Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807046430/bt2517sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807046430/bt2517Isup2.hkl |
CCDC reference: 663658
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (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
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.
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%).
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.
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.
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).
[Cu2(C7H2I3O2)4(H2O)2][Cu2(C7H2I3O2)4(CH4O)2]·2CH4O | Z = 1 |
Mr = 4408.65 | F(000) = 1960 |
Triclinic, P1 | Dx = 2.971 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.9321 (6) Å | Cell parameters from 18920 reflections |
b = 11.9345 (6) Å | θ = 3.0–27.5° |
c = 17.921 (1) Å | µ = 8.43 mm−1 |
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 |
Rigaku R-AXIS RAPID IP diffractometer | 11203 independent reflections |
Radiation source: fine-focus sealed tube | 9161 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.050 |
ω scans | θmax = 27.5°, θmin = 3.0° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −14→15 |
Tmin = 0.084, Tmax = 1.00 | k = −15→14 |
24361 measured reflections | l = −23→23 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.051 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.146 | H-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 parameters | Δρmax = 2.37 e Å−3 |
14 restraints | Δρmin = −1.51 e Å−3 |
[Cu2(C7H2I3O2)4(H2O)2][Cu2(C7H2I3O2)4(CH4O)2]·2CH4O | γ = 91.532 (1)° |
Mr = 4408.65 | V = 2464.0 (2) Å3 |
Triclinic, P1 | Z = 1 |
a = 11.9321 (6) Å | Mo Kα radiation |
b = 11.9345 (6) Å | µ = 8.43 mm−1 |
c = 17.921 (1) Å | T = 295 K |
α = 96.799 (1)° | 0.24 × 0.19 × 0.14 mm |
β = 103.136 (1)° |
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 = 1.00 | Rint = 0.050 |
24361 measured reflections |
R[F2 > 2σ(F2)] = 0.051 | 14 restraints |
wR(F2) = 0.146 | H-atom parameters constrained |
S = 1.06 | Δρmax = 2.37 e Å−3 |
11203 reflections | Δρmin = −1.51 e Å−3 |
449 parameters |
x | y | z | Uiso*/Ueq | ||
I1 | 1.21746 (5) | 1.31313 (5) | 0.68454 (3) | 0.05455 (15) | |
I2 | 1.16902 (5) | 1.60545 (5) | 0.74506 (4) | 0.05628 (16) | |
I3 | 0.72402 (5) | 1.56610 (5) | 0.50800 (4) | 0.05953 (17) | |
I4 | 0.41538 (4) | 0.71789 (4) | 0.45628 (3) | 0.04599 (14) | |
I5 | 0.66311 (5) | 1.18239 (5) | 0.33814 (3) | 0.05117 (15) | |
I6 | 0.35562 (5) | 1.14333 (5) | 0.31042 (4) | 0.05908 (17) | |
