Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
The title cocrystal, [Cu2(C7H2I3O2)4(H2O)2][Cu2(C7H2I3O2)4(CH4O)2]·2CH4O, contains two dinuclear complexes. In both centrosymmetric mol­ecules, four triiodo­benzoates bridge a pair of Cu atoms. The Cu atoms show square-pyramidal coordination; for one, the apical position is occupied by a water mol­ecule, and for the other, this site is occupied by a methanol mol­ecule.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807046430/bt2517sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807046430/bt2517Isup2.hkl
Contains datablock I

CCDC reference: 663658

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.008 Å
  • R factor = 0.051
  • wR factor = 0.146
  • Data-to-parameter ratio = 25.0

checkCIF/PLATON results

No syntax errors found



Alert level A ABSTM02_ALERT_3_A The ratio of expected to reported Tmax/Tmin(RR') is < 0.50 Tmin and Tmax reported: 0.084 1.000 Tmin(prime) and Tmax expected: 0.121 0.307 RR(prime) = 0.213 Please check that your absorption correction is appropriate.
Author Response: The transmission range is given by the ABSCOR program.
PLAT061_ALERT_3_A Tmax/Tmin Range Test RR' too Large .............       0.18
Author Response: The transmission range is given by the ABSCOR program.

Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.31 PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 100 Deg. PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 4 PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.37 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O9 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cu2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cu1 PLAT417_ALERT_2_C Short Inter D-H..H-D H1W2 .. H9O .. 2.13 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact I12 .. O5 .. 3.48 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H10O .. I1 .. 3.10 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2 PLAT731_ALERT_1_C Bond Calc 1.46(2), Rep 1.457(9) ...... 2.22 su-Ra O10 -C30 1.555 1.555 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 C H4 O
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C60 H36 Cu4 I24 O22 Atom count from _chemical_formula_moiety: ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.307 Tmax scaled 0.307 Tmin scaled 0.026
Author Response: The transmission range is given by the ABSCOR program.
PLAT794_ALERT_5_G Check Predicted Bond Valency for Cu1         (2)       2.13
PLAT794_ALERT_5_G Check Predicted Bond Valency for Cu2         (2)       2.13
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......         14

2 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 14 ALERT level C = Check and explain 5 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 6 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion 2 ALERT type 5 Informative message, check

Comment top

There are many examples of di(ligand)tetra(carboxylato)dicopper compounds in which the carboxylate group bridges two copper atoms that are separated by a distance less than the sum of the van der Waals radius of copper. The Cambridge Structural Database (Version 5.28, Nov. 2006) lists more than 500 entries.

Related literature top

There are many examples of such di(ligand)tetra(carboxylato)dicopper compounds in which the carboxylate group bridges two copper atoms that are separated by a distance less than the sum of the van der Waals radius of copper. The Cambridge Structural Database (Version 5.28, November 2006) lists more than 500 entries.

Experimental top

In a long 0.8 cm diameter tube was placed an aqueous (5 ml) solution of copper(II) acetate monohydrate (0.5 mmol). A methanol solution (5 ml) of 2,4,5-triiodobenzoic acid (1 mmol) was layered over this. After several days, blue prisms separated from solution. The C&H elemental percentages were C 16.43 and H 0.58% (versus calculated values of C 16.35 and H 0.82%).

Refinement top

The aromatic rings were refined as rigid hexagons of 1.39 Å sides. The anisotropic temperature factors of the free methanol molecule were restrained to be nearly isotropic. Carbon-bound H atoms were generated geometrically (C–H 0.93 – 0.96 Å) and were included in the refinement in the riding model approximation, with U(H) set to 1.2–1.5Ueq(C). The water and methanolic H atoms were placed in chemically sensible positions on the basis of hydrogen bonding interactions but they were not refined; U(H) was set to 1.5Ueq(O). The final difference Fourier map had peaks/holes in the vicinity of the iodine atoms.

Structure description top

There are many examples of di(ligand)tetra(carboxylato)dicopper compounds in which the carboxylate group bridges two copper atoms that are separated by a distance less than the sum of the van der Waals radius of copper. The Cambridge Structural Database (Version 5.28, Nov. 2006) lists more than 500 entries.

