Literature DB >> 22219770

catena-Poly[[bis-(μ-2-formyl-6-meth-oxy-phenolato)copper(II)sodium]-μ-nitrato].

Po Gao1, Hai-Ge Hou, Ting Gao, Jing-Lin Yang, Yu Yang.   

Abstract

In the title heterodinuclear complex, [CuNa(C(8)H(7)O(3))(2)(NO(3))](n), the Cu(II) ion is five-coordinated in a square-pyramidal arrangement by four atoms of two different ligand molecules in equatorial positions and one remote nitrate O atom in the apical position. The Na(+) ion is eight-coordinated by four ligand O atoms and four nitrate O atoms. The ligand links the Cu(II) and Na ions, forming a layered arrangement extending parallel to (001).

Entities:  

Year:  2011        PMID： 22219770      PMCID： PMC3246950          DOI： 10.1107/S1600536811040025

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


Related literature

For similar nickel–sodium complexes, see Costes et al. (1997a ▶,b ▶).

Experimental

Crystal data

[CuNa(C8H7O3)2(NO3)] M = 450.81 Orthorhombic, a = 7.737 (2) Å b = 13.165 (4) Å c = 16.889 (6) Å V = 1720.2 (9) Å3 Z = 4 Mo Kα radiation μ = 1.35 mm−1 T = 293 K 0.35 × 0.33 × 0.30 mm

Data collection

Rigaku R-AXIS RAPID diffractometer Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.648, T max = 0.691 16868 measured reflections 3926 independent reflections 3692 reflections with I > 2σ(I) R int = 0.025