I7 | 1.38248 (5) | 0.89448 (5) | 1.14510 (4) | 0.06038 (17) | |
I8 | 1.55290 (4) | 0.64621 (5) | 1.12823 (4) | 0.06330 (18) | |
I9 | 1.13581 (5) | 0.38570 (4) | 0.93389 (4) | 0.05658 (16) | |
I10 | 0.88626 (5) | 0.63810 (5) | 0.81397 (4) | 0.06055 (17) | |
I11 | 0.61385 (5) | 0.49247 (5) | 0.71699 (4) | 0.05900 (16) | |
I12 | 0.37236 (4) | 0.80116 (5) | 0.90462 (3) | 0.05159 (15) | |
Cu1 | 0.98855 (7) | 0.97560 (7) | 0.56782 (5) | 0.03541 (19) | |
Cu2 | 1.02862 (6) | 1.00342 (6) | 0.93345 (4) | 0.02765 (16) | |
O1 | 0.9864 (5) | 1.1416 (4) | 0.5920 (3) | 0.0445 (12) | |
O2 | 1.0072 (5) | 1.1823 (4) | 0.4774 (3) | 0.0487 (13) | |
O3 | 0.8236 (4) | 0.9712 (5) | 0.5188 (3) | 0.0488 (13) | |
O4 | 0.8441 (4) | 1.0097 (5) | 0.4027 (3) | 0.0443 (12) | |
O5 | 1.1244 (4) | 0.8783 (4) | 0.9646 (3) | 0.0408 (11) | |
O6 | 1.0761 (4) | 0.8700 (4) | 1.0779 (3) | 0.0440 (12) | |
O7 | 0.8965 (4) | 0.8963 (4) | 0.8912 (3) | 0.0427 (11) | |
O8 | 0.8489 (4) | 0.8904 (4) | 1.0042 (3) | 0.0380 (11) | |
O9 | 1.0766 (6) | 1.0293 (7) | 0.8275 (4) | 0.077 (2) | |
H9o | 1.0351 | 1.0832 | 0.8096 | 0.115* | |
O10 | 0.9491 (14) | 1.1794 (14) | 0.7471 (9) | 0.181 (6) | |
H10o | 1.0010 | 1.2137 | 0.7270 | 0.272* | |
O1w | 0.9549 (6) | 0.9362 (10) | 0.6753 (4) | 0.097 (3) | |
H1w1 | 1.0140 | 0.9077 | 0.7008 | 0.145* | |
H1w2 | 0.9426 | 0.9975 | 0.7015 | 0.145* | |
C1 | 0.9970 (6) | 1.2078 (6) | 0.5447 (4) | 0.0386 (15) | |
C2 | 0.9899 (4) | 1.3311 (3) | 0.5709 (3) | 0.0394 (15) | |
C3 | 1.0703 (3) | 1.3925 (4) | 0.6314 (3) | 0.0384 (15) | |
C4 | 1.0540 (4) | 1.5050 (4) | 0.6545 (2) | 0.0447 (17) | |
C5 | 0.9575 (4) | 1.5562 (3) | 0.6172 (3) | 0.0449 (17) | |
H5 | 0.9466 | 1.6315 | 0.6327 | 0.054* | |
C6 | 0.8771 (3) | 1.4948 (4) | 0.5568 (3) | 0.0416 (16) | |
C7 | 0.8933 (3) | 1.3823 (4) | 0.5336 (2) | 0.0426 (16) | |
H7 | 0.8396 | 1.3412 | 0.4932 | 0.051* | |
C8 | 0.7861 (6) | 0.9872 (6) | 0.4502 (4) | 0.0392 (15) | |
C9 | 0.6566 (2) | 0.9741 (3) | 0.4221 (3) | 0.0340 (14) | |
C10 | 0.5875 (3) | 1.0486 (3) | 0.3809 (3) | 0.0350 (14) | |
C11 | 0.4683 (3) | 1.0310 (3) | 0.3632 (3) | 0.0346 (14) | |
C12 | 0.4181 (2) | 0.9388 (4) | 0.3866 (3) | 0.0408 (16) | |
H12 | 0.3383 | 0.9270 | 0.3748 | 0.049* | |
C13 | 0.4872 (3) | 0.8643 (3) | 0.4278 (3) | 0.0374 (14) | |
C14 | 0.6064 (3) | 0.8819 (3) | 0.4455 (3) | 0.0355 (14) | |
H14 | 0.6526 | 0.8321 | 0.4730 | 0.043* | |
C15 | 1.1284 (6) | 0.8369 (5) | 1.0268 (4) | 0.0339 (14) | |
C16 | 1.1994 (3) | 0.7351 (3) | 1.0369 (3) | 0.0368 (14) | |
C17 | 1.3128 (3) | 0.7405 (3) | 1.0795 (3) | 0.0354 (14) | |