There are many examples of such di(ligand)tetra(carboxylato)dicopper compounds in which the carboxylate group bridges two copper atoms that are separated by a distance less than the sum of the van der Waals radius of copper. The Cambridge Structural Database (Version 5.28, November 2006) lists more than 500 entries.

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO (Rigaku, 1998); data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).

Figures top
[Figure 1] Fig. 1. Thermal ellipsoid plot of the water-coordinated complex. Displacement ellipsoids are drawn at the 50% probability level, and H atoms are drawn as spheres of arbitrary radii. Symmetry code i = 2 - x, 2 - y, 1 - z.
[Figure 2] Fig. 2. Thermal ellipsoid plot of the methanol-coordinated complex. Displacement lelipsoids are drawn at the 50% probability level, and H atoms are drawn as spheres of arbitrary radii. Symmetry code ii = 2 - x, 2 - y, 2 - z.
Diaquatetrakis(2,3,5-triiodobenzoato- κ2O:O')dicopper(II)(Cu–Cu) bis(methanol-κO)tetrakis(2,3,5-triiodobenzoato- κ2O:O')dicopper(II)(Cu–Cu) methanol disolvate top
Crystal data top
[Cu2(C7H2I3O2)4(H2O)2][Cu2(C7H2I3O2)4(CH4O)2]·2CH4OZ = 1
Mr = 4408.65F(000) = 1960
Triclinic, P1Dx = 2.971 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 11.9321 (6) ÅCell parameters from 18920 reflections
b = 11.9345 (6) Åθ = 3.0–27.5°
c = 17.921 (1) ŵ = 8.43 mm1
α = 96.799 (1)°T = 295 K
β = 103.136 (1)°Prism, blue
γ = 91.532 (1)°0.24 × 0.19 × 0.14 mm
V = 2464.0 (2) Å3
Data collection top
Rigaku R-AXIS RAPID IP
diffractometer
11203 independent reflections
Radiation source: fine-focus sealed tube9161 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.050
ω scansθmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 1415
Tmin = 0.084, Tmax = 1.00k = 1514
24361 measured reflectionsl = 2323
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)] = 0.051Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.146H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.078P)2 + 3.5241P]
where P = (Fo2 + 2Fc2)/3
11203 reflections(Δ/σ)max = 0.001
449 parametersΔρmax = 2.37 e Å3
14 restraintsΔρmin = 1.51 e Å3
Crystal data top
[Cu2(C7H2I3O2)4(H2O)2][Cu2(C7H2I3O2)4(CH4O)2]·2CH4Oγ = 91.532 (1)°
Mr = 4408.65V = 2464.0 (2) Å3
Triclinic, P1Z = 1
a = 11.9321 (6) ÅMo Kα radiation
b = 11.9345 (6) ŵ = 8.43 mm1
c = 17.921 (1) ÅT = 295 K
α = 96.799 (1)°0.24 × 0.19 × 0.14 mm
