Literature DB >> 22219775

Poly[bis-[μ-1,3-bis-(diphenyl-phosphan-yl)propane-κP:P']-di-μ-thio-cyanato-κS:N;κN:S-disilver(I)].

Li-Na Cui, Yu-Han Jiang, Li-Li Zhou, Qiong-Hua Jin, Cun-Lin Zhang.   

Abstract

In the title coordinpan>ation polymer, [Ag(2)(NCS)(2)(C(27)H(26)P(2))(2)](n), two centrosymmetrically related Ag(+) cations are linked by two thio-cyanate anions into binuclear eight-membered macrocycles. The Ag⋯Ag separation within the macrocycle is 5.4400 (6) Å. The distorted tetra-hedral coordination about each metal atom is completed by the P atoms of two bridging 1,3-bis-(diphenyl-phosphan-yl)propane ligands, forming polymeric ribbons parallel to the a axis.

Entities:  

Year:  2011        PMID: 22219775      PMCID: PMC3246955          DOI: 10.1107/S1600536811041250

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


Related literature

For silver(I) pan> class="Chemical">complexes containing phosphane ligands and coordinated anions, see: Jin, Hu et al. (2010 ▶); Jin, Song et al. (2010 ▶); Effendy et al. (2007 ▶). For related structures, see: Cui, Hu et al. (2010 ▶); Cui, Jin et al. (2010 ▶); Mu et al. (2010 ▶); Affandi et al. (1997 ▶).

Experimental

Crystal data

[Ag2(pan> class="Chemical">NCS)2(C27H26P2)2] M = 1156.74 Monon class="Chemical">clinpan>in class="Chemical">c, a = 7.5478 (9) Å b = 15.8275 (17) Å n class="Chemical">c = 22.229 (3) Å β = 99.727 (1)° V = 2617.4 (5) Å3 Z = 2 Mo Kα radiation μ = 0.99 mm−1 T = 298 K 0.42 × 0.21 × 0.15 mm

Data collection

Bruker SMART Cpan> class="Chemical">CD area-detector diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2007 ▶) T min = 0.682, T max = 0.866 12975 measured reflen class="Chemical">ctionpan>s 4605 independent reflen class="Chemical">ctions 3068 reflen class="Chemical">ctionpan>s with I > 2σ(I) R int = 0.042

