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The crystal structure of the title compound, [Ag4Br4(C25H22P2)2], was recently reported by Di Nicola, Effendy, Pettinari, Skelton, Somers & White [(2006). Inorg. Chim. Acta, 359, 53–63] in the non-centrosymmetric space group Pca21. We report here a polymorphic structure in a centrosymmetric space group. The molecular structure is essentially the same in both polymorphs.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807005909/xu2135sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807005909/xu2135Isup2.hkl
Contains datablock I

CCDC reference: 643137

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.021 Å
  • Disorder in main residue
  • R factor = 0.066
  • wR factor = 0.196
  • Data-to-parameter ratio = 17.8

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C13B PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C32A PLAT301_ALERT_3_B Main Residue Disorder ......................... 28.00 Perc. PLAT342_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ... 21
Alert level C PLAT026_ALERT_3_C Ratio Observed / Unique Reflections too Low .... 48 Perc. PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.86 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.12 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C19 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C25 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C31B PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C33A PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C11B PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C13A PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C29A PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C32B PLAT245_ALERT_2_C U(iso) H13A Smaller than U(eq) C13B by ... 0.04 AngSq
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 12 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: WinAFC Diffractometer Control Software (Rigaku, 2002); cell refinement: WinAFC Diffractometer Control Software; data reduction: CrystalStructure (Rigaku/MSC, 2004); 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[µ2-bis(diphenylphosphino)methane]di-µ3-bromo-di-µ2-bromo- tetrasilver(I) top
Crystal data top
[Ag4Br4(C25H22P2)2]F(000) = 2928
Mr = 1519.85Dx = 1.965 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 30 reflections
a = 17.272 (3) Åθ = 6.0–15.0°
b = 16.718 (2) ŵ = 4.77 mm1
c = 17.789 (4) ÅT = 293 K
V = 5136.8 (15) Å3Block, colorless