β = 103.136 (1)°
Data collection top
Rigaku R-AXIS RAPID IP
diffractometer
11203 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
9161 reflections with I > 2σ(I)
Tmin = 0.084, Tmax = 1.00Rint = 0.050
24361 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.05114 restraints
wR(F2) = 0.146H-atom parameters constrained
S = 1.06Δρmax = 2.37 e Å3
11203 reflectionsΔρmin = 1.51 e Å3
449 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
I11.21746 (5)1.31313 (5)0.68454 (3)0.05455 (15)
I21.16902 (5)1.60545 (5)0.74506 (4)0.05628 (16)
I30.72402 (5)1.56610 (5)0.50800 (4)0.05953 (17)
I40.41538 (4)0.71789 (4)0.45628 (3)0.04599 (14)
I50.66311 (5)1.18239 (5)0.33814 (3)0.05117 (15)
I60.35562 (5)1.14333 (5)0.31042 (4)0.05908 (17)
I71.38248 (5)0.89448 (5)1.14510 (4)0.06038 (17)
I81.55290 (4)0.64621 (5)1.12823 (4)0.06330 (18)
I91.13581 (5)0.38570 (4)0.93389 (4)0.05658 (16)
I100.88626 (5)0.63810 (5)0.81397 (4)0.06055 (17)
I110.61385 (5)0.49247 (5)0.71699 (4)0.05900 (16)
I120.37236 (4)0.80116 (5)0.90462 (3)0.05159 (15)
Cu10.98855 (7)0.97560 (7)0.56782 (5)0.03541 (19)
Cu21.02862 (6)1.00342 (6)0.93345 (4)0.02765 (16)
O10.9864 (5)1.1416 (4)0.5920 (3)0.0445 (12)
O21.0072 (5)1.1823 (4)0.4774 (3)0.0487 (13)
O30.8236 (4)0.9712 (5)0.5188 (3)0.0488 (13)
O40.8441 (4)1.0097 (5)0.4027 (3)0.0443 (12)
O51.1244 (4)0.8783 (4)0.9646 (3)0.0408 (11)
O61.0761 (4)0.8700 (4)1.0779 (3)0.0440 (12)
O70.8965 (4)0.8963 (4)0.8912 (3)0.0427 (11)
O80.8489 (4)0.8904 (4)1.0042 (3)0.0380 (11)
O91.0766 (6)1.0293 (7)0.8275 (4)0.077 (2)
H9o1.03511.08320.80960.115*
O100.9491 (14)1.1794 (14)0.7471 (9)0.181 (6)
H10o1.00101.21370.72700.272*
O1w0.9549 (6)0.9362 (10)0.6753 (4)0.097 (3)
H1w11.01400.90770.70080.145*
H1w20.94260.99750.70150.145*
C10.9970 (6)1.2078 (6)0.5447 (4)0.0386 (15)
C20.9899 (4)1.3311 (3)0.5709 (3)0.0394 (15)
C31.0703 (3)1.3925 (4)0.6314 (3)0.0384 (15)
C41.0540 (4)1.5050 (4)0.6545 (2)0.0447 (17)
C50.9575 (4)1.5562 (3)0.6172 (3)0.0449 (17)
H50.94661.63150.63270.054*
C60.8771 (3)1.4948 (4)0.5568 (3)0.0416 (16)
C70.8933 (3)1.3823 (4)0.5336 (2)0.0426 (16)
H70.83961.34120.49320.051*
C80.7861 (6)0.9872 (6)0.4502 (4)0.0392 (15)
C90.6566 (2)0.9741 (3)0.4221 (3)0.0340 (14)
C100.5875 (3)1.0486 (3)0.3809 (3)0.0350 (14)
C110.4683 (3)1.0310 (3)0.3632 (3)0.0346 (14)
C120.4181 (2)0.9388 (4)0.3866 (3)0.0408 (16)
H120.33830.92700.37480.049*
C130.4872 (3)0.8643 (3)0.4278 (3)0.0374 (14)
