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In the title complex, (C12H9N2)[ReO4], the ions are connected together via hydrogen bonds. The crystal structure comprises alternating layers of cations and anions aligned along the b-axis direction.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806016771/tk2028sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806016771/tk2028Isup2.hkl
Contains datablock I

CCDC reference: 610911

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.026
  • wR factor = 0.060
  • Data-to-parameter ratio = 15.9

checkCIF/PLATON results

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Alert level C PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 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 0 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, 2001); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: PLATON.

4,7-phenanthrolin-4-ium perrhenate top
Crystal data top
(C12H9N2)[ReO4]F(000) = 808
Mr = 431.41Dx = 2.334 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3551 reflections
a = 7.8374 (16) Åθ = 1.0–27.5°
b = 20.840 (4) ŵ = 9.91 mm1
c = 7.5280 (15) ÅT = 293 K
β = 92.95 (3)°Block, yellow
V = 1227.9 (4) Å30.22 × 0.10 × 0.08 mm
Z = 4
Data collection top
Bruker SMART CCD area-detector
diffractometer
2815 independent reflections
Radiation source: fine-focus sealed tube2267 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
φ and ω scansθmax = 27.5°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
h = 1010
Tmin = 0.32, Tmax = 0.45k = 270
11638 measured reflectionsl = 09
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.026H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.060 w = 1/[σ2(Fo2) + (0.0193P)2 + 1.693P]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max = 0.001
2815 reflectionsΔρmax = 0.78 e Å3
177 parametersΔρmin = 1.09 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00182 (17)
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
C10.3180 (6)0.1092 (3)0.2929 (7)0.0460 (11)
H10.25820.07120.27160.055*
C20.2417 (6)0.1673 (3)0.2541 (7)0.0470 (12)
H20.13100.16880.20330.056*
C30.3294 (6)0.2229 (3)0.2906 (7)0.0436 (11)
H30.27700.26230.26750.052*
C40.4982 (5)0.2210 (2)0.3626 (6)0.0329 (9)
C50.6002 (6)0.2779 (2)0.4030 (6)0.0337 (9)
C60.5400 (7)0.3402 (2)0.3781 (7)0.0451 (12)
H60.42810.34750.33580.054*
C70.6469 (7)0.3907 (3)0.4166 (8)0.0542 (13)
H70.60870.43270.40130.065*
C80.8129 (7)0.3783 (3)0.4785 (8)0.0545 (14)
H80.88470.41320.50210.065*
C90.7704 (6)0.2697 (2)0.4687 (6)0.0374 (10)
C100.8386 (6)0.2069 (3)0.4980 (7)0.0431 (12)
H100.95150.20240.54060.052*
C110.7435 (6)0.1542 (2)0.4653 (7)0.0420 (11)
H110.78900.11360.48800.050*
C120.5733 (6)0.1610 (2)0.3960 (6)0.0331 (9)
N10.4769 (6)0.1077 (2)0.3605 (6)0.0405 (9)
H90.518 (6)0.074 (2)0.370 (6)0.028 (13)*
N20.8756 (5)0.3203 (2)0.5063 (6)0.0480 (11)
O10.0076 (6)0.5055 (3)0.2054 (7)0.0957 (18)
O20.2420 (7)0.4595 (2)0.4438 (6)0.0739 (13)