Z = 40.24 × 0.20 × 0.20 mm
Data collection top
Rigaku AFC-7R
diffractometer
2306 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.033
Graphite monochromatorθmax = 25.5°, θmin = 2.0°
ω/2θ scansh = 620
Absorption correction: ψ scan
(WinAFC Diffractometer Control Software; Rigaku, 2002)
k = 620
Tmin = 0.285, Tmax = 0.385l = 210
5018 measured reflections3 standard reflections every 200 reflections
4778 independent reflections intensity decay: none
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)] = 0.066Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.196H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.08P)2]
where P = (Fo2 + 2Fc2)/3
4778 reflections(Δ/σ)max < 0.001
268 parametersΔρmax = 1.02 e Å3
0 restraintsΔρmin = 1.10 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*/UeqOcc. (<1)
Ag10.51825 (6)0.47959 (7)0.60061 (6)0.0693 (4)
Ag20.34843 (7)0.48795 (7)0.52208 (6)0.0810 (4)
Br10.37730 (8)0.42300 (10)0.64805 (8)0.0768 (5)
Br20.46008 (9)0.61334 (7)0.52755 (8)0.0703 (5)
P10.37603 (16)0.52200 (18)0.31068 (17)0.0464 (8)
P20.25012 (19)0.51402 (19)0.43110 (17)0.0495 (8)
C10.2867 (6)0.5648 (7)0.3478 (6)0.048 (3)
H1A0.29570.62050.36000.057*
H1B0.24730.56290.30900.057*
C11A0.397 (3)0.578 (3)0.230 (3)0.050 (18)*0.50
C11B0.399 (3)0.592 (3)0.232 (2)0.040 (15)*0.50
C12A0.4633 (17)0.5624 (18)0.1876 (16)0.060 (8)*0.50
H12A0.49410.51920.20130.073*0.50
C12B0.4740 (19)0.591 (2)0.2079 (18)0.076 (10)*0.50
H12B0.51220.56270.23320.091*0.50
C13A0.4851 (17)0.6059 (17)0.1284 (16)0.053 (8)*0.50
H13A0.51950.58490.09340.063*0.50
C13B0.491 (3)0.638 (3)0.141 (2)0.104 (15)*0.50
H13B0.54170.64390.12420.125*0.50
C14A0.4576 (19)0.6795 (19)0.1199 (18)0.065 (9)*0.50
H14A0.48360.71570.08940.078*0.50
C14B0.4288 (17)0.6745 (17)0.0996 (17)0.062 (9)*0.50
H14B0.43820.70060.05440.074*0.50
C15A0.3930 (18)0.7016 (18)0.1548 (16)0.076 (8)*0.50
H15A0.36620.74670.13880.091*0.50
C15B0.3570 (18)0.6706 (17)0.1276 (16)0.074 (8)*0.50
H15B0.31830.69940.10340.089*0.50
C16A0.3634 (17)0.6532 (17)0.2204 (16)0.069 (8)*0.50
H16A0.32510.67250.25250.083*0.50
C16B0.3376 (16)0.6282 (16)0.1874 (15)0.063 (7)*0.50
H16B0.28600.62180.20090.075*0.50
C170.3477 (6)0.4261 (7)0.2705 (7)0.050 (3)
C180.3858 (9)0.3580 (8)0.2919 (8)0.076 (4)
H180.42530.36080.32740.091*
C190.3658 (11)0.2860 (9)0.2611 (11)0.106 (6)
H190.38990.23980.27830.127*
C200.3124 (10)0.2802 (9)0.2068 (10)0.095 (5)
H200.30080.23090.18530.113*
C210.2739 (8)0.3502 (11)0.1828 (9)0.087 (5)
