Literature DB >> 22590139

Tetra-kis(4-meth-oxy-anilinium) hexa-chloridobismuthate(III) chloride monohydrate.

Ming-Liang Liu1.   

Abstract

In the crystal of the title compound, (C(7)H(10)NO)(4)[BiCl(6)]Cl·H(2)O, the Bi(III) cation is located on an inversion center and coordinated by six Cl(-) anions in a slightly distorted octa-hedral geometry; the uncoordinated Cl(-) anion and lattice water mol-ecule are located on a twofold rotation axis. Two independent 4-meth-oxy-anilinium cations are linked to the Bi complex, the uncoordinated Cl(-) anion and lattice water mol-ecule via N-H⋯Cl and N-H⋯O hydrogen bonds.

Entities:  

Year:  2012        PMID： 22590139      PMCID： PMC3344373          DOI： 10.1107/S1600536812017096

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For background literature concerning ferroelectric metal-organic complexes, see: Ye et al. (2009 ▶); Zhang et al. (2009 ▶, 2010 ▶). For related structures, see: Liu (2011a ▶,b ▶,c ▶).

Experimental

Crystal data

(C7H10NO)4[BiCl6]Cl·H2O M = 971.79 Monoclinic, a = 25.806 (5) Å b = 7.7081 (15) Å c = 19.550 (4) Å β = 104.27 (3)° V = 3768.8 (13) Å3 Z = 4 Mo Kα radiation μ = 5.22 mm−1 T = 293 K 0.21 × 0.20 × 0.20 mm

Data collection

Rigaku SCXmini diffractometer Absorption correction: multi-scan (CrystalClear; Rigaku, 2005 ▶) T min = 0.350, T max = 0.364 18912 measured reflections 4320 independent reflections 3223 reflections with I > 2σ(I) R int = 0.055