C18 | 1.3761 (3) | 0.6444 (3) | 1.0802 (3) | 0.0394 (15) | |
C19 | 1.3261 (3) | 0.5429 (3) | 1.0382 (3) | 0.0397 (15) | |
H19 | 1.3685 | 0.4786 | 1.0386 | 0.048* | |
C20 | 1.2127 (3) | 0.5375 (3) | 0.9956 (3) | 0.0385 (15) | |
C21 | 1.1493 (3) | 0.6335 (3) | 0.9950 (3) | 0.0365 (15) | |
H21 | 1.0735 | 0.6299 | 0.9665 | 0.044* | |
C22 | 0.8351 (6) | 0.8618 (5) | 0.9338 (4) | 0.0337 (14) | |
C23 | 0.7314 (3) | 0.7821 (3) | 0.8958 (2) | 0.0351 (14) | |
C24 | 0.7315 (3) | 0.6902 (3) | 0.8404 (3) | 0.0358 (14) | |
C25 | 0.6289 (4) | 0.6292 (3) | 0.8038 (2) | 0.0357 (14) | |
C26 | 0.5263 (3) | 0.6601 (3) | 0.8228 (3) | 0.0402 (16) | |
H26 | 0.4577 | 0.6192 | 0.7983 | 0.048* | |
C27 | 0.5263 (3) | 0.7520 (4) | 0.8782 (3) | 0.0364 (14) | |
C28 | 0.6289 (3) | 0.8130 (3) | 0.9147 (2) | 0.0379 (15) | |
H28 | 0.6288 | 0.8745 | 0.9518 | 0.045* | |
C29 | 1.1933 (8) | 1.0578 (10) | 0.8206 (7) | 0.083 (4) | |
H29A | 1.1922 | 1.0662 | 0.7679 | 0.125* | |
H29B | 1.2425 | 0.9985 | 0.8366 | 0.125* | |
H29C | 1.2219 | 1.1274 | 0.8529 | 0.125* | |
C30 | 0.8630 (11) | 1.2632 (11) | 0.7502 (8) | 0.087 (3) | |
H30A | 0.8062 | 1.2359 | 0.7750 | 0.131* | |
H30B | 0.8264 | 1.2762 | 0.6987 | 0.131* | |
H30C | 0.8997 | 1.3326 | 0.7790 | 0.131* |
U11 | U22 | U33 | U12 | U13 | U23 | |
I1 | 0.0427 (3) | 0.0641 (3) | 0.0515 (3) | 0.0108 (2) | −0.0035 (2) | 0.0118 (2) |
I2 | 0.0454 (3) | 0.0580 (3) | 0.0587 (3) | −0.0114 (3) | 0.0063 (2) | −0.0049 (2) |
I3 | 0.0456 (3) | 0.0604 (3) | 0.0766 (4) | 0.0172 (3) | 0.0102 (3) | 0.0293 (3) |
I4 | 0.0468 (3) | 0.0389 (2) | 0.0528 (3) | −0.0049 (2) | 0.0148 (2) | 0.0034 (2) |
I5 | 0.0510 (3) | 0.0535 (3) | 0.0531 (3) | 0.0009 (2) | 0.0138 (2) | 0.0205 (2) |
I6 | 0.0471 (3) | 0.0586 (3) | 0.0710 (4) | 0.0181 (3) | 0.0022 (3) | 0.0256 (3) |
I7 | 0.0575 (3) | 0.0460 (3) | 0.0636 (4) | 0.0062 (3) | −0.0065 (3) | −0.0103 (2) |
I8 | 0.0321 (2) | 0.0648 (3) | 0.0835 (4) | 0.0146 (2) | −0.0063 (3) | 0.0067 (3) |
I9 | 0.0474 (3) | 0.0323 (2) | 0.0854 (4) | 0.0019 (2) | 0.0109 (3) | −0.0023 (2) |
I10 | 0.0411 (3) | 0.0685 (3) | 0.0666 (4) | 0.0092 (3) | 0.0138 (2) | −0.0174 (3) |
I11 | 0.0632 (3) | 0.0478 (3) | 0.0585 (3) | −0.0039 (3) | 0.0112 (3) | −0.0166 (2) |
I12 | 0.0370 (2) | 0.0694 (3) | 0.0492 (3) | 0.0042 (2) | 0.0141 (2) | 0.0025 (2) |
Cu1 | 0.0273 (4) | 0.0489 (5) | 0.0301 (4) | 0.0029 (3) | 0.0070 (3) | 0.0044 (3) |
Cu2 | 0.0285 (3) | 0.0262 (3) | 0.0290 (4) | 0.0054 (3) | 0.0078 (3) | 0.0037 (3) |
O1 | 0.047 (3) | 0.045 (3) | 0.042 (3) | 0.007 (2) | 0.012 (2) | 0.005 (2) |