H210.23590.34730.14590.104*
C220.2929 (8)0.4218 (9)0.2140 (8)0.072 (4)
H220.26880.46830.19730.086*
C230.1801 (7)0.5828 (8)0.4704 (6)0.055 (3)
C240.1231 (7)0.5517 (9)0.5198 (8)0.074 (4)
H240.11910.49710.52920.089*
C250.0726 (10)0.6073 (13)0.5541 (8)0.105 (6)
H250.03440.58770.58610.125*
C260.0765 (10)0.6872 (11)0.5433 (9)0.092 (5)
H260.04340.72170.56890.110*
C270.1302 (8)0.7163 (9)0.4938 (9)0.083 (5)
H270.13150.77080.48370.099*
C280.1829 (8)0.6657 (8)0.4582 (8)0.078 (4)
H280.22010.68710.42620.093*
C29A0.1972 (16)0.4303 (17)0.4053 (16)0.034 (9)*0.50
C29B0.1855 (19)0.4336 (19)0.3858 (19)0.044 (10)*0.50
C30A0.1489 (19)0.427 (2)0.3341 (19)0.055 (10)*0.50
H30A0.14910.46910.29970.066*0.50
C30B0.138 (2)0.452 (2)0.3358 (19)0.065 (11)*0.50
H30B0.13140.50550.32130.078*0.50
C31A0.1023 (17)0.356 (2)0.3221 (17)0.057 (8)*0.50
H31A0.06630.35120.28350.068*0.50
C31B0.0934 (19)0.3880 (19)0.3009 (19)0.074 (10)*0.50
H31B0.06480.39580.25720.089*0.50
C32A0.116 (3)0.296 (3)0.373 (3)0.103 (17)*0.50
H32A0.09270.24760.36180.124*0.50
C32B0.0970 (16)0.307 (2)0.3409 (16)0.053 (7)*0.50
H32B0.06830.26430.32190.064*0.50
C33A0.160 (2)0.297 (2)0.438 (2)0.098 (13)*0.50
H33A0.16230.25290.46970.117*0.50
C33B0.140 (2)0.295 (2)0.402 (2)0.063 (9)*0.50
H33B0.13690.24970.43200.075*0.50
C34A0.1972 (19)0.3625 (19)0.4526 (19)0.069 (10)*0.50
H34A0.22570.36490.49700.083*0.50
C34B0.1930 (16)0.3608 (17)0.4187 (17)0.054 (8)*0.50
H34B0.23300.35250.45280.065*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ag10.0447 (5)0.0876 (8)0.0757 (7)0.0026 (5)0.0106 (5)0.0013 (6)
Ag20.0769 (8)0.1016 (9)0.0646 (7)0.0093 (7)0.0200 (6)0.0100 (7)
Br10.0555 (8)0.1067 (12)0.0682 (9)0.0185 (8)0.0033 (7)0.0307 (9)
Br20.1002 (11)0.0405 (7)0.0703 (9)0.0002 (7)0.0171 (8)0.0045 (7)
P10.0383 (16)0.0485 (17)0.0524 (18)0.0008 (15)0.0033 (14)0.0013 (16)
P20.0427 (16)0.059 (2)0.0474 (17)0.0001 (16)0.0026 (15)0.0035 (16)
C10.043 (6)0.049 (7)0.052 (7)0.006 (6)0.000 (6)0.005 (6)
C170.030 (6)0.055 (8)0.066 (8)0.004 (6)0.008 (6)0.002 (6)
C180.093 (11)0.054 (9)0.079 (10)0.011 (8)0.008 (9)0.001 (8)
C190.138 (17)0.048 (10)0.132 (16)0.009 (10)0.006 (14)0.015 (10)
C200.107 (14)0.057 (10)0.119 (15)0.012 (10)0.013 (12)0.037 (10)
C210.062 (10)0.109 (14)0.089 (12)0.018 (10)0.015 (8)0.031 (10)
C220.071 (9)0.074 (10)0.069 (9)0.007 (8)0.003 (8)0.024 (8)
C230.050 (7)0.074 (9)0.040 (7)0.000 (7)0.001 (6)0.007 (7)
C240.056 (8)0.093 (11)0.073 (9)0.002 (8)0.027 (8)0.011 (8)
C250.092 (13)0.151 (17)0.071 (11)0.004 (13)0.046 (10)0.006 (12)
