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The reaction between the metal diphosphine [Ag2(dppa)2](BF4)2 [dppa is bis­(di­phenyl­phosphino)­amine, C24H21N2P2] and the metal thiol­ate [Bu4N]2[Mo(mnt)3] (mnt is cis-1,2-di­cyano­ethyl­ene-1,2-di­thiol­ate, C4N2S2) gave the title compound, [Ag2(dppa)2(MeCN)2][Mo(mnt)3]. The Ag...Ag distance of 2.9501 (13) Å is shorter than the sum of van der Waals radii for two Ag atoms, indicating a weak metal–metal contact in the complex. The cation lies on an inversion centre and the anion lies on a twofold axis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802018408/cv6151sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802018408/cv6151Isup2.hkl
Contains datablock I

CCDC reference: 200724

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.014 Å
  • R factor = 0.063
  • wR factor = 0.135
  • Data-to-parameter ratio = 15.6

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
ABSTM_02 Alert C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.729 1.000 Tmin' and Tmax expected: 0.677 0.744 RR' = 0.802 Please check that your absorption correction is appropriate. PLAT_371 Alert C Long C(sp2)-C(sp1) Bond C51 - C52 = 1.43 Ang. PLAT_371 Alert C Long C(sp2)-C(sp1) Bond C53 - C54 = 1.42 Ang. PLAT_371 Alert C Long C(sp2)-C(sp1) Bond C55 - C56 = 1.44 Ang. General Notes
ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.744 Tmax scaled 0.744 Tmin scaled 0.543
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
4 Alert Level C = Please check

Computing details top

Data collection: SMART (Siemens, 1994); cell refinement: SMART and SAINT (Siemens, 1994); data reduction: XPREP (Siemens, 1994); program(s) used to solve structure: SHELXTL (Siemens, 1994); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Bis[µ-bis(diphenylphosphino)amine-κP:P']bis[acetonitrilesiliver(I)] tris(cis-1,2-dicyanoethylene 1,2-dithiolate)molybdenate(IV) top
Crystal data top
[Ag2(C24H21N2P2)2(C2H3N)2][Mo(C4N2S2)3]Dx = 1.517 Mg m3
Mr = 1585.1Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PbcnCell parameters from 5955 reflections
a = 17.181 (3) Åθ = 1.5–25.1°
b = 15.313 (3) ŵ = 1.06 mm1
c = 26.386 (5) ÅT = 293 K
V = 6942 (2) Å3Prism, dark-green
Z = 40.36 × 0.34 × 0.28 mm
F(000) = 3176
Data collection top
Siemens SMART CCD
diffractometer
6143 independent reflections
Radiation source: fine-focus sealed tube3749 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.080
