Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807044133/hb2535sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807044133/hb2535Isup2.hkl |
CCDC reference: 663596
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.008 Å
- R factor = 0.039
- wR factor = 0.069
- Data-to-parameter ratio = 42.3
checkCIF/PLATON results
No syntax errors found
Alert level C CELLV02_ALERT_1_C The supplied cell volume s.u. differs from that calculated from the cell parameter s.u.'s by > 2 Calculated cell volume su = 9.11 Cell volume su given = 7.00 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT431_ALERT_2_C Short Inter HL..A Contact Br2 .. Br3 .. 3.57 Ang. PLAT731_ALERT_1_C Bond Calc 0.92(5), Rep 0.922(19) ...... 2.63 su-Ra N2 -H2N 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.92(5), Rep 0.920(19) ...... 2.63 su-Ra N3 -H4N 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.90(5), Rep 0.903(19) ...... 2.63 su-Ra N4 -H5N 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.92(4), Rep 0.920(19) ...... 2.11 su-Ra N4 -H6N 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.95(4), Rep 0.948(19) ...... 2.11 su-Ra O1 -H1W 1.555 1.555 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 Br4 H2 O2 Re
Alert level G ABSTM02_ALERT_3_G The ratio of expected to reported Tmax/Tmin(RR') is < 0.75 Tmin and Tmax reported: 0.340 0.563 Tmin(prime) and Tmax expected: 0.289 0.353 RR(prime) = 0.738 Please check that your absorption correction is appropriate. PLAT794_ALERT_5_G Check Predicted Bond Valency for Re1 (3) 2.36 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 8
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 10 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
(NH4)2ReBr6 was obtained by the method of Watt & Thompson (1963). A mixture of (NH4)2ReBr6 (0.33 g) and 2-amino-6-methylpyridine (0.80 g) was dissolved in 50- ml of ethanol solution, which was heated at 323 K for 10 h followed by slow cooling. After the reaction the mixture colour was yellow–orange. The solution was filtered and the filtrate was left standing for evaporation. After five days, orange plates of (I) appeared. Anal. Calc for C12H20Br5N4O2Re: C 17.19, H 2.57, N 6.68%; found C 16.34, H 2.30, N 6.54%. IR (KBr): 1195(versus), 1200(s), 990(m), 950(s), 1054(m), 980(s), 873(m), 810(s), 730(m), 310(s), 174(m), 159(m).
The N– and O-bound H atoms were located in difference maps and their positions were freely refined with Uiso(H) = 1.2Ueq(carrier). The C-bound H atoms were placed in idealized positions (C—H = 0.93–0.96 Å) and refined as riding with Uiso(H) = 1.2Ueq(C) or 1.5Ueq(methyl C).
The highest difference peak is 0.59 Å from Re1. The deepest difference hole is 0.68 Å from Re1.
This paper reports the crystal structure of a molecular salt containing the [ReVO(H2O)Br4]- anion. All atoms lie on general positions (Fig. 1). The [ReO(H2O)Br4]- anion in (I) shows a distorted trans-ReO2Br4 octahedral geometry about the central Re(V) ion (Table 1). The water molecule is weakly coordinated to rhenium at the base of octahedron with a Re—O distance of 2.206 (3) Å. The Re—Br bond lengths in (I) agree with those in related crystal structures (Abram et al., 1996; Chiozzone et al., 2006; Kochel, 2007).
In the crystal, the component species interact via N—H···Br and O—H···Br hydrogen bonds (Table 2), resulting in alternating layers of anions and cations perpendicular to [010] The shortest Re···Re distances in (I) are 6.819 (3) Å for Re1···Re1i (i = -x, -y + 2, -z + 1) and 8.546 (4) Å for Re1···Re2i (i = -x - 1, -y + 2, -z).
For related structures, see: Abram et al. (1996); Chiozzone et al. (2006); Kochel (2007). For synthetic background, see: Watt & Thompson (1963).