Refinement

R[F 2 > 2σ(F 2)] = 0.038 wR(F 2) = 0.079 S = 1.03 4605 reflen class="Chemical">ctionpan>s 298 parameters H-atom parameters n class="Chemical">conpan>strainpan>ed Δρmax = 0.44 e Å−3 Δρmin = −0.50 e Å−3 Data collepan> class="Chemical">ction: SMART (Bruker, 2007 ▶); cell refinement: SAINT-Plus (Bruker, 2007 ▶); data reduction: SAINT-Plus; 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) global, I. DOI: 10.1107/S1600536811041250/rz2645sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811041250/rz2645Isup2.hkl Additional supplementary materials: crystallographipan> class="Chemical">c information; 3D view; checkCIF report
[Ag2(NCS)2(C27H26P2)2]F(000) = 1176
Mr = 1156.74Dx = 1.468 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 3146 reflections
a = 7.5478 (9) Åθ = 2.3–23.9°
b = 15.8275 (17) ŵ = 0.99 mm1
c = 22.229 (3) ÅT = 298 K
β = 99.727 (1)°Prism, white
V = 2617.4 (5) Å30.42 × 0.21 × 0.15 mm
Z = 2
Bruker SMART CCD area-detector diffractometer4605 independent reflections
Radiation source: fine-focus sealed tube3068 reflections with I > 2σ(I)
graphiteRint = 0.042
φ and ω scansθmax = 25.0°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Bruker, 2007)h = −8→8
Tmin = 0.682, Tmax = 0.866k = −18→18
12975 measured reflectionsl = −26→23
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.038Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.079H-atom parameters constrained
S = 1.03w = 1/[σ2(Fo2) + (0.0218P)2 + 2.1307P] where P = (Fo2 + 2Fc2)/3
4605 reflections(Δ/σ)max = 0.002
298 parametersΔρmax = 0.44 e Å3
0 restraintsΔρmin = −0.50 e Å3
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
Ag10.67725 (4)0.369866 (19)0.563731 (15)0.04506 (12)
P10.84677 (14)0.23813 (6)0.56205 (5)0.0330 (3)
P20.53770 (14)0.35222 (6)0.65884 (5)0.0356 (3)
S10.82981 (18)0.51569 (8)0.57515 (8)0.0920 (6)
N10.5431 (6)0.6134 (3)0.51878 (19)0.0707 (13)
C10.6602 (7)0.5719 (3)0.5414 (2)0.0519 (12)
C21.0481 (5)0.2237 (2)0.61989 (17)0.0356 (9)
H2A1.01490.22700.66010.043*
H2B1.09700.16780.61540.043*
C30.1935 (5)0.2899 (2)0.61504 (18)0.0400 (10)
H3A0.22560.28770.57460.048*
H3B0.14680.34580.62090.048*
C40.3605 (5)0.2739 (2)0.66287 (17)0.0368 (10)
H4A0.40670.21790.65680.044*
H4B0.32760.27560.70320.044*
C50.9279 (5)0.2047 (2)0.49304 (17)0.0350 (9)
C60.9994 (6)0.2658 (3)0.46022 (18)0.0483 (12)
H60.99320.32230.47120.058*
C71.0802 (7)0.2442 (3)0.4110 (2)0.0641 (14)
H71.13060.28590.38980.077*
C81.0861 (7)0.1617 (3)0.3936 (2)0.0651 (14)
H81.14240.14710.36090.078*
C91.0091 (6)0.1002 (3)0.4243 (2)0.0588 (13)
H91.00960.04420.41160.071*
C100.9309 (5)0.1216 (3)0.47387 (18)0.0449 (11)
H100.87950.07980.49470.054*
C110.6995 (5)0.1523 (2)0.57727 (17)0.0343 (10)
C120.5367 (6)0.1429 (3)0.5382 (2)0.0523 (12)
H120.50770.17900.50500.063*
C130.4176 (6)0.0806 (4)0.5481 (2)0.0721 (15)
H130.30980.07430.52130.087*