O2 | 0.059 (3) | 0.047 (3) | 0.042 (3) | 0.002 (3) | 0.016 (2) | 0.003 (2) |
O3 | 0.028 (2) | 0.077 (4) | 0.041 (3) | 0.004 (2) | 0.004 (2) | 0.018 (3) |
O4 | 0.033 (2) | 0.061 (3) | 0.041 (3) | 0.007 (2) | 0.010 (2) | 0.013 (2) |
O5 | 0.041 (3) | 0.037 (2) | 0.047 (3) | 0.016 (2) | 0.012 (2) | 0.007 (2) |
O6 | 0.044 (3) | 0.043 (3) | 0.049 (3) | 0.020 (2) | 0.014 (2) | 0.013 (2) |
O7 | 0.036 (2) | 0.047 (3) | 0.042 (3) | −0.007 (2) | 0.008 (2) | −0.002 (2) |
O8 | 0.040 (2) | 0.038 (2) | 0.035 (3) | −0.005 (2) | 0.009 (2) | 0.0035 (19) |
O9 | 0.091 (5) | 0.101 (5) | 0.049 (4) | −0.007 (4) | 0.040 (4) | 0.010 (4) |
O10 | 0.214 (10) | 0.183 (9) | 0.150 (9) | 0.073 (8) | 0.039 (7) | 0.030 (7) |
O1w | 0.062 (4) | 0.191 (10) | 0.040 (4) | 0.009 (5) | 0.013 (3) | 0.025 (5) |
C1 | 0.032 (3) | 0.047 (4) | 0.034 (4) | 0.007 (3) | 0.003 (3) | 0.006 (3) |
C2 | 0.032 (3) | 0.047 (4) | 0.038 (4) | 0.003 (3) | 0.006 (3) | 0.007 (3) |
C3 | 0.028 (3) | 0.051 (4) | 0.039 (4) | 0.006 (3) | 0.009 (3) | 0.010 (3) |
C4 | 0.038 (4) | 0.044 (4) | 0.052 (4) | −0.003 (3) | 0.009 (3) | 0.006 (3) |
C5 | 0.047 (4) | 0.041 (4) | 0.047 (4) | 0.004 (3) | 0.013 (3) | 0.004 (3) |
C6 | 0.032 (3) | 0.047 (4) | 0.049 (4) | 0.010 (3) | 0.010 (3) | 0.017 (3) |
C7 | 0.037 (3) | 0.047 (4) | 0.042 (4) | 0.004 (3) | 0.005 (3) | 0.005 (3) |
C8 | 0.026 (3) | 0.042 (3) | 0.044 (4) | −0.001 (3) | 0.005 (3) | −0.005 (3) |
C9 | 0.025 (3) | 0.036 (3) | 0.040 (4) | 0.005 (3) | 0.008 (3) | −0.001 (3) |
C10 | 0.042 (3) | 0.032 (3) | 0.031 (3) | 0.000 (3) | 0.010 (3) | 0.002 (2) |
C11 | 0.030 (3) | 0.039 (3) | 0.035 (3) | 0.011 (3) | 0.004 (3) | 0.011 (3) |
C12 | 0.027 (3) | 0.044 (4) | 0.046 (4) | 0.004 (3) | −0.001 (3) | 0.002 (3) |
C13 | 0.036 (3) | 0.037 (3) | 0.037 (4) | 0.003 (3) | 0.006 (3) | 0.000 (3) |
C14 | 0.029 (3) | 0.037 (3) | 0.036 (3) | 0.000 (3) | 0.001 (3) | 0.003 (3) |
C15 | 0.035 (3) | 0.025 (3) | 0.040 (4) | 0.009 (3) | 0.004 (3) | 0.003 (2) |
C16 | 0.037 (3) | 0.033 (3) | 0.044 (4) | 0.015 (3) | 0.013 (3) | 0.008 (3) |
C17 | 0.036 (3) | 0.034 (3) | 0.036 (3) | 0.008 (3) | 0.005 (3) | 0.006 (3) |
C18 | 0.031 (3) | 0.046 (4) | 0.040 (4) | 0.018 (3) | 0.001 (3) | 0.009 (3) |
C19 | 0.038 (3) | 0.032 (3) | 0.049 (4) | 0.014 (3) | 0.005 (3) | 0.012 (3) |
C20 | 0.036 (3) | 0.029 (3) | 0.051 (4) | 0.008 (3) | 0.008 (3) | 0.008 (3) |
C21 | 0.030 (3) | 0.028 (3) | 0.050 (4) | 0.004 (3) | 0.005 (3) | 0.008 (3) |
C22 | 0.035 (3) | 0.028 (3) | 0.038 (4) | 0.001 (3) | 0.006 (3) | 0.009 (3) |
