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The reaction of silver(I) iodide with tri(p-tolyl)phosphine in MeCN solution in 1:3 molar ratio yields a polymorph of the complex of the formula [AgI{P(4-MeC6H4)3}3], with the Ag atom in a distorted tetrahedral environment. A polymorphic structure of this complex (a) is compared with previously published crystal structures (b), determined at different temperatures. The two polymorphs are compared using r.m.s. overlay calculations as well as half-normal probability plots.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768109001372/bp5016sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768109001372/bp5016Isup2.hkl
Contains datablock I

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0108768109001372/bp5016sup3.pdf
Cavity plots and simulated powder patterns

CCDC reference: 689510

Comment top

See manuscript

Experimental top

See manuscript

Refinement top

See manuscript

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND 3.0c (Brandenburg & Putz, 2004); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
See manuscript
(I) top
Crystal data top
C63H63AgIP3F(000) = 4688
Mr = 1147.82Dx = 1.395 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71069 Å
Hall symbol: -C 2ycCell parameters from 8070 reflections
a = 22.745 (3) Åθ = 2.2–28.3°
b = 11.0100 (12) ŵ = 1.06 mm1
c = 44.797 (5) ÅT = 100 K
β = 103.007 (5)°Cuboid, colourless
V = 10930 (2) Å30.26 × 0.2 × 0.17 mm
Z = 8
Data collection top
CCD area detector
diffractometer
12118 reflections with I > 2σ(I)
phi and ω scansRint = 0.033
Absorption correction: multi-scan
SADABS (Bruker, 2004)
θmax = 28.4°, θmin = 0.9°
Tmin = 0.770, Tmax = 0.840h = 3030
88005 measured reflectionsk = 1414
13655 independent reflectionsl = 5959
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.026 w = 1/[σ2(Fo2) + (0.0182P)2 + 18.1054P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.058(Δ/σ)max = 0.004
S = 1.07Δρmax = 0.43 e Å3
13655 reflectionsΔρmin = 0.50 e Å3
623 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.000064 (7)
Primary atom site location: structure-invariant direct methods
Crystal data top
C63H63AgIP3V = 10930 (2) Å3
Mr = 1147.82Z = 8
Monoclinic, C2/cMo Kα radiation
a = 22.745 (3) ŵ = 1.06 mm1
b = 11.0100 (12) ÅT = 100 K
c = 44.797 (5) Å0.26 × 0.2 × 0.17 mm
β = 103.007 (5)°
Data collection top
CCD area detector
diffractometer
13655 independent reflections
Absorption correction: multi-scan
SADABS (Bruker, 2004)
12118 reflections with I > 2σ(I)
Tmin = 0.770, Tmax = 0.840Rint = 0.033
88005 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0260 restraints
wR(F2) = 0.058H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0182P)2 + 18.1054P]
where P = (Fo2 + 2Fc2)/3
13655 reflectionsΔρmax = 0.43 e Å3
623 parametersΔρmin = 0.50 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C2370.66761 (10)0.56920 (18)0.04637 (5)0.0290 (5)
H23A0.63430.56910.02820.044*
H23B0.69930.62450.04310.044*
H23C0.65270.59630.06420.044*
C1110.62321 (8)0.02438 (16)0.16634 (4)0.0165 (3)
C1120.56297 (8)0.04001 (16)0.16822 (4)0.0190 (4)
H1120.53140.01370.15180.023*
C1130.54914 (8)0.09365 (17)0.19384 (4)0.0216 (4)
H1130.50810.10370.19480.026*
C1140.59458 (9)0.13293 (17)0.21820 (4)0.0217 (4)