ω scansθmax = 25.1°, θmin = 1.5°
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
h = 1320
Tmin = 0.729, Tmax = 1.000k = 1817
19737 measured reflectionsl = 3121
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.063Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.135H-atom parameters constrained
S = 1.17 w = 1/[σ2(Fo2) + (0.0205P)2 + 30.6018P]
where P = (Fo2 + 2Fc2)/3
6143 reflections(Δ/σ)max = 0.001
393 parametersΔρmax = 0.40 e Å3
0 restraintsΔρmin = 0.55 e Å3
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mo0.50000.96380 (5)0.75000.0401 (2)
Ag0.49209 (4)0.58946 (4)0.52007 (2)0.0545 (2)
P10.48015 (11)0.52739 (12)0.60463 (7)0.0439 (5)
P20.44075 (11)0.35718 (12)0.55482 (7)0.0436 (5)
N0.4472 (3)0.4243 (4)0.6054 (2)0.0460 (15)
H0A0.43220.40380.63410.055*
N10.3565 (5)0.5771 (6)0.4914 (4)0.097 (3)
C10.2946 (7)0.5602 (7)0.4839 (5)0.091 (3)
C20.2135 (7)0.5395 (8)0.4760 (6)0.159 (7)
H2A0.18970.52560.50790.191*
H2B0.20940.49020.45360.191*
H2C0.18760.58880.46120.191*
C110.4107 (5)0.5851 (5)0.6438 (3)0.052 (2)
C120.3324 (6)0.5746 (7)0.6346 (4)0.087 (3)
H12A0.31610.53590.60950.104*
C130.2771 (7)0.6212 (10)0.6623 (5)0.119 (5)
H13A0.22440.61260.65620.143*
C140.3007 (10)0.6797 (9)0.6984 (6)0.118 (5)
H14A0.26420.71220.71620.142*
C150.3764 (9)0.6897 (7)0.7078 (5)0.105 (4)
H15A0.39210.72920.73260.126*
C160.4320 (6)0.6429 (6)0.6817 (4)0.079 (3)
H16A0.48430.65020.68960.095*
C210.5683 (4)0.5276 (5)0.6421 (3)0.0471 (19)
C220.5783 (6)0.4803 (7)0.6855 (4)0.086 (3)
H22A0.53820.44460.69690.103*
C230.6468 (7)0.4846 (7)0.7125 (4)0.100 (4)
H23A0.65240.45150.74180.120*
C240.7055 (6)0.5358 (7)0.6973 (4)0.082 (3)
H24A0.75130.53890.71590.098*
C250.6969 (6)0.5828 (8)0.6544 (5)0.110 (4)
H25A0.73730.61850.64350.132*
C260.6297 (5)0.5789 (7)0.6268 (4)0.087 (3)
H26A0.62540.61150.59720.105*
C310.3376 (4)0.3330 (5)0.5479 (3)0.0465 (19)
C320.2858 (5)0.3376 (7)0.5874 (4)0.079 (3)
H32A0.30340.35170.61970.095*
C330.2063 (6)0.3209 (8)0.5792 (4)0.097 (4)
H33A0.17120.32480.60590.117*
C340.1808 (6)0.2989 (7)0.5319 (4)0.084 (3)
H34A0.12820.28830.52640.100*
C350.2317 (5)0.2924 (6)0.4930 (4)0.076 (3)
H35A0.21400.27580.46110.091*
C360.3098 (5)0.3104 (5)0.5002 (3)0.062 (2)
H36A0.34400.30740.47300.075*
C410.4824 (4)0.2560 (5)0.5783 (3)0.0473 (19)
C420.5525 (5)0.2589 (6)0.6039 (4)0.070 (3)
H42A0.57660.31240.60970.084*
C430.5873 (6)0.1828 (7)0.6210 (4)0.082 (3)
H43A0.63400.18590.63880.099*