Refinement

R[F 2 > 2σ(F 2)] = 0.031 wR(F 2) = 0.065 S = 1.07 4320 reflections 212 parameters 2 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.46 e Å−3 Δρmin = −0.89 e Å−3 Data collection: CrystalClear (Rigaku, 2005 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812017096/xu5513sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812017096/xu5513Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
(C7H10NO)4[BiCl6]Cl·H2OF(000) = 1920
Mr = 971.79Dx = 1.713 Mg m−3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 3223 reflections
a = 25.806 (5) Åθ = 0–26°
b = 7.7081 (15) ŵ = 5.22 mm−1
c = 19.550 (4) ÅT = 293 K
β = 104.27 (3)°Block, colourless
V = 3768.8 (13) Å30.21 × 0.20 × 0.20 mm
Z = 4
Rigaku SCXmini diffractometer4320 independent reflections
Radiation source: fine-focus sealed tube3223 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.055
CCD_Profile_fitting scansθmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005)h = −33→33
Tmin = 0.350, Tmax = 0.364k = −10→10
18912 measured reflectionsl = −25→25
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.031Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.065H atoms treated by a mixture of independent and constrained refinement
S = 1.07w = 1/[σ2(Fo2) + (0.0215P)2] where P = (Fo2 + 2Fc2)/3
4320 reflections(Δ/σ)max < 0.001
212 parametersΔρmax = 0.46 e Å−3
2 restraintsΔρmin = −0.89 e Å−3
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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.
xyzUiso*/Ueq
O10.28804 (11)0.4079 (3)0.34243 (14)0.0518 (7)
N10.07004 (13)0.4069 (5)0.21893 (18)0.0586 (9)
H1A0.05500.50330.23010.070*
H1B0.06420.39950.17220.070*
H1C0.05580.31520.23500.070*
C10.32410 (19)0.5181 (5)0.3189 (3)0.0680 (14)
H1D0.31260.63640.31970.102*
H1E0.32490.48690.27160.102*
H1F0.35920.50570.34940.102*
C20.21434 (17)0.5117 (4)0.2491 (2)0.0421 (9)
H20.23650.57760.22830.050*
C30.16029 (17)0.5079 (4)0.2199 (2)0.0454 (9)
H30.14580.57090.17900.055*
C40.12749 (15)0.4115 (5)0.2505 (2)0.0404 (9)
C50.14777 (17)0.3185 (5)0.3107 (2)0.0482 (10)
H50.12530.25360.33130.058*
C60.20162 (17)0.3228 (5)0.33989 (19)0.0483 (10)
H60.21560.26060.38110.058*
C70.23587 (15)0.4174 (4)0.30985 (19)0.0358 (8)
O20.23658 (13)0.3700 (4)0.07934 (16)0.0683 (9)
N20.44637 (15)0.5170 (4)0.0738 (2)0.0606 (10)
H2A0.46160.42530.05900.073*
H2B0.44690.60620.04500.073*
H2C0.46440.54470.11730.073*
C80.1924 (2)0.4511 (6)0.0331 (3)0.0781 (16)
H8A0.19280.4259−0.01490.117*
H8B0.19450.57420.04050.117*
H8C0.15980.40810.04220.117*
C90.32753 (18)0.3409 (5)0.1260 (2)0.0548 (11)
H90.31990.27250.16140.066*
C100.37990 (17)0.3753 (5)0.1258 (2)0.0545 (11)
H100.40750.33040.16130.065*
