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The title compound, [Ag4I4(C18H21P)4], has a tetra­meric structure, with the Ag and I atoms alternating in a distorted cubane-like AgI core and with cyclo­hexyl­diphenyl­phosphine ligands capping the Ag corners. Each face is distorted, such that the average Ag...Ag atomic separation is shorter than the average I...I atomic separation by about 1 Å. Two symmetry-unique but structurally similar tetra­mers of the same enanti­omer are each located on a twofold rotation axis, which can be assigned the same helicity, suggesting spontaneous resolution. Three phenyl groups are each disordered over two positions; the site occupancy ratios are between ca 2:1 and 4:1.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807031911/wm2128sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807031911/wm2128Isup2.hkl
Contains datablock I

CCDC reference: 657538

Key indicators

  • Single-crystal X-ray study
  • T = 120 K
  • Mean [sigma](C-C) = 0.012 Å
  • Disorder in main residue
  • R factor = 0.043
  • wR factor = 0.107
  • Data-to-parameter ratio = 22.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT301_ALERT_3_C Main Residue Disorder ......................... 18.00 Perc. PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 12
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 28.34 From the CIF: _reflns_number_total 16990 Count of symmetry unique reflns 9442 Completeness (_total/calc) 179.94% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 7548 Fraction of Friedel pairs measured 0.799 Are heavy atom types Z>Si present yes PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 327
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

The 1:1 AgI:PCyPh2 (PCyPh2 is diphenylcyclohexylphosphine) tetrameric complex is similar to reported analogues with other monodentate phosphine ligands (Bowen et al., 1994; Teo & Calabrese, 1975 and 1976; Meijboom et al., 2006). The silver and iodine atoms alternate in a distorted cubane-like AgI core with phosphine capping the silver corners (Fig. 1). Two symmetry unique but structurally similar tetramers are each located on a twofold axis. Each face is distorted such that the average Ag···Ag atomic separation is shorter than the average I···I atomic separation by about 1 Å. A closer inspection shows that the two faces completed by the twofold axis differ from each other and from the four adjacent faces in that they display the shortest and longest I···I separations for each cubane. If the face with the shortest I···I separation is assigned to be proximal, an inspection of the cyclohexyl fragments clearly show (P) helicity (Eliel et al., 1994) for both symmetry unique molecules (Fig. 2). The starting materials do not display chirality suggesting spontaneous resolution during crystallization. We also note that the proximal and distal planes could easily be inverted by slight distortion of the cubane-like core. Alternatively, concerted rotation along the Ag—P bonds would reverse the helicity. The Flack parameter refined to a value of -0.029 (18) indicating the true hand of the data has been correctly determined.

Related literature top

Background information on similar tetrameric AgI monodentate adducts is given by Bowen et al. (1994), Teo & Calabrese (1975, 1976) and Meijboom et al. (2006). Background reference on helicity is given by Eliel et al. (1994).

Experimental top

Synthesis of [Ag(PCyPh2)I]4: 1 equivalent of AgI and 1.1 equivalents of diphenylcyclohexylphosphine were added in vial containing anhydrous tetrahydrofuran (THF). The mixture was allowed to stir for 3 h at room temperature in darkness. Removal of THF yielded a white powder residue which was washed with several portions of pentane. Colorless crystals were grown by layering pentane over a saturated CH2Cl2 solution at room temperature in the dark (yield 50%).

Refinement top

Three symmetry unique phenyl groups in [Ag(PCyPh2)I]4 were located disordered each in two positions and were treated as rigid flat hexagons having C—C distances constrained to 1.39 Å with refined site occupancies of 67/33, 70/30 and 78/22, respectively, and were subjected to rigid bond restraints. Equal atomic displacement parameters were applied to chemically equivalent atoms in the disordered contributions and bond distances were restrained to be the same. An anti-bumping restraint was applied between C64, a carbon atom of a minor disordered contributor, and C39 in a cyclohexyl ring. H atoms were assigned calculated positions with Uiso restrained to be 1.2Ueq of the bonded C atom and a C—H distance of 0.95–0.99 Å. The highest peak and deepest hole in the final difference map are located 0.97 and 0.72 Å, respectively, from Ag1.

Structure description top

The 1:1 AgI:PCyPh2 (PCyPh2 is diphenylcyclohexylphosphine) tetrameric complex is similar to reported analogues with other monodentate phosphine ligands (Bowen et al., 1994; Teo & Calabrese, 1975 and 1976; Meijboom et al., 2006). The silver and iodine atoms alternate in a distorted cubane-like AgI core with phosphine capping the silver corners (Fig. 1). Two symmetry unique but structurally similar tetramers are each located on a twofold axis. Each face is distorted such that the average Ag···Ag atomic separation is shorter than the average I···I atomic separation by about 1 Å. A closer inspection shows that the two faces completed by the twofold axis differ from each other and from the four adjacent faces in that they display the shortest and longest I···I separations for each cubane. If the face with the shortest I···I separation is assigned to be proximal, an inspection of the cyclohexyl fragments clearly show (P) helicity (Eliel et al., 1994) for both symmetry unique molecules (Fig. 2). The starting materials do not display chirality suggesting spontaneous resolution during crystallization. We also note that the proximal and distal planes could easily be inverted by slight distortion of the cubane-like core. Alternatively, concerted rotation along the Ag—P bonds would reverse the helicity. The Flack parameter refined to a value of -0.029 (18) indicating the true hand of the data has been correctly determined.

Background information on similar tetrameric AgI monodentate adducts is given by Bowen et al. (1994), Teo & Calabrese (1975, 1976) and Meijboom et al. (2006). Background reference on helicity is given by Eliel et al. (1994).

