Download citation
Download citation
link to html
[Rh(μ-I)(COD)]2 was found to crystallize as two different polymorphs in which the Rh dimer adopts either bent or planar geometries with respect to the Rh2I2 core.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S205698902100743X/zl5015sup1.cif
Contains datablocks global, B, P

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205698902100743X/zl5015Bsup2.hkl
Contains datablock B

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205698902100743X/zl5015Psup3.hkl
Contains datablock P

CCDC references: 2097568; 2097567

Key indicators

Structure: B
  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.009 Å
  • R factor = 0.035
  • wR factor = 0.079
  • Data-to-parameter ratio = 17.2
Structure: P
  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.025
  • wR factor = 0.055
  • Data-to-parameter ratio = 17.2

checkCIF/PLATON results

No syntax errors found




Alert level C PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds ............... 0.00938 Ang. PLAT761_ALERT_1_C CIF Contains no X-H Bonds ...................... Please Check PLAT762_ALERT_1_C CIF Contains no X-Y-H or H-Y-H Angles .......... Please Check
Alert level G PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite 8 Note PLAT012_ALERT_1_G N.O.K. _shelx_res_checksum Found in CIF ...... Please Check PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records 1 Report PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 4 Note PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density. 0 Info
0 ALERT level A = Most likely a serious problem - resolve or explain 0 ALERT level B = A potentially serious problem, consider carefully 3 ALERT level C = Check. Ensure it is not caused by an omission or oversight 5 ALERT level G = General information/check it is not something unexpected 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check


Alert level C PLAT761_ALERT_1_C CIF Contains no X-H Bonds ...................... Please Check PLAT762_ALERT_1_C CIF Contains no X-Y-H or H-Y-H Angles .......... Please Check PLAT973_ALERT_2_C Check Calcd Positive Resid. Density on Rh2 1.07 eA-3
Alert level G PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite 16 Note PLAT012_ALERT_1_G N.O.K. _shelx_res_checksum Found in CIF ...... Please Check PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records 1 Report PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) I1 --Rh1 . 6.0 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) I1 --Rh2 . 6.5 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) I2 --Rh2 . 5.5 s.u. PLAT802_ALERT_4_G CIF Input Record(s) with more than 80 Characters 1 Info PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 8 Note PLAT898_ALERT_4_G Second Reported H-M Symbol in CIF Ignored ...... ! Check PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L= 0.600 1 Note PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density. 0 Info
0 ALERT level A = Most likely a serious problem - resolve or explain 0 ALERT level B = A potentially serious problem, consider carefully 3 ALERT level C = Check. Ensure it is not caused by an omission or oversight 11 ALERT level G = General information/check it is not something unexpected 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

For both structures, data collection: APEX3 (Bruker, 2017); cell refinement: SAINT (Bruker, 2017); data reduction: SAINT (Bruker, 2017); program(s) used to solve structure: ShelXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL (Sheldrick, 2015b); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

Di-µ-iodido-bis{[(1,2,5,6-η)-cycloocta-1,4-diene]rhodium(I)} (B) top
Crystal data top
[Rh2I2(C8H12)2]F(000) = 1264
Mr = 675.97Dx = 2.597 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 12.3414 (16) ÅCell parameters from 2574 reflections
b = 11.8176 (17) Åθ = 2.8–23.3°
c = 11.9374 (15) ŵ = 5.47 mm1
β = 96.690 (3)°T = 100 K
V = 1729.2 (4) Å3Block, dark orange
Z = 40.10 × 0.06 × 0.03 mm
Data collection top
Nonius Kappa APEXII
diffractometer
1775 independent reflections
Radiation source: sealed tube, fine-focus1320 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.080
Detector resolution: 7.9 pixels mm-1θmax = 26.4°, θmin = 2.4°
ω and φ scansh = 1515
Absorption correction: multi-scan
(SADABS; Krause et al., 2015)
k = 1414
Tmin = 0.062, Tmax = 0.093l = 1414
15175 measured reflections
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.035Hydrogen site location: mixed
wR(F2) = 0.079H atoms treated by a mixture of independent and constrained refinement
S = 1.03 w = 1/[σ2(Fo2) + (0.0302P)2]
where P = (Fo2 + 2Fc2)/3
1775 reflections(Δ/σ)max < 0.001
103 parametersΔρmax = 1.36 e Å3
4 restraintsΔρmin = 0.79 e Å3
Special details top