C1150.65424 (9)0.12012 (17)0.21589 (4)0.0224 (4)
H1150.68580.14760.23220.027*
C1160.66842 (8)0.06789 (16)0.19024 (4)0.0197 (4)
H1160.70940.06170.1890.024*
C1170.57973 (10)0.1887 (2)0.24639 (5)0.0322 (5)
H11A0.61670.22070.25970.048*
H11B0.55070.25480.24030.048*
H11C0.56220.12660.25750.048*
C1210.63070 (8)0.21322 (16)0.13910 (4)0.0163 (3)
C1220.57870 (8)0.25562 (17)0.14757 (4)0.0206 (4)
H1220.54930.19940.15110.025*
C1230.56978 (9)0.37880 (17)0.15084 (4)0.0222 (4)
H1230.5340.40590.15640.027*
C1240.61211 (9)0.46390 (17)0.14617 (4)0.0228 (4)
C1250.66320 (9)0.42218 (17)0.13718 (5)0.0250 (4)
H1250.69220.47860.13340.03*
C1260.67215 (8)0.29816 (17)0.13369 (4)0.0215 (4)
H1260.70730.27130.12750.026*
C1270.60125 (11)0.59755 (18)0.15038 (6)0.0350 (5)
H12A0.63370.64490.14490.052*
H12B0.60050.61320.17180.052*
H12C0.56250.62120.13720.052*
C1310.58572 (8)0.00920 (16)0.10187 (4)0.0160 (3)
C1320.55948 (8)0.09207 (17)0.07940 (4)0.0201 (4)
H1320.57110.17510.08150.024*
C1330.51620 (9)0.05435 (18)0.05388 (4)0.0241 (4)
H1330.49890.11230.03870.029*
C1340.49784 (9)0.06593 (18)0.05013 (4)0.0228 (4)
C1350.52502 (8)0.14886 (17)0.07238 (4)0.0216 (4)
H1350.51350.23190.07020.026*
C1360.56865 (8)0.11290 (17)0.09776 (4)0.0197 (4)
H1360.58710.17160.11250.024*
C1370.44945 (10)0.1057 (2)0.02296 (5)0.0337 (5)
H13A0.41290.12750.02980.05*
H13B0.46370.17630.01330.05*
H13C0.44040.0390.00810.05*
C2110.72216 (8)0.03792 (16)0.04361 (4)0.0168 (3)
C2120.73900 (9)0.0439 (2)0.01562 (4)0.0274 (4)
H2120.77420.00280.0130.033*
C2130.70462 (10)0.1096 (2)0.00847 (5)0.0309 (5)
H2130.71690.11350.02730.037*
C2140.65254 (9)0.16966 (17)0.00559 (4)0.0229 (4)
C2150.63480 (9)0.16024 (16)0.02190 (4)0.0206 (4)
H2150.59830.19770.0240.025*
C2160.66959 (8)0.09674 (16)0.04656 (4)0.0182 (4)
H2160.65740.09360.06550.022*
C2170.61775 (10)0.2461 (2)0.03164 (5)0.0326 (5)
H21A0.64280.31450.03530.049*
H21B0.60690.19640.05020.049*
H21C0.5810.27690.02630.049*
C2210.84132 (8)0.03990 (16)0.07306 (4)0.0171 (3)
C2220.86694 (8)0.10446 (17)0.05250 (4)0.0209 (4)
H2220.84410.16510.03990.025*
C2230.92588 (9)0.08051 (18)0.05036 (5)0.0242 (4)
H2230.94250.12420.03590.029*
C2240.96111 (8)0.00642 (18)0.06897 (5)0.0241 (4)
C2250.93589 (8)0.06809 (18)0.08998 (4)0.0226 (4)
H2250.95940.12620.10320.027*
C2260.87666 (8)0.04622 (17)0.09200 (4)0.0196 (4)
H2260.860.09020.10640.024*
C2271.02431 (9)0.0334 (2)0.06553 (6)0.0361 (5)
H22A1.04510.08390.08270.054*
H22B1.04640.0430.06540.054*
H22C1.02250.07670.04620.054*
C2310.73882 (8)0.20598 (16)0.06347 (4)0.0155 (3)
C2320.68537 (9)0.22710 (17)0.04187 (4)0.0227 (4)
H2320.6640.16090.03080.027*
C2330.66308 (9)0.34438 (18)0.03637 (5)0.0259 (4)
H2330.62660.35720.02150.031*
C2340.69285 (9)0.44315 (17)0.05202 (4)0.0209 (4)
C2350.74671 (9)0.42198 (17)0.07327 (4)0.0231 (4)
H2350.76850.48850.08390.028*
C2360.76908 (8)0.30518 (17)0.07916 (4)0.0205 (4)
H2360.80550.29260.09410.025*
C3110.86296 (8)0.22523 (16)0.16040 (4)0.0168 (3)
C3120.84113 (8)0.33750 (17)0.16742 (4)0.0203 (4)
H3120.81470.34160.18110.024*
C3130.85774 (8)0.44403 (17)0.15453 (4)0.0220 (4)
H3130.8420.51950.15940.026*
C3140.89687 (8)0.44216 (17)0.13463 (4)0.0202 (4)
C3150.92006 (8)0.32997 (18)0.12861 (4)0.0207 (4)
H3150.9480.32650.11570.025*
C3160.90342 (8)0.22329 (17)0.14093 (4)0.0188 (4)