Data collection: CrysAlis CCD (Oxford Diffraction, 2003); cell refinement: CrysAlis RED (Oxford Diffraction, 2003); data reduction: CrysAlis RED (Oxford Diffraction, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); XP (Bruker, 1999); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
Fig. 1. The molecular structure of (I) showing 50% displacement ellipsoids (arbitrary spheres for the H atoms). | |
Fig. 2. The crystal packing in (I). |
(C6H9N2)2·[ReO(H2O)Br4]·Br | F(000) = 1544 |
Mr = 838.07 | Dx = 2.574 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 5614 reflections |
a = 11.996 (2) Å | θ = 2.7–36.7° |
b = 12.154 (3) Å | µ = 14.87 mm−1 |
c = 18.206 (3) Å | T = 100 K |
β = 125.43 (2)° | Prism, orange |
V = 2162.9 (7) Å3 | 0.08 × 0.08 × 0.07 mm |
Z = 4 |
Kuma KM4 CCD diffractometer | 10288 independent reflections |
Radiation source: fine-focus sealed tube | 5873 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.080 |
ω scans | θmax = 36.7°, θmin = 2.7° |
Absorption correction: numerical (CrysAlis [CrysAlis RED?]; Oxford Diffraction, 2003) | h = −19→19 |
Tmin = 0.340, Tmax = 0.563 | k = −18→20 |
40507 measured reflections | l = −30→24 |
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)] = 0.039 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.069 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.92 | w = 1/[σ2(Fo2) + (0.0236P)2] where P = (Fo2 + 2Fc2)/3 |
10288 reflections | (Δ/σ)max = 0.001 |
243 parameters | Δρmax = 2.13 e Å−3 |
8 restraints | Δρmin = −2.32 e Å−3 |
(C6H9N2)2·[ReO(H2O)Br4]·Br | V = 2162.9 (7) Å3 |
Mr = 838.07 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 11.996 (2) Å | µ = 14.87 mm−1 |
b = 12.154 (3) Å | T = 100 K |
c = 18.206 (3) Å | 0.08 × 0.08 × 0.07 mm |
β = 125.43 (2)° |
Kuma KM4 CCD diffractometer | 10288 independent reflections |
Absorption correction: numerical (CrysAlis [CrysAlis RED?]; Oxford Diffraction, 2003) | 5873 reflections with I > 2σ(I) |
Tmin = 0.340, Tmax = 0.563 | Rint = 0.080 |
40507 measured reflections |
R[F2 > 2σ(F2)] = 0.039 | 8 restraints |
wR(F2) = 0.069 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.92 | Δρmax = 2.13 e Å−3 |
10288 reflections | Δρmin = −2.32 e Å−3 |
243 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
N1 | 0.4220 (4) | 0.6746 (3) | 0.9044 (2) | 0.0208 (7) | |
H1N | 0.409 (5) | 0.7471 (18) | 0.911 (3) | 0.025* | |
N2 | 0.1884 (4) | 0.6673 (3) | 0.8315 (3) | 0.0324 (9) | |
H2N | 0.104 (3) | 0.634 (4) | 0.797 (3) | 0.039* | |
H3N | 0.193 (5) | 0.7408 (18) | 0.844 (3) | 0.039* | |
C2 | 0.3048 (4) | 0.6156 (3) | 0.8599 (3) | 0.0229 (9) | |
C3 | 0.3142 (5) | 0.5033 (3) | 0.8462 (3) | 0.0271 (10) | |