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) top
xyzUiso*/Ueq
I10.52770 (3)0.20354 (3)0.40381 (4)0.02475 (15)
Rh10.38142 (4)0.31608 (4)0.25934 (4)0.02137 (15)
C10.2885 (6)0.3639 (6)0.3898 (6)0.0274 (16)
H10.309 (5)0.316 (5)0.458 (3)0.033*
C20.3652 (5)0.4497 (6)0.3749 (5)0.0255 (15)
H20.433 (3)0.456 (5)0.429 (4)0.031*
C30.3323 (6)0.5616 (5)0.3199 (6)0.0294 (16)
H3A0.3809350.6219810.3542640.035*
H3B0.2567780.5800870.3337930.035*
C40.3390 (6)0.5579 (5)0.1903 (6)0.0312 (17)
H4A0.2823710.6086590.1521820.037*
H4B0.4109720.5872480.1751660.037*
C50.3237 (5)0.4422 (6)0.1410 (6)0.0273 (16)
H50.357 (5)0.418 (5)0.074 (3)0.033*
C60.2378 (5)0.3707 (5)0.1589 (5)0.0229 (15)
H60.219 (5)0.306 (3)0.107 (4)0.028*
C70.1447 (5)0.4044 (6)0.2257 (5)0.0295 (16)
H7A0.0766750.3669410.1924620.035*
H7B0.1334030.4872160.2197590.035*
C80.1680 (5)0.3714 (6)0.3502 (6)0.0286 (16)
H8A0.1344700.4281130.3965800.034*
H8B0.1336570.2973040.3619200.034*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
I10.0234 (3)0.0275 (2)0.0232 (3)0.00135 (18)0.00190 (18)0.00455 (18)
Rh10.0203 (3)0.0237 (3)0.0200 (3)0.0009 (2)0.0018 (2)0.0007 (2)
C10.031 (4)0.029 (4)0.024 (4)0.000 (3)0.007 (3)0.004 (3)
C20.028 (4)0.027 (4)0.022 (4)0.004 (3)0.003 (3)0.004 (3)
C30.030 (4)0.020 (4)0.038 (4)0.005 (3)0.006 (3)0.002 (3)
C40.028 (4)0.024 (4)0.042 (5)0.003 (3)0.006 (3)0.008 (3)
C50.025 (4)0.034 (4)0.022 (4)0.004 (3)0.001 (3)0.004 (3)
C60.025 (4)0.025 (4)0.017 (4)0.002 (3)0.006 (3)0.003 (3)
C70.024 (4)0.029 (4)0.034 (4)0.005 (3)0.001 (3)0.002 (3)
C80.029 (4)0.026 (4)0.031 (4)0.002 (3)0.006 (3)0.005 (3)
Geometric parameters (Å, º) top
I1—Rh12.6975 (7)C1—C81.509 (9)
I1—Rh1i2.7072 (7)C2—C31.510 (9)
Rh1—Rh1i2.9612 (11)C3—C41.560 (9)
Rh1—C12.115 (6)C4—C51.492 (9)
Rh1—C22.122 (6)C5—C61.392 (9)
Rh1—C52.119 (7)C6—C71.526 (9)
Rh1—C62.121 (6)C7—C81.532 (9)
C1—C21.413 (9)
Rh1—I1—Rh1i66.45 (2)C6—Rh1—I1164.61 (18)
I1—Rh1—I1i85.13 (2)C6—Rh1—Rh1i136.51 (18)
I1i—Rh1—Rh1i56.621 (18)C6—Rh1—C290.3 (2)
I1—Rh1—Rh1i56.933 (19)C2—C1—Rh170.8 (4)
C1—Rh1—I1i165.07 (19)C2—C1—C8124.6 (6)
C1—Rh1—I192.3 (2)C8—C1—Rh1112.6 (4)
C1—Rh1—Rh1i132.91 (19)C1—C2—Rh170.3 (4)
C1—Rh1—C239.0 (2)C1—C2—C3122.2 (6)
C1—Rh1—C597.7 (3)C3—C2—Rh1114.2 (5)
C1—Rh1—C681.1 (3)C2—C3—C4111.4 (5)
C2—Rh1—I1i155.75 (18)C5—C4—C3113.4 (5)
C2—Rh1—I193.32 (18)C4—C5—Rh1111.4 (5)
C2—Rh1—Rh1i102.57 (18)C6—C5—Rh170.9 (4)
C5—Rh1—I1157.07 (18)C6—C5—C4124.1 (6)
C5—Rh1—I1i90.08 (18)C5—C6—Rh170.8 (4)
C5—Rh1—Rh1i102.03 (18)C5—C6—C7123.7 (6)
C5—Rh1—C282.0 (3)C7—C6—Rh1114.5 (4)
C5—Rh1—C638.3 (2)C6—C7—C8111.9 (5)
C6—Rh1—I1i97.57 (17)C1—C8—C7112.7 (5)
Symmetry code: (i) x+1, y, z+1/2.
Di-µ-iodido-bis{[(1,2,5,6-η)-cycloocta-1,4-diene]rhodium(I)} (P) top
Crystal data top
[Rh2I2(C8H12)2]F(000) = 1264
Mr = 675.97Dx = 2.621 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 10.4505 (5) ÅCell parameters from 9797 reflections
b = 19.390 (1) Åθ = 2.6–26.4°
c = 8.6271 (4) ŵ = 5.52 mm1
β = 101.523 (2)°T = 100 K
V = 1712.92 (14) Å3Block, yellow-orange
Z = 40.14 × 0.14 × 0.09 mm
Data collection top
Nonius Kappa APEXII
diffractometer
3519 independent reflections
Radiation source: sealed tube, fine-focus2922 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.051
Detector resolution: 7.9 pixels mm-1θmax = 26.4°, θmin = 2.0°
ω and φ scansh = 1313
Absorption correction: multi-scan
(SADABS; Krause et al., 2015)
k = 2424
Tmin = 0.057, Tmax = 0.093l = 910
38760 measured reflections
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.025Hydrogen site location: mixed
wR(F2) = 0.055H atoms treated by a mixture of independent and constrained refinement
S = 1.07 w = 1/[σ2(Fo2) + (0.0284P)2]
where P = (Fo2 + 2Fc2)/3
3519 reflections(Δ/σ)max = 0.001
205 parametersΔρmax = 1.26 e Å3
8 restraintsΔρmin = 0.67 e Å3
Special details top