C440.5542 (7)0.1040 (7)0.6121 (4)0.091 (4)
H44A0.57780.05310.62360.109*
C450.4866 (8)0.1004 (6)0.5865 (5)0.110 (4)
H45A0.46420.04620.57990.132*
C460.4495 (6)0.1753 (6)0.5696 (4)0.087 (3)
H46A0.40240.17120.55240.105*
S10.57730 (12)1.08156 (13)0.78096 (8)0.0533 (5)
N20.5943 (4)1.3207 (5)0.7971 (3)0.069 (2)
C510.5328 (4)1.1784 (4)0.7640 (3)0.0461 (19)
C520.5678 (5)1.2580 (5)0.7814 (3)0.0494 (19)
S20.62374 (11)0.91214 (14)0.72242 (8)0.0563 (5)
S30.45993 (12)0.89637 (13)0.67281 (8)0.0550 (5)
N30.7362 (5)0.7991 (6)0.6239 (4)0.106 (3)
N40.5176 (5)0.7643 (5)0.5621 (3)0.083 (2)
C530.6114 (5)0.8581 (5)0.6654 (3)0.056 (2)
C540.6799 (5)0.8233 (6)0.6427 (3)0.070 (3)
C550.5405 (5)0.8497 (5)0.6444 (3)0.053 (2)
C560.5279 (5)0.8024 (6)0.5980 (3)0.066 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo0.0423 (5)0.0347 (5)0.0433 (5)0.0000.0007 (5)0.000
Ag0.0605 (4)0.0548 (4)0.0483 (3)0.0016 (3)0.0100 (3)0.0144 (3)
P10.0525 (12)0.0397 (10)0.0394 (11)0.0024 (9)0.0061 (9)0.0021 (8)
P20.0500 (12)0.0405 (11)0.0404 (11)0.0082 (9)0.0045 (9)0.0038 (9)
N0.061 (4)0.042 (3)0.034 (3)0.006 (3)0.009 (3)0.001 (3)
N10.061 (5)0.105 (7)0.125 (8)0.015 (5)0.012 (6)0.001 (6)
C10.081 (8)0.085 (8)0.107 (9)0.025 (7)0.002 (8)0.010 (7)
C20.090 (9)0.110 (11)0.28 (2)0.005 (8)0.000 (11)0.048 (12)
C110.053 (5)0.045 (5)0.058 (5)0.001 (4)0.009 (4)0.004 (4)
C120.080 (7)0.096 (8)0.084 (7)0.005 (6)0.017 (6)0.006 (6)
C130.076 (8)0.166 (14)0.115 (11)0.038 (9)0.044 (8)0.019 (10)
C140.145 (13)0.089 (10)0.120 (12)0.040 (10)0.072 (11)0.018 (8)
C150.154 (12)0.053 (6)0.108 (10)0.003 (8)0.068 (10)0.017 (6)
C160.101 (8)0.055 (6)0.081 (7)0.002 (6)0.030 (6)0.014 (5)
C210.056 (5)0.042 (4)0.044 (5)0.004 (4)0.005 (4)0.004 (4)
C220.086 (7)0.095 (8)0.076 (7)0.024 (6)0.024 (6)0.029 (6)
C230.113 (9)0.085 (8)0.103 (9)0.019 (7)0.042 (8)0.022 (7)
C240.068 (7)0.088 (8)0.089 (8)0.015 (6)0.033 (6)0.023 (6)
C250.052 (6)0.148 (12)0.130 (11)0.024 (7)0.014 (7)0.030 (10)
C260.065 (6)0.109 (8)0.088 (7)0.018 (6)0.007 (6)0.036 (7)
C310.052 (5)0.049 (5)0.039 (4)0.011 (4)0.005 (4)0.000 (4)
C320.067 (6)0.115 (8)0.056 (6)0.025 (6)0.011 (5)0.008 (6)
C330.064 (7)0.153 (11)0.074 (8)0.028 (7)0.024 (6)0.010 (7)
C340.052 (6)0.104 (8)0.095 (8)0.022 (6)0.000 (6)0.003 (7)
C350.064 (6)0.093 (7)0.071 (7)0.011 (6)0.007 (5)0.007 (6)
C360.055 (5)0.075 (6)0.057 (5)0.006 (5)0.014 (4)0.004 (5)
C410.060 (5)0.042 (4)0.041 (4)0.003 (4)0.012 (4)0.004 (3)