C23 | 0.033 (3) | 0.032 (3) | 0.040 (4) | 0.005 (3) | 0.007 (3) | 0.007 (3) |
C24 | 0.036 (3) | 0.030 (3) | 0.039 (4) | 0.006 (3) | 0.006 (3) | 0.001 (3) |
C25 | 0.043 (3) | 0.029 (3) | 0.035 (3) | 0.007 (3) | 0.008 (3) | 0.004 (3) |
C26 | 0.039 (3) | 0.035 (3) | 0.041 (4) | −0.003 (3) | 0.002 (3) | 0.001 (3) |
C27 | 0.032 (3) | 0.041 (3) | 0.038 (4) | 0.000 (3) | 0.009 (3) | 0.012 (3) |
C28 | 0.034 (3) | 0.040 (3) | 0.039 (4) | 0.004 (3) | 0.008 (3) | 0.003 (3) |
C29 | 0.095 (8) | 0.093 (8) | 0.095 (9) | 0.039 (6) | 0.067 (7) | 0.053 (7) |
C30 | 0.086 (6) | 0.098 (7) | 0.084 (7) | 0.017 (6) | 0.026 (5) | 0.023 (6) |
I1—C3 | 2.105 (3) | C1—C2 | 1.501 (8) |
I2—C4 | 2.095 (3) | C2—C3 | 1.3900 |
I3—C6 | 2.088 (3) | C2—C7 | 1.3900 |
I4—C13 | 2.092 (3) | C3—C4 | 1.3900 |
I5—C10 | 2.116 (3) | C4—C5 | 1.3900 |
I6—C11 | 2.078 (3) | C5—C6 | 1.3900 |
I7—C17 | 2.100 (3) | C5—H5 | 0.9300 |
I8—C18 | 2.088 (3) | C6—C7 | 1.3900 |
I9—C20 | 2.079 (3) | C7—H7 | 0.9300 |
I10—C24 | 2.100 (3) | C8—C9 | 1.511 (7) |
I11—C25 | 2.091 (3) | C9—C10 | 1.3900 |
I12—C27 | 2.081 (3) | C9—C14 | 1.3900 |
Cu1—O4i | 1.944 (5) | C10—C11 | 1.3900 |
Cu1—O3 | 1.961 (5) | C11—C12 | 1.3900 |
Cu1—O2i | 1.968 (5) | C12—C13 | 1.3900 |
Cu1—O1 | 1.979 (5) | C12—H12 | 0.9300 |
Cu1—O1w | 2.156 (7) | C13—C14 | 1.3900 |
Cu1—Cu1i | 2.6365 (17) | C14—H14 | 0.9300 |
Cu2—O8ii | 1.952 (4) | C15—C16 | 1.505 (7) |
Cu2—O7 | 1.953 (5) | C16—C17 | 1.3900 |
Cu2—O5 | 1.961 (5) | C16—C21 | 1.3900 |
Cu2—O6ii | 1.986 (5) | C17—C18 | 1.3900 |
Cu2—O9 | 2.156 (6) | C18—C19 | 1.3900 |
Cu2—Cu2ii | 2.6355 (15) | C19—C20 | 1.3900 |
O1—C1 | 1.249 (9) | C19—H19 | 0.9300 |
O2—C1 | 1.244 (9) | C20—C21 | 1.3900 |
O2—Cu1i | 1.968 (5) | C21—H21 | 0.9300 |
O3—C8 | 1.248 (9) | C22—C23 | 1.516 (7) |
O4—C8 | 1.259 (9) | C23—C24 | 1.3900 |
O4—Cu1i | 1.944 (5) | C23—C28 | 1.3900 |
O5—C15 | 1.263 (9) | C24—C25 | 1.3900 |
O6—C15 | 1.254 (9) | C25—C26 | 1.3900 |
O6—Cu2ii | 1.986 (5) | C26—C27 | 1.3900 |
O7—C22 | 1.265 (8) | C26—H26 | 0.9300 |
O8—C22 | 1.240 (8) | C27—C28 | 1.3900 |
O8—Cu2ii | 1.952 (4) | C28—H28 | 0.9300 |
O9—C29 | 1.460 (8) | C29—H29A | 0.9600 |
O9—H9o | 0.87 | C29—H29B | 0.9600 |
O10—C30 | 1.457 (9) | C29—H29C | 0.9600 |
O10—H10o | 0.90 | C30—H30A | 0.9600 |
O1w—H1w1 | 0.85 | C30—H30B | 0.9600 |
O1w—H1w2 | 0.86 | C30—H30C | 0.9600 |
O4i—Cu1—O3 | 168.5 (2) | C14—C9—C8 | 114.2 (4) |
O4i—Cu1—O2i | 90.9 (2) | C9—C10—C11 | 120.0 |
O3—Cu1—O2i | 89.1 (3) | C9—C10—I5 | 120.3 (2) |
O4i—Cu1—O1 | 88.6 (2) | C11—C10—I5 | 119.6 (2) |
O3—Cu1—O1 | 89.0 (2) | C12—C11—C10 | 120.0 |
