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Acta Crystallogr Sect E Struct Rep Online. 2009 July 1; 65(Pt 7): m720.
Published online 2009 June 6. doi:  10.1107/S1600536809020388
PMCID: PMC2969192

Dihydro­nium hexa­kis[bromido/chlorido(0.75/0.25)]dicadmate(II)–triphenyl­phosphine oxide (1/6)

Abstract

In the salt, (H3O)2[Cd2Br4.5Cl1.5]·6C18H15OP, the hydro­nium cation forms short O—H(...)O hydrogen bonds to the O atoms of the triphenyl­phosphine oxide units. The centrosymmetric dinuclear anion has two halide atoms functioning in a bridging mode, which confers tetra­hedral coordination to the Cd atom. The three independent halide atoms are each a mixture of bromide and chloride; the occupancies of the Br atoms are 0.6434 (11), 0.7468 (11) and 0.8598 (11).

Related literature

There is only one example of a [(Ph3PO)3·H3O]+ system: for the [Mo6Cl14]2− salt, see: Kozhomuratova et al. (2007 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-65-0m720-scheme1.jpg

Experimental

Crystal data

  • (H3O)2[Cd2Br4.5Cl1.5]·6C18H15OP
  • M r = 2345.24
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-65-0m720-efi1.jpg
  • a = 11.1623 (2) Å
  • b = 15.0677 (3) Å
  • c = 16.0911 (3) Å
  • α = 75.499 (1)°
  • β = 81.013 (1)°
  • γ = 79.605 (1)°
  • V = 2559.57 (8) Å3
  • Z = 1
  • Mo Kα radiation
  • μ = 2.36 mm−1
  • T = 133 K
  • 0.20 × 0.10 × 0.05 mm

Data collection

  • Bruker SMART APEX diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996 [triangle]) T min = 0.650, T max = 0.891
  • 21253 measured reflections
  • 11527 independent reflections
  • 8297 reflections with I > 2σ(I)
  • R int = 0.028

Refinement

  • R[F 2 > 2σ(F 2)] = 0.036
  • wR(F 2) = 0.096
  • S = 0.98
  • 11527 reflections
  • 601 parameters
  • 7 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.93 e Å−3
  • Δρmin = −0.56 e Å−3

Data collection: APEX2 (Bruker, 2007 [triangle]); cell refinement: SAINT (Bruker, 2007 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: X-SEED (Barbour, 2001 [triangle]); software used to prepare material for publication: publCIF (Westrip, 2009 [triangle]).

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809020388/tk2468sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809020388/tk2468Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

We thank the University of Malaya (RG020/09AFR) for supporting this study.

supplementary crystallographic information

Experimental

Cadmium chloride dihydrate (0.22 g, 1 mmol) was dissolved in water (10 ml); triphenylphosphine dibromide (0.8 g, 2 mmol) was dissolved in ethanol (90 ml). The two solutions were mixed and then heated for 1 h. Slow evaporation of the filtrate gave colorless, irregularly-shaped crystals.

Refinement

Hydrogen atoms were placed at calculated positions (C–H 0.95 Å) and were treated as riding on their parent atoms, with U(H) set to 1.2Ueq(C). The acid H-atoms were located in a difference Fourier map, and were refined with a distance restraint of O–H 0.84±0.01 Å; their isotropic temperature factors were refined.

The three independent halogen atoms are each a mixture of bromide and chloride atoms. The total bromide occupancy refined to nearly 2.25; this was then set as exactly 2.25. The occupancies of the Br1, Br2 and Br3 atoms are 0.6434 (11), 0.7468 (11) and 0.8598 (11).

Figures

Fig. 1.
Thermal ellipsoid plot (Barbour, 2001) of 2[Ph3PO.(OH3)] [Cd2Br4.5Cl1.5] at the 70% probability level. Hydrogen atoms are drawn as spheres of arbitrary radius. Hydrogen bonds are drawn as dashed lines. The Br/Cl disorder is not shown.

Crystal data

(H3O)2[Cd2Br4.5Cl1.5]·6C18H15OPZ = 1
Mr = 2345.24F(000) = 1177
Triclinic, P1Dx = 1.521 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 11.1623 (2) ÅCell parameters from 5205 reflections
b = 15.0677 (3) Åθ = 2.2–27.5°
c = 16.0911 (3) ŵ = 2.36 mm1
α = 75.499 (1)°T = 133 K
β = 81.013 (1)°Irregular block, colorless
γ = 79.605 (1)°0.20 × 0.10 × 0.05 mm
V = 2559.57 (8) Å3

Data collection

Bruker SMART APEX diffractometer11527 independent reflections
Radiation source: fine-focus sealed tube8297 reflections with I > 2σ(I)
graphiteRint = 0.028
ω scansθmax = 27.5°, θmin = 1.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −13→14
Tmin = 0.650, Tmax = 0.891k = −19→19
21253 measured reflectionsl = −20→20

