Literature DB >> 21578105

Bis{4'-[(2,3,5,6,8,9,11,12-octa-hydro-1,4,7,10,13-benzopenta-oxacyclo-penta-decin-15-yl)meth-oxy]-2,2':6',2''-terpyridine}cadmium(II) bis-(hexa-fluorido-phosphate) trihydrate: a powder study.

Nadezhda M Kurochkina, Andrey S Kuzovlev, Tamara P Puryaeva, Yurii A Velikodny, Vladimir V Chernyshev.   

Abstract

The asymmetric unit of the title compound, [Cd(C(30)H(31)N(3)O(6))(2)](PF(6))(2)·3H(2)O, contains one half-cation with the Cd(II) center situated on a twofold rotational axis, one hexa-fluoridophosphate anion and two uncoordinated water mol-ecules, one of which is also situated on a twofold rotational axis. The cations are associated into columns along the a axis through π-π inter-actions between the pyridine and benzene rings, with a centroid-centroid distance of 3.72 (5) Å. Inter-molecular O-H⋯O, C-H⋯O and C-H⋯F hydrogen bonds consolidate the crystal packing.

Entities:  

Year:  2009        PMID： 21578105      PMCID： PMC2971444          DOI： 10.1107/S1600536809040926

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


Related literature

For the crystal structures of related complexes with the 4′-(4′′′-benzo-15-crown-5)-meth­yloxy-2,2′:6′,2′′-terpyridine ligand, see: Tsivadze et al. (2008 ▶); Logacheva et al. (2009 ▶). For details of the indexing algorithm, see: Visser (1969 ▶).

Experimental

Crystal data

[Cd(C30H31N3O6)2](PF6)2·3H2O M = 1515.54 Orthorhombic, a = 12.720 (3) Å b = 21.101 (3) Å c = 24.795 (5) Å V = 6655 (2) Å3 Z = 4 Cu Kα1 radiation μ = 3.98 mm−1 T = 295 K Specimen shape: flat sheet 15 × 1 × 1 mm Specimen prepared at 101 kPa Specimen prepared at 295 K Particle morphology: no specific habit, colourless

Data collection

Guinier camera G670 diffractometer Specimen mounting: thin layer in the specimen holder of the camera Specimen mounted in transmission mode Scan method: continuous 2θmin = 4.0, 2θmax = 80.0° Increment in 2θ = 0.01°