C110.35099 (19)0.5412 (5)0.0212 (2)0.0500 (11)
H110.35880.6095−0.01410.060*
C120.28621 (17)0.4080 (5)0.0733 (2)0.0450 (10)
C130.29834 (18)0.5055 (4)0.0210 (2)0.0500 (10)
H130.27090.5483−0.01530.060*
C140.39129 (17)0.4754 (4)0.0737 (2)0.0425 (9)
Bi10.00000.50000.00000.03569 (7)
Cl20.06254 (4)0.23985 (12)0.06560 (5)0.0521 (3)
Cl30.05299 (4)0.74622 (13)0.08758 (6)0.0610 (3)
Cl4−0.05859 (5)0.44282 (15)0.09398 (6)0.0623 (3)
O30.00000.6668 (7)0.25000.112 (2)
Cl10.00000.0822 (2)0.25000.0579 (4)
H3B0.0155 (18)0.741 (2)0.230 (3)0.15 (3)*
U11U22U33U12U13U23
O10.0405 (18)0.0500 (16)0.0567 (17)−0.0059 (14)−0.0034 (14)0.0099 (14)
N10.038 (2)0.071 (2)0.068 (2)−0.0017 (19)0.0168 (19)−0.007 (2)
C10.040 (3)0.066 (3)0.090 (4)−0.011 (2)0.000 (3)0.011 (2)
C20.042 (2)0.042 (2)0.042 (2)−0.0055 (18)0.0093 (18)0.0060 (18)
C30.043 (3)0.049 (2)0.042 (2)0.0016 (19)0.0056 (18)0.0119 (19)
C40.032 (2)0.043 (2)0.049 (2)−0.0043 (18)0.0152 (19)−0.0112 (19)
C50.050 (3)0.047 (2)0.055 (3)−0.0081 (19)0.027 (2)0.001 (2)
C60.063 (3)0.047 (2)0.036 (2)−0.002 (2)0.012 (2)0.0077 (18)
C70.039 (2)0.0319 (19)0.034 (2)−0.0023 (17)0.0050 (18)−0.0041 (16)
O20.047 (2)0.083 (2)0.078 (2)−0.0194 (17)0.0213 (18)−0.0023 (18)
N20.049 (2)0.054 (2)0.081 (3)−0.0016 (16)0.021 (2)−0.0125 (17)
C80.045 (3)0.082 (3)0.107 (4)−0.006 (3)0.018 (3)−0.021 (3)
C90.059 (3)0.052 (2)0.055 (3)−0.010 (2)0.016 (2)0.010 (2)
C100.054 (3)0.047 (2)0.052 (3)−0.001 (2)−0.006 (2)0.006 (2)
C110.056 (3)0.047 (2)0.053 (3)0.0013 (19)0.025 (2)0.0025 (19)
C120.047 (3)0.040 (2)0.051 (3)−0.010 (2)0.019 (2)−0.0103 (19)
C130.049 (3)0.054 (2)0.046 (2)0.013 (2)0.010 (2)0.002 (2)
C140.040 (2)0.034 (2)0.055 (2)−0.0028 (17)0.015 (2)−0.0067 (18)
Bi10.02767 (12)0.03032 (11)0.04936 (13)0.00127 (9)0.01004 (9)0.00439 (10)
Cl20.0438 (6)0.0471 (5)0.0623 (6)0.0162 (5)0.0072 (5)0.0057 (5)
Cl30.0500 (7)0.0438 (6)0.0786 (8)−0.0087 (5)−0.0047 (6)−0.0071 (5)
Cl40.0548 (8)0.0659 (6)0.0779 (8)−0.0033 (5)0.0387 (6)0.0005 (6)
O30.078 (4)0.056 (3)0.217 (7)0.0000.063 (5)0.000
Cl10.0523 (10)0.0516 (8)0.0652 (10)0.0000.0056 (8)0.000
O1—C71.342 (4)N2—H2B0.8910
O1—C11.418 (5)N2—H2C0.8890
N1—C41.459 (5)C8—H8A0.9600
N1—H1A0.8902C8—H8B0.9600
N1—H1B0.8898C8—H8C0.9600
N1—H1C0.8890C9—C101.378 (5)
C1—H1D0.9600C9—C121.387 (5)
C1—H1E0.9600C9—H90.9300
C1—H1F0.9600C10—C141.368 (5)
C2—C31.371 (5)C10—H100.9300
C2—C71.386 (5)C11—C141.365 (6)
C2—H20.9300C11—C131.385 (6)
C3—C41.370 (5)C11—H110.9300
C3—H30.9300C12—C131.367 (5)
C4—C51.367 (5)C13—H130.9300
C5—C61.367 (5)Bi1—Cl4i2.6881 (12)
C5—H50.9300Bi1—Cl42.6881 (12)
C6—C71.383 (5)Bi1—Cl32.6925 (11)
C6—H60.9300Bi1—Cl3i2.6925 (11)
O2—C121.347 (4)Bi1—Cl22.6927 (10)
O2—C81.414 (5)Bi1—Cl2i2.6927 (10)
N2—C141.456 (5)O3—H3B0.846 (10)