H3160.91960.14810.13610.023*
C3170.91164 (9)0.55691 (19)0.11950 (5)0.0278 (4)
H31A0.93810.53760.10560.042*
H31B0.93210.6140.13520.042*
H31C0.87430.59380.10780.042*
C3210.90193 (8)0.01156 (17)0.18353 (4)0.0181 (4)
C3220.95584 (8)0.03913 (18)0.20006 (4)0.0214 (4)
H3220.95920.12470.20270.026*
C3231.00460 (8)0.03490 (19)0.21263 (4)0.0236 (4)
H3231.0410.00090.22370.028*
C3241.00104 (9)0.16074 (19)0.20931 (4)0.0242 (4)
C3250.94749 (9)0.21031 (18)0.19257 (4)0.0240 (4)
H3250.94430.29580.18990.029*
C3260.89848 (9)0.13737 (17)0.17970 (4)0.0206 (4)
H3260.86240.17330.16820.025*
C3271.05435 (10)0.2404 (2)0.22355 (5)0.0339 (5)
H32A1.08940.2170.21550.051*
H32B1.04430.32560.21850.051*
H32C1.06380.23010.24580.051*
C3310.80775 (8)0.10081 (16)0.20589 (4)0.0174 (3)
C3320.83088 (9)0.03257 (18)0.23210 (4)0.0227 (4)
H3320.86440.01950.23260.027*
C3330.80571 (10)0.0395 (2)0.25754 (4)0.0280 (4)
H3330.82260.00760.27520.034*
C3340.75640 (10)0.11377 (19)0.25782 (5)0.0279 (4)
C3370.72863 (12)0.1200 (2)0.28543 (5)0.0436 (6)
H33A0.74150.04930.29860.065*
H33B0.68460.12020.27870.065*
H33C0.74190.19450.2970.065*
C3350.73338 (9)0.18190 (19)0.23166 (5)0.0248 (4)
H3360.70010.23450.23140.03*
C3360.75773 (8)0.17501 (17)0.20600 (4)0.0205 (4)
H3370.74030.22110.18830.025*
P10.64570 (2)0.05189 (4)0.134480 (10)0.01517 (9)
P20.76277 (2)0.05256 (4)0.075737 (10)0.01494 (9)
P30.83375 (2)0.07902 (4)0.170325 (10)0.01502 (9)
Ag10.749448 (6)0.000654 (11)0.128269 (3)0.01451 (4)
I10.748947 (5)0.258264 (10)0.125807 (3)0.02076 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C2370.0292 (11)0.0195 (10)0.0397 (12)0.0063 (8)0.0105 (10)0.0057 (9)
C1110.0161 (8)0.0146 (8)0.0178 (8)0.0019 (7)0.0019 (7)0.0014 (7)
C1120.0144 (8)0.0200 (9)0.0207 (9)0.0009 (7)0.0002 (7)0.0045 (7)
C1130.0167 (9)0.0239 (9)0.0246 (9)0.0007 (8)0.0056 (8)0.0047 (8)
C1140.0237 (9)0.0211 (9)0.0201 (9)0.0003 (8)0.0045 (8)0.0039 (7)
C1150.0195 (9)0.0228 (9)0.0218 (9)0.0012 (8)0.0022 (8)0.0052 (7)
C1160.0152 (8)0.0187 (9)0.0235 (9)0.0005 (7)0.0009 (7)0.0022 (7)
C1170.0309 (11)0.0418 (13)0.0247 (10)0.0042 (10)0.0079 (9)0.0133 (9)
C1210.0153 (8)0.0164 (8)0.0164 (8)0.0001 (7)0.0019 (7)0.0013 (7)
C1220.0196 (9)0.0184 (9)0.0250 (9)0.0028 (7)0.0078 (8)0.0000 (7)
C1230.0233 (9)0.0216 (9)0.0231 (9)0.0023 (8)0.0083 (8)0.0004 (7)
C1240.0283 (10)0.0181 (9)0.0222 (9)0.0002 (8)0.0062 (8)0.0018 (7)
C1250.0239 (10)0.0174 (9)0.0341 (11)0.0028 (8)0.0074 (9)0.0045 (8)
C1260.0178 (9)0.0206 (9)0.0268 (10)0.0005 (8)0.0066 (8)0.0034 (8)
C1270.0421 (13)0.0172 (10)0.0495 (14)0.0031 (9)0.0186 (11)0.0026 (9)
C1310.0130 (8)0.0183 (8)0.0167 (8)0.0001 (7)0.0033 (7)0.0017 (7)
C1320.0232 (9)0.0170 (8)0.0200 (9)0.0010 (7)0.0044 (8)0.0013 (7)
C1330.0274 (10)0.0230 (10)0.0196 (9)0.0053 (8)0.0003 (8)0.0045 (7)
C1340.0202 (9)0.0284 (10)0.0184 (9)0.0022 (8)0.0012 (8)0.0006 (8)
C1350.0212 (9)0.0207 (9)0.0225 (9)0.0046 (8)0.0038 (8)0.0006 (7)
C1360.0188 (9)0.0192 (9)0.0194 (9)0.0011 (7)0.0007 (7)0.0048 (7)
C1370.0342 (12)0.0346 (12)0.0249 (10)0.0021 (10)0.0088 (9)0.0007 (9)
C2110.0186 (9)0.0143 (8)0.0157 (8)0.0022 (7)0.0002 (7)0.0008 (6)
C2120.0233 (10)0.0376 (12)0.0222 (10)0.0075 (9)0.0070 (8)0.0070 (8)
C2130.0282 (11)0.0457 (13)0.0196 (9)0.0029 (10)0.0069 (9)0.0093 (9)
