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
CCDC reference: 610911
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.007 Å
- R factor = 0.026
- wR factor = 0.060
- Data-to-parameter ratio = 15.9
checkCIF/PLATON results
No syntax errors found
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
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 = 431.41 | Dx = 2.334 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 3551 reflections |
a = 7.8374 (16) Å | θ = 1.0–27.5° |
b = 20.840 (4) Å | µ = 9.91 mm−1 |
c = 7.5280 (15) Å | T = 293 K |
β = 92.95 (3)° | Block, yellow |
V = 1227.9 (4) Å3 | 0.22 × 0.10 × 0.08 mm |
Z = 4 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 2815 independent reflections |
Radiation source: fine-focus sealed tube | 2267 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
φ and ω scans | θmax = 27.5°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −10→10 |
Tmin = 0.32, Tmax = 0.45 | k = −27→0 |
11638 measured reflections | l = 0→9 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.026 | H 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 reflections | Δρmax = 0.78 e Å−3 |
177 parameters | Δρmin = −1.09 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction 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 | x | y | z | Uiso*/Ueq | |
C1 | 0.3180 (6) | 0.1092 (3) | 0.2929 (7) | 0.0460 (11) | |
H1 | 0.2582 | 0.0712 | 0.2716 | 0.055* | |
C2 | 0.2417 (6) | 0.1673 (3) | 0.2541 (7) | 0.0470 (12) | |
H2 | 0.1310 | 0.1688 | 0.2033 | 0.056* | |
C3 | 0.3294 (6) | 0.2229 (3) | 0.2906 (7) | 0.0436 (11) | |
H3 | 0.2770 | 0.2623 | 0.2675 | 0.052* | |
C4 | 0.4982 (5) | 0.2210 (2) | 0.3626 (6) | 0.0329 (9) | |
C5 | 0.6002 (6) | 0.2779 (2) | 0.4030 (6) | 0.0337 (9) | |
C6 | 0.5400 (7) | 0.3402 (2) | 0.3781 (7) | 0.0451 (12) | |
H6 | 0.4281 | 0.3475 | 0.3358 | 0.054* | |
C7 | 0.6469 (7) | 0.3907 (3) | 0.4166 (8) | 0.0542 (13) | |
H7 | 0.6087 | 0.4327 | 0.4013 | 0.065* | |
C8 | 0.8129 (7) | 0.3783 (3) | 0.4785 (8) | 0.0545 (14) | |
H8 | 0.8847 | 0.4132 | 0.5021 | 0.065* | |
C9 | 0.7704 (6) | 0.2697 (2) | 0.4687 (6) | 0.0374 (10) | |
C10 | 0.8386 (6) | 0.2069 (3) | 0.4980 (7) | 0.0431 (12) | |
H10 | 0.9515 | 0.2024 | 0.5406 | 0.052* | |
C11 | 0.7435 (6) | 0.1542 (2) | 0.4653 (7) | 0.0420 (11) | |
H11 | 0.7890 | 0.1136 | 0.4880 | 0.050* | |
C12 | 0.5733 (6) | 0.1610 (2) | 0.3960 (6) | 0.0331 (9) | |
N1 | 0.4769 (6) | 0.1077 (2) | 0.3605 (6) | 0.0405 (9) | |
H9 | 0.518 (6) | 0.074 (2) | 0.370 (6) | 0.028 (13)* | |
N2 | 0.8756 (5) | 0.3203 (2) | 0.5063 (6) | 0.0480 (11) | |
O1 | −0.0076 (6) | 0.5055 (3) | 0.2054 (7) | 0.0957 (18) | |
O2 | 0.2420 (7) | 0.4595 (2) | 0.4438 (6) | 0.0739 (13) | |
O3 | 0.1469 (6) | 0.3855 (2) | 0.1502 (6) | 0.0724 (13) | |
O4 | 0.3316 (5) | 0.49769 (19) | 0.1035 (6) | 0.0638 (12) | |
Re1 | 0.17550 (2) | 0.462192 (10) | 0.22432 (3) | 0.04193 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.043 (3) | 0.043 (3) | 0.051 (3) | −0.012 (2) | 0.000 (2) | −0.003 (2) |
C2 | 0.031 (2) | 0.053 (3) | 0.056 (3) | −0.002 (2) | −0.007 (2) | 0.001 (3) |
C3 | 0.034 (2) | 0.042 (3) | 0.053 (3) | 0.004 (2) | −0.006 (2) | 0.005 (2) |
C4 | 0.030 (2) | 0.034 (2) | 0.035 (2) | 0.0010 (18) | 0.0001 (18) | 0.0020 (19) |
