Literature DB >> 21203079

catena-Poly[[(nitrato-κO,O')silver(I)]-μ-1,2-bis-(diphenyl-phosphino)ethane-κP:P'].

Xing-Cong Wang1, Yan-Li Wu, Xiu-Li You.   

Abstract

In the title chain compound, [Ag(NO(3))(C(26)H(24)P(2))](n), the bis-(diphenyl-phosphino)ethane (dppe) units link the Ag(+) ions into chains along [001]. A nitrate anion is coordinated to the Ag atom. There is a centre of symmetry at the mid-point of the ethane C-C bond and a twofold rotation axis passes through the Ag, N and terminal O atoms. Each Ag atom is four-coordinated in a distorted tetra-hedral geometry by two O atoms of the nitrate anion and two P atoms of dppe ligands. The two aromatic rings are oriented at a dihedral angle of 73.77 (3)°.

Entities:  

Year:  2008        PMID: 21203079      PMCID: PMC2961910          DOI: 10.1107/S1600536808019442

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


Related literature

For related literature, see: Harker & Tiekink (1990 ▶); Huang et al. (1991 ▶); Menezes Vicenti & Burrow (2007); Yang et al. (1992 ▶).

Experimental

Crystal data

[Ag(NO3)(C26H24P2)] M = 568.27 Monoclinic, a = 17.123 (3) Å b = 14.064 (3) Å c = 11.120 (2) Å β = 108.33 (3)° V = 2542.0 (9) Å3 Z = 4 Mo Kα radiation μ = 0.95 mm−1 T = 223.2 K 0.30 × 0.26 × 0.20 mm

Data collection

Rigaku Mercury diffractometer Absorption correction: multi-scan (Jacobson, 1998 ▶) T min = 0.704, T max = 0.833 12170 measured reflections 2327 independent reflections 2161 reflections with I > 2σ(I) R int = 0.030