O2i—Cu1—O1 | 168.2 (2) | C12—C11—I6 | 116.2 (2) |
O4i—Cu1—O1w | 99.3 (3) | C10—C11—I6 | 123.6 (2) |
O3—Cu1—O1w | 92.2 (3) | C13—C12—C11 | 120.0 |
O2i—Cu1—O1w | 95.8 (3) | C13—C12—H12 | 120.0 |
O1—Cu1—O1w | 95.9 (3) | C11—C12—H12 | 120.0 |
O4i—Cu1—Cu1i | 85.34 (16) | C12—C13—C14 | 120.0 |
O3—Cu1—Cu1i | 83.20 (16) | C12—C13—I4 | 121.0 (2) |
O2i—Cu1—Cu1i | 84.59 (17) | C14—C13—I4 | 118.9 (2) |
O1—Cu1—Cu1i | 83.64 (16) | C13—C14—C9 | 120.0 |
O1w—Cu1—Cu1i | 175.3 (2) | C13—C14—H14 | 120.0 |
O8ii—Cu2—O7 | 168.1 (2) | C9—C14—H14 | 120.0 |
O8ii—Cu2—O5 | 89.1 (2) | O6—C15—O5 | 126.3 (6) |
O7—Cu2—O5 | 89.9 (2) | O6—C15—C16 | 118.4 (6) |
O8ii—Cu2—O6ii | 89.1 (2) | O5—C15—C16 | 115.2 (6) |
O7—Cu2—O6ii | 89.6 (2) | C17—C16—C21 | 120.0 |
O5—Cu2—O6ii | 168.7 (2) | C17—C16—C15 | 123.5 (3) |
O8ii—Cu2—O9 | 92.7 (2) | C21—C16—C15 | 116.2 (3) |
O7—Cu2—O9 | 99.1 (3) | C16—C17—C18 | 120.0 |
O5—Cu2—O9 | 100.8 (3) | C16—C17—I7 | 118.5 (2) |
O6ii—Cu2—O9 | 90.5 (3) | C18—C17—I7 | 121.5 (2) |
O8ii—Cu2—Cu2ii | 83.02 (15) | C19—C18—C17 | 120.0 |
O7—Cu2—Cu2ii | 85.12 (16) | C19—C18—I8 | 115.8 (2) |
O5—Cu2—Cu2ii | 83.98 (16) | C17—C18—I8 | 123.6 (2) |
O6ii—Cu2—Cu2ii | 84.68 (17) | C18—C19—C20 | 120.0 |
O9—Cu2—Cu2ii | 173.6 (2) | C18—C19—H19 | 120.0 |
C1—O1—Cu1 | 122.6 (5) | C20—C19—H19 | 120.0 |
C1—O2—Cu1i | 122.1 (5) | C19—C20—C21 | 120.0 |
C8—O3—Cu1 | 123.0 (5) | C19—C20—I9 | 120.5 (2) |
C8—O4—Cu1i | 121.1 (4) | C21—C20—I9 | 119.5 (2) |
C15—O5—Cu2 | 123.4 (5) | C20—C21—C16 | 120.0 |
C15—O6—Cu2ii | 121.6 (4) | C20—C21—H21 | 120.0 |
C22—O7—Cu2 | 121.4 (4) | C16—C21—H21 | 120.0 |
C22—O8—Cu2ii | 124.5 (4) | O8—C22—O7 | 126.0 (6) |
C29—O9—Cu2 | 125.2 (6) | O8—C22—C23 | 116.0 (6) |
C29—O9—H9o | 105.5 | O7—C22—C23 | 118.0 (6) |
Cu2—O9—H9o | 105.7 | C24—C23—C28 | 120.0 |
C30—O10—H10o | 103.6 | C24—C23—C22 | 124.8 (4) |
Cu1—O1w—H1w1 | 109.0 | C28—C23—C22 | 114.9 (4) |
Cu1—O1w—H1w2 | 108.7 | C25—C24—C23 | 120.0 |
H1w1—O1w—H1w2 | 108.7 | C25—C24—I10 | 119.3 (2) |
O2—C1—O1 | 127.1 (7) | C23—C24—I10 | 120.7 (2) |
O2—C1—C2 | 116.7 (6) | C26—C25—C24 | 120.0 |
O1—C1—C2 | 116.1 (6) | C26—C25—I11 | 115.4 (2) |
C3—C2—C7 | 120.0 | C24—C25—I11 | 124.6 (2) |
C3—C2—C1 | 123.7 (4) | C25—C26—C27 | 120.0 |
C7—C2—C1 | 116.2 (4) | C25—C26—H26 | 120.0 |
C4—C3—C2 | 120.0 | C27—C26—H26 | 120.0 |
C4—C3—I1 | 121.1 (2) | C26—C27—C28 | 120.0 |
C2—C3—I1 | 118.8 (2) | C26—C27—I12 | 120.2 (2) |
C3—C4—C5 | 120.0 | C28—C27—I12 | 119.8 (2) |
C3—C4—I2 | 123.3 (2) | C27—C28—C23 | 120.0 |
C5—C4—I2 | 116.7 (2) | C27—C28—H28 | 120.0 |
C6—C5—C4 | 120.0 | C23—C28—H28 | 120.0 |