Refinement

R p = 0.020 R wp = 0.024 R exp = 0.015 R B = 0.061 S = 1.67 Wavelength of incident radiation: 1.54059 Å Profile function: split-type pseudo-Voigt (Toraya, 1986 ▶) 2031 reflections 184 parameters 197 restraints H-atom parameters not refined Preferred orientation correction: none Data collection: Huber G640 (Huber, 2002 ▶); cell refinement: MRIA (Zlokazov & Chernyshev, 1992 ▶); data reduction: Huber G640 (Huber, 2002 ▶); method used to solve structure: simulated annealing (Zhukov et al., 2001 ▶); program(s) used to refine structure: MRIA; molecular graphics: PLATON (Spek, 2009 ▶); software used to prepare material for publication: MRIA and SHELXL97 (Sheldrick, 2008 ▶). Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809040926/er2073sup1.cif Rietveld powder data: contains datablocks I. DOI: 10.1107/S1600536809040926/er2073Isup2.rtv Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cd(C30H31N3O6)2](PF6)2·3H2OF(000) = 3104
Mr = 1515.54Dx = 1.513 Mg m−3
Orthorhombic, PccnCu Kα1 radiation, λ = 1.54059 Å
Hall symbol: -P 2ab 2acµ = 3.98 mm−1
a = 12.720 (3) ÅT = 295 K
b = 21.101 (3) ÅParticle morphology: no specific habit
c = 24.795 (5) Åcolourless
V = 6655 (2) Å3flat_sheet, 15 × 1 mm
Z = 4Specimen preparation: Prepared at 295 K and 101 kPa
Guinier camera G670 diffractometerData collection mode: transmission
Radiation source: line-focus sealed tubeScan method: continuous
Curved Germanium (111)2θmin = 4.00°, 2θmax = 80.00°, 2θstep = 0.01°
Specimen mounting: thin layer in the specimen holder of the camera
Refinement on Inet184 parameters
Least-squares matrix: full with fixed elements per cycle197 restraints
Rp = 0.02045 constraints
Rwp = 0.024H-atom parameters not refined
Rexp = 0.015Weighting scheme based on measured s.u.'s
RBragg = 0.061(Δ/σ)max = 0.004
χ2 = 2.785Background function: Chebyshev polynomial up to the 5th order
7601 data pointsPreferred orientation correction: none
Profile function: split-type pseudo-Voigt (Toraya, 1986)
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.
xyzUiso*/Ueq
Cd0.75000.25000.4194 (14)0.058 (5)*
O11.200 (2)0.111 (2)0.408 (3)0.076 (6)*
O21.459 (2)−0.076 (2)0.327 (3)0.076 (6)*
O31.369 (2)−0.199 (3)0.328 (3)0.076 (6)*
O41.460 (2)−0.257 (3)0.426 (3)0.076 (6)*
O51.6125 (19)−0.161 (2)0.470 (3)0.076 (6)*
O61.606 (2)−0.056 (2)0.395 (3)0.076 (6)*
N10.859 (2)0.304 (2)0.355 (3)0.076 (6)*
N20.917 (2)0.204 (3)0.416 (3)0.076 (6)*
N30.761 (2)0.166 (2)0.484 (3)0.076 (6)*
C10.826 (2)0.354 (3)0.325 (3)0.076 (6)*
H10.75900.36980.33090.091*
C20.887 (2)0.382 (3)0.285 (3)0.076 (6)*
H20.86340.41730.26640.091*
C30.986 (3)0.356 (3)0.274 (3)0.076 (6)*
H31.02740.37180.24640.091*