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.096H atoms treated by a mixture of independent and constrained refinement
S = 0.98w = 1/[σ2(Fo2) + (0.0497P)2] where P = (Fo2 + 2Fc2)/3
11527 reflections(Δ/σ)max = 0.001
601 parametersΔρmax = 0.93 e Å3
7 restraintsΔρmin = −0.56 e Å3

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/UeqOcc. (<1)
Cd10.49843 (2)0.596709 (15)0.544155 (16)0.02993 (7)
Br10.31897 (4)0.52389 (3)0.50664 (3)0.03634 (15)0.6434 (11)
Br20.47394 (4)0.56628 (3)0.70646 (3)0.04195 (15)0.7468 (11)
Br30.51554 (4)0.75339 (3)0.44674 (3)0.04616 (15)0.8598 (11)
Cl10.31897 (4)0.52389 (3)0.50664 (3)0.03634 (15)0.36
Cl20.47394 (4)0.56628 (3)0.70646 (3)0.04195 (15)0.25
Cl30.51554 (4)0.75339 (3)0.44674 (3)0.04616 (15)0.14
P10.77902 (8)0.75651 (6)0.79120 (6)0.03052 (19)
P21.04703 (7)0.76284 (5)1.06470 (5)0.02452 (17)
P31.10446 (7)1.03723 (5)0.71506 (5)0.02213 (17)
O10.8679 (2)0.78431 (15)0.83765 (15)0.0373 (6)
O21.0201 (2)0.86060 (14)1.01185 (13)0.0307 (5)
O30.98970 (18)1.02236 (14)0.77588 (13)0.0285 (5)
O40.8825 (2)0.91749 (16)0.89733 (14)0.0289 (5)
H410.876 (4)0.8710 (17)0.878 (2)0.16 (3)*
H420.927 (2)0.898 (2)0.9383 (13)0.038 (11)*
H430.920 (3)0.9536 (19)0.8569 (14)0.052 (12)*
C10.6446 (3)0.7263 (2)0.8628 (2)0.0353 (8)
C20.5511 (4)0.7959 (3)0.8795 (3)0.0566 (11)
H20.55220.85740.84580.068*
C30.4570 (4)0.7774 (4)0.9440 (3)0.0773 (15)
H30.39380.82600.95480.093*
C40.4536 (4)0.6895 (4)0.9928 (3)0.0697 (14)
H40.38790.67671.03720.084*
C50.5457 (5)0.6194 (4)0.9774 (3)0.0672 (13)
H50.54440.55831.01210.081*
C60.6409 (4)0.6371 (3)0.9114 (2)0.0511 (10)
H60.70290.58820.89990.061*
C70.8528 (3)0.6591 (2)0.7477 (2)0.0332 (8)
C80.9792 (3)0.6371 (3)0.7442 (3)0.0462 (9)
H81.02410.67190.76660.055*
C91.0404 (4)0.5647 (3)0.7082 (3)0.0560 (11)
H91.12700.54930.70690.067*
C100.9760 (5)0.5152 (3)0.6743 (2)0.0549 (11)
H101.01830.46620.64870.066*
C110.8506 (4)0.5363 (2)0.6773 (2)0.0502 (11)
H110.80680.50170.65370.060*
C120.7870 (4)0.6077 (2)0.7145 (2)0.0389 (8)
H120.70020.62140.71730.047*
C130.7263 (3)0.8497 (2)0.7052 (2)0.0313 (7)
C140.6436 (3)0.8396 (3)0.6530 (3)0.0484 (10)
H140.61340.78240.66230.058*
C150.6057 (4)0.9135 (3)0.5873 (3)0.0512 (11)
H150.54990.90620.55150.061*
C160.6466 (3)0.9969 (3)0.5729 (2)0.0412 (9)
H160.61931.04700.52770.049*
C170.7274 (3)1.0074 (3)0.6243 (2)0.0449 (9)
H170.75641.06500.61490.054*
C180.7670 (3)0.9338 (2)0.6903 (2)0.0375 (8)
H180.82300.94170.72560.045*
C191.1078 (3)0.6836 (2)0.9960 (2)0.0301 (7)
C201.0993 (3)0.5894 (2)1.0225 (2)0.0347 (8)
H201.05590.56551.07680.042*
C211.1544 (3)0.5306 (2)0.9692 (3)0.0419 (9)
H211.14820.46640.98680.050*
C221.2189 (4)0.5656 (3)0.8899 (3)0.0481 (10)
H221.25720.52490.85380.058*
C231.2275 (4)0.6582 (3)0.8635 (2)0.0480 (10)
H231.27180.68150.80930.058*
C241.1713 (3)0.7180 (2)0.9162 (2)0.0377 (8)
H241.17630.78240.89770.045*
C250.9143 (3)0.72130 (19)1.1300 (2)0.0255 (7)
C260.8974 (3)0.7105 (2)1.2190 (2)0.0304 (7)
H260.95990.72091.24770.036*
C270.7889 (3)0.6842 (2)1.2662 (2)0.0397 (8)
H270.77740.67681.32720.048*
C280.6984 (3)0.6691 (2)1.2248 (3)0.0460 (10)
H280.62470.65051.25720.055*
C290.7147 (3)0.6810 (3)1.1358 (3)0.0473 (10)
H290.65150.67091.10740.057*
C300.8210 (3)0.7070 (2)1.0880 (2)0.0371 (8)