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2002); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. Diagram showing the molecular structure of the 1:1 AgI:PCyPh2 tetrameric complex with ellipsoids drawn at the 30% probability level. A second unique but similar molecule of the title compound, the minor disordered components, and the H atoms are omitted for clarity. [Symmetry operator: i) -x + 1, y, -z + 1.]
[Figure 2] Fig. 2. Abbreviated diagram of the title compound showing (P) helicity of the PCy fragments viewed down the twofold axis with Ag—I—Ag—I face of the shortest I···I distance selected to be proximal. [Symmetry operator: i) -x + 1, y, -z + 1.]
(P)-Tetra-µ3-iodido-tetrakis[(cyclohexyldiphenylphosphine-κP)silver(I)] top
Crystal data top
[Ag4I4(C18H21P)4]F(000) = 3904
Mr = 2012.35Dx = 1.849 Mg m3
Monoclinic, C2Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2yCell parameters from 998 reflections
a = 24.698 (9) Åθ = 2.4–26.6°
b = 12.404 (5) ŵ = 2.91 mm1
c = 24.328 (9) ÅT = 120 K
β = 104.145 (7)°Block, colourless
V = 7227 (5) Å30.15 × 0.14 × 0.09 mm
Z = 4
Data collection top
Bruker APEX
diffractometer
16990 independent reflections
Radiation source: fine-focus sealed tube15397 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.041
Detector resolution: 836.6 pixels mm-1θmax = 28.3°, θmin = 1.7°
ω scansh = 3232
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
k = 1616
Tmin = 0.652, Tmax = 0.767l = 3132
42119 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.043H-atom parameters constrained
wR(F2) = 0.107 w = 1/[σ2(Fo2) + (0.0456P)2 + 26.0708P]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.002
16990 reflectionsΔρmax = 2.48 e Å3
742 parametersΔρmin = 1.27 e Å3
327 restraintsAbsolute structure: Flack (1983), 7870 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.029 (18)
Crystal data top
[Ag4I4(C18H21P)4]V = 7227 (5) Å3
Mr = 2012.35Z = 4
Monoclinic, C2Mo Kα radiation
a = 24.698 (9) ŵ = 2.91 mm1
b = 12.404 (5) ÅT = 120 K
c = 24.328 (9) Å0.15 × 0.14 × 0.09 mm
β = 104.145 (7)°
Data collection top
Bruker APEX
diffractometer
16990 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
15397 reflections with I > 2σ(I)
Tmin = 0.652, Tmax = 0.767Rint = 0.041
42119 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.043H-atom parameters constrained
wR(F2) = 0.107 w = 1/[σ2(Fo2) + (0.0456P)2 + 26.0708P]
where P = (Fo2 + 2Fc2)/3
S = 1.05Δρmax = 2.48 e Å3
16990 reflectionsΔρmin = 1.27 e Å3
742 parametersAbsolute structure: Flack (1983), 7870 Friedel pairs
327 restraintsAbsolute structure parameter: 0.029 (18)
Special details top

Experimental. Data collection is performed with four batch runs at φ = 0.00 ° (600 frames), at φ = 90.00 ° (600 frames), at φ = 180 ° (600 frames) and at φ = 270 ° (600 frames). Frame width = 0.30 ° in ω. Data is merged, corrected for decay, and treated with multi-scan absorption corrections.