H3 | 0.2366 | 0.4591 | 0.8173 | 0.033* | |
C4 | 0.4377 (5) | 0.4602 (4) | 0.8757 (3) | 0.0310 (11) | |
H4 | 0.4440 | 0.3861 | 0.8658 | 0.037* | |
C5 | 0.5566 (5) | 0.5257 (4) | 0.9212 (3) | 0.0318 (11) | |
H5 | 0.6406 | 0.4953 | 0.9406 | 0.038* | |
C6 | 0.5479 (4) | 0.6329 (4) | 0.9365 (3) | 0.0261 (9) | |
C7 | 0.6656 (5) | 0.7116 (5) | 0.9858 (4) | 0.0397 (13) | |
H7A | 0.6761 | 0.7364 | 1.0396 | 0.060* | |
H7B | 0.6482 | 0.7736 | 0.9478 | 0.060* | |
H7C | 0.7478 | 0.6753 | 1.0016 | 0.060* | |
N3 | 0.1990 (3) | 0.6251 (3) | 0.5887 (2) | 0.0182 (7) | |
H4N | 0.265 (3) | 0.621 (4) | 0.578 (3) | 0.022* | |
N4 | 0.2592 (4) | 0.4446 (3) | 0.6379 (3) | 0.0278 (8) | |
H5N | 0.334 (3) | 0.457 (4) | 0.639 (3) | 0.033* | |
H6N | 0.239 (5) | 0.379 (2) | 0.653 (3) | 0.033* | |
C11 | 0.1736 (4) | 0.5308 (3) | 0.6153 (3) | 0.0205 (8) | |
C12 | 0.0562 (5) | 0.5275 (4) | 0.6155 (3) | 0.0275 (10) | |
H12 | 0.0324 | 0.4632 | 0.6311 | 0.033* | |
C13 | −0.0216 (5) | 0.6198 (4) | 0.5926 (3) | 0.0321 (11) | |
H13 | −0.0980 | 0.6187 | 0.5938 | 0.039* | |
C14 | 0.0113 (5) | 0.7163 (4) | 0.5672 (3) | 0.0288 (10) | |
H14 | −0.0421 | 0.7791 | 0.5527 | 0.035* | |
C15 | 0.1211 (4) | 0.7179 (3) | 0.5638 (3) | 0.0212 (8) | |
C16 | 0.1635 (4) | 0.8130 (3) | 0.5331 (3) | 0.0250 (9) | |
H16A | 0.1512 | 0.7943 | 0.4776 | 0.038* | |
H16B | 0.2581 | 0.8296 | 0.5781 | 0.038* | |
H16C | 0.1086 | 0.8760 | 0.5239 | 0.038* | |
Re1 | −0.237586 (16) | 0.926025 (12) | 0.281334 (11) | 0.01677 (4) | |
Br1 | −0.06351 (4) | 1.03636 (3) | 0.27687 (3) | 0.02292 (9) | |
Br2 | −0.38484 (4) | 1.09524 (3) | 0.23272 (3) | 0.02134 (9) | |
Br3 | −0.44110 (4) | 0.81224 (3) | 0.23999 (3) | 0.02152 (9) | |
Br4 | −0.12108 (4) | 0.75203 (3) | 0.28299 (3) | 0.02382 (9) | |
O1 | −0.3328 (3) | 0.9120 (2) | 0.1355 (2) | 0.0197 (6) | |
O2 | −0.1646 (3) | 0.9336 (2) | 0.3918 (2) | 0.0248 (6) | |
Br5 | 0.34325 (4) | 0.88956 (3) | 0.98187 (3) | 0.02261 (9) | |
H1W | −0.324 (5) | 0.978 (2) | 0.111 (3) | 0.027* | |
H2W | −0.426 (2) | 0.897 (4) | 0.088 (2) | 0.027* |
U11 | U22 | U33 | U12 | U13 | U23 | |
N1 | 0.0184 (17) | 0.0190 (16) | 0.027 (2) | −0.0032 (14) | 0.0139 (16) | −0.0034 (14) |
N2 | 0.0181 (19) | 0.029 (2) | 0.041 (3) | −0.0060 (17) | 0.0119 (19) | −0.0156 (18) |
C2 | 0.024 (2) | 0.025 (2) | 0.020 (2) | −0.0060 (18) | 0.0128 (19) | −0.0040 (17) |
C3 | 0.035 (3) | 0.023 (2) | 0.029 (3) | −0.0080 (19) | 0.021 (2) | −0.0075 (18) |
C4 | 0.045 (3) | 0.022 (2) | 0.026 (2) | 0.008 (2) | 0.021 (2) | −0.0002 (18) |
C5 | 0.026 (2) | 0.039 (3) | 0.029 (3) | 0.014 (2) | 0.015 (2) | −0.001 (2) |
C6 | 0.021 (2) | 0.037 (2) | 0.024 (2) | −0.0022 (19) | 0.015 (2) | −0.0027 (19) |