C6—C5—H5 | 120.0 | O9—C29—H29A | 109.5 |
C4—C5—H5 | 120.0 | O9—C29—H29B | 109.5 |
C7—C6—C5 | 120.0 | H29A—C29—H29B | 109.5 |
C7—C6—I3 | 119.6 (2) | O9—C29—H29C | 109.5 |
C5—C6—I3 | 120.1 (2) | H29A—C29—H29C | 109.5 |
C6—C7—C2 | 120.0 | H29B—C29—H29C | 109.5 |
C6—C7—H7 | 120.0 | O10—C30—H30A | 109.5 |
C2—C7—H7 | 120.0 | O10—C30—H30B | 109.5 |
O3—C8—O4 | 127.3 (6) | H30A—C30—H30B | 109.5 |
O3—C8—C9 | 114.9 (6) | O10—C30—H30C | 109.5 |
O4—C8—C9 | 117.8 (6) | H30A—C30—H30C | 109.5 |
C10—C9—C14 | 120.0 | H30B—C30—H30C | 109.5 |
C10—C9—C8 | 125.7 (4) | ||
O4i—Cu1—O1—C1 | 84.2 (6) | C9—C10—C11—C12 | 0.0 |
O3—Cu1—O1—C1 | −84.5 (6) | I5—C10—C11—C12 | 175.7 (3) |
O2i—Cu1—O1—C1 | −3.5 (14) | C9—C10—C11—I6 | 174.6 (4) |
O1w—Cu1—O1—C1 | −176.6 (6) | I5—C10—C11—I6 | −9.7 (3) |
Cu1i—Cu1—O1—C1 | −1.2 (5) | C10—C11—C12—C13 | 0.0 |
O4i—Cu1—O3—C8 | 7.2 (17) | I6—C11—C12—C13 | −175.0 (3) |
O2i—Cu1—O3—C8 | −83.1 (6) | C11—C12—C13—C14 | 0.0 |
O1—Cu1—O3—C8 | 85.2 (6) | C11—C12—C13—I4 | −175.1 (3) |
O1w—Cu1—O3—C8 | −178.9 (7) | C12—C13—C14—C9 | 0.0 |
Cu1i—Cu1—O3—C8 | 1.5 (6) | I4—C13—C14—C9 | 175.2 (3) |
O8ii—Cu2—O5—C15 | 84.4 (5) | C10—C9—C14—C13 | 0.0 |
O7—Cu2—O5—C15 | −83.8 (5) | C8—C9—C14—C13 | 175.9 (5) |
O6ii—Cu2—O5—C15 | 3.2 (14) | Cu2ii—O6—C15—O5 | 1.5 (9) |
O9—Cu2—O5—C15 | 176.9 (5) | Cu2ii—O6—C15—C16 | −175.6 (4) |
Cu2ii—Cu2—O5—C15 | 1.3 (5) | Cu2—O5—C15—O6 | −2.1 (9) |
O8ii—Cu2—O7—C22 | −1.6 (14) | Cu2—O5—C15—C16 | 175.1 (3) |
O5—Cu2—O7—C22 | 83.5 (5) | O6—C15—C16—C17 | −85.1 (6) |
O6ii—Cu2—O7—C22 | −85.2 (5) | O5—C15—C16—C17 | 97.5 (6) |
O9—Cu2—O7—C22 | −175.7 (6) | O6—C15—C16—C21 | 100.8 (6) |
Cu2ii—Cu2—O7—C22 | −0.5 (5) | O5—C15—C16—C21 | −76.6 (6) |
O8ii—Cu2—O9—C29 | 30.5 (9) | C21—C16—C17—C18 | 0.0 |
O7—Cu2—O9—C29 | −150.7 (8) | C15—C16—C17—C18 | −173.9 (5) |
O5—Cu2—O9—C29 | −59.1 (9) | C21—C16—C17—I7 | −177.8 (3) |
O6ii—Cu2—O9—C29 | 119.7 (9) | C15—C16—C17—I7 | 8.3 (5) |
Cu1i—O2—C1—O1 | −1.2 (11) | C16—C17—C18—C19 | 0.0 |
Cu1i—O2—C1—C2 | −177.5 (4) | I7—C17—C18—C19 | 177.8 (4) |
Cu1—O1—C1—O2 | 1.9 (10) | C16—C17—C18—I8 | 170.8 (4) |
Cu1—O1—C1—C2 | 178.2 (4) | I7—C17—C18—I8 | −11.4 (4) |
O2—C1—C2—C3 | −117.9 (6) | C17—C18—C19—C20 | 0.0 |
O1—C1—C2—C3 | 65.4 (7) | I8—C18—C19—C20 | −171.5 (3) |
O2—C1—C2—C7 | 65.3 (7) | C18—C19—C20—C21 | 0.0 |
O1—C1—C2—C7 | −111.4 (6) | C18—C19—C20—I9 | −179.1 (4) |
C7—C2—C3—C4 | 0.0 | C19—C20—C21—C16 | 0.0 |
C1—C2—C3—C4 | −176.7 (6) | I9—C20—C21—C16 | 179.1 (4) |
C7—C2—C3—I1 | −178.4 (4) | C17—C16—C21—C20 | 0.0 |
C1—C2—C3—I1 | 4.9 (5) | C15—C16—C21—C20 | 174.3 (5) |