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 > 2σ(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*/UeqOcc. (<1)
Ag10.57326 (3)0.94301 (5)0.52831 (3)0.06118 (18)
Ag20.49338 (3)0.74512 (5)0.57164 (2)0.04812 (14)
Ag31.01975 (3)0.55462 (5)0.07637 (3)0.05755 (17)
Ag40.93112 (2)0.35289 (4)0.00325 (3)0.04431 (13)
I10.591930 (19)0.70934 (4)0.53562 (2)0.04137 (11)
I20.48125 (2)0.97682 (4)0.58617 (2)0.05396 (13)
I30.90958 (2)0.58414 (3)0.00354 (2)0.04997 (13)
I41.027377 (18)0.32713 (3)0.098437 (18)0.03722 (9)
P10.65521 (8)1.04838 (16)0.57606 (8)0.0425 (4)
P20.46790 (7)0.64854 (14)0.64952 (7)0.0333 (3)
P31.04524 (11)0.66022 (16)0.16369 (9)0.0521 (5)
P40.84888 (7)0.24331 (15)0.00446 (7)0.0372 (4)
C10.6946 (3)1.1312 (6)0.4848 (3)0.0504 (18)
H1A0.68151.20280.49410.060*
H1B0.66331.09540.45770.060*
C20.7433 (3)1.1453 (6)0.4577 (4)0.056 (2)
H2A0.77321.18680.48370.067*
H2B0.73091.18700.42220.067*
C30.7666 (4)1.0373 (7)0.4447 (4)0.055 (2)
H3A0.73820.99950.41520.066*
H3B0.79991.04960.42960.066*
C40.7824 (4)0.9681 (8)0.4965 (4)0.063 (2)
H4A0.81441.00100.52390.076*
H4B0.79410.89620.48600.076*
C50.7329 (4)0.9549 (6)0.5246 (4)0.055 (2)
H5A0.70240.91440.49890.066*
H5B0.74520.91310.56020.066*
C60.7114 (3)1.0649 (6)0.5376 (3)0.0465 (17)
H6A0.74311.10300.56380.056*
C70.7451 (7)1.0293 (11)0.6723 (6)0.049 (3)0.67 (4)
H7A0.75811.09490.65990.059*0.67 (4)
C80.7783 (4)0.9733 (16)0.7177 (6)0.065 (3)0.67 (4)
H8A0.81401.00070.73640.078*0.67 (4)
C90.7593 (8)0.8773 (13)0.7358 (6)0.084 (5)0.67 (4)
H9A0.78200.83910.76680.101*0.67 (4)
C100.7071 (10)0.8373 (14)0.7084 (7)0.091 (6)0.67 (4)
H10A0.69420.77170.72080.109*0.67 (4)
C110.6739 (7)0.8933 (16)0.6630 (7)0.073 (5)0.67 (4)
H11A0.63830.86590.64430.088*0.67 (4)
C120.6929 (6)0.9892 (11)0.6449 (5)0.048 (2)0.67 (4)
C730.7553 (11)1.002 (3)0.6688 (12)0.049 (3)0.33 (4)
H73A0.77891.04770.65340.059*0.33 (4)
C740.7773 (10)0.944 (3)0.7179 (13)0.065 (3)0.33 (4)
H74A0.81590.94940.73610.078*0.33 (4)
C750.7428 (18)0.877 (3)0.7405 (12)0.084 (5)0.33 (4)
H75A0.75790.83760.77410.101*0.33 (4)
C760.6864 (17)0.869 (3)0.7139 (16)0.091 (6)0.33 (4)
H76A0.66280.82410.72930.109*0.33 (4)
C770.6644 (11)0.928 (3)0.6647 (15)0.073 (5)0.33 (4)
H77A0.62580.92240.64650.088*0.33 (4)
C780.6989 (12)0.994 (2)0.6422 (10)0.048 (2)0.33 (4)
C130.6649 (4)1.2421 (7)0.6414 (4)0.056 (2)
H13A0.69081.20520.67070.067*
C140.6532 (4)1.3491 (7)0.6486 (4)0.056 (2)
H14A0.66941.38420.68340.068*
C150.6181 (4)1.4050 (7)0.6054 (4)0.054 (2)
H15A0.61131.47950.60970.065*
C160.5931 (4)1.3525 (7)0.5562 (4)0.058 (2)
H16A0.56881.39110.52650.069*
C170.6029 (4)1.2434 (8)0.5491 (4)0.058 (2)
H17A0.58451.20740.51520.069*
C180.6396 (3)1.1876 (6)0.5920 (3)0.0392 (15)
C190.5484 (3)0.7426 (6)0.7368 (4)0.0514 (18)
H19A0.51960.79740.73820.062*
H19B0.56910.76690.70900.062*
C200.5890 (4)0.7326 (7)0.7957 (4)0.056 (2)
H20A0.60950.80130.80540.068*
H20B0.56740.71940.82450.068*
C210.6300 (3)0.6427 (8)0.7976 (4)0.057 (2)
H21A0.65610.66280.77430.068*
H21B0.65210.63330.83720.068*
C220.6030 (4)0.5390 (7)0.7768 (4)0.059 (2)
H22A0.58170.51250.80370.071*
H22B0.63210.48500.77540.071*
C230.5634 (4)0.5501 (7)0.7177 (4)0.058 (2)
H23A0.58510.56970.68990.069*
H23B0.54480.48010.70610.069*
C240.5200 (3)0.6348 (5)0.7175 (3)0.0374 (14)
H24A0.49940.61300.74640.045*
C250.4719 (4)0.4442 (7)0.6074 (4)0.057 (2)
H25A0.50200.47330.59420.068*
C260.4587 (4)0.3355 (8)0.5979 (4)0.065 (2)
H26A0.48070.29070.58030.078*
C270.4141 (4)0.2941 (7)0.6140 (4)0.061 (2)
H27A0.40530.21970.60860.074*
C280.3817 (4)0.3604 (8)0.6382 (4)0.066 (2)
H28A0.34920.33250.64750.079*
C290.3963 (4)0.4690 (7)0.6492 (4)0.0551 (19)
H29A0.37410.51400.66650.066*
C300.4429 (3)0.5105 (6)0.6349 (3)0.0372 (14)
C310.3631 (3)0.7377 (6)0.6252 (3)0.0455 (16)
H31A0.36400.72130.58730.055*
C320.3156 (4)0.7850 (7)0.6361 (4)0.059 (2)
H32A0.28380.79730.60580.071*
C330.3145 (4)0.8136 (8)0.6895 (4)0.064 (2)
H33A0.28200.84580.69660.077*
C340.3611 (4)0.7957 (9)0.7339 (4)0.069 (3)
H34A0.36110.81820.77120.083*
C350.4076 (4)0.7448 (7)0.7234 (3)0.0533 (19)
H35A0.43890.73050.75400.064*
C360.4087 (3)0.7146 (6)0.6692 (3)0.0395 (14)
C370.9802 (4)0.5462 (6)0.2222 (4)0.070 (2)
H37A0.96520.50650.18640.084*
H37B1.01420.50830.24320.084*
C380.9372 (4)0.5445 (8)0.2572 (5)0.078 (2)
H38A0.92430.46940.25950.093*
H38B0.95510.56850.29620.093*
C390.8893 (4)0.6122 (7)0.2347 (5)0.086 (2)
H39A0.86750.61860.26370.103*