C2140.0225 (9)0.0211 (9)0.0216 (9)0.0039 (8)0.0021 (8)0.0048 (7)
C2150.0191 (9)0.0153 (8)0.0254 (9)0.0000 (7)0.0007 (8)0.0007 (7)
C2160.0213 (9)0.0161 (8)0.0171 (8)0.0017 (7)0.0039 (7)0.0006 (7)
C2170.0294 (11)0.0341 (12)0.0292 (11)0.0013 (10)0.0041 (9)0.0135 (9)
C2210.0166 (8)0.0179 (9)0.0157 (8)0.0013 (7)0.0012 (7)0.0042 (7)
C2220.0200 (9)0.0190 (9)0.0221 (9)0.0026 (7)0.0016 (8)0.0004 (7)
C2230.0224 (10)0.0260 (10)0.0249 (10)0.0077 (8)0.0069 (8)0.0022 (8)
C2240.0163 (9)0.0273 (10)0.0273 (10)0.0024 (8)0.0018 (8)0.0089 (8)
C2250.0192 (9)0.0246 (10)0.0212 (9)0.0043 (8)0.0011 (8)0.0035 (8)
C2260.0201 (9)0.0209 (9)0.0165 (8)0.0010 (7)0.0013 (7)0.0022 (7)
C2270.0201 (10)0.0436 (13)0.0456 (13)0.0020 (10)0.0093 (10)0.0023 (11)
C2310.0172 (8)0.0153 (8)0.0142 (8)0.0006 (7)0.0042 (7)0.0006 (6)
C2320.0224 (9)0.0197 (9)0.0227 (9)0.0002 (8)0.0021 (8)0.0012 (7)
C2330.0227 (10)0.0261 (10)0.0256 (10)0.0053 (8)0.0018 (8)0.0043 (8)
C2340.0235 (9)0.0185 (9)0.0228 (9)0.0036 (8)0.0093 (8)0.0043 (7)
C2350.0244 (10)0.0174 (9)0.0266 (10)0.0034 (8)0.0037 (8)0.0020 (8)
C2360.0193 (9)0.0193 (9)0.0208 (9)0.0003 (7)0.0001 (7)0.0017 (7)
C3110.0134 (8)0.0196 (9)0.0156 (8)0.0020 (7)0.0007 (7)0.0009 (7)
C3120.0189 (9)0.0214 (9)0.0209 (9)0.0008 (7)0.0050 (8)0.0011 (7)
C3130.0205 (9)0.0181 (9)0.0271 (10)0.0014 (7)0.0049 (8)0.0003 (7)
C3140.0152 (8)0.0221 (9)0.0211 (9)0.0024 (7)0.0007 (7)0.0023 (7)
C3150.0153 (8)0.0268 (10)0.0199 (9)0.0036 (8)0.0037 (7)0.0002 (7)
C3160.0155 (8)0.0218 (9)0.0186 (8)0.0008 (7)0.0029 (7)0.0026 (7)
C3170.0232 (10)0.0268 (10)0.0331 (11)0.0026 (8)0.0063 (9)0.0084 (9)
C3210.0164 (8)0.0225 (9)0.0148 (8)0.0019 (7)0.0025 (7)0.0004 (7)
C3220.0190 (9)0.0248 (10)0.0196 (9)0.0008 (8)0.0022 (8)0.0043 (7)
C3230.0149 (9)0.0348 (11)0.0187 (9)0.0020 (8)0.0012 (7)0.0053 (8)
C3240.0225 (9)0.0326 (11)0.0164 (9)0.0097 (8)0.0023 (8)0.0006 (8)
C3250.0266 (10)0.0230 (9)0.0209 (9)0.0058 (8)0.0025 (8)0.0002 (8)
C3260.0195 (9)0.0226 (9)0.0181 (8)0.0006 (8)0.0009 (7)0.0000 (7)
C3270.0301 (11)0.0429 (13)0.0254 (10)0.0171 (10)0.0005 (9)0.0017 (9)
C3310.0159 (8)0.0196 (9)0.0160 (8)0.0047 (7)0.0023 (7)0.0035 (7)
C3320.0214 (9)0.0255 (10)0.0198 (9)0.0009 (8)0.0016 (8)0.0007 (8)
C3330.0333 (11)0.0331 (11)0.0168 (9)0.0058 (9)0.0040 (8)0.0021 (8)
C3340.0295 (11)0.0332 (11)0.0232 (10)0.0094 (9)0.0107 (9)0.0068 (9)
C3370.0507 (15)0.0550 (16)0.0318 (12)0.0063 (13)0.0234 (12)0.0052 (11)
C3350.0203 (9)0.0275 (10)0.0276 (10)0.0048 (8)0.0074 (8)0.0091 (8)
C3360.0178 (9)0.0219 (9)0.0213 (9)0.0045 (7)0.0029 (7)0.0030 (7)
P10.0126 (2)0.0146 (2)0.0179 (2)0.00063 (17)0.00255 (17)0.00174 (17)
P20.0159 (2)0.0147 (2)0.0133 (2)0.00025 (17)0.00162 (17)0.00018 (16)
P30.0127 (2)0.0174 (2)0.0140 (2)0.00021 (17)0.00097 (17)0.00116 (17)
Ag10.01342 (6)0.01470 (7)0.01467 (6)0.00023 (5)0.00160 (5)0.00015 (5)
I10.02249 (7)0.01317 (6)0.02471 (7)0.00125 (5)0.00129 (5)0.00072 (4)
Geometric parameters (Å, º) top
C237—C2341.501 (3)C223—H2230.95
C237—H23A0.98C224—C2251.385 (3)
C237—H23B0.98C224—C2271.509 (3)
C237—H23C0.98C225—C2261.391 (3)
C111—C1161.392 (2)C225—H2250.95
C111—C1121.402 (2)C226—H2260.95
C111—P11.8256 (18)C227—H22A0.98
C112—C1131.388 (3)C227—H22B0.98
C112—H1120.95C227—H22C0.98
C113—C1141.392 (3)C231—C2321.392 (3)
C113—H1130.95C231—C2361.394 (3)