C2—C3—C4—C5 | 0.0 | Cu2ii—O8—C22—O7 | −0.4 (10) |
I1—C3—C4—C5 | 178.4 (4) | Cu2ii—O8—C22—C23 | −177.5 (4) |
C2—C3—C4—I2 | 179.8 (4) | Cu2—O7—C22—O8 | 0.7 (10) |
I1—C3—C4—I2 | −1.8 (4) | Cu2—O7—C22—C23 | 177.7 (4) |
C3—C4—C5—C6 | 0.0 | O8—C22—C23—C24 | −138.5 (5) |
I2—C4—C5—C6 | −179.8 (4) | O7—C22—C23—C24 | 44.2 (7) |
C4—C5—C6—C7 | 0.0 | O8—C22—C23—C28 | 47.5 (6) |
C4—C5—C6—I3 | 173.8 (4) | O7—C22—C23—C28 | −129.8 (5) |
C5—C6—C7—C2 | 0.0 | C28—C23—C24—C25 | 0.0 |
I3—C6—C7—C2 | −173.8 (4) | C22—C23—C24—C25 | −173.7 (5) |
C3—C2—C7—C6 | 0.0 | C28—C23—C24—I10 | −177.6 (3) |
C1—C2—C7—C6 | 176.9 (5) | C22—C23—C24—I10 | 8.7 (5) |
Cu1—O3—C8—O4 | −1.1 (11) | C23—C24—C25—C26 | 0.0 |
Cu1—O3—C8—C9 | 176.9 (4) | I10—C24—C25—C26 | 177.6 (3) |
Cu1i—O4—C8—O3 | −0.4 (11) | C23—C24—C25—I11 | 178.0 (3) |
Cu1i—O4—C8—C9 | −178.4 (4) | I10—C24—C25—I11 | −4.4 (3) |
O3—C8—C9—C10 | 133.2 (6) | C24—C25—C26—C27 | 0.0 |
O4—C8—C9—C10 | −48.6 (8) | I11—C25—C26—C27 | −178.1 (3) |
O3—C8—C9—C14 | −42.4 (7) | C25—C26—C27—C28 | 0.0 |
O4—C8—C9—C14 | 135.8 (6) | C25—C26—C27—I12 | 178.4 (3) |
C14—C9—C10—C11 | 0.0 | C26—C27—C28—C23 | 0.0 |
C8—C9—C10—C11 | −175.4 (5) | I12—C27—C28—C23 | −178.4 (3) |
C14—C9—C10—I5 | −175.6 (3) | C24—C23—C28—C27 | 0.0 |
C8—C9—C10—I5 | 9.0 (5) | C22—C23—C28—C27 | 174.3 (5) |
Symmetry codes: (i) −x+2, −y+2, −z+1; (ii) −x+2, −y+2, −z+2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w2···O9 | 0.86 | 2.43 | 2.86 (1) | 112 |
O1w—H1w2···O10 | 0.86 | 2.22 | 3.04 (2) | 161 |
O9—H9o···O10 | 0.87 | 1.86 | 2.71 (2) | 165 |
O10—H10o···I1 | 0.90 | 3.10 | 3.98 (2) | 168 |
Experimental details
Crystal data | |
Chemical formula | [Cu2(C7H2I3O2)4(H2O)2][Cu2(C7H2I3O2)4(CH4O)2]·2CH4O |
Mr | 4408.65 |
Crystal system, space group | Triclinic, 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) |
V (Å3) | 2464.0 (2) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 8.43 |
Crystal size (mm) | 0.24 × 0.19 × 0.14 |
Data collection | |
Diffractometer | Rigaku R-AXIS RAPID IP |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.084, 1.00 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 24361, 11203, 9161 |
Rint | 0.050 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.051, 0.146, 1.06 |
No. of reflections | 11203 |
No. of parameters | 449 |
No. of restraints | 14 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 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).
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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.