C140.6064 (3)0.8819 (3)0.4455 (3)0.0355 (14)
H140.65260.83210.47300.043*
C151.1284 (6)0.8369 (5)1.0268 (4)0.0339 (14)
C161.1994 (3)0.7351 (3)1.0369 (3)0.0368 (14)
C171.3128 (3)0.7405 (3)1.0795 (3)0.0354 (14)
C181.3761 (3)0.6444 (3)1.0802 (3)0.0394 (15)
C191.3261 (3)0.5429 (3)1.0382 (3)0.0397 (15)
H191.36850.47861.03860.048*
C201.2127 (3)0.5375 (3)0.9956 (3)0.0385 (15)
C211.1493 (3)0.6335 (3)0.9950 (3)0.0365 (15)
H211.07350.62990.96650.044*
C220.8351 (6)0.8618 (5)0.9338 (4)0.0337 (14)
C230.7314 (3)0.7821 (3)0.8958 (2)0.0351 (14)
C240.7315 (3)0.6902 (3)0.8404 (3)0.0358 (14)
C250.6289 (4)0.6292 (3)0.8038 (2)0.0357 (14)
C260.5263 (3)0.6601 (3)0.8228 (3)0.0402 (16)
H260.45770.61920.79830.048*
C270.5263 (3)0.7520 (4)0.8782 (3)0.0364 (14)
C280.6289 (3)0.8130 (3)0.9147 (2)0.0379 (15)
H280.62880.87450.95180.045*
C291.1933 (8)1.0578 (10)0.8206 (7)0.083 (4)
H29A1.19221.06620.76790.125*
H29B1.24250.99850.83660.125*
H29C1.22191.12740.85290.125*
C300.8630 (11)1.2632 (11)0.7502 (8)0.087 (3)
H30A0.80621.23590.77500.131*
H30B0.82641.27620.69870.131*
H30C0.89971.33260.77900.131*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
I10.0427 (3)0.0641 (3)0.0515 (3)0.0108 (2)0.0035 (2)0.0118 (2)
I20.0454 (3)0.0580 (3)0.0587 (3)0.0114 (3)0.0063 (2)0.0049 (2)
I30.0456 (3)0.0604 (3)0.0766 (4)0.0172 (3)0.0102 (3)0.0293 (3)
I40.0468 (3)0.0389 (2)0.0528 (3)0.0049 (2)0.0148 (2)0.0034 (2)
I50.0510 (3)0.0535 (3)0.0531 (3)0.0009 (2)0.0138 (2)0.0205 (2)
I60.0471 (3)0.0586 (3)0.0710 (4)0.0181 (3)0.0022 (3)0.0256 (3)
I70.0575 (3)0.0460 (3)0.0636 (4)0.0062 (3)0.0065 (3)0.0103 (2)
I80.0321 (2)0.0648 (3)0.0835 (4)0.0146 (2)0.0063 (3)0.0067 (3)
I90.0474 (3)0.0323 (2)0.0854 (4)0.0019 (2)0.0109 (3)0.0023 (2)
I100.0411 (3)0.0685 (3)0.0666 (4)0.0092 (3)0.0138 (2)0.0174 (3)
I110.0632 (3)0.0478 (3)0.0585 (3)0.0039 (3)0.0112 (3)0.0166 (2)
I120.0370 (2)0.0694 (3)0.0492 (3)0.0042 (2)0.0141 (2)0.0025 (2)
Cu10.0273 (4)0.0489 (5)0.0301 (4)0.0029 (3)0.0070 (3)0.0044 (3)
Cu20.0285 (3)0.0262 (3)0.0290 (4)0.0054 (3)0.0078 (3)0.0037 (3)
O10.047 (3)0.045 (3)0.042 (3)0.007 (2)0.012 (2)0.005 (2)
O20.059 (3)0.047 (3)0.042 (3)0.002 (3)0.016 (2)0.003 (2)
O30.028 (2)0.077 (4)0.041 (3)0.004 (2)0.004 (2)0.018 (3)
O40.033 (2)0.061 (3)0.041 (3)0.007 (2)0.010 (2)0.013 (2)
O50.041 (3)0.037 (2)0.047 (3)0.016 (2)0.012 (2)0.007 (2)
O60.044 (3)0.043 (3)0.049 (3)0.020 (2)0.014 (2)0.013 (2)