Refinement

R[F 2 > 2σ(F 2)] = 0.021 wR(F 2) = 0.057 S = 1.03 3926 reflections 255 parameters H-atom parameters constrained Δρmax = 0.22 e Å−3 Δρmin = −0.21 e Å−3 Absolute structure: Flack (1983 ▶), 1671 Friedel pairs Flack parameter: 0.007 (8) Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: CrystalClear (Rigaku/MSC, 2002 ▶); 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: SHELXL97 . Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536811040025/ng5236sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811040025/ng5236Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[CuNa(C8H7O3)2(NO3)]F(000) = 916
Mr = 450.81Dx = 1.741 Mg m−3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 15663 reflections
a = 7.737 (2) Åθ = 3.1–27.5°
b = 13.165 (4) ŵ = 1.35 mm−1
c = 16.889 (6) ÅT = 293 K
V = 1720.2 (9) Å3Block, brown
Z = 40.35 × 0.33 × 0.30 mm
Rigaku R-AXIS RAPID diffractometer3926 independent reflections
Radiation source: fine-focus sealed tube3692 reflections with I > 2σ(I)
graphiteRint = 0.025
ω scansθmax = 27.5°, θmin = 3.1°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)h = −9→10
Tmin = 0.648, Tmax = 0.691k = −17→16
16868 measured reflectionsl = −21→21
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.021H-atom parameters constrained
wR(F2) = 0.057w = 1/[σ2(Fo2) + (0.0375P)2] where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.001
3926 reflectionsΔρmax = 0.22 e Å−3
255 parametersΔρmin = −0.21 e Å−3
0 restraintsAbsolute structure: Flack (1983), 1671 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: 0.007 (8)
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.
xyzUiso*/Ueq
C10.0679 (2)0.92359 (12)0.67688 (10)0.0321 (3)
C20.0859 (2)1.02319 (13)0.70061 (11)0.0375 (4)
H20.03781.07490.67030.045*
C30.1765 (2)1.04734 (13)0.77039 (12)0.0411 (4)
H30.18951.11480.78560.049*
C40.2450 (3)0.97166 (13)0.81555 (10)0.0406 (4)
H40.30250.98780.86220.049*
C50.2298 (2)0.86831 (12)0.79230 (10)0.0331 (3)
C60.14000 (19)0.84231 (11)0.72185 (10)0.0293 (3)
C70.3021 (2)0.79245 (15)0.84132 (11)0.0401 (4)
H70.34520.81490.88970.048*
C8−0.0953 (3)0.96653 (15)0.56154 (13)0.0484 (5)
H8A−0.17811.00340.59260.073*
H8B−0.15290.93410.51800.073*
H8C−0.00951.01260.54160.073*
C90.0758 (2)0.44760 (12)0.54819 (9)0.0309 (3)
C100.0625 (3)0.34687 (13)0.52792 (12)0.0421 (4)
H100.00320.32810.48230.051*
C110.1387 (3)0.27166 (13)0.57635 (13)0.0495 (5)
H110.12920.20360.56220.059*
C120.2248 (3)0.29714 (13)0.64274 (12)0.0446 (5)
H120.27380.24660.67400.054*
C130.2416 (3)0.40139 (11)0.66559 (10)0.0337 (3)
C140.1682 (2)0.47851 (12)0.61750 (9)0.0287 (3)
C150.3276 (2)0.42379 (13)0.73717 (11)0.0379 (4)
H150.37280.36880.76480.046*
C16−0.0964 (3)0.50378 (17)0.43943 (13)0.0513 (5)
H16A−0.02410.47280.40000.077*
H16B−0.14580.56500.41850.077*
H16C−0.18720.45770.45380.077*
Cu10.25742 (3)0.636953 (13)0.726538 (11)0.03049 (6)
N10.5362 (2)0.72115 (11)0.60308 (10)0.0391 (3)
Na10.03464 (14)0.71081 (6)0.56511 (5)0.0556 (2)
O1−0.01427 (18)0.89168 (9)0.60950 (8)0.0423 (3)
O20.11760 (15)0.74989 (9)0.69651 (7)0.0349 (3)
O30.31612 (18)0.69909 (10)0.82857 (8)0.0433 (3)
O40.00468 (16)0.52733 (9)0.50775 (7)0.0367 (3)
O50.17851 (16)0.57479 (8)0.63174 (7)0.0330 (2)
O60.34982 (16)0.50983 (9)0.76779 (8)0.0386 (3)
O70.51745 (17)0.70304 (11)0.67537 (8)0.0449 (3)
O80.4100 (2)0.74389 (12)0.56117 (8)0.0547 (4)
O90.6790 (2)0.7162 (2)0.57232 (13)0.0937 (7)
U11U22U33U12U13U23
C10.0297 (8)0.0350 (8)0.0315 (8)0.0009 (7)0.0035 (7)−0.0002 (7)
C20.0381 (9)0.0324 (8)0.0421 (10)0.0028 (7)0.0080 (7)0.0033 (7)
C30.0414 (9)0.0336 (8)0.0482 (10)−0.0039 (7)0.0074 (9)−0.0076 (8)
C40.0388 (9)0.0458 (9)0.0373 (8)−0.0037 (10)0.0026 (9)−0.0099 (7)
C50.0318 (8)0.0379 (8)0.0296 (7)0.0008 (8)0.0032 (6)−0.0020 (6)
C60.0266 (7)0.0320 (7)0.0294 (7)0.0012 (6)0.0037 (6)−0.0007 (6)
C70.0437 (10)0.0507 (9)0.0258 (8)0.0024 (8)−0.0044 (7)−0.0043 (7)
C80.0524 (12)0.0468 (10)0.0461 (11)0.0120 (10)−0.0117 (9)0.0078 (9)
C90.0315 (8)0.0313 (7)0.0299 (8)0.0006 (7)0.0048 (7)0.0017 (6)
C100.0514 (10)0.0351 (8)0.0399 (9)−0.0018 (8)0.0041 (8)−0.0086 (8)
C110.0703 (14)0.0269 (7)0.0513 (12)0.0020 (9)0.0068 (11)−0.0041 (8)
C120.0541 (12)0.0288 (7)0.0508 (10)0.0105 (9)0.0092 (10)0.0069 (7)
C130.0352 (8)0.0291 (6)0.0367 (8)0.0024 (8)0.0045 (8)0.0056 (6)
C140.0289 (7)0.0278 (7)0.0293 (8)0.0006 (6)0.0053 (6)0.0029 (6)
C150.0399 (9)0.0345 (8)0.0394 (10)0.0085 (8)0.0024 (8)0.0116 (7)
C160.0540 (12)0.0548 (11)0.0453 (11)−0.0040 (10)−0.0180 (10)−0.0021 (9)