C140.4571 (7)0.0281 (3)0.5973 (3)0.0702 (15)
H140.3768−0.01420.60370.084*
C150.6145 (7)0.0377 (3)0.6370 (2)0.0641 (14)
H150.64070.00260.67090.077*
C160.7344 (6)0.0994 (3)0.6269 (2)0.0480 (11)
H160.84140.10550.65420.058*
C170.4373 (5)0.4470 (2)0.68533 (19)0.0369 (10)
C180.3580 (6)0.5036 (3)0.6417 (2)0.0508 (12)
H180.36700.49490.60090.061*
C190.2658 (7)0.5725 (3)0.6579 (3)0.0698 (15)
H190.21190.60990.62800.084*
C200.2531 (7)0.5864 (3)0.7180 (3)0.0699 (16)
H200.18970.63270.72900.084*
C210.3336 (7)0.5319 (3)0.7613 (2)0.0666 (14)
H210.32650.54160.80210.080*
C220.4260 (6)0.4621 (3)0.7455 (2)0.0532 (12)
H220.48060.42530.77560.064*
C230.7159 (5)0.3225 (2)0.72144 (18)0.0376 (10)
C240.8650 (6)0.3745 (3)0.7347 (2)0.0527 (12)
H240.86770.42520.71360.063*
C251.0084 (6)0.3527 (3)0.7782 (2)0.0658 (15)
H251.10650.38890.78660.079*
C261.0090 (7)0.2786 (4)0.8094 (2)0.0685 (15)
H261.10630.26450.83920.082*
C270.8650 (7)0.2248 (3)0.7963 (2)0.0623 (14)
H270.86600.17350.81680.075*
C280.7187 (6)0.2465 (3)0.75300 (19)0.0490 (11)
H280.62120.20990.74480.059*
U11U22U33U12U13U23
Ag10.0491 (2)0.03714 (18)0.0486 (2)0.00698 (17)0.00730 (15)0.00473 (16)
P10.0307 (6)0.0291 (6)0.0388 (6)0.0003 (4)0.0047 (5)0.0014 (4)
P20.0317 (6)0.0380 (6)0.0375 (6)−0.0022 (5)0.0072 (5)−0.0028 (5)
S10.0498 (9)0.0493 (8)0.1629 (16)−0.0138 (7)−0.0224 (10)0.0306 (9)
N10.067 (3)0.062 (3)0.072 (3)−0.004 (2)−0.021 (2)0.019 (2)
C10.060 (3)0.039 (3)0.051 (3)−0.018 (2)−0.004 (3)0.006 (2)
C20.033 (2)0.036 (2)0.038 (2)−0.0019 (18)0.0040 (19)−0.0019 (18)
C30.035 (2)0.037 (2)0.046 (3)−0.0038 (19)0.000 (2)−0.0005 (19)
C40.032 (2)0.033 (2)0.045 (3)−0.0007 (18)0.005 (2)−0.0008 (19)
C50.032 (2)0.035 (2)0.037 (2)−0.0003 (18)0.0022 (19)0.0000 (18)
C60.067 (3)0.038 (3)0.040 (3)−0.009 (2)0.009 (2)0.001 (2)
C70.091 (4)0.059 (3)0.046 (3)−0.025 (3)0.025 (3)−0.006 (2)
C80.078 (4)0.077 (4)0.046 (3)−0.013 (3)0.028 (3)−0.016 (3)
C90.078 (4)0.048 (3)0.053 (3)0.001 (3)0.019 (3)−0.017 (2)
C100.051 (3)0.038 (3)0.047 (3)−0.007 (2)0.012 (2)−0.001 (2)
C110.031 (2)0.033 (2)0.041 (3)−0.0021 (17)0.011 (2)−0.0036 (18)
C120.043 (3)0.059 (3)0.052 (3)−0.009 (2)−0.001 (2)0.004 (2)
C130.039 (3)0.096 (4)0.078 (4)−0.026 (3)0.001 (3)−0.014 (3)
C140.059 (4)0.067 (4)0.091 (4)−0.031 (3)0.029 (3)−0.007 (3)
C150.064 (4)0.048 (3)0.082 (4)−0.013 (3)0.016 (3)0.021 (3)
C160.039 (3)0.048 (3)0.056 (3)−0.006 (2)0.006 (2)0.012 (2)
C170.027 (2)0.036 (2)0.047 (3)−0.0043 (18)0.003 (2)−0.003 (2)
C180.051 (3)0.043 (3)0.056 (3)0.000 (2)0.001 (2)−0.010 (2)
C190.065 (4)0.041 (3)0.098 (4)0.008 (3)−0.002 (3)0.000 (3)
C200.051 (3)0.042 (3)0.117 (5)0.004 (2)0.017 (3)−0.028 (3)
C210.068 (4)0.066 (3)0.069 (4)−0.002 (3)0.023 (3)−0.026 (3)
C220.057 (3)0.054 (3)0.049 (3)0.003 (2)0.009 (2)−0.006 (2)
C230.033 (2)0.040 (2)0.040 (2)0.0045 (19)0.008 (2)−0.0065 (19)