C7 | 0.021 (2) | 0.054 (3) | 0.047 (3) | −0.012 (2) | 0.021 (2) | −0.015 (3) |
N3 | 0.0143 (16) | 0.0228 (17) | 0.0180 (17) | 0.0015 (14) | 0.0096 (15) | −0.0032 (13) |
N4 | 0.031 (2) | 0.0208 (19) | 0.035 (2) | 0.0061 (17) | 0.0214 (19) | 0.0049 (16) |
C11 | 0.024 (2) | 0.0206 (19) | 0.014 (2) | −0.0007 (17) | 0.0095 (18) | 0.0008 (15) |
C12 | 0.024 (2) | 0.034 (2) | 0.028 (3) | −0.0007 (19) | 0.017 (2) | 0.0030 (19) |
C13 | 0.022 (2) | 0.045 (3) | 0.037 (3) | 0.004 (2) | 0.021 (2) | 0.006 (2) |
C14 | 0.021 (2) | 0.029 (2) | 0.034 (3) | 0.0073 (19) | 0.015 (2) | 0.004 (2) |
C15 | 0.022 (2) | 0.0206 (19) | 0.018 (2) | 0.0020 (17) | 0.0097 (18) | 0.0008 (16) |
C16 | 0.022 (2) | 0.0187 (19) | 0.027 (2) | 0.0003 (17) | 0.010 (2) | 0.0014 (17) |
Re1 | 0.01591 (7) | 0.01429 (7) | 0.01882 (8) | 0.00079 (6) | 0.00933 (6) | 0.00002 (6) |
Br1 | 0.0185 (2) | 0.01779 (18) | 0.0319 (2) | −0.00143 (16) | 0.01433 (19) | −0.00067 (16) |
Br2 | 0.0206 (2) | 0.01803 (18) | 0.0250 (2) | 0.00517 (15) | 0.01295 (18) | 0.00171 (15) |
Br3 | 0.0198 (2) | 0.02158 (19) | 0.0243 (2) | −0.00228 (16) | 0.01344 (18) | 0.00220 (16) |
Br4 | 0.0198 (2) | 0.01426 (18) | 0.0349 (3) | 0.00186 (15) | 0.01442 (19) | −0.00040 (16) |
O1 | 0.0256 (15) | 0.0159 (13) | 0.0201 (15) | 0.0004 (12) | 0.0147 (13) | 0.0013 (11) |
O2 | 0.0258 (15) | 0.0221 (14) | 0.0218 (16) | 0.0022 (13) | 0.0111 (13) | 0.0022 (12) |
Br5 | 0.0247 (2) | 0.02478 (19) | 0.0205 (2) | −0.00570 (17) | 0.01438 (18) | −0.00151 (16) |
N1—C2 | 1.352 (5) | N4—H5N | 0.903 (19) |
N1—C6 | 1.363 (5) | N4—H6N | 0.920 (19) |
N1—H1N | 0.913 (19) | C11—C12 | 1.411 (6) |
N2—C2 | 1.331 (6) | C12—C13 | 1.361 (6) |
N2—H2N | 0.922 (19) | C12—H12 | 0.9300 |
N2—H3N | 0.915 (19) | C13—C14 | 1.399 (6) |
C2—C3 | 1.404 (6) | C13—H13 | 0.9300 |
C3—C4 | 1.354 (6) | C14—C15 | 1.354 (6) |
C3—H3 | 0.9300 | C14—H14 | 0.9300 |
C4—C5 | 1.410 (7) | C15—C16 | 1.496 (6) |
C4—H4 | 0.9300 | C16—H16A | 0.9600 |
C5—C6 | 1.349 (6) | C16—H16B | 0.9600 |
C5—H5 | 0.9300 | C16—H16C | 0.9600 |
C6—C7 | 1.498 (6) | Re1—O2 | 1.667 (3) |
C7—H7A | 0.9600 | Re1—O1 | 2.206 (3) |
C7—H7B | 0.9600 | Re1—Br3 | 2.5117 (6) |
C7—H7C | 0.9600 | Re1—Br2 | 2.5141 (6) |
N3—C11 | 1.347 (5) | Re1—Br1 | 2.5223 (5) |
N3—C15 | 1.363 (5) | Re1—Br4 | 2.5254 (6) |
N3—H4N | 0.920 (19) | O1—H1W | 0.948 (19) |
N4—C11 | 1.354 (5) | O1—H2W | 0.955 (19) |
C2—N1—C6 | 124.7 (4) | C13—C12—C11 | 118.9 (4) |
C2—N1—H1N | 113 (3) | C13—C12—H12 | 120.6 |
C6—N1—H1N | 122 (3) | C11—C12—H12 | 120.6 |
C2—N2—H2N | 124 (3) | C12—C13—C14 | 121.2 (4) |
C2—N2—H3N | 118 (3) | C12—C13—H13 | 119.4 |
H2N—N2—H3N | 118 (4) | C14—C13—H13 | 119.4 |
N2—C2—N1 | 118.4 (4) | C15—C14—C13 | 119.7 (4) |
N2—C2—C3 | 124.3 (4) | C15—C14—H14 | 120.2 |