H300.83120.71531.02690.045*
C311.1628 (3)0.7585 (2)1.13150 (19)0.0246 (6)
C321.2048 (3)0.8411 (2)1.1285 (2)0.0276 (7)
H321.17020.89741.09310.033*
C331.2963 (3)0.8413 (2)1.1767 (2)0.0390 (9)
H331.32420.89791.17450.047*
C341.3477 (3)0.7599 (3)1.2282 (2)0.0419 (9)
H341.41050.76071.26140.050*
C351.3079 (3)0.6769 (3)1.2315 (2)0.0379 (8)
H351.34370.62091.26660.046*
C361.2160 (3)0.6763 (2)1.1834 (2)0.0330 (8)
H361.18870.61941.18560.040*
C371.2285 (3)1.04350 (19)0.7715 (2)0.0245 (7)
C381.2051 (3)1.0362 (2)0.8601 (2)0.0302 (7)
H381.12591.02670.88920.036*
C391.2966 (3)1.0426 (2)0.9059 (2)0.0397 (8)
H391.28011.03740.96650.048*
C401.4112 (3)1.0564 (3)0.8646 (2)0.0420 (9)
H401.47351.06150.89640.050*
C411.4359 (3)1.0629 (3)0.7761 (2)0.0412 (9)
H41A1.51561.07140.74750.049*
C421.3450 (3)1.0571 (2)0.7303 (2)0.0340 (8)
H42A1.36181.06240.66970.041*
C431.0715 (3)1.14445 (19)0.63665 (19)0.0255 (7)
C440.9536 (3)1.1932 (2)0.6446 (2)0.0297 (7)
H440.89341.16830.68860.036*
C450.9236 (4)1.2784 (2)0.5885 (2)0.0397 (9)
H450.84271.31120.59360.048*
C461.0109 (4)1.3149 (2)0.5258 (2)0.0466 (10)
H460.99111.37400.48860.056*
C471.1273 (4)1.2663 (3)0.5167 (3)0.0542 (11)
H471.18681.29150.47230.065*
C481.1586 (3)1.1809 (2)0.5717 (2)0.0425 (9)
H481.23901.14770.56490.051*
C511.1527 (3)0.9460 (2)0.65886 (19)0.0248 (7)
C521.0762 (3)0.9363 (2)0.6022 (2)0.0364 (8)
H521.00710.98210.58910.044*
C531.0996 (3)0.8607 (2)0.5647 (2)0.0417 (9)
H531.04630.85410.52680.050*
C541.2010 (3)0.7948 (2)0.5830 (2)0.0383 (8)
H541.21720.74250.55790.046*
C551.2784 (3)0.8046 (2)0.6371 (2)0.0417 (9)
H551.34920.75990.64810.050*
C561.2547 (3)0.8790 (2)0.6762 (2)0.0336 (8)
H561.30790.88420.71480.040*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Cd10.02838 (13)0.02682 (13)0.03454 (15)−0.00040 (9)−0.00221 (10)−0.01039 (10)
Br10.0245 (2)0.0356 (2)0.0516 (3)0.00557 (16)−0.00932 (19)−0.0189 (2)
Br20.0390 (3)0.0480 (3)0.0349 (3)0.00852 (18)−0.00424 (18)−0.0130 (2)
Br30.0531 (3)0.0293 (2)0.0501 (3)−0.01052 (17)0.0123 (2)−0.00627 (18)
Cl10.0245 (2)0.0356 (2)0.0516 (3)0.00557 (16)−0.00932 (19)−0.0189 (2)
Cl20.0390 (3)0.0480 (3)0.0349 (3)0.00852 (18)−0.00424 (18)−0.0130 (2)
Cl30.0531 (3)0.0293 (2)0.0501 (3)−0.01052 (17)0.0123 (2)−0.00627 (18)
P10.0294 (5)0.0313 (4)0.0342 (5)−0.0064 (3)−0.0102 (4)−0.0082 (4)
P20.0319 (4)0.0191 (4)0.0227 (4)−0.0026 (3)−0.0059 (3)−0.0042 (3)
P30.0224 (4)0.0204 (4)0.0212 (4)−0.0015 (3)−0.0004 (3)−0.0027 (3)
O10.0388 (14)0.0324 (12)0.0453 (15)−0.0043 (10)−0.0203 (11)−0.0088 (11)
O20.0424 (14)0.0239 (11)0.0248 (12)−0.0014 (9)−0.0087 (10)−0.0032 (9)
O30.0240 (11)0.0293 (11)0.0265 (12)−0.0031 (9)0.0027 (9)−0.0002 (9)
O40.0318 (13)0.0282 (12)0.0232 (12)−0.0044 (10)−0.0039 (10)0.0009 (10)
C10.037 (2)0.048 (2)0.0265 (18)−0.0140 (16)−0.0096 (15)−0.0085 (16)
C20.045 (2)0.058 (3)0.062 (3)−0.0005 (19)0.004 (2)−0.016 (2)
C30.054 (3)0.105 (4)0.065 (3)−0.003 (3)0.011 (2)−0.024 (3)
C40.046 (3)0.119 (5)0.044 (3)−0.022 (3)−0.001 (2)−0.015 (3)
C50.077 (3)0.082 (3)0.043 (3)−0.040 (3)−0.003 (2)0.002 (2)
C60.060 (3)0.057 (3)0.036 (2)−0.016 (2)−0.0075 (19)−0.0042 (19)
C70.043 (2)0.0297 (17)0.0268 (18)−0.0061 (14)−0.0080 (15)−0.0034 (14)