C5 | 0.033 (2) | 0.032 (2) | 0.037 (2) | −0.0004 (18) | 0.0034 (18) | −0.0016 (19) |
C6 | 0.044 (3) | 0.038 (3) | 0.053 (3) | 0.006 (2) | −0.001 (2) | 0.001 (2) |
C7 | 0.061 (3) | 0.033 (3) | 0.069 (4) | 0.000 (3) | 0.001 (3) | −0.002 (3) |
C8 | 0.057 (3) | 0.041 (3) | 0.066 (4) | −0.016 (3) | 0.005 (3) | −0.011 (3) |
C9 | 0.033 (2) | 0.044 (3) | 0.035 (2) | −0.003 (2) | 0.0027 (19) | −0.007 (2) |
C10 | 0.030 (2) | 0.050 (3) | 0.049 (3) | 0.005 (2) | 0.000 (2) | −0.001 (2) |
C11 | 0.041 (3) | 0.034 (2) | 0.050 (3) | 0.009 (2) | −0.004 (2) | −0.001 (2) |
C12 | 0.031 (2) | 0.034 (2) | 0.034 (2) | −0.0012 (18) | 0.0034 (18) | −0.0030 (19) |
N1 | 0.044 (2) | 0.028 (2) | 0.049 (2) | 0.002 (2) | 0.0028 (19) | 0.0006 (19) |
N2 | 0.040 (2) | 0.051 (3) | 0.053 (3) | −0.008 (2) | −0.001 (2) | −0.009 (2) |
O1 | 0.067 (3) | 0.146 (5) | 0.075 (3) | 0.056 (3) | 0.011 (3) | −0.002 (3) |
O2 | 0.092 (3) | 0.072 (3) | 0.056 (2) | 0.014 (3) | −0.013 (2) | −0.002 (2) |
O3 | 0.087 (3) | 0.054 (2) | 0.078 (3) | −0.031 (2) | 0.016 (2) | −0.013 (2) |
O4 | 0.062 (3) | 0.045 (2) | 0.087 (3) | −0.013 (2) | 0.028 (2) | −0.004 (2) |
Re1 | 0.03602 (12) | 0.03890 (12) | 0.05083 (13) | 0.00132 (10) | 0.00177 (8) | −0.00112 (11) |
Geometric parameters (Å, º) top
C1—N1 | 1.321 (6) | C8—N2 | 1.317 (7) |
C1—C2 | 1.376 (8) | C8—H8 | 0.9300 |
C1—H1 | 0.9300 | C9—N2 | 1.360 (6) |
C2—C3 | 1.368 (7) | C9—C10 | 1.427 (7) |
C2—H2 | 0.9300 | C10—C11 | 1.344 (7) |
C3—C4 | 1.404 (6) | C10—H10 | 0.9300 |
C3—H3 | 0.9300 | C11—C12 | 1.414 (6) |
C4—C12 | 1.398 (6) | C11—H11 | 0.9300 |
C4—C5 | 1.455 (6) | C12—N1 | 1.362 (6) |
C5—C6 | 1.391 (6) | N1—H9 | 0.77 (5) |
C5—C9 | 1.409 (6) | Re1—O1 | 1.696 (5) |
C6—C7 | 1.367 (7) | Re1—O2 | 1.708 (4) |
C6—H6 | 0.9300 | Re1—O3 | 1.704 (4) |
C7—C8 | 1.383 (8) | Re1—O4 | 1.728 (4) |
C7—H7 | 0.9300 | | |
| | | |
N1—C1—C2 | 119.5 (5) | C7—C8—H8 | 117.9 |
N1—C1—H1 | 120.2 | N2—C9—C5 | 122.1 (5) |
C2—C1—H1 | 120.2 | N2—C9—C10 | 117.5 (4) |
C3—C2—C1 | 119.6 (5) | C5—C9—C10 | 120.4 (4) |
C3—C2—H2 | 120.2 | C11—C10—C9 | 121.5 (4) |
C1—C2—H2 | 120.2 | C11—C10—H10 | 119.3 |
C2—C3—C4 | 120.4 (5) | C9—C10—H10 | 119.3 |
C2—C3—H3 | 119.8 | C10—C11—C12 | 119.2 (5) |
C4—C3—H3 | 119.8 | C10—C11—H11 | 120.4 |
C12—C4—C3 | 118.4 (4) | C12—C11—H11 | 120.4 |
C12—C4—C5 | 118.0 (4) | N1—C12—C4 | 118.0 (4) |
C3—C4—C5 | 123.6 (4) | N1—C12—C11 | 119.5 (4) |
C6—C5—C9 | 118.0 (4) | C4—C12—C11 | 122.5 (4) |
C6—C5—C4 | 123.7 (4) | C1—N1—C12 | 124.0 (5) |
C9—C5—C4 | 118.3 (4) | C1—N1—H9 | 116 (4) |
C7—C6—C5 | 119.3 (5) | C12—N1—H9 | 120 (4) |
C7—C6—H6 | 120.3 | C8—N2—C9 | 117.5 (5) |
C5—C6—H6 | 120.3 | O1—Re1—O2 | 108.3 (2) |
C6—C7—C8 | 118.9 (5) | O1—Re1—O3 | 112.1 (3) |
C6—C7—H7 | 120.5 | O1—Re1—O4 | 110.3 (3) |
C8—C7—H7 | 120.5 | O2—Re1—O3 | 108.3 (2) |
N2—C8—C7 | 124.2 (5) | O2—Re1—O4 | 109.5 (2) |
N2—C8—H8 | 117.9 | O3—Re1—O4 | 108.3 (2) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H9···O4i | 0.77 (5) | 1.98 (5) | 2.746 (6) | 168 (5) |
C1—H1···O1ii | 0.93 | 2.41 | 3.254 (7) | 151 |
C1—H1···O2iii | 0.93 | 2.55 | 3.024 (7) | 112 |
C2—H2···N2iv | 0.93 | 2.44 | 3.350 (7) | 166 |
C10—H10···O3v | 0.93 | 2.50 | 3.252 (7) | 138 |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) −x, y−1/2, −z+1/2; (iii) x, −y+1/2, z−1/2; (iv) x−1, −y+1/2, z−1/2; (v) x+1, −y+1/2, z+1/2. |