C240.044 (3)0.053 (3)0.058 (3)0.001 (2)−0.001 (2)−0.012 (2)
C250.038 (3)0.080 (4)0.075 (4)−0.001 (3)−0.005 (3)−0.029 (3)
C260.047 (3)0.089 (4)0.063 (4)0.025 (3)−0.009 (3)−0.008 (3)
C270.057 (3)0.069 (3)0.060 (3)0.021 (3)0.007 (3)0.011 (3)
C280.038 (3)0.056 (3)0.054 (3)0.003 (2)0.010 (2)0.002 (2)
Ag1—N1i2.274 (4)C11—C161.374 (5)
Ag1—P12.4499 (10)C11—C121.388 (5)
Ag1—P22.5316 (11)C12—C131.377 (6)
Ag1—S12.5726 (13)C12—H120.9300
P1—C111.823 (4)C13—C141.365 (7)
P1—C51.823 (4)C13—H130.9300
P1—C21.832 (4)C14—C151.363 (6)
P2—C171.823 (4)C14—H140.9300
P2—C231.826 (4)C15—C161.376 (5)
P2—C41.837 (4)C15—H150.9300
S1—C11.633 (5)C16—H160.9300
N1—C11.147 (5)C17—C221.375 (5)
N1—Ag1i2.274 (4)C17—C181.380 (5)
C2—C3ii1.535 (5)C18—C191.374 (6)
C2—H2A0.9700C18—H180.9300
C2—H2B0.9700C19—C201.375 (7)
C3—C41.527 (5)C19—H190.9300
C3—C2iii1.535 (5)C20—C211.356 (7)
C3—H3A0.9700C20—H200.9300
C3—H3B0.9700C21—C221.384 (6)
C4—H4A0.9700C21—H210.9300
C4—H4B0.9700C22—H220.9300
C5—C61.376 (5)C23—C241.386 (5)
C5—C101.384 (5)C23—C281.391 (5)
C6—C71.382 (6)C24—C251.369 (6)
C6—H60.9300C24—H240.9300
C7—C81.365 (6)C25—C261.362 (7)
C7—H70.9300C25—H250.9300
C8—C91.373 (6)C26—C271.372 (7)
C8—H80.9300C26—H260.9300
C9—C101.378 (5)C27—C281.381 (6)
C9—H90.9300C27—H270.9300
C10—H100.9300C28—H280.9300
N1i—Ag1—P1113.55 (11)C5—C10—H10119.6
N1i—Ag1—P2109.61 (12)C16—C11—C12117.8 (4)
P1—Ag1—P2102.18 (4)C16—C11—P1124.3 (3)
N1i—Ag1—S1103.26 (10)C12—C11—P1117.9 (3)
P1—Ag1—S1122.60 (4)C13—C12—C11120.7 (4)
P2—Ag1—S1105.01 (5)C13—C12—H12119.7
C11—P1—C5103.99 (17)C11—C12—H12119.7
C11—P1—C2103.66 (17)C14—C13—C12120.2 (5)
C5—P1—C2101.39 (17)C14—C13—H13119.9
C11—P1—Ag1107.16 (12)C12—C13—H13119.9
C5—P1—Ag1120.68 (12)C15—C14—C13119.9 (5)
C2—P1—Ag1117.99 (12)C15—C14—H14120.0
C17—P2—C23105.00 (18)C13—C14—H14120.0
C17—P2—C4101.19 (17)C14—C15—C16119.9 (5)
C23—P2—C4103.73 (18)C14—C15—H15120.1
C17—P2—Ag1115.67 (13)C16—C15—H15120.1
C23—P2—Ag1107.94 (13)C11—C16—C15121.5 (4)
C4—P2—Ag1121.62 (13)C11—C16—H16119.3
C1—S1—Ag198.04 (15)C15—C16—H16119.3
C1—N1—Ag1i145.6 (4)C22—C17—C18118.7 (4)
N1—C1—S1177.9 (4)C22—C17—P2123.7 (3)
C3ii—C2—P1112.6 (3)C18—C17—P2117.5 (3)
C3ii—C2—H2A109.1C19—C18—C17120.7 (4)
P1—C2—H2A109.1C19—C18—H18119.7
C3ii—C2—H2B109.1C17—C18—H18119.7
P1—C2—H2B109.1C18—C19—C20120.2 (5)
H2A—C2—H2B107.8C18—C19—H19119.9
C4—C3—C2iii110.7 (3)C20—C19—H19119.9
C4—C3—H3A109.5C21—C20—C19119.5 (5)
C2iii—C3—H3A109.5C21—C20—H20120.3
C4—C3—H3B109.5C19—C20—H20120.3
C2iii—C3—H3B109.5C20—C21—C22120.8 (5)
H3A—C3—H3B108.1C20—C21—H21119.6
C3—C4—P2112.1 (3)C22—C21—H21119.6
C3—C4—H4A109.2C17—C22—C21120.2 (4)
P2—C4—H4A109.2C17—C22—H22119.9
C3—C4—H4B109.2C21—C22—H22119.9
P2—C4—H4B109.2C24—C23—C28117.7 (4)
H4A—C4—H4B107.9C24—C23—P2118.4 (3)
C6—C5—C10118.5 (4)C28—C23—P2123.6 (3)
C6—C5—P1117.4 (3)C25—C24—C23121.1 (5)
C10—C5—P1124.1 (3)C25—C24—H24119.4
C5—C6—C7120.7 (4)C23—C24—H24119.4