C80.041 (2)0.043 (2)0.055 (3)−0.0032 (16)−0.0058 (18)−0.0131 (19)
C90.054 (3)0.050 (2)0.053 (3)0.011 (2)−0.002 (2)−0.007 (2)
C100.090 (4)0.035 (2)0.032 (2)0.002 (2)−0.002 (2)−0.0052 (17)
C110.094 (4)0.0259 (19)0.033 (2)−0.015 (2)−0.015 (2)−0.0005 (16)
C120.053 (2)0.0317 (18)0.033 (2)−0.0150 (16)−0.0104 (17)−0.0006 (15)
C130.0230 (17)0.0373 (18)0.0339 (19)0.0008 (13)−0.0084 (14)−0.0096 (15)
C140.045 (2)0.040 (2)0.065 (3)0.0020 (17)−0.030 (2)−0.013 (2)
C150.045 (2)0.062 (3)0.053 (3)0.0124 (19)−0.0332 (19)−0.022 (2)
C160.036 (2)0.047 (2)0.035 (2)0.0091 (16)−0.0091 (16)−0.0056 (17)
C170.041 (2)0.049 (2)0.039 (2)−0.0114 (17)−0.0064 (17)0.0052 (18)
C180.037 (2)0.045 (2)0.0312 (19)−0.0132 (16)−0.0108 (15)−0.0003 (16)
C190.0349 (18)0.0274 (16)0.0304 (18)−0.0001 (13)−0.0098 (14)−0.0103 (14)
C200.039 (2)0.0289 (17)0.040 (2)−0.0037 (14)−0.0050 (16)−0.0141 (15)
C210.040 (2)0.0305 (18)0.063 (3)0.0009 (15)−0.0147 (19)−0.0238 (18)
C220.047 (2)0.054 (2)0.049 (2)0.0075 (18)−0.0099 (19)−0.030 (2)
C230.056 (3)0.053 (2)0.033 (2)0.0010 (19)−0.0001 (18)−0.0168 (18)
C240.045 (2)0.0380 (19)0.0288 (19)−0.0012 (15)−0.0023 (16)−0.0105 (16)
C250.0270 (17)0.0191 (14)0.0319 (18)0.0009 (12)−0.0064 (13)−0.0099 (13)
C260.0318 (18)0.0304 (17)0.0327 (19)−0.0055 (13)−0.0053 (14)−0.0127 (14)
C270.037 (2)0.043 (2)0.039 (2)−0.0089 (16)0.0055 (16)−0.0129 (17)
C280.0265 (19)0.044 (2)0.072 (3)−0.0051 (15)0.0046 (18)−0.027 (2)
C290.031 (2)0.050 (2)0.073 (3)−0.0054 (16)−0.0127 (19)−0.031 (2)
C300.033 (2)0.0347 (18)0.049 (2)−0.0011 (14)−0.0125 (17)−0.0188 (17)
C310.0269 (16)0.0278 (16)0.0194 (15)−0.0050 (12)−0.0016 (12)−0.0062 (13)
C320.0262 (17)0.0302 (16)0.0276 (17)−0.0079 (13)0.0015 (13)−0.0092 (14)
C330.0299 (19)0.045 (2)0.048 (2)−0.0136 (15)0.0039 (16)−0.0199 (18)
C340.0245 (18)0.065 (3)0.042 (2)−0.0080 (17)−0.0060 (16)−0.0217 (19)
C350.0294 (19)0.050 (2)0.0303 (19)0.0016 (15)−0.0084 (15)−0.0034 (16)
C360.0345 (19)0.0327 (18)0.0281 (18)−0.0057 (14)−0.0003 (15)−0.0017 (14)
C370.0230 (16)0.0189 (14)0.0285 (17)−0.0008 (11)0.0008 (13)−0.0033 (12)
C380.0250 (17)0.0363 (18)0.0278 (18)−0.0014 (13)−0.0001 (14)−0.0083 (14)
C390.037 (2)0.054 (2)0.0302 (19)−0.0072 (16)−0.0008 (16)−0.0147 (17)
C400.037 (2)0.053 (2)0.041 (2)−0.0088 (17)−0.0122 (17)−0.0137 (18)
C410.033 (2)0.052 (2)0.040 (2)−0.0152 (16)0.0025 (16)−0.0121 (18)
C420.0347 (19)0.0400 (19)0.0266 (18)−0.0124 (15)0.0008 (15)−0.0039 (15)
C430.0314 (17)0.0219 (15)0.0216 (16)−0.0006 (12)−0.0044 (13)−0.0037 (12)
C440.0338 (18)0.0322 (17)0.0211 (16)0.0033 (13)−0.0037 (13)−0.0079 (14)
C450.058 (2)0.0327 (19)0.0253 (18)0.0140 (16)−0.0148 (17)−0.0092 (15)
C460.072 (3)0.0263 (18)0.039 (2)−0.0036 (18)−0.021 (2)0.0045 (16)
C470.058 (3)0.050 (2)0.041 (2)−0.018 (2)−0.0057 (19)0.0216 (19)
C480.037 (2)0.044 (2)0.036 (2)−0.0037 (16)−0.0021 (16)0.0080 (17)
C510.0278 (17)0.0242 (15)0.0209 (16)−0.0038 (12)−0.0001 (13)−0.0039 (12)
C520.0321 (19)0.0363 (19)0.041 (2)0.0053 (14)−0.0087 (16)−0.0138 (16)
C530.039 (2)0.045 (2)0.048 (2)−0.0053 (16)−0.0091 (17)−0.0222 (18)
C540.051 (2)0.0277 (17)0.038 (2)−0.0037 (15)−0.0015 (17)−0.0155 (15)
C550.046 (2)0.0314 (19)0.043 (2)0.0132 (15)−0.0089 (18)−0.0109 (16)
C560.039 (2)0.0276 (17)0.0328 (19)0.0047 (14)−0.0076 (15)−0.0088 (14)

