Literature DB >> 22199479

Bis[bis-(2,2'-bipyridine-κN,N')chloridocopper(II)] bis-(μ-2,6-pyridine-dicarboxyl-ato)-κO,N,O:O;κO:O,N,O-bis-[aqua-dichloridobismuthate(III)] penta-hydrate.

Hong-Wei Wang, Wan-Lan Liu, Yu-Quan Feng.   

Abstract

In the title compound, [CuCl(C(10)H(8)N(2))(2)](2)[Bi(2)Cl(4)(C(7)H(3)NO(4))(2)(H(2)O)(2)]·5H(2)O, the dianion [Bi(2)Cl(4)(C(7)H(3)NO(4))(2)(H(2)O)(2)](2-) is located about an inversion center. The Cu(II) atom of the cation is coordinated by four N atoms of the two chelating 2,2'-bypyridine ligands and one Cl(-) ion, completing a distorted trigonal-bipyramidal coordination environment. In the anion, each Bi(III) atom is seven-coordinate and is bonded to a tridentate pyridine-2,6-dicarboxyl-ate ligand, a water mol-ecule, two chloride ions and a bridging carboxyl-ate O atom of another carboxyl-ate ligand. The coordination geometry of Bi(III) is distorted penta-gonal-bipyramidal with the Cl(-) ions located in axial positions. The structure of the dianion is additionally stabilized by an intra-molecular O-H⋯O hydrogen bond between the coordinated water mol-ecule and carboxyl-ate O atom. In the crystal, O-H⋯O hydrogen bonds occur . The H atoms of the solvent water mol-ecules could not be located.

Entities:  

Year:  2011        PMID: 22199479      PMCID: PMC3238588          DOI: 10.1107/S1600536811045259

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


Related literature

For examples of bis­muth(III) coordination compounds, see: Sun et al. (2004 ▶); Jiang et al. (2006 ▶); Meng & Zhang (2011 ▶).

Experimental

Crystal data

[CuCl(C10H8N2)2]2[Bi2Cl4(C7H3NO4)2(H2O)2]·5H2O M = 1838.72 Monoclinic, a = 22.880 (6) Å b = 22.044 (6) Å c = 13.628 (4) Å β = 110.130 (4)° V = 6454 (3) Å3 Z = 4 Mo Kα radiation μ = 6.41 mm−1 T = 296 K 0.18 × 0.16 × 0.15 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2008 ▶) T min = 0.392, T max = 0.447 16290 measured reflections 5684 independent reflections 4963 reflections with I > 2σ(I) R int = 0.025