H39B0.86520.57540.20140.103*
C400.9015 (4)0.7225 (7)0.2172 (5)0.075 (2)
H40A0.91570.76700.25140.090*
H40B0.86640.75590.19520.090*
C410.9441 (4)0.7227 (7)0.1814 (4)0.070 (2)
H41A0.92680.69120.14380.083*
H41B0.95450.79810.17550.083*
C420.9957 (4)0.6603 (6)0.2083 (4)0.0654 (19)
H42A1.01400.69670.24480.078*
C431.0662 (4)0.8782 (7)0.1958 (4)0.063 (2)
H43A1.06480.85530.23270.075*
C441.0755 (4)0.9838 (8)0.1865 (5)0.074 (3)
H44A1.07971.03490.21640.089*
C451.0787 (4)1.0152 (6)0.1339 (6)0.073 (3)
H45A1.08601.08880.12760.088*
C461.0716 (4)0.9445 (7)0.0901 (5)0.075 (3)
H46A1.07350.96890.05360.090*
C471.0614 (4)0.8354 (7)0.0989 (4)0.060 (2)
H47A1.05650.78500.06870.072*
C481.0588 (3)0.8027 (5)0.1521 (3)0.0489 (18)
C491.1575 (14)0.603 (5)0.1732 (14)0.063 (3)0.22 (3)
H49A1.14720.59950.13300.076*0.22 (3)
C501.2121 (12)0.581 (4)0.203 (2)0.074 (4)0.22 (3)
H50A1.23910.56240.18240.089*0.22 (3)
C511.2271 (11)0.587 (4)0.261 (2)0.078 (4)0.22 (3)
H51A1.26440.57160.28140.094*0.22 (3)
C521.1875 (18)0.614 (4)0.2909 (15)0.090 (5)0.22 (3)
H52A1.19780.61790.33110.107*0.22 (3)
C531.1329 (16)0.636 (4)0.2616 (16)0.072 (4)0.22 (3)
H53A1.10590.65500.28180.086*0.22 (3)
C541.1179 (10)0.631 (5)0.2028 (16)0.058 (3)0.22 (3)
C851.1550 (4)0.6036 (11)0.1920 (5)0.063 (3)0.78 (3)
H85A1.15030.60610.15210.076*0.78 (3)
C861.2076 (3)0.5856 (10)0.2274 (6)0.074 (4)0.78 (3)
H86A1.23890.57570.21170.089*0.78 (3)
C871.2144 (4)0.5819 (10)0.2858 (6)0.078 (4)0.78 (3)
H87A1.25030.56960.31000.094*0.78 (3)
C881.1686 (6)0.5964 (10)0.3088 (4)0.090 (5)0.78 (3)
H88A1.17330.59390.34870.107*0.78 (3)
C891.1160 (5)0.6144 (11)0.2734 (4)0.072 (4)0.78 (3)
H89A1.08480.62430.28910.086*0.78 (3)
C901.1092 (4)0.6181 (11)0.2150 (4)0.058 (3)0.78 (3)
C550.8124 (3)0.1958 (6)0.1115 (3)0.0410 (15)
H55A0.82030.11860.10280.049*
H55B0.84700.23000.11650.049*
C560.7666 (3)0.2062 (6)0.1663 (3)0.055 (2)
H56A0.78000.17490.19800.066*
H56B0.73340.16460.16260.066*
C570.7499 (3)0.3227 (6)0.1800 (3)0.0526 (19)
H57A0.78150.36210.18880.063*
H57B0.71810.32530.21390.063*
C580.7333 (3)0.3771 (8)0.1309 (3)0.060 (2)
H58A0.72550.45430.13990.072*
H58B0.69880.34360.12510.072*
C590.7791 (3)0.3674 (6)0.0770 (3)0.052 (2)
H59A0.76660.40120.04540.062*
H59B0.81260.40670.08160.062*
C600.7944 (3)0.2495 (6)0.0624 (3)0.0432 (16)
H60A0.76040.21150.05680.052*
C610.7774 (9)0.2483 (14)0.0737 (10)0.057 (3)0.297 (12)
H61A0.76890.17720.05970.069*0.297 (12)
C620.7485 (9)0.294 (2)0.1103 (11)0.070 (4)0.297 (12)
H62A0.72010.25340.12140.084*0.297 (12)
C630.7610 (9)0.398 (2)0.1307 (9)0.081 (6)0.297 (12)
H63A0.74120.42850.15570.097*0.297 (12)
C640.8024 (9)0.4563 (17)0.1145 (9)0.070 (4)0.297 (12)
H64A0.81100.52740.12850.084*0.297 (12)
C650.8314 (8)0.4111 (17)0.0779 (9)0.055 (3)0.297 (12)
H65A0.85970.45120.06680.066*0.297 (12)
C660.8189 (9)0.3071 (17)0.0575 (9)0.036 (2)0.297 (12)
C790.7599 (3)0.2106 (7)0.0582 (4)0.057 (3)0.703 (12)
H79A0.75360.14400.03830.069*0.703 (12)
C800.7248 (3)0.2428 (8)0.0918 (4)0.070 (4)0.703 (12)
H80A0.69440.19830.09500.084*0.703 (12)
C810.7341 (4)0.3402 (9)0.1209 (4)0.081 (6)0.703 (12)
H81A0.71000.36220.14390.097*0.703 (12)
C820.7785 (4)0.4053 (8)0.1163 (4)0.070 (4)0.703 (12)
H82A0.78490.47190.13610.084*0.703 (12)
C830.8137 (3)0.3731 (7)0.0826 (4)0.055 (3)0.703 (12)
H83A0.84410.41760.07950.066*0.703 (12)
C840.8044 (3)0.2757 (7)0.0536 (3)0.036 (2)0.703 (12)
C670.9137 (3)0.0797 (5)0.0602 (3)0.0364 (13)
H67A0.93890.13650.07500.044*
C680.9272 (3)0.0280 (6)0.0768 (3)0.0462 (16)
H68A0.96170.04380.10290.055*
C690.8908 (4)0.1097 (6)0.0555 (3)0.0516 (19)
H69A0.90000.18170.06760.062*
C700.8409 (4)0.0888 (7)0.0167 (4)0.061 (2)
H70A0.81640.14590.00090.073*
C710.8271 (4)0.0183 (7)0.0011 (4)0.058 (2)
H71A0.79210.03370.02430.070*
C720.8630 (3)0.1016 (5)0.0216 (3)0.0390 (14)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ag10.0498 (3)0.0511 (4)0.0721 (4)0.0034 (3)0.0053 (3)0.0026 (3)
Ag20.0504 (3)0.0512 (3)0.0477 (3)0.0002 (3)0.0214 (3)0.0046 (3)
Ag30.0764 (4)0.0337 (3)0.0575 (4)0.0062 (3)0.0067 (3)0.0041 (3)
Ag40.0405 (3)0.0304 (3)0.0569 (3)0.0017 (2)0.0022 (2)0.0028 (2)
I10.0359 (2)0.0399 (2)0.0495 (3)0.00681 (18)0.01294 (19)0.00699 (19)
I20.0532 (3)0.0412 (3)0.0620 (3)0.0034 (2)0.0033 (2)0.0064 (2)
I30.0619 (3)0.0273 (2)0.0531 (3)0.0066 (2)0.0005 (2)0.00548 (19)
I40.0363 (2)0.02788 (19)0.0439 (2)0.00317 (16)0.00288 (17)0.00464 (17)
P10.0396 (9)0.0375 (9)0.0478 (10)0.0014 (8)0.0057 (8)0.0066 (8)