O70.036 (2)0.047 (3)0.042 (3)0.007 (2)0.008 (2)0.002 (2)
O80.040 (2)0.038 (2)0.035 (3)0.005 (2)0.009 (2)0.0035 (19)
O90.091 (5)0.101 (5)0.049 (4)0.007 (4)0.040 (4)0.010 (4)
O100.214 (10)0.183 (9)0.150 (9)0.073 (8)0.039 (7)0.030 (7)
O1w0.062 (4)0.191 (10)0.040 (4)0.009 (5)0.013 (3)0.025 (5)
C10.032 (3)0.047 (4)0.034 (4)0.007 (3)0.003 (3)0.006 (3)
C20.032 (3)0.047 (4)0.038 (4)0.003 (3)0.006 (3)0.007 (3)
C30.028 (3)0.051 (4)0.039 (4)0.006 (3)0.009 (3)0.010 (3)
C40.038 (4)0.044 (4)0.052 (4)0.003 (3)0.009 (3)0.006 (3)
C50.047 (4)0.041 (4)0.047 (4)0.004 (3)0.013 (3)0.004 (3)
C60.032 (3)0.047 (4)0.049 (4)0.010 (3)0.010 (3)0.017 (3)
C70.037 (3)0.047 (4)0.042 (4)0.004 (3)0.005 (3)0.005 (3)
C80.026 (3)0.042 (3)0.044 (4)0.001 (3)0.005 (3)0.005 (3)
C90.025 (3)0.036 (3)0.040 (4)0.005 (3)0.008 (3)0.001 (3)
C100.042 (3)0.032 (3)0.031 (3)0.000 (3)0.010 (3)0.002 (2)
C110.030 (3)0.039 (3)0.035 (3)0.011 (3)0.004 (3)0.011 (3)
C120.027 (3)0.044 (4)0.046 (4)0.004 (3)0.001 (3)0.002 (3)
C130.036 (3)0.037 (3)0.037 (4)0.003 (3)0.006 (3)0.000 (3)
C140.029 (3)0.037 (3)0.036 (3)0.000 (3)0.001 (3)0.003 (3)
C150.035 (3)0.025 (3)0.040 (4)0.009 (3)0.004 (3)0.003 (2)
C160.037 (3)0.033 (3)0.044 (4)0.015 (3)0.013 (3)0.008 (3)
C170.036 (3)0.034 (3)0.036 (3)0.008 (3)0.005 (3)0.006 (3)
C180.031 (3)0.046 (4)0.040 (4)0.018 (3)0.001 (3)0.009 (3)
C190.038 (3)0.032 (3)0.049 (4)0.014 (3)0.005 (3)0.012 (3)
C200.036 (3)0.029 (3)0.051 (4)0.008 (3)0.008 (3)0.008 (3)
C210.030 (3)0.028 (3)0.050 (4)0.004 (3)0.005 (3)0.008 (3)
C220.035 (3)0.028 (3)0.038 (4)0.001 (3)0.006 (3)0.009 (3)
C230.033 (3)0.032 (3)0.040 (4)0.005 (3)0.007 (3)0.007 (3)
C240.036 (3)0.030 (3)0.039 (4)0.006 (3)0.006 (3)0.001 (3)
C250.043 (3)0.029 (3)0.035 (3)0.007 (3)0.008 (3)0.004 (3)
C260.039 (3)0.035 (3)0.041 (4)0.003 (3)0.002 (3)0.001 (3)
C270.032 (3)0.041 (3)0.038 (4)0.000 (3)0.009 (3)0.012 (3)
C280.034 (3)0.040 (3)0.039 (4)0.004 (3)0.008 (3)0.003 (3)
C290.095 (8)0.093 (8)0.095 (9)0.039 (6)0.067 (7)0.053 (7)
C300.086 (6)0.098 (7)0.084 (7)0.017 (6)0.026 (5)0.023 (6)
Geometric parameters (Å, º) top
I1—C32.105 (3)C1—C21.501 (8)
I2—C42.095 (3)C2—C31.3900
I3—C62.088 (3)C2—C71.3900
I4—C132.092 (3)C3—C41.3900
I5—C102.116 (3)C4—C51.3900
I6—C112.078 (3)C5—C61.3900
I7—C172.100 (3)C5—H50.9300
I8—C182.088 (3)C6—C71.3900
I9—C202.079 (3)C7—H70.9300
I10—C242.100 (3)C8—C91.511 (7)
I11—C252.091 (3)C9—C101.3900
I12—C272.081 (3)C9—C141.3900
Cu1—O4i1.944 (5)C10—C111.3900