Refinement

R[F 2 > 2σ(F 2)] = 0.035 wR(F 2) = 0.087 S = 1.07 2327 reflections 151 parameters H-atom parameters constrained Δρmax = 0.97 e Å−3 Δρmin = −0.45 e Å−3 Data collection: CrystalClear (Rigaku/MSC, 2001 ▶); cell refinement: CrystalClear; data reduction: CrystalStructure (Rigaku/MSC, 2004 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXL97; software used to prepare material for publication: SHELXL97. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808019442/hk2480sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808019442/hk2480Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ag(NO3)(C26H24P2)]F000 = 1152
Mr = 568.27Dx = 1.485 Mg m3
Monoclinic, C2/cMo Kα radiation λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 5049 reflections
a = 17.123 (3) Åθ = 3.5–25.3º
b = 14.064 (3) ŵ = 0.95 mm1
c = 11.120 (2) ÅT = 223.2 K
β = 108.33 (3)ºBlock, colorless
V = 2542.0 (9) Å30.30 × 0.26 × 0.20 mm
Z = 4
Rigaku Mercury diffractometer2327 independent reflections
Radiation source: fine-focus sealed tube2161 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.031
Detector resolution: 14.6306 pixels mm-1θmax = 25.3º
T = 223.15 Kθmin = 3.5º
ω scansh = −20→19
Absorption correction: multi-scan(Jacobson, 1998)k = −16→15
Tmin = 0.704, Tmax = 0.833l = −13→13
12170 measured reflections
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.035H-atom parameters constrained
wR(F2) = 0.087  w = 1/[σ2(Fo2) + (0.0457P)2 + 4.2828P] where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max < 0.001
2327 reflectionsΔρmax = 0.97 e Å3
151 parametersΔρmin = −0.45 e Å3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Experimental. no
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 > 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
Ag10.00000.33644 (2)0.25000.03718 (14)
P10.08413 (5)0.39847 (5)0.13087 (7)0.02910 (19)
O10.06120 (15)0.17517 (16)0.3151 (2)0.0493 (6)
O20.00000.0421 (3)0.25000.0783 (13)
N10.00000.1292 (3)0.25000.0409 (9)
C10.18506 (17)0.4287 (2)0.2384 (3)0.0342 (7)
C20.2341 (2)0.5014 (3)0.2188 (3)0.0486 (8)
H2A0.21600.53810.14570.058*
C30.3100 (2)0.5200 (3)0.3075 (4)0.0635 (11)
H3A0.34260.56930.29430.076*
C40.3370 (2)0.4648 (3)0.4153 (4)0.0633 (11)
H4A0.38780.47710.47500.076*
C50.2902 (2)0.3933 (3)0.4345 (4)0.0612 (11)
H5A0.30940.35600.50690.073*
C60.2142 (2)0.3747 (3)0.3484 (3)0.0472 (8)
H6A0.18220.32570.36390.057*
C70.10284 (19)0.3224 (2)0.0110 (3)0.0351 (7)
C80.1568 (2)0.3472 (3)−0.0540 (4)0.0529 (9)
H8A0.18490.4048−0.03670.064*
C90.1693 (3)0.2867 (3)−0.1445 (4)0.0690 (12)
H9A0.20500.3040−0.18880.083*
C100.1292 (3)0.2022 (3)−0.1684 (4)0.0702 (13)
H10A0.13850.1613−0.22820.084*
C110.0753 (3)0.1761 (3)−0.1058 (4)0.0677 (13)
H11A0.04770.1183−0.12370.081*
C120.0620 (2)0.2364 (2)−0.0154 (3)0.0490 (9)
H12A0.02550.21890.02740.059*
C130.04348 (17)0.5080 (2)0.0442 (3)0.0339 (6)
H13A0.04320.55820.10390.041*
H13B0.07870.5278−0.00460.041*
U11U22U33U12U13U23
Ag10.0364 (2)0.0378 (2)0.0391 (2)0.0000.01439 (15)0.000
P10.0287 (4)0.0281 (4)0.0297 (4)0.0031 (3)0.0081 (3)0.0020 (3)
O10.0397 (13)0.0446 (14)0.0527 (14)0.0038 (10)−0.0010 (11)0.0004 (11)
O20.077 (3)0.038 (2)0.118 (4)0.0000.029 (3)0.000
N10.042 (2)0.033 (2)0.049 (2)0.0000.0154 (19)0.000
C10.0290 (15)0.0384 (16)0.0348 (15)0.0051 (12)0.0096 (13)−0.0052 (13)
C20.0403 (19)0.049 (2)0.054 (2)−0.0047 (15)0.0113 (16)−0.0005 (16)
C30.0357 (19)0.063 (3)0.088 (3)−0.0127 (17)0.014 (2)−0.018 (2)
C40.0361 (19)0.082 (3)0.059 (2)0.006 (2)−0.0046 (18)−0.028 (2)
C50.047 (2)0.083 (3)0.043 (2)0.015 (2)−0.0008 (18)−0.0020 (19)
C60.0372 (18)0.062 (2)0.0404 (18)0.0085 (16)0.0087 (15)0.0075 (16)
C70.0380 (17)0.0331 (16)0.0326 (15)0.0098 (12)0.0088 (13)−0.0003 (12)
C80.054 (2)0.052 (2)0.060 (2)−0.0011 (17)0.0288 (19)−0.0087 (17)
C90.077 (3)0.081 (3)0.062 (3)0.013 (2)0.040 (2)−0.015 (2)
C100.097 (3)0.063 (3)0.049 (2)0.027 (2)0.021 (2)−0.014 (2)
C110.107 (4)0.040 (2)0.047 (2)0.000 (2)0.011 (2)−0.0088 (17)
C120.071 (2)0.0376 (18)0.0369 (17)−0.0022 (16)0.0145 (17)0.0004 (14)
C130.0335 (16)0.0294 (15)0.0366 (15)0.0031 (12)0.0080 (13)0.0042 (12)
Ag1—P12.4066 (9)C5—C61.376 (5)
Ag1—P1i2.4066 (9)C5—H5A0.9300
Ag1—O1i2.508 (2)C6—H6A0.9300
Ag1—O12.508 (2)C7—C121.381 (5)
P1—C71.815 (3)C7—C81.386 (5)
P1—C11.816 (3)C8—C91.385 (5)
P1—C131.834 (3)C8—H8A0.9300
O1—N11.250 (3)C9—C101.357 (7)
O2—N11.225 (5)C9—H9A0.9300
N1—O1i1.250 (3)C10—C111.370 (7)
C1—C21.382 (5)C10—H10A0.9300
C1—C61.393 (4)C11—C121.387 (5)
C2—C31.388 (5)C11—H11A0.9300
C2—H2A0.9300C12—H12A0.9300
C3—C41.381 (6)C13—C13ii1.521 (6)
C3—H3A0.9300C13—H13A0.9700
C4—C51.343 (6)C13—H13B0.9700
C4—H4A0.9300
P1—Ag1—P1i137.49 (4)C4—C5—H5A119.6
P1—Ag1—O1i115.92 (7)C6—C5—H5A119.6
P1i—Ag1—O1i102.63 (7)C5—C6—C1120.4 (4)
P1—Ag1—O1102.63 (6)C5—C6—H6A119.8
P1i—Ag1—O1115.92 (7)C1—C6—H6A119.8
O1i—Ag1—O150.52 (11)C12—C7—C8119.1 (3)
C7—P1—C1105.68 (14)C12—C7—P1118.6 (3)
C7—P1—C13103.59 (14)C8—C7—P1122.4 (3)
C1—P1—C13105.93 (14)C9—C8—C7120.3 (4)
C7—P1—Ag1117.71 (11)C9—C8—H8A119.8
C1—P1—Ag1109.46 (10)C7—C8—H8A119.8
C13—P1—Ag1113.56 (10)C10—C9—C8119.8 (4)
N1—O1—Ag195.88 (19)C10—C9—H9A120.1
O2—N1—O1121.14 (18)C8—C9—H9A120.1
O2—N1—O1i121.14 (18)C9—C10—C11121.0 (4)
O1—N1—O1i117.7 (4)C9—C10—H10A119.5
C2—C1—C6118.3 (3)C11—C10—H10A119.5
C2—C1—P1124.7 (2)C10—C11—C12119.7 (4)
C6—C1—P1117.0 (3)C10—C11—H11A120.2
C1—C2—C3120.5 (4)C12—C11—H11A120.2
C1—C2—H2A119.8C7—C12—C11120.1 (4)
C3—C2—H2A119.8C7—C12—H12A119.9
C4—C3—C2119.6 (4)C11—C12—H12A119.9
C4—C3—H3A120.2C13ii—C13—P1110.4 (3)
C2—C3—H3A120.2C13ii—C13—H13A109.6
C5—C4—C3120.4 (3)P1—C13—H13A109.6
C5—C4—H4A119.8C13ii—C13—H13B109.6
C3—C4—H4A119.8P1—C13—H13B109.6
C4—C5—C6120.9 (4)H13A—C13—H13B108.1
Ag1—P12.4066 (9)
Ag1—O12.508 (2)
P1—Ag1—P1i137.49 (4)
P1—Ag1—O1i115.92 (7)
P1—Ag1—O1102.63 (6)
O1i—Ag1—O150.52 (11)

Symmetry code: (i) .

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