C114—C1151.391 (3)C231—P21.8214 (18)
C114—C1171.509 (3)C232—C2331.389 (3)
C115—C1161.386 (3)C232—H2320.95
C115—H1150.95C233—C2341.385 (3)
C116—H1160.95C233—H2330.95
C117—H11A0.98C234—C2351.392 (3)
C117—H11B0.98C235—C2361.386 (3)
C117—H11C0.98C235—H2350.95
C121—C1261.387 (2)C236—H2360.95
C121—C1221.401 (2)C311—C3121.394 (3)
C121—P11.8292 (18)C311—C3161.403 (2)
C122—C1231.384 (3)C311—P31.8340 (18)
C122—H1220.95C312—C3131.397 (3)
C123—C1241.393 (3)C312—H3120.95
C123—H1230.95C313—C3141.394 (3)
C124—C1251.391 (3)C313—H3130.95
C124—C1271.511 (3)C314—C3151.393 (3)
C125—C1261.395 (3)C314—C3171.507 (3)
C125—H1250.95C315—C3161.386 (3)
C126—H1260.95C315—H3150.95
C127—H12A0.98C316—H3160.95
C127—H12B0.98C317—H31A0.98
C127—H12C0.98C317—H31B0.98
C131—C1321.390 (2)C317—H31C0.98
C131—C1361.400 (2)C321—C3261.396 (3)
C131—P11.8218 (18)C321—C3221.398 (3)
C132—C1331.394 (3)C321—P31.8267 (18)
C132—H1320.95C322—C3231.389 (3)
C133—C1341.387 (3)C322—H3220.95
C133—H1330.95C323—C3241.394 (3)
C134—C1351.390 (3)C323—H3230.95
C134—C1371.511 (3)C324—C3251.390 (3)
C135—C1361.388 (3)C324—C3271.516 (3)
C135—H1350.95C325—C3261.389 (3)
C136—H1360.95C325—H3250.95
C137—H13A0.98C326—H3260.95
C137—H13B0.98C327—H32A0.98
C137—H13C0.98C327—H32B0.98
C211—C2161.392 (3)C327—H32C0.98
C211—C2121.393 (3)C331—C3321.394 (3)
C211—P21.8216 (18)C331—C3361.402 (3)
C212—C2131.385 (3)C331—P31.8355 (18)
C212—H2120.95C332—C3331.388 (3)
C213—C2141.388 (3)C332—H3320.95
C213—H2130.95C333—C3341.390 (3)
C214—C2151.383 (3)C333—H3330.95
C214—C2171.510 (3)C334—C3351.391 (3)
C215—C2161.393 (3)C334—C3371.512 (3)
C215—H2150.95C337—H33A0.98
C216—H2160.95C337—H33B0.98
C217—H21A0.98C337—H33C0.98
C217—H21B0.98C335—C3361.386 (3)
C217—H21C0.98C335—H3360.95
C221—C2221.391 (3)C336—H3370.95
C221—C2261.399 (3)P1—Ag12.5053 (5)
C221—P21.8228 (18)P2—Ag12.5087 (5)
C222—C2231.390 (3)P3—Ag12.5238 (5)
C222—H2220.95Ag1—I12.8383 (4)
C223—C2241.397 (3)
C234—C237—H23A109.5C224—C227—H22A109.5
C234—C237—H23B109.5C224—C227—H22B109.5
H23A—C237—H23B109.5H22A—C227—H22B109.5
C234—C237—H23C109.5C224—C227—H22C109.5
H23A—C237—H23C109.5H22A—C227—H22C109.5
H23B—C237—H23C109.5H22B—C227—H22C109.5
C116—C111—C112118.33 (16)C232—C231—C236118.32 (16)
C116—C111—P1118.10 (13)C232—C231—P2121.30 (14)
C112—C111—P1123.57 (13)C236—C231—P2119.62 (13)
C113—C112—C111120.54 (17)C233—C232—C231120.35 (18)
C113—C112—H112119.7C233—C232—H232119.8
C111—C112—H112119.7C231—C232—H232119.8
C112—C113—C114120.93 (17)C234—C233—C232121.52 (18)
C112—C113—H113119.5C234—C233—H233119.2
C114—C113—H113119.5C232—C233—H233119.2
C115—C114—C113118.32 (17)C233—C234—C235118.00 (17)
C115—C114—C117120.62 (18)C233—C234—C237121.03 (18)
C113—C114—C117121.07 (18)C235—C234—C237120.96 (18)
C116—C115—C114121.10 (17)C236—C235—C234120.96 (18)
C116—C115—H115119.4C236—C235—H235119.5
C114—C115—H115119.5C234—C235—H235119.5
C115—C116—C111120.72 (17)C235—C236—C231120.83 (17)
C115—C116—H116119.6C235—C236—H236119.6
C111—C116—H116119.6C231—C236—H236119.6
C114—C117—H11A109.5C312—C311—C316118.06 (17)
C114—C117—H11B109.5C312—C311—P3123.82 (14)
H11A—C117—H11B109.5C316—C311—P3117.48 (14)
C114—C117—H11C109.5C311—C312—C313120.52 (17)
H11A—C117—H11C109.5C311—C312—H312119.7
H11B—C117—H11C109.5C313—C312—H312119.7
C126—C121—C122118.10 (17)C314—C313—C312121.54 (17)