Cu1—O31.961 (5)C11—C121.3900
Cu1—O2i1.968 (5)C12—C131.3900
Cu1—O11.979 (5)C12—H120.9300
Cu1—O1w2.156 (7)C13—C141.3900
Cu1—Cu1i2.6365 (17)C14—H140.9300
Cu2—O8ii1.952 (4)C15—C161.505 (7)
Cu2—O71.953 (5)C16—C171.3900
Cu2—O51.961 (5)C16—C211.3900
Cu2—O6ii1.986 (5)C17—C181.3900
Cu2—O92.156 (6)C18—C191.3900
Cu2—Cu2ii2.6355 (15)C19—C201.3900
O1—C11.249 (9)C19—H190.9300
O2—C11.244 (9)C20—C211.3900
O2—Cu1i1.968 (5)C21—H210.9300
O3—C81.248 (9)C22—C231.516 (7)
O4—C81.259 (9)C23—C241.3900
O4—Cu1i1.944 (5)C23—C281.3900
O5—C151.263 (9)C24—C251.3900
O6—C151.254 (9)C25—C261.3900
O6—Cu2ii1.986 (5)C26—C271.3900
O7—C221.265 (8)C26—H260.9300
O8—C221.240 (8)C27—C281.3900
O8—Cu2ii1.952 (4)C28—H280.9300
O9—C291.460 (8)C29—H29A0.9600
O9—H9o0.87C29—H29B0.9600
O10—C301.457 (9)C29—H29C0.9600
O10—H10o0.90C30—H30A0.9600
O1w—H1w10.85C30—H30B0.9600
O1w—H1w20.86C30—H30C0.9600
O4i—Cu1—O3168.5 (2)C14—C9—C8114.2 (4)
O4i—Cu1—O2i90.9 (2)C9—C10—C11120.0
O3—Cu1—O2i89.1 (3)C9—C10—I5120.3 (2)
O4i—Cu1—O188.6 (2)C11—C10—I5119.6 (2)
O3—Cu1—O189.0 (2)C12—C11—C10120.0
O2i—Cu1—O1168.2 (2)C12—C11—I6116.2 (2)
O4i—Cu1—O1w99.3 (3)C10—C11—I6123.6 (2)
O3—Cu1—O1w92.2 (3)C13—C12—C11120.0
O2i—Cu1—O1w95.8 (3)C13—C12—H12120.0
O1—Cu1—O1w95.9 (3)C11—C12—H12120.0
O4i—Cu1—Cu1i85.34 (16)C12—C13—C14120.0
O3—Cu1—Cu1i83.20 (16)C12—C13—I4121.0 (2)
O2i—Cu1—Cu1i84.59 (17)C14—C13—I4118.9 (2)
O1—Cu1—Cu1i83.64 (16)C13—C14—C9120.0
O1w—Cu1—Cu1i175.3 (2)C13—C14—H14120.0
O8ii—Cu2—O7168.1 (2)C9—C14—H14120.0
O8ii—Cu2—O589.1 (2)O6—C15—O5126.3 (6)
O7—Cu2—O589.9 (2)O6—C15—C16118.4 (6)
O8ii—Cu2—O6ii89.1 (2)O5—C15—C16115.2 (6)
O7—Cu2—O6ii89.6 (2)C17—C16—C21120.0
O5—Cu2—O6ii168.7 (2)C17—C16—C15123.5 (3)
O8ii—Cu2—O992.7 (2)C21—C16—C15116.2 (3)
O7—Cu2—O999.1 (3)C16—C17—C18120.0
O5—Cu2—O9100.8 (3)C16—C17—I7118.5 (2)
O6ii—Cu2—O990.5 (3)C18—C17—I7121.5 (2)
O8ii—Cu2—Cu2ii83.02 (15)C19—C18—C17120.0
O7—Cu2—Cu2ii85.12 (16)C19—C18—I8115.8 (2)
O5—Cu2—Cu2ii83.98 (16)C17—C18—I8123.6 (2)
O6ii—Cu2—Cu2ii84.68 (17)C18—C19—C20120.0
O9—Cu2—Cu2ii173.6 (2)C18—C19—H19120.0
C1—O1—Cu1122.6 (5)C20—C19—H19120.0
C1—O2—Cu1i122.1 (5)C19—C20—C21120.0
C8—O3—Cu1123.0 (5)C19—C20—I9120.5 (2)
C8—O4—Cu1i121.1 (4)C21—C20—I9119.5 (2)
C15—O5—Cu2123.4 (5)C20—C21—C16120.0
C15—O6—Cu2ii121.6 (4)C20—C21—H21120.0
C22—O7—Cu2121.4 (4)C16—C21—H21120.0
C22—O8—Cu2ii124.5 (4)O8—C22—O7126.0 (6)
C29—O9—Cu2125.2 (6)O8—C22—C23116.0 (6)
C29—O9—H9o105.5O7—C22—C23118.0 (6)