C260.088 (13)0.108 (14)0.079 (11)0.003 (11)0.000 (10)0.020 (10)
C270.045 (8)0.082 (10)0.121 (13)0.012 (7)0.012 (9)0.003 (10)
C280.063 (9)0.069 (10)0.100 (12)0.005 (8)0.029 (9)0.015 (9)
Geometric parameters (Å, º) top
Ag1—P1i2.414 (3)C18—C191.368 (19)
Ag1—Br12.7449 (17)C18—H180.9300
Ag1—Br22.7746 (17)C19—C201.34 (2)
Ag1—Br2i2.7840 (18)C19—H190.9300
Ag1—Ag2i3.2188 (16)C20—C211.41 (2)
Ag1—Ag23.2518 (16)C20—H200.9300
Ag2—P22.386 (3)C21—C221.360 (18)
Ag2—Br12.5395 (18)C21—H210.9300
Ag2—Br22.8500 (19)C22—H220.9300
P1—C11A1.74 (5)C23—C281.404 (17)
P1—C171.823 (12)C23—C241.418 (17)
P1—C11.825 (10)C24—C251.41 (2)
P1—C11B1.87 (4)C24—H240.9300
P2—C29A1.73 (3)C25—C261.35 (2)
P2—C231.810 (12)C25—H250.9300
P2—C11.820 (11)C26—C271.368 (19)
P2—C29B1.92 (3)C26—H260.9300
C1—H1A0.9700C27—C281.394 (18)
C1—H1B0.9700C27—H270.9300
C11A—C12A1.40 (5)C28—H280.9300
C11A—C16A1.40 (5)C29A—C34A1.41 (4)
C11B—C12B1.36 (5)C29A—C30A1.52 (4)
C11B—C16B1.45 (5)C29B—C30B1.25 (5)
C12A—C13A1.33 (4)C29B—C34B1.36 (4)
C12A—H12A0.9300C30A—C31A1.46 (4)
C12B—C13B1.46 (5)C30A—H30A0.9300
C12B—H12B0.9300C30B—C31B1.46 (5)
C13A—C14A1.33 (5)C30B—H30B0.9300
C13A—H13A0.9300C31A—C32A1.36 (5)
C13B—C14B1.43 (5)C31A—H31A0.9300
C13B—H13B0.9300C31B—C32B1.54 (4)
C14A—C15A1.33 (4)C31B—H31B0.9300
C14A—H14A0.9300C32A—C33A1.38 (6)
C14B—C15B1.34 (4)C32A—H32A0.9300
C14B—H14B0.9300C32B—C33B1.34 (5)
C15A—C16A1.51 (4)C32B—H32B0.9300
C15A—H15A0.9300C33A—C34A1.30 (5)
C15B—C16B1.32 (3)C33A—H33A0.9300
C15B—H15B0.9300C33B—C34B1.45 (4)
C16A—H16A0.9300C33B—H33B0.9300
C16B—H16B0.9300C34A—H34A0.9300
C17—C181.368 (16)C34B—H34B0.9300
C17—C221.383 (16)
P1i—Ag1—Br1117.79 (9)C16B—C15B—H15B117.9
P1i—Ag1—Br2126.09 (9)C14B—C15B—H15B117.9
Br1—Ag1—Br295.77 (6)C11A—C16A—C15A116 (3)
P1i—Ag1—Br2i115.31 (9)C11A—C16A—H16A121.9
Br1—Ag1—Br2i100.29 (6)C15A—C16A—H16A121.9
Br2—Ag1—Br2i96.59 (5)C15B—C16B—C11B118 (3)
P1i—Ag1—Ag2i84.49 (8)C15B—C16B—H16B120.8
Br1—Ag1—Ag2i154.30 (5)C11B—C16B—H16B120.8
Br2—Ag1—Ag2i78.79 (5)C18—C17—C22119.3 (12)
Br2i—Ag1—Ag2i56.13 (4)C18—C17—P1119.6 (10)
P1i—Ag1—Ag2164.53 (9)C22—C17—P1120.9 (10)
Br1—Ag1—Ag249.22 (4)C19—C18—C17119.9 (15)
Br2—Ag1—Ag255.77 (4)C19—C18—H18120.1
Br2i—Ag1—Ag278.08 (5)C17—C18—H18120.1
Ag2i—Ag1—Ag2110.29 (4)C20—C19—C18121.8 (16)
P2—Ag2—Br1144.73 (10)C20—C19—H19119.1
P2—Ag2—Br2111.73 (9)C18—C19—H19119.1
Br1—Ag2—Br298.72 (6)C19—C20—C21118.8 (14)
P2—Ag2—Ag1i91.05 (9)C19—C20—H20120.6
Br1—Ag2—Ag1i122.00 (6)C21—C20—H20120.6