C420.051 (5)0.054 (5)0.106 (8)0.016 (4)0.007 (5)0.011 (5)
C430.062 (6)0.083 (7)0.103 (8)0.017 (6)0.016 (6)0.023 (6)
C440.095 (8)0.073 (8)0.105 (9)0.029 (7)0.027 (7)0.031 (7)
C450.165 (13)0.036 (5)0.129 (10)0.005 (7)0.024 (10)0.019 (6)
C460.106 (8)0.060 (6)0.096 (8)0.011 (6)0.026 (7)0.017 (6)
S10.0546 (12)0.0419 (11)0.0633 (13)0.0020 (10)0.0142 (10)0.0006 (10)
N20.094 (6)0.056 (5)0.058 (5)0.010 (4)0.002 (4)0.013 (4)
C510.058 (5)0.035 (4)0.045 (5)0.005 (3)0.004 (4)0.000 (3)
C520.065 (5)0.040 (4)0.043 (5)0.002 (4)0.000 (4)0.003 (4)
S20.0449 (11)0.0642 (13)0.0597 (13)0.0008 (11)0.0019 (10)0.0102 (11)
S30.0512 (11)0.0583 (13)0.0553 (12)0.0019 (10)0.0027 (10)0.0153 (10)
N30.077 (6)0.126 (8)0.114 (8)0.028 (6)0.029 (6)0.026 (6)
N40.089 (6)0.092 (6)0.068 (5)0.021 (5)0.006 (5)0.023 (5)
C530.056 (5)0.049 (5)0.063 (5)0.016 (4)0.013 (5)0.001 (4)
C540.067 (6)0.078 (7)0.065 (6)0.012 (5)0.002 (5)0.013 (5)
C550.060 (5)0.050 (5)0.050 (5)0.002 (4)0.007 (4)0.002 (4)
C560.075 (6)0.067 (6)0.056 (6)0.008 (5)0.003 (5)0.012 (5)
Geometric parameters (Å, º) top
Mo—S2i2.382 (2)C23—H23A0.9300
Mo—S22.382 (2)C24—C251.348 (14)
Mo—S12.384 (2)C24—H24A0.9300
Mo—S1i2.384 (2)C25—C261.367 (13)
Mo—S32.385 (2)C25—H25A0.9300
Mo—S3i2.385 (2)C26—H26A0.9300
Ag—P2ii2.430 (2)C31—C321.373 (10)
Ag—P12.434 (2)C31—C361.388 (10)
Ag—N12.457 (9)C32—C331.406 (12)
Ag—Agii2.9501 (13)C32—H32A0.9300
P1—N1.677 (6)C33—C341.366 (13)
P1—C211.808 (8)C33—H33A0.9300
P1—C111.809 (8)C34—C351.350 (12)
P2—N1.688 (6)C34—H34A0.9300
P2—C411.816 (7)C35—C361.384 (11)
P2—C311.820 (8)C35—H35A0.9300
P2—Agii2.430 (2)C36—H36A0.9300
N—H0A0.8600C41—C461.378 (11)
N1—C11.111 (13)C41—C421.381 (11)
C1—C21.445 (15)C42—C431.385 (12)
C2—H2A0.9600C42—H42A0.9300
C2—H2B0.9600C43—C441.355 (13)
C2—H2C0.9600C43—H43A0.9300
C11—C121.377 (12)C44—C451.346 (14)
C11—C161.384 (11)C44—H44A0.9300
C12—C131.394 (14)C45—C461.386 (13)
C12—H12A0.9300C45—H45A0.9300
C13—C141.369 (17)C46—H46A0.9300
C13—H13A0.9300S1—C511.727 (7)
C14—C151.332 (17)N2—C521.140 (9)
C14—H14A0.9300C51—C51i1.349 (14)
C15—C161.379 (13)C51—C521.434 (10)
C15—H15A0.9300S2—C531.730 (9)
C16—H16A0.9300S3—C551.730 (8)
C21—C221.365 (11)N3—C541.149 (10)
C21—C261.376 (11)N4—C561.127 (10)
C22—C231.379 (13)C53—C551.345 (10)
C22—H22A0.9300C53—C541.423 (11)
C23—C241.338 (13)C55—C561.437 (11)
S2i—Mo—S2141.21 (11)C21—C22—H22A119.5
S2i—Mo—S1130.07 (8)C23—C22—H22A119.5
S2—Mo—S181.88 (7)C24—C23—C22121.0 (10)
S2i—Mo—S1i81.88 (7)C24—C23—H23A119.5