Refinement

R[F 2 > 2σ(F 2)] = 0.025 wR(F 2) = 0.063 S = 1.04 5684 reflections 408 parameters 3 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.88 e Å−3 Δρmin = −0.74 e Å−3 Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT (Bruker, 2008 ▶); data reduction: SAINT; 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/S1600536811045259/gk2419sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811045259/gk2419Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[CuCl(C10H8N2)2]2[Bi2Cl4(C7H3NO4)2(H2O)2]·5H2OF(000) = 3528
Mr = 1838.72Dx = 1.882 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 8126 reflections
a = 22.880 (6) Åθ = 2.4–28.1°
b = 22.044 (6) ŵ = 6.41 mm1
c = 13.628 (4) ÅT = 296 K
β = 110.130 (4)°Block, blue
V = 6454 (3) Å30.18 × 0.16 × 0.15 mm
Z = 4
Bruker APEXII CCD diffractometer5684 independent reflections
Radiation source: fine-focus sealed tube4963 reflections with I > 2σ(I)
graphiteRint = 0.025
φ and ω scansθmax = 25.0°, θmin = 1.8°
Absorption correction: multi-scan (SADABS; Bruker, 2008)h = −27→23
Tmin = 0.392, Tmax = 0.447k = −26→26
16290 measured reflectionsl = −16→14
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.025Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.063H atoms treated by a mixture of independent and constrained refinement
S = 1.04w = 1/[σ2(Fo2) + (0.0312P)2 + 11.1454P] where P = (Fo2 + 2Fc2)/3
5684 reflections(Δ/σ)max = 0.002
408 parametersΔρmax = 0.88 e Å3
3 restraintsΔρmin = −0.74 e Å3
xyzUiso*/Ueq
Bi10.025844 (6)0.242343 (7)0.610971 (11)0.02982 (6)
C10.12686 (18)0.23152 (18)0.8542 (3)0.0326 (9)
C20.16677 (19)0.24402 (17)0.7868 (3)0.0327 (9)
C30.23102 (19)0.25200 (18)0.8283 (4)0.0402 (10)
H3A0.25210.25020.90000.048*
C40.2625 (2)0.2627 (2)0.7598 (4)0.0526 (13)
H4A0.30550.26830.78560.063*
C50.2309 (2)0.2652 (2)0.6536 (4)0.0457 (11)
H5A0.25220.27120.60730.055*
C60.16695 (18)0.25867 (17)0.6173 (3)0.0321 (9)
C70.1267 (2)0.26348 (19)0.5032 (4)0.0379 (10)
C80.1129 (2)0.0957 (2)0.1789 (4)0.0517 (12)
H8A0.09510.08750.10790.062*
C90.0795 (2)0.1308 (2)0.2266 (4)0.0578 (13)
H9A0.04030.14580.18830.069*
C100.1061 (3)0.1424 (2)0.3317 (5)0.0612 (14)
H10A0.08450.16460.36630.073*
C110.1655 (2)0.1207 (2)0.3858 (4)0.0525 (12)
H11A0.18420.12870.45670.063*
C120.1965 (2)0.08714 (19)0.3336 (4)0.0416 (10)
C130.2607 (2)0.0635 (2)0.3840 (3)0.0413 (10)
C140.2988 (2)0.0786 (2)0.4839 (4)0.0592 (13)
H14A0.28460.10480.52420.071*
C150.3586 (2)0.0543 (3)0.5239 (4)0.0638 (14)
H15A0.38480.06460.59070.077*
C160.3783 (2)0.0150 (2)0.4636 (4)0.0610 (14)
H16A0.4180−0.00190.48890.073*
C170.3379 (2)0.0010 (2)0.3640 (4)0.0538 (12)
H17A0.3510−0.02590.32320.065*
C180.1123 (2)−0.0074 (2)−0.0053 (4)0.0475 (11)
H18A0.1014−0.03360.03900.057*
C190.0703 (2)0.0024 (2)−0.1038 (4)0.0530 (12)
H19A0.0315−0.0163−0.12560.064*
C200.0872 (2)0.0408 (2)−0.1695 (4)0.0538 (12)