C126—C121—P1118.90 (14)C314—C313—H313119.2
C122—C121—P1123.00 (14)C312—C313—H313119.2
C123—C122—C121120.54 (17)C315—C314—C313117.44 (17)
C123—C122—H122119.7C315—C314—C317121.60 (17)
C121—C122—H122119.7C313—C314—C317120.94 (18)
C122—C123—C124121.37 (18)C316—C315—C314121.68 (17)
C122—C123—H123119.3C316—C315—H315119.2
C124—C123—H123119.3C314—C315—H315119.2
C125—C124—C123118.19 (18)C315—C316—C311120.70 (17)
C125—C124—C127121.90 (18)C315—C316—H316119.7
C123—C124—C127119.90 (18)C311—C316—H316119.7
C124—C125—C126120.55 (18)C314—C317—H31A109.5
C124—C125—H125119.7C314—C317—H31B109.5
C126—C125—H125119.7H31A—C317—H31B109.5
C121—C126—C125121.22 (17)C314—C317—H31C109.5
C121—C126—H126119.4H31A—C317—H31C109.5
C125—C126—H126119.4H31B—C317—H31C109.5
C124—C127—H12A109.5C326—C321—C322118.66 (17)
C124—C127—H12B109.5C326—C321—P3118.80 (14)
H12A—C127—H12B109.5C322—C321—P3122.22 (14)
C124—C127—H12C109.5C323—C322—C321120.36 (18)
H12A—C127—H12C109.5C323—C322—H322119.8
H12B—C127—H12C109.5C321—C322—H322119.8
C132—C131—C136118.31 (16)C322—C323—C324121.20 (18)
C132—C131—P1122.23 (14)C322—C323—H323119.4
C136—C131—P1119.25 (13)C324—C323—H323119.4
C131—C132—C133120.50 (17)C325—C324—C323118.06 (18)
C131—C132—H132119.8C325—C324—C327121.37 (19)
C133—C132—H132119.8C323—C324—C327120.57 (19)
C134—C133—C132121.42 (18)C326—C325—C324121.38 (19)
C134—C133—H133119.3C326—C325—H325119.3
C132—C133—H133119.3C324—C325—H325119.3
C133—C134—C135117.85 (17)C325—C326—C321120.32 (18)
C133—C134—C137121.25 (18)C325—C326—H326119.8
C135—C134—C137120.89 (18)C321—C326—H326119.8
C136—C135—C134121.38 (18)C324—C327—H32A109.5
C136—C135—H135119.3C324—C327—H32B109.5
C134—C135—H135119.3H32A—C327—H32B109.5
C135—C136—C131120.50 (17)C324—C327—H32C109.5
C135—C136—H136119.7H32A—C327—H32C109.5
C131—C136—H136119.7H32B—C327—H32C109.5
C134—C137—H13A109.5C332—C331—C336117.64 (17)
C134—C137—H13B109.5C332—C331—P3121.78 (14)
H13A—C137—H13B109.5C336—C331—P3119.98 (14)
C134—C137—H13C109.5C333—C332—C331120.99 (19)
H13A—C137—H13C109.5C333—C332—H332119.5
H13B—C137—H13C109.5C331—C332—H332119.5
C216—C211—C212118.66 (17)C332—C333—C334121.51 (19)
C216—C211—P2118.24 (13)C332—C333—H333119.2
C212—C211—P2122.95 (14)C334—C333—H333119.2
C213—C212—C211120.30 (19)C333—C334—C335117.46 (18)
C213—C212—H212119.8C333—C334—C337121.4 (2)
C211—C212—H212119.8C335—C334—C337121.2 (2)
C212—C213—C214121.37 (19)C334—C337—H33A109.5
C212—C213—H213119.3C334—C337—H33B109.5
C214—C213—H213119.3H33A—C337—H33B109.5
C215—C214—C213118.23 (18)C334—C337—H33C109.5
C215—C214—C217121.51 (19)H33A—C337—H33C109.5
C213—C214—C217120.24 (18)H33B—C337—H33C109.5
C214—C215—C216121.05 (18)C336—C335—C334121.63 (19)
C214—C215—H215119.5C336—C335—H336119.2
C216—C215—H215119.5C334—C335—H336119.2
C211—C216—C215120.33 (17)C335—C336—C331120.75 (18)
C211—C216—H216119.8C335—C336—H337119.6
C215—C216—H216119.8C331—C336—H337119.6
C214—C217—H21A109.5C131—P1—C111102.55 (8)
C214—C217—H21B109.5C131—P1—C121102.49 (8)
H21A—C217—H21B109.5C111—P1—C121105.43 (8)
C214—C217—H21C109.5C131—P1—Ag1113.91 (6)
H21A—C217—H21C109.5C111—P1—Ag1114.66 (6)
H21B—C217—H21C109.5C121—P1—Ag1116.18 (6)
C222—C221—C226118.60 (17)C231—P2—C211101.81 (8)
C222—C221—P2124.57 (14)C231—P2—C221106.38 (8)
C226—C221—P2116.72 (14)C211—P2—C221103.67 (8)