C41.021 (2)0.305 (3)0.305 (3)0.076 (6)*
H41.08780.28790.29960.091*
C50.955 (2)0.278 (3)0.344 (3)0.076 (6)*
C60.989 (2)0.225 (3)0.380 (3)0.076 (6)*
C71.087 (3)0.195 (3)0.373 (3)0.076 (6)*
H71.13370.20800.34710.091*
C81.111 (2)0.143 (3)0.407 (4)0.076 (6)*
C91.036 (2)0.125 (3)0.447 (3)0.076 (6)*
H91.05240.09280.47160.091*
C100.940 (3)0.154 (3)0.449 (3)0.076 (6)*
C110.854 (2)0.135 (3)0.487 (4)0.076 (6)*
C120.866 (3)0.082 (3)0.522 (3)0.076 (6)*
H120.92820.05890.52080.091*
C130.786 (2)0.066 (3)0.556 (3)0.076 (6)*
H130.79390.03230.58010.091*
C140.692 (2)0.100 (3)0.555 (3)0.076 (6)*
H140.63600.08970.57740.091*
C150.683 (3)0.149 (3)0.518 (4)0.076 (6)*
H150.62060.17220.51660.091*
C161.289 (3)0.129 (3)0.371 (3)0.076 (6)*
H16A1.31370.17130.38010.091*
H16B1.26470.12910.33420.091*
C171.375 (2)0.081 (3)0.379 (3)0.076 (6)*
C181.374 (2)0.025 (3)0.348 (3)0.076 (6)*
H181.32130.01900.32240.091*
C191.450 (2)−0.021 (4)0.356 (4)0.076 (6)*
C201.533 (2)−0.010 (3)0.394 (4)0.076 (6)*
C211.534 (3)0.045 (3)0.424 (3)0.076 (6)*
H211.58540.05080.45000.091*
C221.456 (3)0.091 (3)0.416 (3)0.076 (6)*
H221.45790.12870.43560.091*
C231.374 (3)−0.094 (3)0.293 (3)0.076 (6)*
H23A1.3070−0.08690.31060.091*
H23B1.3750−0.06990.25960.091*
C241.386 (2)−0.163 (3)0.280 (3)0.076 (6)*
H24A1.3360−0.17590.25290.091*
H24B1.4564−0.17140.26670.091*
C251.425 (3)−0.258 (3)0.328 (3)0.076 (6)*
H25A1.4982−0.25140.31970.091*
H25B1.3957−0.28590.29990.091*
C261.413 (2)−0.289 (3)0.383 (3)0.076 (6)*
H26A1.3382−0.29380.39050.091*
H26B1.4423−0.33160.38110.091*
C271.575 (3)−0.263 (3)0.426 (3)0.076 (6)*
H27A1.6059−0.24540.39390.091*
H27B1.5957−0.30710.42990.091*
C281.604 (2)−0.224 (3)0.477 (4)0.076 (6)*
H28A1.5510−0.23190.50450.091*
H28B1.6703−0.23980.49080.091*
C291.700 (3)−0.133 (4)0.445 (4)0.076 (6)*
H29A1.7112−0.15110.40970.091*
H29B1.7629−0.13980.46670.091*
C301.675 (3)−0.061 (3)0.441 (4)0.076 (6)*
H30A1.6398−0.04640.47340.091*
H30B1.7384−0.03670.43570.091*
P10.9384 (18)−0.019 (2)0.343 (2)0.106 (11)*
F110.8318 (18)0.013 (2)0.360 (2)0.183 (12)*
F121.0448 (17)−0.052 (2)0.3259 (19)0.183 (12)*
F130.9814 (18)−0.012 (2)0.402 (2)0.183 (12)*
F140.984 (2)0.046 (2)0.327 (2)0.183 (12)*
F150.8942 (17)−0.029 (2)0.284 (2)0.183 (12)*
F160.8922 (18)−0.086 (2)0.359 (2)0.183 (12)*
O1W0.25000.25000.287 (2)0.120 (12)*
H1W0.24800.22000.26410.180*
O2W0.2037 (18)0.154 (2)0.206 (3)0.106 (12)*
H2W10.15450.14110.18580.159*
H2W20.24130.12350.21710.159*
Cd—N12.42 (6)C13—C141.39 (6)
Cd—N22.34 (3)C14—C151.39 (10)
Cd—N32.39 (6)C16—C171.51 (7)
Cd—N1i2.42 (6)C17—C181.41 (9)
Cd—N2i2.34 (3)C17—C221.40 (8)
Cd—N3i2.39 (6)C18—C191.38 (8)
P1—F151.58 (7)C19—C201.43 (10)
P1—F161.56 (6)C20—C211.38 (10)
P1—F121.57 (4)C21—C221.39 (7)