P20.0306 (8)0.0367 (9)0.0320 (8)0.0008 (7)0.0063 (6)0.0012 (7)
P30.0752 (15)0.0266 (9)0.0516 (11)0.0001 (9)0.0101 (10)0.0013 (8)
P40.0325 (8)0.0401 (9)0.0380 (8)0.0070 (7)0.0069 (7)0.0079 (7)
C10.057 (5)0.041 (4)0.054 (4)0.008 (3)0.015 (4)0.011 (3)
C20.050 (5)0.038 (4)0.082 (6)0.007 (3)0.023 (4)0.005 (4)
C30.055 (5)0.048 (4)0.067 (5)0.003 (4)0.022 (4)0.005 (4)
C40.067 (6)0.053 (5)0.075 (6)0.014 (4)0.027 (5)0.003 (5)
C50.077 (6)0.034 (4)0.057 (5)0.005 (4)0.021 (4)0.006 (3)
C60.053 (4)0.041 (4)0.048 (4)0.007 (3)0.017 (3)0.004 (3)
C70.036 (6)0.059 (8)0.052 (5)0.021 (5)0.009 (4)0.002 (5)
C80.064 (5)0.084 (10)0.045 (4)0.015 (5)0.008 (4)0.002 (6)
C90.104 (11)0.102 (8)0.044 (6)0.004 (8)0.011 (6)0.022 (5)
C100.108 (11)0.097 (12)0.060 (7)0.020 (9)0.005 (8)0.039 (8)
C110.077 (7)0.069 (11)0.070 (6)0.008 (7)0.013 (5)0.030 (8)
C120.039 (4)0.049 (4)0.057 (4)0.008 (3)0.015 (3)0.014 (3)
C730.036 (6)0.059 (8)0.052 (5)0.021 (5)0.009 (4)0.002 (5)
C740.064 (5)0.084 (10)0.045 (4)0.015 (5)0.008 (4)0.002 (6)
C750.104 (11)0.102 (8)0.044 (6)0.004 (8)0.011 (6)0.022 (5)
C760.108 (11)0.097 (12)0.060 (7)0.020 (9)0.005 (8)0.039 (8)
C770.077 (7)0.069 (11)0.070 (6)0.008 (7)0.013 (5)0.030 (8)
C780.039 (4)0.049 (4)0.057 (4)0.008 (3)0.015 (3)0.014 (3)
C130.052 (5)0.050 (5)0.059 (5)0.011 (4)0.001 (4)0.011 (4)
C140.058 (5)0.058 (5)0.049 (4)0.002 (4)0.005 (4)0.001 (4)
C150.057 (5)0.047 (4)0.067 (5)0.008 (4)0.029 (4)0.001 (4)
C160.064 (5)0.060 (5)0.053 (5)0.025 (4)0.021 (4)0.013 (4)
C170.057 (5)0.068 (6)0.051 (4)0.018 (4)0.017 (4)0.003 (4)
C180.039 (3)0.039 (4)0.039 (3)0.000 (3)0.008 (3)0.007 (3)
C190.040 (4)0.038 (4)0.068 (5)0.004 (3)0.001 (3)0.003 (4)
C200.056 (5)0.049 (5)0.055 (5)0.006 (4)0.006 (4)0.016 (4)
C210.046 (4)0.069 (6)0.050 (5)0.006 (4)0.001 (3)0.006 (4)
C220.061 (5)0.054 (5)0.051 (5)0.018 (4)0.007 (4)0.002 (4)
C230.052 (5)0.053 (5)0.062 (5)0.015 (4)0.002 (4)0.007 (4)
C240.033 (3)0.035 (3)0.040 (3)0.001 (3)0.000 (3)0.007 (3)
C250.054 (5)0.060 (5)0.055 (5)0.020 (4)0.013 (4)0.020 (4)
C260.071 (6)0.061 (5)0.065 (5)0.007 (5)0.021 (4)0.023 (5)
C270.085 (7)0.046 (5)0.050 (4)0.022 (4)0.008 (4)0.013 (4)
C280.059 (5)0.057 (5)0.079 (6)0.021 (4)0.013 (5)0.002 (5)
C290.054 (5)0.051 (4)0.061 (5)0.006 (4)0.015 (4)0.001 (4)
C300.035 (3)0.039 (3)0.035 (3)0.006 (3)0.003 (3)0.001 (3)
C310.042 (4)0.048 (4)0.048 (4)0.004 (3)0.014 (3)0.002 (3)
C320.046 (5)0.060 (5)0.068 (5)0.010 (4)0.005 (4)0.003 (4)
C330.046 (5)0.064 (6)0.086 (6)0.011 (4)0.023 (4)0.014 (5)
C340.071 (6)0.079 (7)0.065 (6)0.007 (5)0.030 (5)0.020 (5)
C350.053 (4)0.055 (5)0.050 (4)0.003 (4)0.008 (3)0.007 (4)
C360.035 (3)0.039 (3)0.047 (4)0.004 (3)0.015 (3)0.001 (3)
C370.099 (5)0.040 (3)0.079 (5)0.006 (4)0.035 (4)0.010 (4)
C380.103 (6)0.054 (4)0.086 (5)0.006 (4)0.042 (4)0.012 (4)
C390.097 (5)0.068 (5)0.100 (6)0.006 (4)0.039 (5)0.017 (4)
C400.080 (5)0.058 (4)0.085 (5)0.012 (4)0.017 (4)0.010 (4)
C410.077 (5)0.050 (4)0.076 (5)0.001 (3)0.007 (4)0.022 (4)
C420.087 (5)0.037 (3)0.074 (5)0.007 (3)0.024 (4)0.008 (3)
C430.073 (6)0.039 (4)0.071 (6)0.001 (4)0.007 (5)0.012 (4)
C440.057 (6)0.044 (5)0.108 (8)0.004 (4)0.007 (5)0.021 (5)
C450.042 (5)0.028 (4)0.161 (11)0.002 (3)0.046 (6)0.009 (5)
C460.089 (7)0.031 (4)0.121 (9)0.003 (4)0.057 (7)0.015 (5)
C470.076 (6)0.034 (4)0.076 (6)0.003 (4)0.033 (5)0.003 (4)
C480.060 (5)0.023 (3)0.060 (5)0.003 (3)0.008 (4)0.003 (3)
C490.083 (6)0.056 (6)0.047 (6)0.008 (5)0.008 (5)0.004 (6)
C500.083 (6)0.066 (6)0.067 (8)0.009 (6)0.007 (6)0.004 (7)
C510.089 (7)0.065 (6)0.067 (8)0.024 (7)0.007 (6)0.004 (8)
C520.111 (9)0.098 (9)0.045 (6)0.050 (9)0.007 (5)0.006 (7)
C530.085 (7)0.075 (9)0.052 (6)0.010 (7)0.009 (5)0.001 (6)
C540.083 (6)0.034 (5)0.048 (6)0.018 (5)0.000 (4)0.003 (5)
C850.083 (6)0.056 (6)0.047 (6)0.008 (5)0.008 (5)0.004 (6)
C860.083 (6)0.066 (6)0.067 (8)0.009 (6)0.007 (6)0.004 (7)
C870.089 (7)0.065 (6)0.067 (8)0.024 (7)0.007 (6)0.004 (8)
C880.111 (9)0.098 (9)0.045 (6)0.050 (9)0.007 (5)0.006 (7)
C890.085 (7)0.075 (9)0.052 (6)0.010 (7)0.009 (5)0.001 (6)
C900.083 (6)0.034 (5)0.048 (6)0.018 (5)0.000 (4)0.003 (5)
C550.033 (3)0.042 (4)0.045 (4)0.000 (3)0.005 (3)0.002 (3)
C560.053 (4)0.067 (5)0.042 (4)0.017 (4)0.006 (3)0.002 (4)
C570.049 (4)0.067 (5)0.041 (4)0.000 (4)0.010 (3)0.019 (4)
C580.048 (4)0.081 (6)0.052 (5)0.021 (4)0.013 (4)0.020 (4)
C590.046 (4)0.065 (5)0.046 (4)0.018 (4)0.014 (3)0.020 (4)
C600.028 (3)0.053 (4)0.043 (4)0.006 (3)0.001 (3)0.013 (3)