Geometric parameters (Å, °)

Cd1—Br32.5066 (4)C22—C231.370 (5)
Cd1—Br22.5156 (5)C22—H220.9500
Cd1—Cl1i2.6479 (4)C23—C241.392 (5)
Cd1—Br1i2.6479 (4)C23—H230.9500
Cd1—Br12.6616 (5)C24—H240.9500
Br1—Cd1i2.6479 (4)C25—C261.387 (4)
P1—O11.502 (2)C25—C301.400 (4)
P1—C131.793 (3)C26—C271.391 (4)
P1—C71.794 (3)C26—H260.9500
P1—C11.797 (3)C27—C281.373 (5)
P2—O21.509 (2)C27—H270.9500
P2—C311.788 (3)C28—C291.386 (6)
P2—C251.791 (3)C28—H280.9500
P2—C191.801 (3)C29—C301.373 (5)
P3—O31.500 (2)C29—H290.9500
P3—C511.789 (3)C30—H300.9500
P3—C371.798 (3)C31—C321.396 (4)
P3—C431.802 (3)C31—C361.399 (4)
O4—H410.851 (10)C32—C331.376 (5)
O4—H420.846 (10)C32—H320.9500
O4—H430.848 (10)C33—C341.381 (5)
C1—C61.379 (5)C33—H330.9500
C1—C21.386 (5)C34—C351.386 (5)
C2—C31.371 (6)C34—H340.9500
C2—H20.9500C35—C361.380 (5)
C3—C41.364 (7)C35—H350.9500
C3—H30.9500C36—H360.9500
C4—C51.377 (7)C37—C421.389 (4)
C4—H40.9500C37—C381.390 (4)
C5—C61.391 (6)C38—C391.379 (5)
C5—H50.9500C38—H380.9500
C6—H60.9500C39—C401.373 (5)
C7—C81.385 (5)C39—H390.9500
C7—C121.400 (5)C40—C411.389 (5)
C8—C91.384 (5)C40—H400.9500
C8—H80.9500C41—C421.371 (5)
C9—C101.376 (6)C41—H41A0.9500
C9—H90.9500C42—H42A0.9500
C10—C111.374 (6)C43—C481.389 (4)
C10—H100.9500C43—C441.391 (4)
C11—C121.390 (5)C44—C451.390 (4)
C11—H110.9500C44—H440.9500
C12—H120.9500C45—C461.371 (5)
C13—C181.374 (5)C45—H450.9500
C13—C141.393 (5)C46—C471.377 (5)
C14—C151.384 (5)C46—H460.9500
C14—H140.9500C47—C481.387 (5)
C15—C161.367 (5)C47—H470.9500
C15—H150.9500C48—H480.9500
C16—C171.368 (5)C51—C561.392 (4)
C16—H160.9500C51—C521.392 (4)
C17—C181.390 (5)C52—C531.384 (4)
C17—H170.9500C52—H520.9500
C18—H180.9500C53—C541.380 (5)
C19—C241.391 (5)C53—H530.9500
C19—C201.392 (4)C54—C551.368 (5)
C20—C211.384 (4)C54—H540.9500
C20—H200.9500C55—C561.382 (4)
C21—C221.392 (5)C55—H550.9500
C21—H210.9500C56—H560.9500
Br3—Cd1—Br2123.627 (16)C21—C22—H22119.8
Br3—Cd1—Cl1i108.515 (16)C22—C23—C24119.9 (4)
Br2—Cd1—Cl1i108.971 (16)C22—C23—H23120.1
Br3—Cd1—Br1i108.515 (16)C24—C23—H23120.1
Br2—Cd1—Br1i108.971 (16)C19—C24—C23120.0 (3)
Cl1i—Cd1—Br1i0.00 (2)C19—C24—H24120.0
Br3—Cd1—Br1110.821 (17)C23—C24—H24120.0
Br2—Cd1—Br1105.115 (17)C26—C25—C30119.7 (3)
Cl1i—Cd1—Br196.353 (14)C26—C25—P2122.1 (2)
Br1i—Cd1—Br196.353 (14)C30—C25—P2118.0 (3)
Cd1i—Br1—Cd183.647 (14)C25—C26—C27120.0 (3)