P1—F131.57 (7)C23—C241.50 (9)
P1—F111.58 (4)C25—C261.51 (10)
P1—F141.56 (6)C27—C281.55 (11)
O1—C161.50 (8)C29—C301.56 (10)
O1—C81.32 (5)C1—H10.93
O2—C231.42 (7)C2—H20.93
O2—C191.37 (10)C3—H30.93
O3—C241.43 (10)C4—H40.93
O3—C251.45 (8)C7—H70.93
O4—C261.40 (9)C9—H90.93
O4—C271.47 (5)C12—H120.93
O5—C291.40 (7)C13—H130.93
O5—C281.34 (8)C14—H140.93
O6—C201.34 (6)C15—H150.93
O6—C301.44 (10)C16—H16B0.97
O1W—H1W0.85C16—H16A0.97
O2W—H2W20.85C18—H180.93
O2W—H2W10.85C21—H210.93
N1—C51.36 (5)C22—H220.93
N1—C11.34 (8)C23—H23A0.97
N2—C61.35 (8)C23—H23B0.97
N2—C101.37 (9)C24—H24B0.97
N3—C151.35 (8)C24—H24A0.97
N3—C111.35 (5)C25—H25A0.97
C1—C21.39 (9)C25—H25B0.97
C2—C31.40 (5)C26—H26A0.97
C3—C41.40 (9)C26—H26B0.97
C4—C51.40 (8)C27—H27B0.97
C5—C61.49 (9)C27—H27A0.97
C6—C71.42 (6)C28—H28B0.97
C7—C81.40 (10)C28—H28A0.97
C8—C91.43 (9)C29—H29A0.97
C9—C101.37 (5)C29—H29B0.97
C10—C111.50 (9)C30—H30B0.97
C11—C121.41 (10)C30—H30A0.97
C12—C131.38 (8)
N1—Cd—N269.5 (17)C19—C20—C21119 (5)
N1—Cd—N3139.8 (11)C20—C21—C22121 (6)
N1—Cd—N1i96 (2)C17—C22—C21120 (6)
N1—Cd—N2i107.5 (19)O2—C23—C24108 (4)
N1—Cd—N3i97.7 (18)O3—C24—C23109 (6)
N2—Cd—N370.3 (17)O3—C25—C26109 (5)
N1i—Cd—N2107.5 (19)O4—C26—C25117 (5)
N2—Cd—N2i176 (3)O4—C27—C28101 (5)
N2—Cd—N3i112.6 (18)O5—C28—C27116 (7)
N1i—Cd—N397.7 (18)O5—C29—C30106 (4)
N2i—Cd—N3112.6 (18)O6—C30—C29104 (6)
N3—Cd—N3i96 (2)N1—C1—H1119.02
N1i—Cd—N2i69.5 (18)C2—C1—H1118.21
N1i—Cd—N3i139.8 (11)C3—C2—H2120.64
N2i—Cd—N3i70.3 (17)C1—C2—H2121.06
F13—P1—F15179 (3)C2—C3—H3120.96
F13—P1—F1689 (3)C4—C3—H3120.23
F14—P1—F1590 (3)C5—C4—H4119.17
F14—P1—F16180 (4)C3—C4—H4120.66
F15—P1—F1690 (3)C6—C7—H7120.20
F11—P1—F12179 (4)C8—C7—H7121.61
F11—P1—F1390 (3)C8—C9—H9119.78
F11—P1—F1490 (3)C10—C9—H9120.01
F11—P1—F1590 (3)C11—C12—H12120.36
F11—P1—F1690 (2)C13—C12—H12120.20
F12—P1—F1390 (3)C12—C13—H13120.62
F12—P1—F1490 (2)C14—C13—H13119.68
F12—P1—F1590 (3)C13—C14—H14121.76
F12—P1—F1691 (3)C15—C14—H14120.43
F13—P1—F1491 (3)N3—C15—H15117.54
C8—O1—C16120 (6)C14—C15—H15119.07
C19—O2—C23118 (4)O1—C16—H16A109.92
C24—O3—C25113 (5)O1—C16—H16B110.65
C26—O4—C27113 (5)C17—C16—H16A109.67
C28—O5—C29122 (5)H16A—C16—H16B108.72
C20—O6—C30119 (7)C17—C16—H16B110.61
H1W—O1W—H1Wii96C17—C18—H18119.46
H2W1—O2W—H2W2111C19—C18—H18120.31
Cd—N1—C5117 (4)C22—C21—H21120.53
Cd—N1—C1123 (3)C20—C21—H21118.82
C1—N1—C5120 (5)C17—C22—H22119.39
C6—N2—C10120 (4)C21—C22—H22120.13
Cd—N2—C6120 (4)O2—C23—H23B110.81
Cd—N2—C10120 (3)O2—C23—H23A111.11
C11—N3—C15119 (6)H23A—C23—H23B108.32
Cd—N3—C11116 (5)C24—C23—H23A109.67
Cd—N3—C15125 (3)C24—C23—H23B108.88
N1—C1—C2123 (4)O3—C24—H24A109.30
C1—C2—C3118 (6)C23—C24—H24B110.14
C2—C3—C4119 (5)O3—C24—H24B109.01
C3—C4—C5120 (4)C23—C24—H24A110.90