N1—C2—C3 | 117.3 (4) | C13—C14—H14 | 120.2 |
C4—C3—C2 | 119.2 (4) | C14—C15—N3 | 118.1 (4) |
C4—C3—H3 | 120.4 | C14—C15—C16 | 125.4 (4) |
C2—C3—H3 | 120.4 | N3—C15—C16 | 116.5 (4) |
C3—C4—C5 | 121.1 (4) | C15—C16—H16A | 109.5 |
C3—C4—H4 | 119.5 | C15—C16—H16B | 109.5 |
C5—C4—H4 | 119.5 | H16A—C16—H16B | 109.5 |
C6—C5—C4 | 119.6 (4) | C15—C16—H16C | 109.5 |
C6—C5—H5 | 120.2 | H16A—C16—H16C | 109.5 |
C4—C5—H5 | 120.2 | H16B—C16—H16C | 109.5 |
C5—C6—N1 | 118.1 (4) | O2—Re1—O1 | 178.68 (12) |
C5—C6—C7 | 125.6 (4) | O2—Re1—Br3 | 97.54 (10) |
N1—C6—C7 | 116.4 (4) | O1—Re1—Br3 | 82.06 (8) |
C6—C7—H7A | 109.5 | O2—Re1—Br2 | 98.64 (10) |
C6—C7—H7B | 109.5 | O1—Re1—Br2 | 82.62 (7) |
H7A—C7—H7B | 109.5 | Br3—Re1—Br2 | 88.99 (2) |
C6—C7—H7C | 109.5 | O2—Re1—Br1 | 98.28 (10) |
H7A—C7—H7C | 109.5 | O1—Re1—Br1 | 82.12 (8) |
H7B—C7—H7C | 109.5 | Br3—Re1—Br1 | 164.174 (16) |
C11—N3—C15 | 124.7 (3) | Br2—Re1—Br1 | 88.83 (2) |
C11—N3—H4N | 116 (3) | O2—Re1—Br4 | 97.56 (10) |
C15—N3—H4N | 119 (3) | O1—Re1—Br4 | 81.18 (7) |
C11—N4—H5N | 116 (3) | Br3—Re1—Br4 | 88.71 (2) |
C11—N4—H6N | 118 (3) | Br2—Re1—Br4 | 163.793 (16) |
H5N—N4—H6N | 125 (4) | Br1—Re1—Br4 | 89.02 (2) |
N3—C11—N4 | 118.5 (4) | Re1—O1—H1W | 112 (3) |
N3—C11—C12 | 117.4 (4) | Re1—O1—H2W | 129 (3) |
N4—C11—C12 | 124.1 (4) | H1W—O1—H2W | 97 (4) |
C6—N1—C2—N2 | −179.4 (4) | C15—N3—C11—N4 | 179.7 (4) |
C6—N1—C2—C3 | 0.2 (6) | C15—N3—C11—C12 | 1.5 (6) |
N2—C2—C3—C4 | 178.0 (4) | N3—C11—C12—C13 | −2.6 (6) |
N1—C2—C3—C4 | −1.6 (6) | N4—C11—C12—C13 | 179.2 (4) |
C2—C3—C4—C5 | 1.2 (7) | C11—C12—C13—C14 | 1.4 (7) |
C3—C4—C5—C6 | 0.6 (7) | C12—C13—C14—C15 | 1.1 (7) |
C4—C5—C6—N1 | −2.0 (7) | C13—C14—C15—N3 | −2.2 (7) |
C4—C5—C6—C7 | 178.3 (5) | C13—C14—C15—C16 | 176.5 (4) |
C2—N1—C6—C5 | 1.6 (6) | C11—N3—C15—C14 | 1.0 (6) |
C2—N1—C6—C7 | −178.7 (4) | C11—N3—C15—C16 | −177.8 (4) |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1N···Br5 | 0.92 (3) | 2.54 (5) | 3.354 (4) | 148 (5) |
O1—H1W···Br5i | 0.95 (4) | 2.25 (4) | 3.176 (3) | 165 (4) |
N2—H2N···Br1ii | 0.92 (5) | 2.76 (5) | 3.573 (5) | 148 (4) |
N2—H2N···Br4ii | 0.92 (5) | 2.91 (5) | 3.424 (6) | 117 (4) |
O1—H2W···Br5iii | 0.95 (3) | 2.28 (3) | 3.225 (4) | 170 (4) |
N2—H3N···Br5 | 0.92 (2) | 2.75 (4) | 3.514 (4) | 141 (3) |
N3—H4N···Br5iv | 0.92 (5) | 2.42 (5) | 3.273 (4) | 154 (4) |
N4—H5N···Br2v | 0.90 (5) | 2.83 (5) | 3.592 (6) | 143 (4) |
N4—H6N···Br4vi | 0.92 (4) | 2.79 (5) | 3.647 (5) | 155 (5) |
Symmetry codes: (i) −x, −y+2, −z+1; (ii) x, −y+3/2, z+1/2; (iii) x−1, y, z−1; (iv) x, −y+3/2, z−1/2; (v) x+1, −y+3/2, z+1/2; (vi) −x, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | (C6H9N2)2·[ReO(H2O)Br4]·Br |