Cu2—O9—H9o105.7C24—C23—C28120.0
C30—O10—H10o103.6C24—C23—C22124.8 (4)
Cu1—O1w—H1w1109.0C28—C23—C22114.9 (4)
Cu1—O1w—H1w2108.7C25—C24—C23120.0
H1w1—O1w—H1w2108.7C25—C24—I10119.3 (2)
O2—C1—O1127.1 (7)C23—C24—I10120.7 (2)
O2—C1—C2116.7 (6)C26—C25—C24120.0
O1—C1—C2116.1 (6)C26—C25—I11115.4 (2)
C3—C2—C7120.0C24—C25—I11124.6 (2)
C3—C2—C1123.7 (4)C25—C26—C27120.0
C7—C2—C1116.2 (4)C25—C26—H26120.0
C4—C3—C2120.0C27—C26—H26120.0
C4—C3—I1121.1 (2)C26—C27—C28120.0
C2—C3—I1118.8 (2)C26—C27—I12120.2 (2)
C3—C4—C5120.0C28—C27—I12119.8 (2)
C3—C4—I2123.3 (2)C27—C28—C23120.0
C5—C4—I2116.7 (2)C27—C28—H28120.0
C6—C5—C4120.0C23—C28—H28120.0
C6—C5—H5120.0O9—C29—H29A109.5
C4—C5—H5120.0O9—C29—H29B109.5
C7—C6—C5120.0H29A—C29—H29B109.5
C7—C6—I3119.6 (2)O9—C29—H29C109.5
C5—C6—I3120.1 (2)H29A—C29—H29C109.5
C6—C7—C2120.0H29B—C29—H29C109.5
C6—C7—H7120.0O10—C30—H30A109.5
C2—C7—H7120.0O10—C30—H30B109.5
O3—C8—O4127.3 (6)H30A—C30—H30B109.5
O3—C8—C9114.9 (6)O10—C30—H30C109.5
O4—C8—C9117.8 (6)H30A—C30—H30C109.5
C10—C9—C14120.0H30B—C30—H30C109.5
C10—C9—C8125.7 (4)
O4i—Cu1—O1—C184.2 (6)C9—C10—C11—C120.0
O3—Cu1—O1—C184.5 (6)I5—C10—C11—C12175.7 (3)
O2i—Cu1—O1—C13.5 (14)C9—C10—C11—I6174.6 (4)
O1w—Cu1—O1—C1176.6 (6)I5—C10—C11—I69.7 (3)
Cu1i—Cu1—O1—C11.2 (5)C10—C11—C12—C130.0
O4i—Cu1—O3—C87.2 (17)I6—C11—C12—C13175.0 (3)
O2i—Cu1—O3—C883.1 (6)C11—C12—C13—C140.0
O1—Cu1—O3—C885.2 (6)C11—C12—C13—I4175.1 (3)
O1w—Cu1—O3—C8178.9 (7)C12—C13—C14—C90.0
Cu1i—Cu1—O3—C81.5 (6)I4—C13—C14—C9175.2 (3)
O8ii—Cu2—O5—C1584.4 (5)C10—C9—C14—C130.0
O7—Cu2—O5—C1583.8 (5)C8—C9—C14—C13175.9 (5)
O6ii—Cu2—O5—C153.2 (14)Cu2ii—O6—C15—O51.5 (9)
O9—Cu2—O5—C15176.9 (5)Cu2ii—O6—C15—C16175.6 (4)
Cu2ii—Cu2—O5—C151.3 (5)Cu2—O5—C15—O62.1 (9)
O8ii—Cu2—O7—C221.6 (14)Cu2—O5—C15—C16175.1 (3)
O5—Cu2—O7—C2283.5 (5)O6—C15—C16—C1785.1 (6)
O6ii—Cu2—O7—C2285.2 (5)O5—C15—C16—C1797.5 (6)
O9—Cu2—O7—C22175.7 (6)O6—C15—C16—C21100.8 (6)
Cu2ii—Cu2—O7—C220.5 (5)O5—C15—C16—C2176.6 (6)
O8ii—Cu2—O9—C2930.5 (9)C21—C16—C17—C180.0
O7—Cu2—O9—C29150.7 (8)C15—C16—C17—C18173.9 (5)
O5—Cu2—O9—C2959.1 (9)C21—C16—C17—I7177.8 (3)
O6ii—Cu2—O9—C29119.7 (9)C15—C16—C17—I78.3 (5)
Cu1i—O2—C1—O11.2 (11)C16—C17—C18—C190.0
Cu1i—O2—C1—C2177.5 (4)I7—C17—C18—C19177.8 (4)
Cu1—O1—C1—O21.9 (10)C16—C17—C18—I8170.8 (4)
Cu1—O1—C1—C2178.2 (4)I7—C17—C18—I811.4 (4)
O2—C1—C2—C3117.9 (6)C17—C18—C19—C200.0
O1—C1—C2—C365.4 (7)I8—C18—C19—C20171.5 (3)
O2—C1—C2—C765.3 (7)C18—C19—C20—C210.0