C5—C6—H6119.6C26—C25—C24120.7 (5)
C7—C6—H6119.7C26—C25—H25119.6
C8—C7—C6120.1 (4)C24—C25—H25119.6
C8—C7—H7119.9C25—C26—C27119.5 (5)
C6—C7—H7119.9C25—C26—H26120.2
C7—C8—C9120.0 (4)C27—C26—H26120.2
C7—C8—H8120.0C26—C27—C28120.3 (5)
C9—C8—H8120.0C26—C27—H27119.8
C8—C9—C10119.8 (4)C28—C27—H27119.8
C8—C9—H9120.1C27—C28—C23120.6 (4)
C10—C9—H9120.1C27—C28—H28119.7
C9—C10—C5120.8 (4)C23—C28—H28119.7
C9—C10—H10119.6
N1i—Ag1—P1—C11−72.24 (18)C5—P1—C11—C16113.2 (3)
P2—Ag1—P1—C1145.70 (13)C2—P1—C11—C167.6 (4)
S1—Ag1—P1—C11162.61 (14)Ag1—P1—C11—C16−117.9 (3)
N1i—Ag1—P1—C546.28 (19)C5—P1—C11—C12−70.8 (3)
P2—Ag1—P1—C5164.22 (15)C2—P1—C11—C12−176.4 (3)
S1—Ag1—P1—C5−78.87 (15)Ag1—P1—C11—C1258.1 (3)
N1i—Ag1—P1—C2171.41 (18)C16—C11—C12—C13−2.1 (6)
P2—Ag1—P1—C2−70.65 (14)P1—C11—C12—C13−178.4 (4)
S1—Ag1—P1—C246.26 (15)C11—C12—C13—C141.1 (7)
N1i—Ag1—P2—C17−71.60 (18)C12—C13—C14—C150.5 (8)
P1—Ag1—P2—C17167.68 (14)C13—C14—C15—C16−1.1 (8)
S1—Ag1—P2—C1738.74 (15)C12—C11—C16—C151.6 (6)
N1i—Ag1—P2—C23171.17 (17)P1—C11—C16—C15177.6 (3)
P1—Ag1—P2—C2350.46 (14)C14—C15—C16—C110.0 (7)
S1—Ag1—P2—C23−78.48 (14)C23—P2—C17—C22−32.1 (4)
N1i—Ag1—P2—C451.68 (18)C4—P2—C17—C2275.6 (4)
P1—Ag1—P2—C4−69.03 (15)Ag1—P2—C17—C22−150.9 (3)
S1—Ag1—P2—C4162.02 (15)C23—P2—C17—C18152.4 (3)
N1i—Ag1—S1—C124.7 (2)C4—P2—C17—C18−99.9 (3)
P1—Ag1—S1—C1154.31 (17)Ag1—P2—C17—C1833.6 (4)
P2—Ag1—S1—C1−90.17 (18)C22—C17—C18—C19−1.5 (6)
C11—P1—C2—C3ii179.5 (3)P2—C17—C18—C19174.2 (3)
C5—P1—C2—C3ii71.8 (3)C17—C18—C19—C200.6 (7)
Ag1—P1—C2—C3ii−62.3 (3)C18—C19—C20—C210.6 (8)
C2iii—C3—C4—P2−179.7 (3)C19—C20—C21—C22−0.9 (8)
C17—P2—C4—C369.1 (3)C18—C17—C22—C211.2 (6)
C23—P2—C4—C3177.8 (3)P2—C17—C22—C21−174.2 (3)
Ag1—P2—C4—C3−60.7 (3)C20—C21—C22—C170.0 (7)
C11—P1—C5—C6161.6 (3)C17—P2—C23—C24−68.3 (3)
C2—P1—C5—C6−91.1 (3)C4—P2—C23—C24−174.1 (3)
Ag1—P1—C5—C641.5 (4)Ag1—P2—C23—C2455.6 (3)
C11—P1—C5—C10−22.2 (4)C17—P2—C23—C28118.0 (3)
C2—P1—C5—C1085.2 (4)C4—P2—C23—C2812.2 (4)
Ag1—P1—C5—C10−142.3 (3)Ag1—P2—C23—C28−118.1 (3)
C10—C5—C6—C7−3.1 (6)C28—C23—C24—C25−1.3 (6)
P1—C5—C6—C7173.3 (4)P2—C23—C24—C25−175.4 (3)
C5—C6—C7—C81.5 (7)C23—C24—C25—C260.6 (7)
C6—C7—C8—C91.1 (8)C24—C25—C26—C270.8 (7)
C7—C8—C9—C10−2.1 (8)C25—C26—C27—C28−1.5 (7)
C8—C9—C10—C50.4 (7)C26—C27—C28—C230.8 (7)
C6—C5—C10—C92.2 (6)C24—C23—C28—C270.6 (6)
P1—C5—C10—C9−174.1 (3)P2—C23—C28—C27174.4 (3)
  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.  (Methanol-κO)(perchlorato-κO)bis-(triphenyl-phosphine-κP)silver(I).

Authors:  Li-Na Cui; Qiong-Hua Jin; Ke-Yi Hu; Cun-Lin Zhang
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-07-21

3.  (Perchlorato-κO)tris-(triphenyl-phosphine-κP)silver(I).

Authors:  Li-Na Cui; Ke-Yi Hu; Qiong-Hua Jin; Cun-Lin Zhang
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-07-03
  3 in total

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