C610.030 (6)0.084 (10)0.058 (7)0.003 (6)0.011 (5)0.016 (7)
C620.035 (7)0.108 (13)0.070 (8)0.002 (6)0.019 (6)0.029 (8)
C630.059 (9)0.142 (18)0.046 (6)0.025 (9)0.017 (7)0.016 (9)
C640.049 (8)0.104 (13)0.061 (7)0.012 (7)0.021 (6)0.001 (8)
C650.050 (7)0.063 (9)0.052 (6)0.005 (6)0.015 (5)0.010 (6)
C660.023 (5)0.049 (7)0.034 (4)0.001 (4)0.003 (4)0.016 (4)
C790.030 (6)0.084 (10)0.058 (7)0.003 (6)0.011 (5)0.016 (7)
C800.035 (7)0.108 (13)0.070 (8)0.002 (6)0.019 (6)0.029 (8)
C810.059 (9)0.142 (18)0.046 (6)0.025 (9)0.017 (7)0.016 (9)
C820.049 (8)0.104 (13)0.061 (7)0.012 (7)0.021 (6)0.001 (8)
C830.050 (7)0.063 (9)0.052 (6)0.005 (6)0.015 (5)0.010 (6)
C840.023 (5)0.049 (7)0.034 (4)0.001 (4)0.003 (4)0.016 (4)
C670.036 (3)0.032 (3)0.039 (3)0.001 (3)0.006 (3)0.003 (3)
C680.046 (4)0.035 (3)0.053 (4)0.000 (3)0.004 (3)0.006 (3)
C690.067 (5)0.035 (4)0.049 (4)0.008 (4)0.007 (4)0.009 (3)
C700.077 (6)0.046 (5)0.056 (5)0.029 (4)0.010 (4)0.010 (4)
C710.048 (4)0.062 (5)0.058 (5)0.017 (4)0.003 (4)0.017 (4)
C720.035 (3)0.033 (3)0.047 (4)0.002 (3)0.006 (3)0.002 (3)
Geometric parameters (Å, º) top
Ag1—P12.450 (2)C29—H29A0.9500
Ag1—I2i2.8129 (13)C31—C361.382 (10)
Ag1—I12.9334 (14)C31—C321.392 (11)
Ag1—I22.9808 (13)C31—H31A0.9500
Ag2—P22.4503 (19)C32—C331.353 (12)
Ag2—I12.8163 (11)C32—H32A0.9500
Ag2—I22.9199 (14)C33—C341.391 (13)
Ag2—I1i2.9595 (11)C33—H33A0.9500
Ag3—P32.444 (2)C34—C351.387 (12)
Ag3—I42.8700 (13)C34—H34A0.9500
Ag3—I32.8846 (12)C35—C361.379 (10)
Ag3—I3ii2.9355 (12)C35—H35A0.9500
Ag4—P42.450 (2)C37—C381.515 (10)
Ag4—I42.9029 (10)C37—C421.526 (9)
Ag4—I4ii2.9175 (12)C37—H37A0.9900
Ag4—I32.9176 (13)C37—H37B0.9900
I1—Ag2i2.9593 (11)C38—C391.445 (10)
I2—Ag1i2.8129 (13)C38—H38A0.9900
I3—Ag3ii2.9355 (12)C38—H38B0.9900
I4—Ag4ii2.9176 (12)C39—C401.486 (10)
P1—C181.831 (7)C39—H39A0.9900
P1—C781.831 (14)C39—H39B0.9900
P1—C121.858 (8)C40—C411.520 (10)
P1—C61.865 (8)C40—H40A0.9900
P2—C301.825 (7)C40—H40B0.9900
P2—C361.838 (7)C41—C421.499 (10)
P2—C241.839 (7)C41—H41A0.9900
P3—C421.822 (9)C41—H41B0.9900
P3—C901.834 (6)C42—H42A1.0000
P3—C481.834 (7)C43—C441.358 (13)
P3—C541.850 (16)C43—C481.396 (11)
P4—C661.818 (12)C43—H43A0.9500
P4—C721.821 (7)C44—C451.359 (16)
P4—C601.843 (7)C44—H44A0.9500
P4—C841.854 (5)C45—C461.358 (15)
C1—C61.495 (11)C45—H45A0.9500
C1—C21.517 (11)C46—C471.403 (11)
C1—H1A0.9900C46—H46A0.9500
C1—H1B0.9900C47—C481.371 (12)
C2—C31.521 (11)C47—H47A0.9500
C2—H2A0.9900C49—C501.3900
C2—H2B0.9900C49—C541.3900
C3—C41.496 (13)C49—H49A0.9500
C3—H3A0.9900C50—C511.3705
C3—H3B0.9900C50—H50A0.9500
C4—C51.549 (12)C51—C521.3900
C4—H4A0.9900C51—H51A0.9500
C4—H4B0.9900C52—C531.3900
C5—C61.525 (10)C52—H52A0.9500
C5—H5A0.9900C53—C541.3900
C5—H5B0.9900C53—H53A0.9500
C6—H6A1.0000C85—C861.3900
C7—C81.3900C85—C901.3900
C7—C121.3900C85—H85A0.9500
C7—H7A0.9500C86—C871.3900
C8—C91.3900C86—H86A0.9500
C8—H8A0.9500C87—C881.3900
C9—C101.3900C87—H87A0.9500
C9—H9A0.9500C88—C891.3900
C10—C111.3900C88—H88A0.9500
C10—H10A0.9500C89—C901.3900
C11—C121.3900C89—H89A0.9500
C11—H11A0.9500C55—C601.526 (8)
C73—C741.3900C55—C561.529 (8)
C73—C781.3900C55—H55A0.9900
C73—H73A0.9500C55—H55B0.9900
C74—C751.3900C56—C571.516 (9)
C74—H74A0.9500C56—H56A0.9900
C75—C761.3900C56—H56B0.9900
C75—H75A0.9500C57—C581.513 (9)
C76—C771.3900C57—H57A0.9900
C76—H76A0.9500C57—H57B0.9900
C77—C781.3900C58—C591.512 (9)
C77—H77A0.9500C58—H58A0.9900
C13—C141.378 (12)C58—H58B0.9900
C13—C181.387 (11)C59—C601.530 (9)
C13—H13A0.9500C59—H59A0.9900
C14—C151.374 (12)C59—H59B0.9900
C14—H14A0.9500C60—H60A1.0000
C15—C161.370 (12)C61—C621.3900
C15—H15A0.9500C61—C661.3900
C16—C171.392 (12)C61—H61A0.9500
C16—H16A0.9500C62—C631.3900
C17—C181.389 (11)C62—H62A0.9500
C17—H17A0.9500C63—C641.3900
C19—C241.530 (10)C63—H63A0.9500
C19—C201.540 (11)C64—C651.3900
C19—H19A0.9900C64—H64A0.9500
C19—H19B0.9900C65—C661.3900
C20—C211.500 (12)C65—H65A0.9500
C20—H20A0.9900C79—C801.3900
C20—H20B0.9900C79—C841.3900
C21—C221.480 (13)C79—H79A0.9500
C21—H21A0.9900C80—C811.3900
C21—H21B0.9900C80—H80A0.9500
C22—C231.536 (11)C81—C821.3900
C22—H22A0.9900C81—H81A0.9500
C22—H22B0.9900C82—C831.3900
C23—C241.500 (10)C82—H82A0.9500
C23—H23A0.9900C83—C841.3900
C23—H23B0.9900C83—H83A0.9500
C24—H24A1.0000C67—C721.395 (9)
C25—C301.367 (11)C67—C681.412 (10)
C25—C261.393 (13)C67—H67A0.9500
C25—H25A0.9500C68—C691.370 (10)
C26—C271.355 (13)C68—H68A0.9500
C26—H26A0.9500C69—C701.382 (12)