H20A0.05950.0486−0.23640.065*
C210.1451 (2)0.0674 (2)−0.1356 (4)0.0461 (11)
H21A0.15720.0926−0.17990.055*
C220.18524 (18)0.05626 (17)−0.0343 (3)0.0349 (9)
C230.24907 (18)0.08145 (18)0.0105 (3)0.0367 (10)
C240.2784 (2)0.1136 (2)−0.0478 (4)0.0468 (11)
H24A0.25730.1218−0.11810.056*
C250.3389 (2)0.1332 (2)0.0002 (4)0.0553 (13)
H25A0.35940.1540−0.03780.066*
C260.3683 (2)0.1215 (2)0.1044 (4)0.0535 (12)
H26A0.40890.13460.13850.064*
C270.3365 (2)0.0900 (2)0.1577 (4)0.0488 (11)
H27A0.35650.08260.22860.059*
Cl10.03209 (6)0.36683 (7)0.61824 (12)0.0693 (4)
Cl20.03436 (7)0.12583 (6)0.58147 (13)0.0695 (4)
Cl30.22828 (6)−0.08940 (5)0.17806 (10)0.0560 (3)
Cu10.22536 (2)0.01472 (2)0.17652 (4)0.04341 (14)
N10.13659 (14)0.24776 (13)0.6839 (3)0.0299 (7)
N20.16967 (16)0.07324 (16)0.2309 (3)0.0413 (8)
N30.28081 (16)0.02474 (16)0.3248 (3)0.0440 (9)
N40.16815 (15)0.01917 (15)0.0295 (3)0.0386 (8)
N50.27864 (15)0.06980 (15)0.1128 (3)0.0390 (8)
O10.06762 (13)0.23135 (14)0.8042 (2)0.0413 (7)
O20.15260 (13)0.22296 (15)0.9484 (2)0.0471 (7)
O30.06808 (14)0.25476 (14)0.4818 (2)0.0455 (8)
O40.15195 (14)0.27517 (16)0.4391 (2)0.0516 (8)
O5−0.06953 (17)0.2428 (2)0.4468 (3)0.0731 (12)
O1W0.00000.5052 (4)0.75000.173 (4)
H1−0.073 (5)0.257 (5)0.389 (4)0.208*
H2−0.103 (3)0.233 (5)0.454 (9)0.208*
O3W−0.0652 (3)0.2915 (3)0.2650 (4)0.151 (3)
O2W0.4613 (3)−0.0920 (3)0.3689 (4)0.1270 (19)
U11U22U33U12U13U23
Bi10.02219 (9)0.04836 (10)0.01923 (9)0.00043 (6)0.00754 (6)−0.00092 (6)
C10.028 (2)0.044 (2)0.025 (2)0.0032 (17)0.0069 (17)−0.0018 (17)
C20.029 (2)0.038 (2)0.029 (2)0.0015 (15)0.0080 (18)−0.0032 (17)
C30.027 (2)0.057 (3)0.032 (3)−0.0022 (17)0.0046 (18)−0.0015 (19)
C40.022 (2)0.083 (3)0.047 (3)−0.005 (2)0.004 (2)0.007 (2)
C50.034 (2)0.064 (3)0.045 (3)−0.005 (2)0.021 (2)0.002 (2)
C60.028 (2)0.042 (2)0.028 (2)−0.0020 (16)0.0118 (18)−0.0032 (17)
C70.037 (2)0.049 (2)0.032 (2)−0.0020 (18)0.018 (2)−0.0033 (19)
C80.055 (3)0.054 (3)0.044 (3)0.006 (2)0.014 (2)0.003 (2)
C90.053 (3)0.059 (3)0.063 (4)0.001 (2)0.022 (3)0.002 (3)
C100.069 (4)0.059 (3)0.067 (4)0.000 (3)0.039 (3)−0.008 (3)
C110.064 (3)0.051 (3)0.046 (3)−0.012 (2)0.023 (2)−0.009 (2)
C120.047 (3)0.040 (2)0.039 (3)−0.0089 (19)0.017 (2)0.002 (2)
C130.049 (3)0.046 (2)0.030 (2)−0.012 (2)0.015 (2)0.0052 (19)
C140.063 (3)0.079 (4)0.035 (3)−0.017 (3)0.016 (2)−0.009 (3)
C150.059 (3)0.089 (4)0.035 (3)−0.017 (3)0.006 (3)−0.002 (3)
C160.048 (3)0.073 (4)0.051 (3)−0.005 (2)0.002 (2)0.014 (3)
C170.053 (3)0.060 (3)0.046 (3)0.004 (2)0.013 (2)0.008 (2)
C180.043 (3)0.055 (3)0.041 (3)−0.008 (2)0.011 (2)0.005 (2)
C190.038 (2)0.062 (3)0.052 (3)−0.003 (2)0.007 (2)−0.003 (2)
C200.046 (3)0.067 (3)0.037 (3)0.007 (2)−0.001 (2)−0.001 (2)
C210.052 (3)0.049 (3)0.037 (3)0.005 (2)0.016 (2)0.006 (2)
C220.040 (2)0.035 (2)0.032 (2)0.0012 (17)0.0138 (18)−0.0058 (18)
C230.045 (3)0.033 (2)0.036 (3)0.0007 (17)0.020 (2)−0.0029 (18)