O1—P1—C13111.51 (14)C25—C26—H26120.0
O1—P1—C7109.07 (15)C27—C26—H26120.0
C13—P1—C7109.32 (15)C28—C27—C26120.1 (3)
O1—P1—C1111.14 (15)C28—C27—H27120.0
C13—P1—C1106.26 (16)C26—C27—H27120.0
C7—P1—C1109.49 (16)C27—C28—C29119.9 (3)
O2—P2—C31108.70 (13)C27—C28—H28120.0
O2—P2—C25113.11 (13)C29—C28—H28120.0
C31—P2—C25109.99 (14)C30—C29—C28120.9 (3)
O2—P2—C19110.91 (14)C30—C29—H29119.6
C31—P2—C19106.83 (14)C28—C29—H29119.6
C25—P2—C19107.12 (14)C29—C30—C25119.4 (3)
O3—P3—C51111.76 (13)C29—C30—H30120.3
O3—P3—C37111.35 (13)C25—C30—H30120.3
C51—P3—C37107.96 (14)C32—C31—C36118.9 (3)
O3—P3—C43107.67 (13)C32—C31—P2117.8 (2)
C51—P3—C43108.35 (13)C36—C31—P2123.3 (2)
C37—P3—C43109.71 (14)C33—C32—C31120.2 (3)
H41—O4—H42107.4 (16)C33—C32—H32119.9
H41—O4—H43107.4 (16)C31—C32—H32119.9
H42—O4—H43108.3 (15)C32—C33—C34120.4 (3)
C6—C1—C2118.9 (4)C32—C33—H33119.8
C6—C1—P1121.0 (3)C34—C33—H33119.8
C2—C1—P1119.4 (3)C33—C34—C35120.2 (3)
C3—C2—C1121.0 (4)C33—C34—H34119.9
C3—C2—H2119.5C35—C34—H34119.9
C1—C2—H2119.5C36—C35—C34119.6 (3)
C4—C3—C2120.3 (5)C36—C35—H35120.2
C4—C3—H3119.9C34—C35—H35120.2
C2—C3—H3119.9C35—C36—C31120.6 (3)
C3—C4—C5119.7 (4)C35—C36—H36119.7
C3—C4—H4120.2C31—C36—H36119.7
C5—C4—H4120.2C42—C37—C38118.9 (3)
C4—C5—C6120.5 (5)C42—C37—P3123.1 (2)
C4—C5—H5119.7C38—C37—P3117.9 (2)
C6—C5—H5119.7C39—C38—C37120.1 (3)
C1—C6—C5119.6 (4)C39—C38—H38120.0
C1—C6—H6120.2C37—C38—H38120.0
C5—C6—H6120.2C40—C39—C38120.5 (3)
C8—C7—C12119.6 (3)C40—C39—H39119.7
C8—C7—P1118.4 (3)C38—C39—H39119.7
C12—C7—P1121.9 (3)C39—C40—C41119.9 (3)
C9—C8—C7120.4 (4)C39—C40—H40120.1
C9—C8—H8119.8C41—C40—H40120.1
C7—C8—H8119.8C42—C41—C40119.8 (3)
C10—C9—C8120.0 (4)C42—C41—H41A120.1
C10—C9—H9120.0C40—C41—H41A120.1
C8—C9—H9120.0C41—C42—C37120.8 (3)
C11—C10—C9120.2 (4)C41—C42—H42A119.6
C11—C10—H10119.9C37—C42—H42A119.6
C9—C10—H10119.9C48—C43—C44119.5 (3)
C10—C11—C12120.7 (4)C48—C43—P3123.1 (2)
C10—C11—H11119.6C44—C43—P3117.3 (2)
C12—C11—H11119.6C45—C44—C43120.2 (3)
C11—C12—C7119.1 (4)C45—C44—H44119.9
C11—C12—H12120.5C43—C44—H44119.9
C7—C12—H12120.5C46—C45—C44119.9 (3)
C18—C13—C14118.6 (3)C46—C45—H45120.1
C18—C13—P1119.8 (3)C44—C45—H45120.1
C14—C13—P1121.6 (3)C45—C46—C47120.2 (3)
C15—C14—C13119.5 (4)C45—C46—H46119.9
C15—C14—H14120.2C47—C46—H46119.9
C13—C14—H14120.2C46—C47—C48120.7 (3)
C16—C15—C14121.5 (4)C46—C47—H47119.7