O30.1469 (6)0.3855 (2)0.1502 (6)0.0724 (13)
O40.3316 (5)0.49769 (19)0.1035 (6)0.0638 (12)
Re10.17550 (2)0.462192 (10)0.22432 (3)0.04193 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.043 (3)0.043 (3)0.051 (3)0.012 (2)0.000 (2)0.003 (2)
C20.031 (2)0.053 (3)0.056 (3)0.002 (2)0.007 (2)0.001 (3)
C30.034 (2)0.042 (3)0.053 (3)0.004 (2)0.006 (2)0.005 (2)
C40.030 (2)0.034 (2)0.035 (2)0.0010 (18)0.0001 (18)0.0020 (19)
C50.033 (2)0.032 (2)0.037 (2)0.0004 (18)0.0034 (18)0.0016 (19)
C60.044 (3)0.038 (3)0.053 (3)0.006 (2)0.001 (2)0.001 (2)
C70.061 (3)0.033 (3)0.069 (4)0.000 (3)0.001 (3)0.002 (3)
C80.057 (3)0.041 (3)0.066 (4)0.016 (3)0.005 (3)0.011 (3)
C90.033 (2)0.044 (3)0.035 (2)0.003 (2)0.0027 (19)0.007 (2)
C100.030 (2)0.050 (3)0.049 (3)0.005 (2)0.000 (2)0.001 (2)
C110.041 (3)0.034 (2)0.050 (3)0.009 (2)0.004 (2)0.001 (2)
C120.031 (2)0.034 (2)0.034 (2)0.0012 (18)0.0034 (18)0.0030 (19)
N10.044 (2)0.028 (2)0.049 (2)0.002 (2)0.0028 (19)0.0006 (19)
N20.040 (2)0.051 (3)0.053 (3)0.008 (2)0.001 (2)0.009 (2)
O10.067 (3)0.146 (5)0.075 (3)0.056 (3)0.011 (3)0.002 (3)
O20.092 (3)0.072 (3)0.056 (2)0.014 (3)0.013 (2)0.002 (2)
O30.087 (3)0.054 (2)0.078 (3)0.031 (2)0.016 (2)0.013 (2)
O40.062 (3)0.045 (2)0.087 (3)0.013 (2)0.028 (2)0.004 (2)
Re10.03602 (12)0.03890 (12)0.05083 (13)0.00132 (10)0.00177 (8)0.00112 (11)
Geometric parameters (Å, º) top
C1—N11.321 (6)C8—N21.317 (7)
C1—C21.376 (8)C8—H80.9300
C1—H10.9300C9—N21.360 (6)
C2—C31.368 (7)C9—C101.427 (7)
C2—H20.9300C10—C111.344 (7)
C3—C41.404 (6)C10—H100.9300
C3—H30.9300C11—C121.414 (6)
C4—C121.398 (6)C11—H110.9300
C4—C51.455 (6)C12—N11.362 (6)
C5—C61.391 (6)N1—H90.77 (5)
C5—C91.409 (6)Re1—O11.696 (5)
C6—C71.367 (7)Re1—O21.708 (4)
C6—H60.9300Re1—O31.704 (4)
C7—C81.383 (8)Re1—O41.728 (4)
C7—H70.9300
N1—C1—C2119.5 (5)C7—C8—H8117.9
N1—C1—H1120.2N2—C9—C5122.1 (5)
C2—C1—H1120.2N2—C9—C10117.5 (4)
C3—C2—C1119.6 (5)C5—C9—C10120.4 (4)
C3—C2—H2120.2C11—C10—C9121.5 (4)
C1—C2—H2120.2C11—C10—H10119.3
C2—C3—C4120.4 (5)C9—C10—H10119.3
C2—C3—H3119.8C10—C11—C12119.2 (5)
C4—C3—H3119.8C10—C11—H11120.4
C12—C4—C3118.4 (4)C12—C11—H11120.4
C12—C4—C5118.0 (4)N1—C12—C4118.0 (4)
C3—C4—C5123.6 (4)N1—C12—C11119.5 (4)
C6—C5—C9118.0 (4)C4—C12—C11122.5 (4)
C6—C5—C4123.7 (4)C1—N1—C12124.0 (5)
C9—C5—C4118.3 (4)C1—N1—H9116 (4)
C7—C6—C5119.3 (5)C12—N1—H9120 (4)
C7—C6—H6120.3C8—N2—C9117.5 (5)
C5—C6—H6120.3O1—Re1—O2108.3 (2)
C6—C7—C8118.9 (5)O1—Re1—O3112.1 (3)
C6—C7—H7120.5O1—Re1—O4110.3 (3)
C8—C7—H7120.5O2—Re1—O3108.3 (2)
N2—C8—C7124.2 (5)O2—Re1—O4109.5 (2)
N2—C8—H8117.9O3—Re1—O4108.3 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H9···O4i0.77 (5)1.98 (5)2.746 (6)168 (5)
C1—H1···O1ii0.932.413.254 (7)151
C1—H1···O2iii0.932.553.024 (7)112
C2—H2···N2iv0.932.443.350 (7)166
C10—H10···O3v0.932.503.252 (7)138
Symmetry codes: (i) x+1, y1/2, z+1/2; (ii) x, y1/2, z+1/2; (iii) x, y+1/2, z1/2; (iv) x1, y+1/2, z1/2; (v) x+1, y+1/2, z+1/2.
 

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