C240.060 (3)0.046 (3)0.038 (3)−0.008 (2)0.021 (2)−0.003 (2)
C250.067 (3)0.048 (3)0.061 (4)−0.019 (2)0.036 (3)−0.009 (2)
C260.049 (3)0.052 (3)0.060 (4)−0.015 (2)0.019 (3)−0.009 (2)
C270.047 (3)0.054 (3)0.041 (3)−0.005 (2)0.009 (2)−0.003 (2)
Cl10.0662 (9)0.0669 (8)0.0728 (10)−0.0064 (6)0.0214 (7)−0.0097 (7)
Cl20.0781 (9)0.0537 (7)0.0808 (10)0.0080 (6)0.0326 (8)0.0003 (7)
Cl30.0835 (9)0.0496 (6)0.0356 (6)0.0040 (6)0.0213 (6)0.0012 (5)
Cu10.0458 (3)0.0514 (3)0.0292 (3)−0.0035 (2)0.0081 (2)0.0028 (2)
N10.0232 (16)0.0408 (19)0.0261 (19)0.0002 (12)0.0092 (14)−0.0019 (14)
N20.045 (2)0.046 (2)0.034 (2)−0.0004 (16)0.0153 (17)0.0033 (16)
N30.044 (2)0.050 (2)0.033 (2)−0.0016 (17)0.0084 (17)0.0047 (17)
N40.0390 (19)0.044 (2)0.031 (2)−0.0048 (15)0.0089 (15)−0.0021 (16)
N50.0378 (19)0.046 (2)0.031 (2)−0.0052 (15)0.0085 (16)−0.0026 (16)
O10.0284 (15)0.070 (2)0.0261 (16)0.0004 (13)0.0101 (12)0.0002 (14)
O20.0369 (16)0.077 (2)0.0258 (17)0.0039 (15)0.0083 (13)0.0036 (15)
O30.0317 (16)0.080 (2)0.0268 (17)−0.0045 (13)0.0126 (13)−0.0020 (14)
O40.0481 (18)0.082 (2)0.0329 (18)−0.0098 (16)0.0247 (15)−0.0006 (17)
O50.036 (2)0.143 (4)0.032 (2)0.0002 (19)0.0021 (16)0.001 (2)
O1W0.187 (9)0.111 (6)0.191 (11)0.0000.026 (8)0.000
O3W0.221 (6)0.136 (5)0.053 (3)−0.077 (5)−0.009 (4)0.012 (3)
O2W0.149 (5)0.119 (4)0.110 (5)0.006 (4)0.040 (4)−0.011 (3)
Bi1—O32.297 (3)C14—H14A0.9300
Bi1—N12.385 (3)C15—C161.373 (8)
Bi1—O12.485 (3)C15—H15A0.9300
Bi1—O52.531 (4)C16—C171.390 (7)
Bi1—Cl22.6174 (15)C16—H16A0.9300
Bi1—Cl12.7479 (16)C17—N31.336 (5)
C1—O21.229 (5)C17—H17A0.9300
C1—O11.290 (5)C18—N41.336 (5)
C1—C21.527 (6)C18—C191.372 (6)
C2—N11.335 (5)C18—H18A0.9300
C2—C31.393 (6)C19—C201.380 (7)
C3—C41.382 (7)C19—H19A0.9300
C3—H3A0.9300C20—C211.375 (6)
C4—C51.379 (7)C20—H20A0.9300
C4—H4A0.9300C21—C221.392 (6)
C5—C61.382 (6)C21—H21A0.9300
C5—H5A0.9300C22—N41.347 (5)
C6—N11.341 (5)C22—C231.483 (5)
C6—C71.515 (6)C23—N51.349 (5)
C7—O41.229 (5)C23—C241.396 (6)
C7—O31.285 (5)C24—C251.381 (6)
C8—N21.341 (6)C24—H24A0.9300
C8—C91.395 (7)C25—C261.371 (7)
C8—H8A0.9300C25—H25A0.9300
C9—C101.374 (7)C26—C271.381 (6)
C9—H9A0.9300C26—H26A0.9300
C10—C111.390 (7)C27—N51.329 (5)
C10—H10A0.9300C27—H27A0.9300
C11—C121.380 (6)Cl3—Cu12.2962 (14)
C11—H11A0.9300Cu1—N41.983 (3)
C12—N21.355 (6)Cu1—N31.994 (4)
C12—C131.485 (6)Cu1—N52.107 (3)
C13—N31.360 (6)Cu1—N22.118 (4)
C13—C141.380 (6)O5—H10.83 (2)
C14—C151.393 (7)O5—H20.83 (2)
O3—Bi1—N169.30 (11)N3—C17—C16122.3 (5)
O3—Bi1—O1135.54 (10)N3—C17—H17A118.9
N1—Bi1—O166.26 (10)C16—C17—H17A118.9
O3—Bi1—O577.55 (13)N4—C18—C19122.7 (4)
N1—Bi1—O5146.83 (13)N4—C18—H18A118.6
O1—Bi1—O5146.85 (12)C19—C18—H18A118.6
O3—Bi1—Cl285.76 (8)C18—C19—C20118.2 (4)
N1—Bi1—Cl289.34 (8)C18—C19—H19A120.9
O1—Bi1—Cl292.60 (8)C20—C19—H19A120.9
O5—Bi1—Cl287.41 (12)C19—C20—C21119.8 (4)
O3—Bi1—Cl183.01 (8)C19—C20—H20A120.1
N1—Bi1—Cl184.28 (8)C21—C20—H20A120.1