Br2—Ag2—Ag1i54.20 (4)C22—C21—C20119.5 (14)
P2—Ag2—Ag1160.25 (9)C22—C21—H21120.2
Br1—Ag2—Ag154.93 (4)C20—C21—H21120.2
Br2—Ag2—Ag153.60 (4)C21—C22—C17120.5 (14)
Ag1i—Ag2—Ag169.71 (4)C21—C22—H22119.8
Ag2—Br1—Ag175.85 (5)C17—C22—H22119.8
Ag1—Br2—Ag1i83.41 (5)C28—C23—C24118.8 (12)
Ag1—Br2—Ag270.63 (4)C28—C23—P2123.0 (10)
Ag1i—Br2—Ag269.67 (4)C24—C23—P2118.0 (10)
C11A—P1—C17101.7 (15)C25—C24—C23117.0 (14)
C11A—P1—C1105.3 (16)C25—C24—H24121.5
C17—P1—C1105.0 (5)C23—C24—H24121.5
C17—P1—C11B108.2 (14)C26—C25—C24123.9 (16)
C1—P1—C11B101.9 (15)C26—C25—H25118.0
C11A—P1—Ag1i112.7 (16)C24—C25—H25118.0
C17—P1—Ag1i116.7 (4)C25—C26—C27118.4 (16)
C1—P1—Ag1i114.0 (4)C25—C26—H26120.8
C11B—P1—Ag1i109.8 (14)C27—C26—H26120.8
C29A—P2—C23105.2 (10)C26—C27—C28121.3 (15)
C29A—P2—C1110.1 (10)C26—C27—H27119.3
C23—P2—C1104.5 (5)C28—C27—H27119.3
C23—P2—C29B102.6 (10)C27—C28—C23120.4 (13)
C1—P2—C29B100.7 (10)C27—C28—H28119.8
C29A—P2—Ag2114.0 (10)C23—C28—H28119.8
C23—P2—Ag2109.3 (4)C34A—C29A—C30A118 (3)
C1—P2—Ag2113.0 (4)C34A—C29A—P2119 (2)
C29B—P2—Ag2124.7 (10)C30A—C29A—P2123 (2)
P2—C1—P1113.9 (6)C30B—C29B—C34B127 (4)
P2—C1—H1A108.8C30B—C29B—P2120 (3)
P1—C1—H1A108.8C34B—C29B—P2113 (3)
P2—C1—H1B108.8C31A—C30A—C29A117 (3)
P1—C1—H1B108.8C31A—C30A—H30A121.5
H1A—C1—H1B107.7C29A—C30A—H30A121.5
C12A—C11A—C16A116 (4)C29B—C30B—C31B118 (4)
C12A—C11A—P1121 (3)C29B—C30B—H30B121.2
C16A—C11A—P1120 (3)C31B—C30B—H30B121.2
C12B—C11B—C16B122 (4)C32A—C31A—C30A114 (3)
C12B—C11B—P1115 (3)C32A—C31A—H31A123.0
C16B—C11B—P1121 (3)C30A—C31A—H31A123.0
C13A—C12A—C11A124 (3)C30B—C31B—C32B116 (3)
C13A—C12A—H12A117.9C30B—C31B—H31B122.2
C11A—C12A—H12A117.9C32B—C31B—H31B122.2
C11B—C12B—C13B116 (4)C31A—C32A—C33A130 (4)
C11B—C12B—H12B122.0C31A—C32A—H32A115.0
C13B—C12B—H12B122.0C33A—C32A—H32A115.0
C14A—C13A—C12A120 (3)C33B—C32B—C31B122 (3)
C14A—C13A—H13A120.2C33B—C32B—H32B118.0
C12A—C13A—H13A120.2C31B—C32B—H32B119.1
C14B—C13B—C12B120 (4)C34A—C33A—C32A117 (4)
C14B—C13B—H13B120.1C34A—C33A—H33A121.7
C12B—C13B—H13B120.1C32A—C33A—H33A121.7
C13A—C14A—C15A120 (3)C32B—C33B—C34B114 (3)
C13A—C14A—H14A119.8C32B—C33B—H33B123.0
C15A—C14A—H14A119.8C34B—C33B—H33B123.0
C15B—C14B—C13B119 (3)C33A—C34A—C29A124 (4)
C15B—C14B—H14B120.5C33A—C34A—H34A118.1
C13B—C14B—H14B120.5C29A—C34A—H34A118.1
C14A—C15A—C16A120 (3)C29B—C34B—C33B122 (3)
C14A—C15A—H15A120.1C29B—C34B—H34B119.0
C16A—C15A—H15A120.1C33B—C34B—H34B119.0
C16B—C15B—C14B124 (3)
Symmetry code: (i) x+1, y+1, z+1.
 

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