C27—C281.378 (13)C69—H69A0.9500
C27—H27A0.9500C70—C711.400 (12)
C28—C291.403 (12)C70—H70A0.9500
C28—H28A0.9500C71—C721.375 (10)
C29—C301.381 (10)C71—H71A0.9500
P1—Ag1—I2i122.00 (5)C29—C28—H28A119.8
P1—Ag1—I1113.51 (5)C30—C29—C28120.2 (8)
I2i—Ag1—I1103.73 (3)C30—C29—H29A119.9
P1—Ag1—I2109.75 (6)C28—C29—H29A119.9
I2i—Ag1—I2102.17 (4)C25—C30—C29117.8 (7)
I1—Ag1—I2103.71 (3)C25—C30—P2117.9 (5)
P2—Ag2—I1124.64 (5)C29—C30—P2124.3 (6)
P2—Ag2—I2109.52 (5)C36—C31—C32120.4 (7)
I1—Ag2—I2108.35 (2)C36—C31—H31A119.8
P2—Ag2—I1i110.27 (5)C32—C31—H31A119.8
I1—Ag2—I1i100.68 (3)C33—C32—C31120.6 (8)
I2—Ag2—I1i100.50 (2)C33—C32—H32A119.7
P3—Ag3—I4111.91 (6)C31—C32—H32A119.7
P3—Ag3—I3118.03 (7)C32—C33—C34119.8 (8)
I4—Ag3—I3104.40 (2)C32—C33—H33A120.1
P3—Ag3—I3ii116.12 (7)C34—C33—H33A120.1
I4—Ag3—I3ii102.95 (3)C35—C34—C33119.7 (8)
I3—Ag3—I3ii101.63 (4)C35—C34—H34A120.2
P4—Ag4—I4116.69 (5)C33—C34—H34A120.2
P4—Ag4—I4ii114.43 (5)C36—C35—C34120.7 (8)
I4—Ag4—I4ii105.99 (3)C36—C35—H35A119.6
P4—Ag4—I3113.15 (5)C34—C35—H35A119.6
I4—Ag4—I3102.74 (2)C35—C36—C31118.7 (7)
I4ii—Ag4—I3102.23 (2)C35—C36—P2125.0 (6)
Ag2—I1—Ag174.23 (2)C31—C36—P2116.2 (5)
Ag2—I1—Ag2i76.55 (3)C38—C37—C42112.7 (7)
Ag1—I1—Ag2i74.39 (2)C38—C37—H37A109.0
Ag1i—I2—Ag276.81 (2)C42—C37—H37A109.0
Ag1i—I2—Ag175.36 (4)C38—C37—H37B109.0
Ag2—I2—Ag172.05 (2)C42—C37—H37B109.0
Ag3—I3—Ag474.43 (2)H37A—C37—H37B107.8
Ag3—I3—Ag3ii76.51 (4)C39—C38—C37113.6 (7)
Ag4—I3—Ag3ii74.78 (2)C39—C38—H38A108.8
Ag3—I4—Ag474.87 (2)C37—C38—H38A108.9
Ag3—I4—Ag4ii75.78 (2)C39—C38—H38B108.9
Ag4—I4—Ag4ii72.57 (3)C37—C38—H38B108.9
C18—P1—C78105.6 (11)H38A—C38—H38B107.7
C18—P1—C12105.4 (5)C38—C39—C40116.1 (7)
C18—P1—C6102.9 (3)C38—C39—H39A108.3
C78—P1—C697.5 (11)C40—C39—H39A108.3
C12—P1—C6103.0 (6)C38—C39—H39B108.3
C18—P1—Ag1114.3 (2)C40—C39—H39B108.3
C78—P1—Ag1117.5 (11)H39A—C39—H39B107.4
C12—P1—Ag1113.0 (5)C39—C40—C41112.5 (7)
C6—P1—Ag1116.7 (3)C39—C40—H40A109.1
C30—P2—C36102.5 (3)C41—C40—H40A109.1
C30—P2—C24102.5 (3)C39—C40—H40B109.1
C36—P2—C24103.5 (3)C41—C40—H40B109.1
C30—P2—Ag2116.5 (2)H40A—C40—H40B107.8
C36—P2—Ag2110.7 (2)C42—C41—C40112.7 (7)
C24—P2—Ag2119.1 (2)C42—C41—H41A109.1
C42—P3—C90100.8 (5)C40—C41—H41A109.1
C42—P3—C48105.4 (4)C42—C41—H41B109.1
C90—P3—C48102.7 (5)C40—C41—H41B109.1
C42—P3—C54113.7 (13)H41A—C41—H41B107.8
C48—P3—C5494.5 (18)C41—C42—C37110.0 (7)
C42—P3—Ag3116.7 (3)C41—C42—P3111.4 (6)
C90—P3—Ag3115.8 (4)C37—C42—P3111.9 (6)
C48—P3—Ag3113.6 (3)C41—C42—H42A107.8
C54—P3—Ag3110.6 (16)C37—C42—H42A107.8
C66—P4—C72110.2 (8)P3—C42—H42A107.8
C66—P4—C60105.8 (8)C44—C43—C48121.0 (10)
C72—P4—C60107.5 (3)C44—C43—H43A119.5
C72—P4—C8499.9 (4)C48—C43—H43A119.5
C60—P4—C8498.1 (4)C43—C44—C45119.0 (10)
C66—P4—Ag4104.5 (6)C43—C44—H44A120.5
C72—P4—Ag4115.2 (2)C45—C44—H44A120.5
C60—P4—Ag4113.3 (2)C46—C45—C44121.9 (8)
C84—P4—Ag4120.7 (3)C46—C45—H45A119.1
C6—C1—C2110.7 (7)C44—C45—H45A119.1
C6—C1—H1A109.5C45—C46—C47119.8 (10)
C2—C1—H1A109.5C45—C46—H46A120.1
C6—C1—H1B109.5C47—C46—H46A120.1
C2—C1—H1B109.5C48—C47—C46118.7 (9)
H1A—C1—H1B108.1C48—C47—H47A120.6
C1—C2—C3111.7 (7)C46—C47—H47A120.6
C1—C2—H2A109.3C47—C48—C43119.6 (7)
C3—C2—H2A109.3C47—C48—P3118.8 (6)
C1—C2—H2B109.3C43—C48—P3121.6 (7)
C3—C2—H2B109.3C50—C49—C54120.0
H2A—C2—H2B107.9C50—C49—H49A120.0
C4—C3—C2111.3 (7)C54—C49—H49A120.0
C4—C3—H3A109.4C51—C50—C49120.0
C2—C3—H3A109.4C51—C50—H50A120.0
C4—C3—H3B109.4C49—C50—H50A120.0
C2—C3—H3B109.4C52—C51—C50120.0
H3A—C3—H3B108.0C52—C51—H51A120.0
C3—C4—C5111.2 (7)C50—C51—H51A120.0
C3—C4—H4A109.4C51—C52—C53120.0
C5—C4—H4A109.4C51—C52—H52A120.0
C3—C4—H4B109.4C53—C52—H52A120.0
C5—C4—H4B109.4C54—C53—C52120.0
H4A—C4—H4B108.0C54—C53—H53A120.0
C6—C5—C4110.4 (7)C52—C53—H53A120.0
C6—C5—H5A109.6C53—C54—C49120.0
C4—C5—H5A109.6C53—C54—P3120 (2)
C6—C5—H5B109.6C49—C54—P3120 (2)
C4—C5—H5B109.6C86—C85—C90120.0
H5A—C5—H5B108.1C86—C85—H85A120.0
C1—C6—C5110.6 (7)C90—C85—H85A120.0
C1—C6—P1114.0 (6)C85—C86—C87120.0
C5—C6—P1110.2 (5)C85—C86—H86A120.0
C1—C6—H6A107.2C87—C86—H86A120.0
C5—C6—H6A107.2C88—C87—C86120.0
P1—C6—H6A107.2C88—C87—H87A120.0
C8—C7—C12120.0C86—C87—H87A120.0
C8—C7—H7A120.0C87—C88—C89120.0
C12—C7—H7A120.0C87—C88—H88A120.0
C9—C8—C7120.0C89—C88—H88A120.0
C9—C8—H8A120.0C90—C89—C88120.0
C7—C8—H8A120.0C90—C89—H89A120.0
C8—C9—C10120.0C88—C89—H89A120.0
C8—C9—H9A120.0C89—C90—C85120.0
C10—C9—H9A120.0C89—C90—P3125.0 (6)
C11—C10—C9120.0C85—C90—P3114.4 (5)
C11—C10—H10A120.0C60—C55—C56110.5 (5)
