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The title compound, (C5H6N)2[CdBr4]·H2O, consists of discrete anions, cations and solvent water mol­ecules. Both pyridinium cations and the tetra­bromo­cadmate anion possess a crystallographically imposed mirror symmetry. The solvent water mol­ecule and one pyridinium cation form intermol­ecular N—H...O and O—H...Br hydrogen bonds, giving a three-dimensional hydrogen-bonded structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804029897/rz6012sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804029897/rz6012Isup2.hkl
Contains datablock I

CCDC reference: 262254

Key indicators

  • Single-crystal X-ray study
  • T = 223 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.030
  • wR factor = 0.077
  • Data-to-parameter ratio = 23.0

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1 ... ?
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 1 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 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, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXTL.

Bis(pyridinium) tetrabromocadmate(II) monohydrate top
Crystal data top
(C5H6N)2[CdBr4]·H2OF(000) = 1136
Mr = 610.27Dx = 2.311 Mg m3
Orthorhombic, PnmaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2nCell parameters from 2299 reflections
a = 14.951 (2) Åθ = 2.1–28.3°
b = 9.1564 (15) ŵ = 10.35 mm1
c = 12.815 (2) ÅT = 223 K
V = 1754.3 (5) Å3Prismatic, colourless
Z = 40.15 × 0.12 × 0.10 mm
Data collection top
Bruker AXS APEX CCD
diffractometer
2299 independent reflections
Radiation source: fine-focus sealed tube1776 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.060
ω scansθmax = 28.3°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1919
Tmin = 0.234, Tmax = 0.355k = 1212
22963 measured reflectionsl = 1717
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)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.077H atoms treated by a mixture of independent and constrained refinement
S = 1.10 w = 1/[σ2(Fo2) + (0.0272P)2 + 2.3887P]
where P = (Fo2 + 2Fc2)/3
2299 reflections(Δ/σ)max < 0.001
100 parametersΔρmax = 0.66 e Å3
0 restraintsΔρmin = 0.66 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
Cd10.37721 (3)0.25000.75084 (4)0.03605 (13)
Br10.34626 (3)0.02430 (6)0.86495 (4)0.04565 (14)
Br20.54582 (4)0.25000.70170 (5)0.04547 (18)
Br30.29500 (5)0.25000.57349 (6)0.0527 (2)
O10.5712 (4)0.25000.9546 (4)0.0560 (14)
N10.3121 (4)0.75000.5065 (5)0.0622 (18)
H10.26290.75000.47040.075*
N20.4451 (4)0.25000.1020 (4)0.0407 (13)
H20.48800.25000.05620.049*
C30.3471 (4)0.8746 (6)0.5322 (4)0.0545 (14)
H30.31760.96150.51360.065*
C40.4229 (4)0.8813 (7)0.5837 (4)0.0702 (18)
H40.44790.97180.60250.084*
C50.4655 (6)0.75000.6099 (7)0.090 (4)
H50.52110.75000.64420.108*
C60.4133 (3)0.1227 (5)0.1360 (4)0.0439 (11)
H60.43790.03480.11120.053*
C70.3455 (3)0.1200 (5)0.2061 (4)0.0439 (11)
H70.32250.03050.23000.053*
C80.3109 (4)0.25000.2419 (5)0.0422 (15)
H80.26390.25000.29050.051*
H90.629 (5)0.25000.952 (6)0.05 (2)*
H100.569 (6)0.25000.884 (7)0.08 (3)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.0342 (2)0.0373 (2)0.0366 (2)0.0000.0030 (2)0.000
Br10.0463 (3)0.0434 (3)0.0472 (3)0.0070 (2)0.0024 (2)0.0083 (2)
Br20.0356 (3)0.0657 (5)0.0351 (4)0.0000.0053 (3)0.000
Br30.0520 (4)0.0547 (4)0.0514 (4)0.0000.0226 (3)0.000
O10.038 (3)0.094 (4)0.036 (3)0.0000.006 (2)0.000
N10.044 (4)0.092 (6)0.051 (4)0.0000.007 (3)0.000
N20.041 (3)0.051 (3)0.030 (3)0.0000.006 (2)0.000
C30.058 (3)0.047 (3)0.058 (3)0.013 (3)0.011 (3)0.001 (3)
C40.079 (5)0.075 (4)0.056 (4)0.024 (4)0.012 (3)0.033 (3)
C50.048 (5)0.170 (12)0.053 (5)0.0000.024 (4)0.000
C60.043 (3)0.038 (3)0.051 (3)0.005 (2)0.006 (2)0.004 (2)
C70.042 (3)0.040 (3)0.050 (3)0.004 (2)0.006 (2)0.007 (2)
C80.028 (3)0.055 (4)0.043 (4)0.0000.010 (3)0.000
Geometric parameters (Å, º) top
Cd1—Br1i2.5736 (6)C3—C41.314 (8)
Cd1—Br12.5736 (6)C3—H30.9400
Cd1—Br32.5838 (9)C4—C51.402 (8)
Cd1—Br22.5983 (9)C4—H40.9400
O1—H90.86 (8)C5—H50.9400
O1—H100.90 (9)C6—C71.355 (6)
N1—C31.297 (6)C6—H60.9400
N1—H10.8700C7—C81.377 (6)
N2—C61.331 (5)C7—H70.9400
N2—H20.8700C8—H80.9400
Br1i—Cd1—Br1106.84 (3)C3—C4—C5118.2 (6)
Br1i—Cd1—Br3114.474 (19)C3—C4—H4120.9
Br1—Cd1—Br3114.474 (19)C5—C4—H4120.9
Br1i—Cd1—Br2108.188 (18)C4ii—C5—C4118.2 (8)
Br1—Cd1—Br2108.188 (18)C4ii—C5—H5120.9
Br3—Cd1—Br2104.38 (3)C4—C5—H5120.9
H9—O1—H1090 (7)N2—C6—C7120.0 (5)
C3ii—N1—C3123.2 (7)N2—C6—H6120.0
C3ii—N1—H1118.4C7—C6—H6120.0
C3—N1—H1118.4C6—C7—C8119.1 (5)
C6—N2—C6i122.2 (6)C6—C7—H7120.5
C6—N2—H2118.9C8—C7—H7120.5
C6i—N2—H2118.9C7—C8—C7i119.7 (6)
N1—C3—C4121.1 (6)C7—C8—H8120.1
N1—C3—H3119.5C7i—C8—H8120.1
C4—C3—H3119.5
C3ii—N1—C3—C42.3 (12)C6i—N2—C6—C71.0 (10)
N1—C3—C4—C50.3 (10)N2—C6—C7—C80.5 (8)
C3—C4—C5—C4ii2.7 (13)C6—C7—C8—C7i0.0 (10)
Symmetry codes: (i) x, y+1/2, z; (ii) x, y+3/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O1iii0.871.802.669 (7)176
O1—H9···Br3iv0.86 (8)2.50 (8)3.365 (6)175 (7)
O1—H10···Br20.90 (9)2.36 (9)3.263 (6)174 (8)
Symmetry codes: (iii) x, y, z1; (iv) x+1/2, y, z+3/2.
 

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