O1—Bi1—Cl193.61 (8)C20—C21—C22119.2 (4)
O5—Bi1—Cl192.67 (12)C20—C21—H21A120.4
Cl2—Bi1—Cl1168.47 (5)C22—C21—H21A120.4
O2—C1—O1126.1 (4)N4—C22—C21120.6 (4)
O2—C1—C2119.0 (3)N4—C22—C23115.2 (4)
O1—C1—C2114.9 (4)C21—C22—C23124.2 (4)
N1—C2—C3120.7 (4)N5—C23—C24121.1 (4)
N1—C2—C1116.3 (3)N5—C23—C22115.3 (3)
C3—C2—C1123.0 (4)C24—C23—C22123.6 (4)
C4—C3—C2118.1 (4)C25—C24—C23119.3 (4)
C4—C3—H3A121.0C25—C24—H24A120.4
C2—C3—H3A121.0C23—C24—H24A120.4
C5—C4—C3120.5 (4)C26—C25—C24119.2 (4)
C5—C4—H4A119.7C26—C25—H25A120.4
C3—C4—H4A119.7C24—C25—H25A120.4
C6—C5—C4118.7 (4)C25—C26—C27118.6 (4)
C6—C5—H5A120.6C25—C26—H26A120.7
C4—C5—H5A120.6C27—C26—H26A120.7
N1—C6—C5120.5 (4)N5—C27—C26123.3 (5)
N1—C6—C7115.7 (3)N5—C27—H27A118.4
C5—C6—C7123.8 (4)C26—C27—H27A118.4
O4—C7—O3125.5 (4)N4—Cu1—N3170.69 (14)
O4—C7—C6118.4 (4)N4—Cu1—N580.20 (13)
O3—C7—C6116.1 (4)N3—Cu1—N595.56 (14)
N2—C8—C9123.0 (5)N4—Cu1—N293.21 (14)
N2—C8—H8A118.5N3—Cu1—N280.07 (15)
C9—C8—H8A118.5N5—Cu1—N2107.23 (14)
C10—C9—C8118.2 (5)N4—Cu1—Cl393.77 (10)
C10—C9—H9A120.9N3—Cu1—Cl395.46 (11)
C8—C9—H9A120.9N5—Cu1—Cl3124.09 (10)
C9—C10—C11119.2 (5)N2—Cu1—Cl3128.65 (10)
C9—C10—H10A120.4C2—N1—C6121.4 (3)
C11—C10—H10A120.4C2—N1—Bi1121.7 (3)
C12—C11—C10119.7 (5)C6—N1—Bi1116.8 (3)
C12—C11—H11A120.2C8—N2—C12118.3 (4)
C10—C11—H11A120.2C8—N2—Cu1129.0 (3)
N2—C12—C11121.4 (4)C12—N2—Cu1112.6 (3)
N2—C12—C13115.1 (4)C17—N3—C13119.5 (4)
C11—C12—C13123.5 (4)C17—N3—Cu1123.7 (3)
N3—C13—C14120.6 (4)C13—N3—Cu1116.4 (3)
N3—C13—C12115.4 (4)C18—N4—C22119.4 (4)
C14—C13—C12124.0 (4)C18—N4—Cu1123.7 (3)
C13—C14—C15119.7 (5)C22—N4—Cu1116.5 (3)
C13—C14—H14A120.1C27—N5—C23118.5 (4)
C15—C14—H14A120.1C27—N5—Cu1129.0 (3)
C16—C15—C14119.2 (5)C23—N5—Cu1112.3 (3)
C16—C15—H15A120.4C1—O1—Bi1120.7 (2)
C14—C15—H15A120.4C7—O3—Bi1121.7 (3)
C15—C16—C17118.6 (5)Bi1—O5—H1128 (8)
C15—C16—H16A120.7Bi1—O5—H2117 (8)
C17—C16—H16A120.7H1—O5—H2114 (5)
D—H···AD—HH···AD···AD—H···A
O5—H1···O3W0.83 (2)1.92 (3)2.733 (7)169 (11)
O5—H2···O2i0.83 (2)2.04 (6)2.777 (5)147 (10)
Table 1

Selected bond lengths (Å)

Bi1—O32.297 (3)
Bi1—N12.385 (3)
Bi1—O12.485 (3)
Bi1—O52.531 (4)
Bi1—Cl22.6174 (15)
Bi1—Cl12.7479 (16)
Cl3—Cu12.2962 (14)
Cu1—N41.983 (3)
Cu1—N31.994 (4)
Cu1—N52.107 (3)
Cu1—N22.118 (4)
Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
O5—H1⋯O3W0.83 (2)1.92 (3)2.733 (7)169 (11)
O5—H2⋯O2i0.83 (2)2.04 (6)2.777 (5)147 (10)

Symmetry code: (i) .

  3 in total

Review 1.  Bismuth in medicine.

Authors:  Hongzhe Sun; Li Zhang; Ka-Yee Szeto
Journal:  Met Ions Biol Syst       Date:  2004

2.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

3.  2-(2-Pyrid-yl)pyridinium (2,2'-bipyridine-κN,N')tetra-kis-(nitrato-κO,O')bis-muthate(III).

Authors:  Zhao-Hui Meng; Shu-Shen Zhang
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-09-20
  3 in total

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