C16—C15—H15119.2C48—C47—H47119.7
C14—C15—H15119.2C47—C48—C43119.5 (3)
C15—C16—C17119.2 (3)C47—C48—H48120.3
C15—C16—H16120.4C43—C48—H48120.3
C17—C16—H16120.4C56—C51—C52118.7 (3)
C16—C17—C18120.0 (4)C56—C51—P3123.3 (2)
C16—C17—H17120.0C52—C51—P3117.6 (2)
C18—C17—H17120.0C53—C52—C51120.9 (3)
C13—C18—C17121.1 (3)C53—C52—H52119.6
C13—C18—H18119.4C51—C52—H52119.6
C17—C18—H18119.4C54—C53—C52119.5 (3)
C24—C19—C20119.8 (3)C54—C53—H53120.3
C24—C19—P2117.9 (2)C52—C53—H53120.3
C20—C19—P2122.1 (3)C55—C54—C53120.2 (3)
C21—C20—C19119.7 (3)C55—C54—H54119.9
C21—C20—H20120.2C53—C54—H54119.9
C19—C20—H20120.2C54—C55—C56120.8 (3)
C20—C21—C22120.1 (3)C54—C55—H55119.6
C20—C21—H21120.0C56—C55—H55119.6
C22—C21—H21120.0C55—C56—C51120.0 (3)
C23—C22—C21120.5 (3)C55—C56—H56120.0
C23—C22—H22119.8C51—C56—H56120.0
Br3—Cd1—Br1—Cd1i112.593 (17)C19—P2—C25—C30−55.2 (3)
Br2—Cd1—Br1—Cd1i−111.648 (16)C30—C25—C26—C270.9 (4)
Cl1i—Cd1—Br1—Cd1i0.0P2—C25—C26—C27175.5 (2)
Br1i—Cd1—Br1—Cd1i0.0C25—C26—C27—C280.0 (5)
O1—P1—C1—C6−87.6 (3)C26—C27—C28—C29−0.7 (5)
C13—P1—C1—C6150.9 (3)C27—C28—C29—C300.6 (5)
C7—P1—C1—C632.9 (3)C28—C29—C30—C250.3 (5)
O1—P1—C1—C282.3 (3)C26—C25—C30—C29−1.0 (4)
C13—P1—C1—C2−39.2 (3)P2—C25—C30—C29−175.8 (3)
C7—P1—C1—C2−157.1 (3)O2—P2—C31—C322.7 (3)
C6—C1—C2—C31.0 (6)C25—P2—C31—C32−121.6 (2)
P1—C1—C2—C3−169.2 (4)C19—P2—C31—C32122.4 (2)
C1—C2—C3—C4−0.4 (8)O2—P2—C31—C36−174.6 (2)
C2—C3—C4—C50.5 (8)C25—P2—C31—C3661.0 (3)
C3—C4—C5—C6−1.3 (7)C19—P2—C31—C36−54.9 (3)
C2—C1—C6—C5−1.7 (6)C36—C31—C32—C33−0.7 (4)
P1—C1—C6—C5168.3 (3)P2—C31—C32—C33−178.1 (2)
C4—C5—C6—C11.9 (7)C31—C32—C33—C340.3 (5)
O1—P1—C7—C8−14.2 (3)C32—C33—C34—C350.3 (5)
C13—P1—C7—C8108.0 (3)C33—C34—C35—C36−0.4 (5)
C1—P1—C7—C8−136.0 (3)C34—C35—C36—C310.0 (5)
O1—P1—C7—C12168.5 (3)C32—C31—C36—C350.6 (4)
C13—P1—C7—C12−69.4 (3)P2—C31—C36—C35177.9 (2)
C1—P1—C7—C1246.6 (3)O3—P3—C37—C42−179.9 (2)
C12—C7—C8—C9−0.1 (6)C51—P3—C37—C4257.1 (3)
P1—C7—C8—C9−177.6 (3)C43—P3—C37—C42−60.8 (3)
C7—C8—C9—C101.2 (6)O3—P3—C37—C38−1.2 (3)
C8—C9—C10—C11−1.1 (6)C51—P3—C37—C38−124.2 (2)
C9—C10—C11—C120.0 (6)C43—P3—C37—C38117.9 (2)
C10—C11—C12—C71.0 (5)C42—C37—C38—C390.2 (4)
C8—C7—C12—C11−0.9 (5)P3—C37—C38—C39−178.6 (2)
P1—C7—C12—C11176.4 (3)C37—C38—C39—C400.1 (5)
O1—P1—C13—C18−0.9 (3)C38—C39—C40—C41−0.8 (5)