C223—C222—C221120.18 (18)C231—P2—Ag1114.12 (6)
C223—C222—H222119.9C211—P2—Ag1117.81 (6)
C221—C222—H222119.9C221—P2—Ag1111.78 (6)
C222—C223—C224121.42 (18)C321—P3—C311103.31 (8)
C222—C223—H223119.3C321—P3—C331101.89 (8)
C224—C223—H223119.3C311—P3—C331107.51 (8)
C225—C224—C223118.13 (18)C321—P3—Ag1119.94 (6)
C225—C224—C227121.50 (19)C311—P3—Ag1112.33 (6)
C223—C224—C227120.35 (19)C331—P3—Ag1110.75 (6)
C224—C225—C226120.95 (18)P1—Ag1—P2111.460 (16)
C224—C225—H225119.5P1—Ag1—P3114.405 (17)
C226—C225—H225119.5P2—Ag1—P3112.781 (17)
C225—C226—C221120.69 (18)P1—Ag1—I1103.853 (11)
C225—C226—H226119.7P2—Ag1—I1101.373 (12)
C221—C226—H226119.7P3—Ag1—I1111.844 (12)
C116—C111—C112—C1132.3 (3)C337—C334—C335—C336178.68 (19)
P1—C111—C112—C113176.83 (15)C334—C335—C336—C3311.6 (3)
C111—C112—C113—C1140.1 (3)C332—C331—C336—C3351.5 (3)
C112—C113—C114—C1151.7 (3)P3—C331—C336—C335172.80 (14)
C112—C113—C114—C117178.59 (19)C132—C131—P1—C111136.81 (15)
C113—C114—C115—C1161.0 (3)C136—C131—P1—C11148.58 (16)
C117—C114—C115—C116179.32 (19)C132—C131—P1—C12127.64 (17)
C114—C115—C116—C1111.4 (3)C136—C131—P1—C121157.75 (14)
C112—C111—C116—C1153.0 (3)C132—C131—P1—Ag198.69 (15)
P1—C111—C116—C115176.14 (15)C136—C131—P1—Ag175.91 (15)
C126—C121—C122—C1231.0 (3)C116—C111—P1—C131146.23 (15)
P1—C121—C122—C123179.75 (15)C112—C111—P1—C13134.64 (17)
C121—C122—C123—C1240.6 (3)C116—C111—P1—C121106.83 (15)
C122—C123—C124—C1251.9 (3)C112—C111—P1—C12172.29 (17)
C122—C123—C124—C127179.15 (19)C116—C111—P1—Ag122.24 (16)
C123—C124—C125—C1261.5 (3)C112—C111—P1—Ag1158.64 (14)
C127—C124—C125—C126179.5 (2)C126—C121—P1—C131113.80 (15)
C122—C121—C126—C1251.3 (3)C122—C121—P1—C13165.46 (17)
P1—C121—C126—C125179.35 (15)C126—C121—P1—C111139.22 (15)
C124—C125—C126—C1210.1 (3)C122—C121—P1—C11141.51 (17)
C136—C131—C132—C1331.6 (3)C126—C121—P1—Ag111.05 (17)
P1—C131—C132—C133176.21 (14)C122—C121—P1—Ag1169.68 (13)
C131—C132—C133—C1340.3 (3)C232—C231—P2—C21122.59 (17)
C132—C133—C134—C1351.4 (3)C236—C231—P2—C211167.51 (15)
C132—C133—C134—C137177.96 (19)C232—C231—P2—C221130.84 (15)
C133—C134—C135—C1360.7 (3)C236—C231—P2—C22159.26 (16)
C137—C134—C135—C136178.68 (19)C232—C231—P2—Ag1105.43 (15)
C134—C135—C136—C1311.1 (3)C236—C231—P2—Ag164.47 (15)
C132—C131—C136—C1352.3 (3)C216—C211—P2—C231100.58 (15)
P1—C131—C136—C135177.08 (14)C212—C211—P2—C23174.82 (18)
C216—C211—C212—C2131.5 (3)C216—C211—P2—C221149.09 (14)
P2—C211—C212—C213176.84 (17)C212—C211—P2—C22135.51 (18)
C211—C212—C213—C2140.7 (3)C216—C211—P2—Ag125.04 (16)
C212—C213—C214—C2151.4 (3)C212—C211—P2—Ag1159.56 (14)
C212—C213—C214—C217176.7 (2)C222—C221—P2—C23128.79 (18)
C213—C214—C215—C2162.8 (3)C226—C221—P2—C231154.99 (14)
C217—C214—C215—C216175.30 (18)C222—C221—P2—C21178.14 (17)
C212—C211—C216—C2150.1 (3)C226—C221—P2—C21198.08 (15)
P2—C211—C216—C215175.67 (14)C222—C221—P2—Ag1153.96 (14)
C214—C215—C216—C2112.1 (3)C226—C221—P2—Ag129.82 (15)
C226—C221—C222—C2231.9 (3)C326—C321—P3—C311150.71 (15)
P2—C221—C222—C223174.24 (14)C322—C321—P3—C31135.87 (17)
C221—C222—C223—C2241.2 (3)C326—C321—P3—C33197.83 (15)
C222—C223—C224—C2250.5 (3)C322—C321—P3—C33175.58 (17)
C222—C223—C224—C227178.14 (19)C326—C321—P3—Ag124.79 (17)
C223—C224—C225—C2261.5 (3)C322—C321—P3—Ag1161.80 (13)
C227—C224—C225—C226177.13 (19)C312—C311—P3—C321138.15 (16)