Mr | 838.07 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 100 |
a, b, c (Å) | 11.996 (2), 12.154 (3), 18.206 (3) |
β (°) | 125.43 (2) |
V (Å3) | 2162.9 (7) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 14.87 |
Crystal size (mm) | 0.08 × 0.08 × 0.07 |
Data collection | |
Diffractometer | Kuma KM4 CCD |
Absorption correction | Numerical (CrysAlis [CrysAlis RED?]; Oxford Diffraction, 2003) |
Tmin, Tmax | 0.340, 0.563 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 40507, 10288, 5873 |
Rint | 0.080 |
(sin θ/λ)max (Å−1) | 0.840 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.039, 0.069, 0.92 |
No. of reflections | 10288 |
No. of parameters | 243 |
No. of restraints | 8 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 2.13, −2.32 |
Computer programs: CrysAlis CCD (Oxford Diffraction, 2003), CrysAlis RED (Oxford Diffraction, 2003), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), PLATON (Spek, 2003); XP (Bruker, 1999).
Re1—O2 | 1.667 (3) | Re1—Br2 | 2.5141 (6) |
Re1—O1 | 2.206 (3) | Re1—Br1 | 2.5223 (5) |
Re1—Br3 | 2.5117 (6) | Re1—Br4 | 2.5254 (6) |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1N···Br5 | 0.92 (3) | 2.54 (5) | 3.354 (4) | 148 (5) |
O1—H1W···Br5i | 0.95 (4) | 2.25 (4) | 3.176 (3) | 165 (4) |
N2—H2N···Br1ii | 0.92 (5) | 2.76 (5) | 3.573 (5) | 148 (4) |
N2—H2N···Br4ii | 0.92 (5) | 2.91 (5) | 3.424 (6) | 117 (4) |
O1—H2W···Br5iii | 0.95 (3) | 2.28 (3) | 3.225 (4) | 170 (4) |
N2—H3N···Br5 | 0.92 (2) | 2.75 (4) | 3.514 (4) | 141 (3) |
N3—H4N···Br5iv | 0.92 (5) | 2.42 (5) | 3.273 (4) | 154 (4) |
N4—H5N···Br2v | 0.90 (5) | 2.83 (5) | 3.592 (6) | 143 (4) |
N4—H6N···Br4vi | 0.92 (4) | 2.79 (5) | 3.647 (5) | 155 (5) |
Symmetry codes: (i) −x, −y+2, −z+1; (ii) x, −y+3/2, z+1/2; (iii) x−1, y, z−1; (iv) x, −y+3/2, z−1/2; (v) x+1, −y+3/2, z+1/2; (vi) −x, −y+1, −z+1. |
This paper reports the crystal structure of a molecular salt containing the [ReVO(H2O)Br4]- anion. All atoms lie on general positions (Fig. 1). The [ReO(H2O)Br4]- anion in (I) shows a distorted trans-ReO2Br4 octahedral geometry about the central Re(V) ion (Table 1). The water molecule is weakly coordinated to rhenium at the base of octahedron with a Re—O distance of 2.206 (3) Å. The Re—Br bond lengths in (I) agree with those in related crystal structures (Abram et al., 1996; Chiozzone et al., 2006; Kochel, 2007).
In the crystal, the component species interact via N—H···Br and O—H···Br hydrogen bonds (Table 2), resulting in alternating layers of anions and cations perpendicular to [010] The shortest Re···Re distances in (I) are 6.819 (3) Å for Re1···Re1i (i = -x, -y + 2, -z + 1) and 8.546 (4) Å for Re1···Re2i (i = -x - 1, -y + 2, -z).