Cu10.03520 (10)0.02981 (9)0.02645 (10)0.00292 (9)−0.00451 (9)0.00259 (7)
N10.0461 (9)0.0354 (7)0.0357 (8)−0.0090 (7)0.0044 (7)0.0047 (6)
Na10.0954 (7)0.0374 (4)0.0340 (4)0.0132 (4)−0.0188 (4)0.0012 (3)
O10.0518 (7)0.0344 (6)0.0407 (7)0.0082 (6)−0.0130 (6)0.0016 (5)
O20.0404 (6)0.0302 (5)0.0340 (6)0.0051 (5)−0.0081 (5)−0.0019 (5)
O30.0581 (8)0.0437 (6)0.0282 (6)0.0092 (6)−0.0082 (6)0.0006 (5)
O40.0423 (7)0.0344 (6)0.0334 (6)0.0006 (6)−0.0082 (5)0.0009 (5)
O50.0434 (6)0.0244 (5)0.0312 (6)−0.0007 (5)−0.0066 (5)0.0042 (4)
O60.0415 (6)0.0402 (6)0.0343 (6)0.0054 (5)−0.0075 (6)0.0078 (5)
O70.0448 (7)0.0593 (8)0.0305 (6)−0.0087 (6)−0.0033 (6)0.0084 (6)
O80.0627 (9)0.0642 (9)0.0373 (8)−0.0019 (8)−0.0063 (7)0.0162 (7)
O90.0520 (10)0.158 (2)0.0716 (13)−0.0040 (12)0.0224 (9)0.0250 (14)
C1—O11.370 (2)C14—O51.2925 (19)
C1—C21.378 (2)C15—O61.257 (2)
C1—C61.426 (2)C15—H150.9300
C2—C31.407 (3)C16—O41.428 (2)
C2—H20.9300C16—H16A0.9600
C3—C41.362 (3)C16—H16B0.9600
C3—H30.9300C16—H16C0.9600
C4—C51.421 (2)Cu1—O51.8989 (12)
C4—H40.9300Cu1—O21.9074 (12)
C5—C71.413 (2)Cu1—O61.9487 (12)
C5—C61.420 (2)Cu1—O31.9608 (14)
C6—O21.3013 (19)Cu1—O72.3560 (14)
C7—O31.252 (2)Cu1—Na13.3688 (11)
C7—H70.9300N1—O91.223 (2)
C8—O11.421 (2)N1—O81.243 (2)
C8—H8A0.9600N1—O71.252 (2)
C8—H8B0.9600N1—Na1i2.978 (2)
C8—H8C0.9600Na1—O22.3667 (16)
C9—O41.368 (2)Na1—O52.3900 (14)
C9—C101.373 (2)Na1—O8ii2.4154 (17)
C9—C141.431 (2)Na1—O12.5249 (15)
C10—C111.413 (3)Na1—O42.6129 (16)
C10—H100.9300Na1—O9ii2.749 (2)
C11—C121.347 (3)Na1—O9iii2.755 (2)
C11—H110.9300Na1—O82.937 (2)
C12—C131.431 (2)Na1—N1ii2.978 (2)
C12—H120.9300O8—Na1i2.4154 (17)
C13—C151.411 (3)O9—Na1i2.749 (2)
C13—C141.419 (2)O9—Na1iv2.755 (2)
O1—C1—C2125.48 (15)O8—N1—O7120.68 (16)
O1—C1—C6113.20 (14)O9—N1—Na1i67.31 (13)
C2—C1—C6121.31 (16)O8—N1—Na1i51.77 (9)
C1—C2—C3120.59 (16)O7—N1—Na1i170.58 (13)
C1—C2—H2119.7O2—Na1—O566.12 (4)
C3—C2—H2119.7O2—Na1—O8ii151.95 (6)
C4—C3—C2119.82 (16)O5—Na1—O8ii141.87 (6)
C4—C3—H3120.1O2—Na1—O163.72 (4)
C2—C3—H3120.1O5—Na1—O1129.54 (5)
C3—C4—C5120.89 (17)O8ii—Na1—O188.25 (6)
C3—C4—H4119.6O2—Na1—O4124.94 (5)
C5—C4—H4119.6O5—Na1—O461.52 (4)
C7—C5—C6120.96 (15)O8ii—Na1—O482.27 (5)
C7—C5—C4118.82 (16)O1—Na1—O4165.61 (6)
C6—C5—C4120.21 (15)O2—Na1—O9ii127.27 (7)
O2—C6—C5124.49 (14)O5—Na1—O9ii118.04 (7)
O2—C6—C1118.32 (15)O8ii—Na1—O9ii47.97 (5)
C5—C6—C1117.18 (14)O1—Na1—O9ii88.98 (7)
O3—C7—C5128.84 (17)O4—Na1—O9ii92.63 (7)
O3—C7—H7115.6O2—Na1—O9iii102.93 (7)
C5—C7—H7115.6O5—Na1—O9iii117.63 (7)
O1—C8—H8A109.5O8ii—Na1—O9iii68.52 (6)
O1—C8—H8B109.5O1—Na1—O9iii79.21 (7)
H8A—C8—H8B109.5O4—Na1—O9iii87.24 (7)
O1—C8—H8C109.5O9ii—Na1—O9iii115.72 (6)
H8A—C8—H8C109.5O2—Na1—O873.79 (5)
H8B—C8—H8C109.5O5—Na1—O870.20 (5)
O4—C9—C10125.88 (16)O8ii—Na1—O8109.77 (5)
O4—C9—C14113.03 (14)O1—Na1—O890.86 (5)
C10—C9—C14121.08 (16)O4—Na1—O8102.50 (6)
C9—C10—C11120.06 (18)O9ii—Na1—O861.80 (5)
C9—C10—H10120.0O9iii—Na1—O8169.91 (7)
C11—C10—H10120.0O2—Na1—N1ii145.87 (6)
C12—C11—C10120.92 (16)O5—Na1—N1ii132.26 (6)
C12—C11—H11119.5O8ii—Na1—N1ii23.83 (5)
C10—C11—H11119.5O1—Na1—N1ii90.01 (5)
C11—C12—C13120.54 (17)O4—Na1—N1ii85.69 (5)
C11—C12—H12119.7O9ii—Na1—N1ii24.23 (5)
C13—C12—H12119.7O9iii—Na1—N1ii92.20 (6)
C15—C13—C14121.97 (15)O8—Na1—N1ii85.98 (5)
C15—C13—C12118.31 (16)O2—Na1—Cu133.40 (3)
C14—C13—C12119.70 (16)O5—Na1—Cu133.32 (3)
O5—C14—C13124.79 (15)O8ii—Na1—Cu1171.94 (5)
O5—C14—C9117.52 (14)O1—Na1—Cu196.23 (4)
C13—C14—C9117.69 (15)O4—Na1—Cu194.51 (4)
O6—C15—C13127.26 (15)O9ii—Na1—Cu1125.19 (5)
O6—C15—H15116.4O9iii—Na1—Cu1118.86 (6)
C13—C15—H15116.4O8—Na1—Cu163.60 (3)
O4—C16—H16A109.5N1ii—Na1—Cu1148.94 (5)
O4—C16—H16B109.5C1—O1—C8117.75 (14)
H16A—C16—H16B109.5C1—O1—Na1117.80 (10)
O4—C16—H16C109.5C8—O1—Na1123.41 (12)
H16A—C16—H16C109.5C6—O2—Cu1124.46 (10)
H16B—C16—H16C109.5C6—O2—Na1123.21 (11)
O5—Cu1—O285.95 (5)Cu1—O2—Na1103.51 (5)
O5—Cu1—O692.82 (5)C7—O3—Cu1122.72 (12)
O2—Cu1—O6166.56 (5)C9—O4—C16117.21 (14)
O5—Cu1—O3174.40 (6)C9—O4—Na1119.25 (10)
O2—Cu1—O392.28 (5)C16—O4—Na1123.29 (11)
O6—Cu1—O387.66 (6)C14—O5—Cu1126.82 (10)
O5—Cu1—O797.15 (5)C14—O5—Na1128.20 (11)
O2—Cu1—O795.67 (5)Cu1—O5—Na1102.93 (5)
O6—Cu1—O797.76 (5)C15—O6—Cu1125.21 (11)
O3—Cu1—O788.31 (6)N1—O7—Cu1121.78 (11)
O5—Cu1—Na143.75 (4)N1—O8—Na1i104.40 (12)
O2—Cu1—Na143.08 (4)N1—O8—Na1136.74 (11)
O6—Cu1—Na1136.46 (4)Na1i—O8—Na1116.83 (6)
O3—Cu1—Na1135.18 (4)N1—O9—Na1i88.46 (14)
O7—Cu1—Na191.92 (4)N1—O9—Na1iv157.32 (17)
O9—N1—O8118.74 (18)Na1i—O9—Na1iv112.18 (7)
O9—N1—O7120.58 (18)
Table 1