C9—C10—H10A120.0C60—C55—H55A109.5
C12—C11—C10120.0C56—C55—H55A109.5
C12—C11—H11A120.0C60—C55—H55B109.5
C10—C11—H11A120.0C56—C55—H55B109.5
C11—C12—C7120.0H55A—C55—H55B108.1
C11—C12—P1119.3 (9)C57—C56—C55112.0 (6)
C7—C12—P1119.5 (10)C57—C56—H56A109.2
C74—C73—C78120.0C55—C56—H56A109.2
C74—C73—H73A120.0C57—C56—H56B109.2
C78—C73—H73A120.0C55—C56—H56B109.2
C73—C74—C75120.0H56A—C56—H56B107.9
C73—C74—H74A120.0C58—C57—C56111.4 (6)
C75—C74—H74A120.0C58—C57—H57A109.4
C74—C75—C76120.0C56—C57—H57A109.4
C74—C75—H75A120.0C58—C57—H57B109.4
C76—C75—H75A120.0C56—C57—H57B109.4
C77—C76—C75120.0H57A—C57—H57B108.0
C77—C76—H76A120.0C59—C58—C57111.1 (6)
C75—C76—H76A120.0C59—C58—H58A109.4
C76—C77—C78120.0C57—C58—H58A109.4
C76—C77—H77A120.0C59—C58—H58B109.4
C78—C77—H77A120.0C57—C58—H58B109.4
C77—C78—C73120.0H58A—C58—H58B108.0
C77—C78—P1106 (2)C58—C59—C60111.5 (7)
C73—C78—P1134 (2)C58—C59—H59A109.3
C14—C13—C18121.0 (8)C60—C59—H59A109.3
C14—C13—H13A119.5C58—C59—H59B109.3
C18—C13—H13A119.5C60—C59—H59B109.3
C15—C14—C13120.1 (8)H59A—C59—H59B108.0
C15—C14—H14A119.9C55—C60—C59109.8 (6)
C13—C14—H14A119.9C55—C60—P4112.5 (4)
C16—C15—C14119.5 (8)C59—C60—P4109.3 (5)
C16—C15—H15A120.3C55—C60—H60A108.4
C14—C15—H15A120.3C59—C60—H60A108.4
C15—C16—C17121.1 (8)P4—C60—H60A108.4
C15—C16—H16A119.5C62—C61—C66120.0
C17—C16—H16A119.5C62—C61—H61A120.0
C18—C17—C16119.5 (8)C66—C61—H61A120.0
C18—C17—H17A120.3C61—C62—C63120.0
C16—C17—H17A120.3C61—C62—H62A120.0
C13—C18—C17118.7 (7)C63—C62—H62A120.0
C13—C18—P1124.7 (6)C62—C63—C64120.0
C17—C18—P1116.3 (6)C62—C63—H63A120.0
C24—C19—C20111.2 (6)C64—C63—H63A120.0
C24—C19—H19A109.4C65—C64—C63120.0
C20—C19—H19A109.4C65—C64—H64A120.0
C24—C19—H19B109.4C63—C64—H64A120.0
C20—C19—H19B109.4C66—C65—C64120.0
H19A—C19—H19B108.0C66—C65—H65A120.0
C21—C20—C19111.7 (7)C64—C65—H65A120.0
C21—C20—H20A109.3C65—C66—C61120.0
C19—C20—H20A109.3C65—C66—P4124.3 (11)
C21—C20—H20B109.3C61—C66—P4115.4 (11)
C19—C20—H20B109.3C80—C79—C84120.0
H20A—C20—H20B107.9C80—C79—H79A120.0
C22—C21—C20113.1 (7)C84—C79—H79A120.0
C22—C21—H21A109.0C81—C80—C79120.0
C20—C21—H21A109.0C81—C80—H80A120.0
C22—C21—H21B109.0C79—C80—H80A120.0
C20—C21—H21B109.0C80—C81—C82120.0
H21A—C21—H21B107.8C80—C81—H81A120.0
C21—C22—C23111.9 (7)C82—C81—H81A120.0
C21—C22—H22A109.2C83—C82—C81120.0
C23—C22—H22A109.2C83—C82—H82A120.0
C21—C22—H22B109.2C81—C82—H82A120.0
C23—C22—H22B109.2C84—C83—C82120.0
H22A—C22—H22B107.9C84—C83—H83A120.0
C24—C23—C22110.9 (7)C82—C83—H83A120.0
C24—C23—H23A109.5C83—C84—C79120.0
C22—C23—H23A109.5C83—C84—P4117.8 (4)
C24—C23—H23B109.5C79—C84—P4122.0 (4)
C22—C23—H23B109.5C72—C67—C68119.1 (6)
H23A—C23—H23B108.0C72—C67—H67A120.4
C23—C24—C19109.7 (6)C68—C67—H67A120.4
C23—C24—P2114.2 (5)C69—C68—C67120.3 (7)
C19—C24—P2111.3 (5)C69—C68—H68A119.8
C23—C24—H24A107.1C67—C68—H68A119.8
C19—C24—H24A107.1C68—C69—C70120.8 (7)
P2—C24—H24A107.1C68—C69—H69A119.6
C30—C25—C26122.3 (8)C70—C69—H69A119.6
C30—C25—H25A118.8C69—C70—C71118.8 (8)
C26—C25—H25A118.8C69—C70—H70A120.6
C27—C26—C25119.5 (8)C71—C70—H70A120.6
C27—C26—H26A120.3C72—C71—C70121.4 (8)
C25—C26—H26A120.3C72—C71—H71A119.3
C26—C27—C28119.7 (8)C70—C71—H71A119.3
C26—C27—H27A120.2C71—C72—C67119.5 (7)
C28—C27—H27A120.2C71—C72—P4124.9 (6)
C27—C28—C29120.3 (8)C67—C72—P4115.6 (5)
C27—C28—H28A119.8
Symmetry codes: (i) x+1, y, z+1; (ii) x+2, y, z.

Experimental details

Crystal data
Chemical formula[Ag4I4(C18H21P)4]
Mr2012.35
Crystal system, space groupMonoclinic, C2
Temperature (K)120
a, b, c (Å)24.698 (9), 12.404 (5), 24.328 (9)
β (°) 104.145 (7)
V3)7227 (5)
Z4
Radiation typeMo Kα
µ (mm1)2.91
Crystal size (mm)0.15 × 0.14 × 0.09
Data collection
DiffractometerBruker APEX
Absorption correctionMulti-scan
(SADABS; Bruker, 2002)
Tmin, Tmax0.652, 0.767
No. of measured, independent and
observed [I > 2σ(I)] reflections
42119, 16990, 15397
Rint0.041
(sin θ/λ)max1)0.668
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.043, 0.107, 1.05
No. of reflections16990
No. of parameters742
No. of restraints327
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0456P)2 + 26.0708P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)2.48, 1.27
Absolute structureFlack (1983), 7870 Friedel pairs
Absolute structure parameter0.029 (18)

Computer programs: SMART (Bruker, 2002), SAINT (Bruker, 2002), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2002), SHELXTL.

 

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