S2—Mo—S1i130.07 (8)C22—C23—H23A119.5
S1—Mo—S1i81.70 (10)C23—C24—C25118.9 (10)
S2i—Mo—S381.93 (8)C23—C24—H24A120.6
S2—Mo—S381.54 (7)C25—C24—H24A120.6
S1—Mo—S3141.35 (8)C24—C25—C26121.1 (10)
S1i—Mo—S382.77 (7)C24—C25—H25A119.5
S2i—Mo—S3i81.54 (7)C26—C25—H25A119.5
S2—Mo—S3i81.93 (8)C25—C26—C21121.1 (10)
S1—Mo—S3i82.77 (7)C25—C26—H26A119.5
S1i—Mo—S3i141.35 (8)C21—C26—H26A119.5
S3—Mo—S3i128.69 (11)C32—C31—C36118.5 (7)
P2ii—Ag—P1156.48 (7)C32—C31—P2123.0 (6)
P2ii—Ag—N1103.0 (2)C36—C31—P2118.5 (6)
P1—Ag—N199.9 (2)C31—C32—C33120.2 (9)
P2ii—Ag—Agii88.65 (5)C31—C32—H32A119.9
P1—Ag—Agii88.52 (5)C33—C32—H32A119.9
N1—Ag—Agii84.5 (2)C34—C33—C32119.8 (9)
N—P1—C21106.1 (3)C34—C33—H33A120.1
N—P1—C11103.3 (3)C32—C33—H33A120.1
C21—P1—C11103.8 (4)C35—C34—C33120.3 (9)
N—P1—Ag114.0 (2)C35—C34—H34A119.8
C21—P1—Ag115.5 (3)C33—C34—H34A119.8
C11—P1—Ag112.9 (3)C34—C35—C36120.6 (9)
N—P2—C41102.9 (3)C34—C35—H35A119.7
N—P2—C31105.5 (3)C36—C35—H35A119.7
C41—P2—C31104.2 (4)C35—C36—C31120.5 (8)
N—P2—Agii114.0 (2)C35—C36—H36A119.7
C41—P2—Agii112.2 (2)C31—C36—H36A119.7
C31—P2—Agii116.7 (3)C46—C41—C42118.0 (8)
P1—N—P2125.9 (3)C46—C41—P2123.1 (7)
P1—N—H0A117.1C42—C41—P2118.9 (6)
P2—N—H0A117.1C41—C42—C43120.5 (9)
C1—N1—Ag168.3 (10)C41—C42—H42A119.7
N1—C1—C2178.0 (15)C43—C42—H42A119.7
C1—C2—H2A109.5C44—C43—C42120.8 (10)
C1—C2—H2B109.5C44—C43—H43A119.6
H2A—C2—H2B109.5C42—C43—H43A119.6
C1—C2—H2C109.5C45—C44—C43119.1 (10)
H2A—C2—H2C109.5C45—C44—H44A120.4
H2B—C2—H2C109.5C43—C44—H44A120.4
C12—C11—C16117.4 (8)C44—C45—C46121.6 (10)
C12—C11—P1119.1 (7)C44—C45—H45A119.2
C16—C11—P1123.4 (7)C46—C45—H45A119.2
C11—C12—C13120.8 (11)C41—C46—C45120.0 (10)
C11—C12—H12A119.6C41—C46—H46A120.0
C13—C12—H12A119.6C45—C46—H46A120.0
C14—C13—C12119.9 (13)C51—S1—Mo108.3 (2)
C14—C13—H13A120.1C51i—C51—C52121.7 (4)
C12—C13—H13A120.1C51i—C51—S1120.8 (2)
C15—C14—C13119.7 (13)C52—C51—S1117.5 (5)
C15—C14—H14A120.2N2—C52—C51177.3 (9)
C13—C14—H14A120.2C53—S2—Mo108.4 (3)
C14—C15—C16121.4 (13)C55—S3—Mo108.6 (3)
C14—C15—H15A119.3C55—C53—C54122.6 (8)
C16—C15—H15A119.3C55—C53—S2121.1 (6)
C15—C16—C11120.7 (11)C54—C53—S2116.3 (7)
C15—C16—H16A119.6N3—C54—C53176.8 (11)
C11—C16—H16A119.6C53—C55—C56122.5 (8)
C22—C21—C26116.9 (8)C53—C55—S3120.4 (6)
C22—C21—P1124.3 (7)C56—C55—S3117.2 (6)
C26—C21—P1118.8 (6)N4—C56—C55178.9 (11)
C21—C22—C23121.1 (9)
Symmetry codes: (i) x+1, y, z+3/2; (ii) x+1, y+1, z+1.
 

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