O1—C1—C2—C7111.4 (6)C18—C19—C20—I9179.1 (4)
C7—C2—C3—C40.0C19—C20—C21—C160.0
C1—C2—C3—C4176.7 (6)I9—C20—C21—C16179.1 (4)
C7—C2—C3—I1178.4 (4)C17—C16—C21—C200.0
C1—C2—C3—I14.9 (5)C15—C16—C21—C20174.3 (5)
C2—C3—C4—C50.0Cu2ii—O8—C22—O70.4 (10)
I1—C3—C4—C5178.4 (4)Cu2ii—O8—C22—C23177.5 (4)
C2—C3—C4—I2179.8 (4)Cu2—O7—C22—O80.7 (10)
I1—C3—C4—I21.8 (4)Cu2—O7—C22—C23177.7 (4)
C3—C4—C5—C60.0O8—C22—C23—C24138.5 (5)
I2—C4—C5—C6179.8 (4)O7—C22—C23—C2444.2 (7)
C4—C5—C6—C70.0O8—C22—C23—C2847.5 (6)
C4—C5—C6—I3173.8 (4)O7—C22—C23—C28129.8 (5)
C5—C6—C7—C20.0C28—C23—C24—C250.0
I3—C6—C7—C2173.8 (4)C22—C23—C24—C25173.7 (5)
C3—C2—C7—C60.0C28—C23—C24—I10177.6 (3)
C1—C2—C7—C6176.9 (5)C22—C23—C24—I108.7 (5)
Cu1—O3—C8—O41.1 (11)C23—C24—C25—C260.0
Cu1—O3—C8—C9176.9 (4)I10—C24—C25—C26177.6 (3)
Cu1i—O4—C8—O30.4 (11)C23—C24—C25—I11178.0 (3)
Cu1i—O4—C8—C9178.4 (4)I10—C24—C25—I114.4 (3)
O3—C8—C9—C10133.2 (6)C24—C25—C26—C270.0
O4—C8—C9—C1048.6 (8)I11—C25—C26—C27178.1 (3)
O3—C8—C9—C1442.4 (7)C25—C26—C27—C280.0
O4—C8—C9—C14135.8 (6)C25—C26—C27—I12178.4 (3)
C14—C9—C10—C110.0C26—C27—C28—C230.0
C8—C9—C10—C11175.4 (5)I12—C27—C28—C23178.4 (3)
C14—C9—C10—I5175.6 (3)C24—C23—C28—C270.0
C8—C9—C10—I59.0 (5)C22—C23—C28—C27174.3 (5)
Symmetry codes: (i) x+2, y+2, z+1; (ii) x+2, y+2, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w2···O90.862.432.86 (1)112
O1w—H1w2···O100.862.223.04 (2)161
O9—H9o···O100.871.862.71 (2)165
O10—H10o···I10.903.103.98 (2)168

Experimental details

Crystal data
Chemical formula[Cu2(C7H2I3O2)4(H2O)2][Cu2(C7H2I3O2)4(CH4O)2]·2CH4O
Mr4408.65
Crystal system, space groupTriclinic, P1
Temperature (K)295
a, b, c (Å)11.9321 (6), 11.9345 (6), 17.921 (1)
α, β, γ (°)96.799 (1), 103.136 (1), 91.532 (1)
V3)2464.0 (2)
Z1
Radiation typeMo Kα
µ (mm1)8.43
Crystal size (mm)0.24 × 0.19 × 0.14
Data collection
DiffractometerRigaku R-AXIS RAPID IP
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.084, 1.00
No. of measured, independent and
observed [I > 2σ(I)] reflections
24361, 11203, 9161
Rint0.050
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.051, 0.146, 1.06
No. of reflections11203
No. of parameters449
No. of restraints14
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)2.37, 1.51

Computer programs: RAPID-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001), publCIF (Westrip, 2007).

 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds