) | 3.231 (5) | 138 (6) |
C9—H9···Cl1iii | 0.95 | 2.77 | 3.650 (7) | 155 |
C12—H12A···Cl3 | 0.98 | 2.79 | 3.733 (8) | 162 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y, −z; (iii) −x+1, −y, −z+1. |
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