C4—C5—C6123 (3)H24A—C24—H24B108.67
N1—C5—C4120 (6)O3—C25—H25B109.47
N1—C5—C6117 (5)C26—C25—H25A110.35
C5—C6—C7122 (5)C26—C25—H25B111.70
N2—C6—C5116 (3)H25A—C25—H25B107.65
N2—C6—C7122 (6)O3—C25—H25A108.83
C6—C7—C8118 (5)O4—C26—H26A108.81
O1—C8—C9115 (7)O4—C26—H26B108.62
O1—C8—C7126 (6)C25—C26—H26B107.92
C7—C8—C9118 (4)H26A—C26—H26B106.66
C8—C9—C10120 (6)C25—C26—H26A107.84
N2—C10—C9121 (5)O4—C27—H27A111.94
C9—C10—C11124 (6)C28—C27—H27A111.83
N2—C10—C11115 (4)C28—C27—H27B111.22
N3—C11—C12121 (5)O4—C27—H27B110.64
N3—C11—C10118 (7)H27A—C27—H27B109.95
C10—C11—C12121 (4)C27—C28—H28A108.37
C11—C12—C13119 (4)C27—C28—H28B108.17
C12—C13—C14120 (6)H28A—C28—H28B107.24
C13—C14—C15118 (5)O5—C28—H28B108.40
N3—C15—C14123 (4)O5—C28—H28A108.38
O1—C16—C17107 (5)C30—C29—H29A111.02
C16—C17—C18119 (5)O5—C29—H29A110.53
C16—C17—C22122 (6)O5—C29—H29B110.18
C18—C17—C22119 (5)H29A—C29—H29B108.73
C17—C18—C19120 (6)C30—C29—H29B110.29
O2—C19—C18125 (7)O6—C30—H30B111.22
C18—C19—C20120 (7)O6—C30—H30A110.53
O2—C19—C20115 (5)H30A—C30—H30B109.26
O6—C20—C19114 (7)C29—C30—H30A110.60
O6—C20—C21127 (6)C29—C30—H30B110.91
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O2W0.852.082.91 (6)165
C3—H3···F15iii0.932.443.21 (7)140
C4—H4···O1Wiv0.932.233.17 (4)178
C4—H4···O1Wi0.932.233.17 (4)178
C7—H7···O1Wiv0.932.283.20 (7)175
C7—H7···O1Wi0.932.283.20 (7)175
C12—H12···F13v0.932.443.10 (7)128
C15—H15···O4v0.932.513.23 (8)135
C22—H22···O5vi0.932.603.31 (10)133
C23—H23B···F15vii0.972.363.23 (8)149
C30—H30B···F11iv0.972.463.23 (8)137
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1W—H1W⋯O2W0.852.082.91 (6)165
C3—H3⋯F15i0.932.443.21 (7)140
C4—H4⋯O1Wii0.932.233.17 (4)178
C4—H4⋯O1Wiii0.932.233.17 (4)178
C7—H7⋯O1Wii0.932.283.20 (7)175
C7—H7⋯O1Wiii0.932.283.20 (7)175
C12—H12⋯F13iv0.932.443.10 (7)128
C15—H15⋯O4iv0.932.513.23 (8)135
C22—H22⋯O5v0.932.603.31 (10)133
C23—H23B⋯F15vi0.972.363.23 (8)149
C30—H30B⋯F11ii0.972.463.23 (8)137

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

  3 in total

1.  A short history of SHELX.

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

2.  Ni(II), Co(II), Cu(II), Zn(II) and Na(I) complexes of a hybrid ligand 4'-(4'''-benzo-15-crown-5)-methyloxy-2,2':6',2''-terpyridine.

Authors:  Nadezhda M Logacheva; Vladimir E Baulin; Aslan Yu Tsivadze; Elena N Pyatova; Irina S Ivanova; Yurii A Velikodny; Vladimir V Chernyshev
Journal:  Dalton Trans       Date:  2009-02-11       Impact factor: 4.390

3.  Structure validation in chemical crystallography.

Authors:  Anthony L Spek
Journal:  Acta Crystallogr D Biol Crystallogr       Date:  2009-01-20
  3 in total

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