C7—P1—C13—C18−121.6 (3)C39—C40—C41—C421.1 (6)
C1—P1—C13—C18120.3 (3)C40—C41—C42—C37−0.8 (5)
O1—P1—C13—C14179.7 (3)C38—C37—C42—C410.2 (5)
C7—P1—C13—C1459.0 (3)P3—C37—C42—C41178.9 (3)
C1—P1—C13—C14−59.0 (3)O3—P3—C43—C48178.2 (3)
C18—C13—C14—C150.7 (5)C51—P3—C43—C48−60.8 (3)
P1—C13—C14—C15−180.0 (3)C37—P3—C43—C4856.9 (3)
C13—C14—C15—C16−0.6 (6)O3—P3—C43—C440.4 (3)
C14—C15—C16—C170.3 (6)C51—P3—C43—C44121.4 (2)
C15—C16—C17—C180.0 (5)C37—P3—C43—C44−121.0 (2)
C14—C13—C18—C17−0.4 (5)C48—C43—C44—C45−0.6 (5)
P1—C13—C18—C17−179.8 (3)P3—C43—C44—C45177.3 (2)
C16—C17—C18—C130.0 (5)C43—C44—C45—C46−0.9 (5)
O2—P2—C19—C2427.5 (3)C44—C45—C46—C471.9 (6)
C31—P2—C19—C24−90.8 (3)C45—C46—C47—C48−1.4 (6)
C25—P2—C19—C24151.4 (3)C46—C47—C48—C43−0.2 (6)
O2—P2—C19—C20−156.4 (3)C44—C43—C48—C471.2 (5)
C31—P2—C19—C2085.3 (3)P3—C43—C48—C47−176.6 (3)
C25—P2—C19—C20−32.5 (3)O3—P3—C51—C56−107.6 (3)
C24—C19—C20—C210.1 (5)C37—P3—C51—C5615.1 (3)
P2—C19—C20—C21−175.9 (3)C43—P3—C51—C56133.9 (3)
C19—C20—C21—C220.6 (5)O3—P3—C51—C5264.9 (3)
C20—C21—C22—C23−0.6 (6)C37—P3—C51—C52−172.3 (2)
C21—C22—C23—C24−0.1 (6)C43—P3—C51—C52−53.6 (3)
C20—C19—C24—C23−0.8 (5)C56—C51—C52—C531.0 (5)
P2—C19—C24—C23175.4 (3)P3—C51—C52—C53−171.9 (3)
C22—C23—C24—C190.8 (6)C51—C52—C53—C54−0.8 (5)
O2—P2—C25—C26−107.3 (3)C52—C53—C54—C55−0.5 (6)
C31—P2—C25—C2614.4 (3)C53—C54—C55—C561.7 (6)
C19—P2—C25—C26130.2 (3)C54—C55—C56—C51−1.6 (5)
O2—P2—C25—C3067.3 (3)C52—C51—C56—C550.2 (5)
C31—P2—C25—C30−170.9 (2)P3—C51—C56—C55172.6 (3)

Symmetry codes: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O4—H41···O10.85 (1)1.62 (1)2.472 (3)177 (4)
O4—H42···O20.85 (1)1.63 (1)2.471 (3)176 (3)
O4—H43···O30.85 (1)1.63 (1)2.481 (3)177 (3)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: TK2468).

References

  • Barbour, L. J. (2001). J. Supramol. Chem.1, 189–191.
  • Bruker (2007). APEX2 and SAINT Bruker AXS Inc., Madison, Wisconsin, USA.
  • Kozhomuratova, Z. S., Mironov, Yu. V., Shestopalov, M. A., Drebushchak, I. V., Moroz, N. K., Naumov, D. Y., Smolentsev, A. I., Uskov, E. M. & Fedorov, V. E. (2007). Eur. J. Inorg. Chem. pp. 2055–2060.
  • Sheldrick, G. M. (1996). SADABS University of Göttingen, Germany.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Westrip, S. P. (2009). publCIF In preparation.

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