N2—H2A0.8910
C7—O1—C1118.4 (3)O2—C8—H8B109.5
C4—N1—H1A109.5H8A—C8—H8B109.5
C4—N1—H1B109.4O2—C8—H8C109.5
H1A—N1—H1B109.4H8A—C8—H8C109.5
C4—N1—H1C109.6H8B—C8—H8C109.5
H1A—N1—H1C109.5C10—C9—C12120.1 (4)
H1B—N1—H1C109.4C10—C9—H9120.0
O1—C1—H1D109.5C12—C9—H9120.0
O1—C1—H1E109.5C14—C10—C9120.1 (4)
H1D—C1—H1E109.5C14—C10—H10119.9
O1—C1—H1F109.5C9—C10—H10119.9
H1D—C1—H1F109.5C14—C11—C13119.6 (4)
H1E—C1—H1F109.5C14—C11—H11120.2
C3—C2—C7119.9 (4)C13—C11—H11120.2
C3—C2—H2120.1O2—C12—C13125.7 (4)
C7—C2—H2120.1O2—C12—C9115.3 (4)
C4—C3—C2120.3 (4)C13—C12—C9119.0 (4)
C4—C3—H3119.9C12—C13—C11120.8 (4)
C2—C3—H3119.9C12—C13—H13119.6
C5—C4—C3120.9 (4)C11—C13—H13119.6
C5—C4—N1119.0 (4)C11—C14—C10120.4 (4)
C3—C4—N1120.1 (4)C11—C14—N2118.8 (4)
C6—C5—C4118.8 (4)C10—C14—N2120.8 (4)
C6—C5—H5120.6Cl4i—Bi1—Cl4180.00 (3)
C4—C5—H5120.6Cl4i—Bi1—Cl392.06 (4)
C5—C6—C7121.7 (4)Cl4—Bi1—Cl387.94 (4)
C5—C6—H6119.1Cl4i—Bi1—Cl3i87.94 (4)
C7—C6—H6119.1Cl4—Bi1—Cl3i92.06 (4)
O1—C7—C6116.2 (3)Cl3—Bi1—Cl3i180.00 (7)
O1—C7—C2125.4 (3)Cl4i—Bi1—Cl294.33 (4)
C6—C7—C2118.5 (4)Cl4—Bi1—Cl285.67 (4)
C12—O2—C8118.8 (4)Cl3—Bi1—Cl294.08 (4)
C14—N2—H2A109.5Cl3i—Bi1—Cl285.92 (4)
C14—N2—H2B109.6Cl4i—Bi1—Cl2i85.67 (4)
H2A—N2—H2B109.3Cl4—Bi1—Cl2i94.33 (4)
C14—N2—H2C109.6Cl3—Bi1—Cl2i85.92 (4)
H2A—N2—H2C109.4Cl3i—Bi1—Cl2i94.08 (4)
H2B—N2—H2C109.5Cl2—Bi1—Cl2i180.00 (6)
O2—C8—H8A109.5
C7—C2—C3—C40.2 (5)C12—C9—C10—C14−0.2 (6)
C2—C3—C4—C50.4 (6)C8—O2—C12—C13−7.6 (6)
C2—C3—C4—N1−179.6 (3)C8—O2—C12—C9172.2 (4)
C3—C4—C5—C6−0.2 (6)C10—C9—C12—O2−178.5 (3)
N1—C4—C5—C6179.8 (3)C10—C9—C12—C131.2 (6)
C4—C5—C6—C7−0.5 (6)O2—C12—C13—C11177.9 (4)
C1—O1—C7—C6−172.6 (4)C9—C12—C13—C11−1.8 (6)
C1—O1—C7—C28.1 (5)C14—C11—C13—C121.3 (6)
C5—C6—C7—O1−178.4 (3)C13—C11—C14—C10−0.2 (6)
C5—C6—C7—C21.0 (5)C13—C11—C14—N2−178.9 (3)
C3—C2—C7—O1178.5 (3)C9—C10—C14—C11−0.3 (6)
C3—C2—C7—C6−0.8 (5)C9—C10—C14—N2178.3 (3)
D—H···AD—HH···AD···AD—H···A
N1—H1A···O30.892.012.862 (5)161
N1—H1B···Cl20.892.413.224 (4)152
N1—H1C···Cl10.892.373.231 (4)165
N2—H2A···Cl3ii0.892.673.411 (4)141
N2—H2A···Cl2iii0.892.683.330 (4)131
N2—H2B···Cl4iv0.892.783.312 (3)120
N2—H2B···Cl3v0.892.833.648 (4)153
N2—H2C···Cl1iv0.892.553.418 (4)167
O3—H3B···Cl1vi0.85 (1)2.70 (2)3.202 (6)119 (2)
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
N1—H1A⋯O30.892.012.862 (5)161
N1—H1B⋯Cl20.892.413.224 (4)152
N1—H1C⋯Cl10.892.373.231 (4)165
N2—H2A⋯Cl3i0.892.673.411 (4)141
N2—H2A⋯Cl2ii0.892.683.330 (4)131
N2—H2B⋯Cl4iii0.892.783.312 (3)120
N2—H2B⋯Cl3iv0.892.833.648 (4)153
N2—H2C⋯Cl1iii0.892.553.418 (4)167
O3—H3B⋯Cl1v0.85 (1)2.70 (2)3.202 (6)119 (2)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

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