C224—C225—C226—C2210.8 (3)C316—C311—P3—C32151.19 (15)
C222—C221—C226—C2250.9 (3)C312—C311—P3—C33130.89 (18)
P2—C221—C226—C225175.52 (14)C316—C311—P3—C331158.45 (14)
C236—C231—C232—C2330.2 (3)C312—C311—P3—Ag191.19 (15)
P2—C231—C232—C233169.81 (15)C316—C311—P3—Ag179.46 (14)
C231—C232—C233—C2340.1 (3)C332—C331—P3—C32113.82 (17)
C232—C233—C234—C2351.0 (3)C336—C331—P3—C321175.28 (15)
C232—C233—C234—C237178.65 (19)C332—C331—P3—C311122.07 (16)
C233—C234—C235—C2361.6 (3)C336—C331—P3—C31167.03 (16)
C237—C234—C235—C236178.02 (18)C332—C331—P3—Ag1114.87 (15)
C234—C235—C236—C2311.4 (3)C336—C331—P3—Ag156.02 (16)
C232—C231—C236—C2350.4 (3)C131—P1—Ag1—P243.85 (6)
P2—C231—C236—C235170.61 (15)C111—P1—Ag1—P2161.57 (6)
C316—C311—C312—C3132.1 (3)C121—P1—Ag1—P274.94 (7)
P3—C311—C312—C313168.50 (14)C131—P1—Ag1—P3173.29 (6)
C311—C312—C313—C3140.7 (3)C111—P1—Ag1—P368.99 (7)
C312—C313—C314—C3151.5 (3)C121—P1—Ag1—P354.50 (7)
C312—C313—C314—C317176.52 (18)C131—P1—Ag1—I164.52 (6)
C313—C314—C315—C3162.3 (3)C111—P1—Ag1—I153.20 (6)
C317—C314—C315—C316175.70 (18)C121—P1—Ag1—I1176.69 (6)
C314—C315—C316—C3110.9 (3)C231—P2—Ag1—P149.17 (7)
C312—C311—C316—C3151.3 (3)C211—P2—Ag1—P170.16 (7)
P3—C311—C316—C315169.89 (14)C221—P2—Ag1—P1169.94 (6)
C326—C321—C322—C3230.7 (3)C231—P2—Ag1—P381.12 (7)
P3—C321—C322—C323172.75 (14)C211—P2—Ag1—P3159.56 (7)
C321—C322—C323—C3240.4 (3)C221—P2—Ag1—P339.65 (6)
C322—C323—C324—C3251.1 (3)C231—P2—Ag1—I1159.14 (6)
C322—C323—C324—C327179.13 (18)C211—P2—Ag1—I139.81 (7)
C323—C324—C325—C3260.7 (3)C221—P2—Ag1—I180.09 (6)
C327—C324—C325—C326179.55 (18)C321—P3—Ag1—P1143.72 (7)
C324—C325—C326—C3210.4 (3)C311—P3—Ag1—P194.69 (6)
C322—C321—C326—C3251.1 (3)C331—P3—Ag1—P125.53 (7)
P3—C321—C326—C325172.57 (14)C321—P3—Ag1—P287.50 (7)
C336—C331—C332—C3331.0 (3)C311—P3—Ag1—P234.08 (7)
P3—C331—C332—C333172.06 (15)C331—P3—Ag1—P2154.31 (6)
C331—C332—C333—C3340.5 (3)C321—P3—Ag1—I126.00 (7)
C332—C333—C334—C3350.5 (3)C311—P3—Ag1—I1147.59 (6)
C332—C333—C334—C337179.3 (2)C331—P3—Ag1—I192.19 (6)
C333—C334—C335—C3361.1 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C326—H326···I10.952.993.9335 (19)172

Experimental details

Crystal data
Chemical formulaC63H63AgIP3
Mr1147.82
Crystal system, space groupMonoclinic, C2/c
Temperature (K)100
a, b, c (Å)22.745 (3), 11.0100 (12), 44.797 (5)
β (°) 103.007 (5)
V3)10930 (2)
Z8
Radiation typeMo Kα
µ (mm1)1.06
Crystal size (mm)0.26 × 0.2 × 0.17
Data collection
DiffractometerCCD area detector
diffractometer
Absorption correctionMulti-scan
SADABS (Bruker, 2004)
Tmin, Tmax0.770, 0.840
No. of measured, independent and
observed [I > 2σ(I)] reflections
88005, 13655, 12118
Rint0.033
(sin θ/λ)max1)0.669
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.026, 0.058, 1.07
No. of reflections13655
No. of parameters623
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0182P)2 + 18.1054P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)0.43, 0.50

Computer programs: APEX2 (Bruker, 2005), SAINT-Plus (Bruker, 2004), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), DIAMOND 3.0c (Brandenburg & Putz, 2004), WinGX (Farrugia, 1999).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C326—H326···I10.952.993.9335 (19)171.9
 

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