Selected bond lengths (Å)

Cu1—O51.8989 (12)
Cu1—O21.9074 (12)
Cu1—O61.9487 (12)
Cu1—O31.9608 (14)
Cu1—O72.3560 (14)
Na1—O22.3667 (16)
Na1—O52.3900 (14)
Na1—O8i2.4154 (17)
Na1—O12.5249 (15)
Na1—O42.6129 (16)
Na1—O9i2.749 (2)
Na1—O9ii2.755 (2)
Na1—O82.937 (2)

Symmetry codes: (i) ; (ii) .

  2 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.  A General Route to Strictly Dinuclear Cu(II)/Ln(III) Complexes. Structural Determination and Magnetic Behavior of Two Cu(II)/Gd(III) Complexes.

Authors:  J.-P. Costes; F. Dahan; A. Dupuis; J.-P. Laurent
Journal:  Inorg Chem       Date:  1997-07-30       Impact factor: 5.165
  2 in total
  2 in total

1.  catena-Poly[[bis-(μ-2-formyl-6-meth-oxy-phenolato-1:2κO,O:O,O)copper(II)sodium]-μ-tetra-fluorido-borate-1:1'κF:F'].

Authors:  Yu Yang; Po Gao; Jing-Lin Yang; Hai-Ge Hou; Ting Gao
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-12-10

2.  catena-Poly[copper(II)-bis-(μ-2-formyl-6-meth-oxy-phenolato-κO,O:O,O)-[(methanol-κO)sodium]-μ-perchlorato-κO:O'].

Authors:  Ting Gao; Po Gao; Hong-Feng Li; Ju-Wen Zhang; Li-Li Xu
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2012-01-14
  2 in total

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