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) top
xyzUiso*/Ueq
I10.73024 (3)0.56233 (2)0.46409 (3)0.02018 (8)
I20.89372 (2)0.46580 (2)0.19408 (3)0.02188 (8)
Rh10.80485 (3)0.42940 (2)0.45350 (4)0.01765 (9)
Rh20.72305 (3)0.57016 (2)0.14928 (4)0.01730 (9)
C10.7956 (4)0.3230 (2)0.3955 (5)0.0205 (9)
H10.778 (4)0.318 (2)0.280 (2)0.025*
C20.9215 (4)0.3392 (2)0.4781 (5)0.0229 (9)
H20.990 (3)0.346 (2)0.416 (4)0.027*
C30.9741 (4)0.3226 (2)0.6498 (5)0.0253 (10)
H3A1.0598150.3455830.6834850.030*
H3B0.9884540.2722700.6608750.030*
C40.8836 (4)0.3453 (2)0.7597 (5)0.0261 (10)
H4A0.8276460.3060030.7768780.031*
H4B0.9370290.3585490.8635190.031*
C50.7978 (4)0.4056 (2)0.6927 (5)0.0241 (10)
H50.814 (4)0.4466 (15)0.756 (5)0.029*
C60.6732 (4)0.3985 (2)0.5982 (5)0.0198 (9)
H60.607 (3)0.4340 (16)0.602 (5)0.024*
C70.6093 (4)0.3303 (2)0.5424 (5)0.0234 (9)
H7A0.5290710.3391820.4621280.028*
H7B0.5834540.3065260.6329500.028*
C80.6995 (4)0.2832 (2)0.4711 (5)0.0240 (9)
H8A0.7483120.2531060.5552560.029*
H8B0.6459110.2532370.3903850.029*
C90.6610 (4)0.5469 (2)0.0943 (5)0.0206 (9)
H90.679 (4)0.4967 (11)0.103 (5)0.025*
C100.7642 (4)0.5945 (2)0.0773 (5)0.0208 (9)
H100.847 (3)0.5720 (19)0.087 (5)0.025*
C110.7443 (4)0.6700 (2)0.1207 (5)0.0247 (10)
H11A0.6651440.6751010.2047670.030*
H11B0.8199210.6869150.1629120.030*
C120.7293 (4)0.7139 (2)0.0242 (5)0.0237 (9)
H12A0.8166050.7298100.0791900.028*
H12B0.6762060.7552120.0127300.028*
C130.6659 (4)0.6751 (2)0.1393 (5)0.0228 (9)
H130.685 (4)0.693 (2)0.250 (3)0.027*
C140.5529 (4)0.6343 (2)0.0998 (5)0.0210 (9)
H140.501 (3)0.626 (2)0.181 (4)0.025*
C150.4755 (4)0.6267 (2)0.0676 (5)0.0240 (9)
H15A0.4857980.6690820.1280310.029*
H15B0.3817410.6217030.0646950.029*
C160.5200 (4)0.5641 (2)0.1526 (5)0.0233 (9)
H16A0.4661460.5236460.1368710.028*
H16B0.5049850.5737090.2675010.028*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
I10.02462 (15)0.01759 (15)0.01827 (15)0.00106 (11)0.00414 (11)0.00015 (11)
I20.02106 (15)0.02275 (16)0.02346 (15)0.00440 (11)0.00840 (11)0.00442 (12)
Rh10.01825 (17)0.01641 (17)0.01870 (17)0.00044 (13)0.00467 (13)0.00062 (13)
Rh20.01825 (17)0.01664 (17)0.01712 (17)0.00074 (13)0.00379 (13)0.00049 (13)
C10.028 (2)0.014 (2)0.021 (2)0.0024 (17)0.0100 (18)0.0021 (18)
C20.024 (2)0.018 (2)0.029 (2)0.0044 (18)0.0087 (18)0.0019 (19)
C30.021 (2)0.026 (2)0.029 (2)0.0061 (18)0.0056 (18)0.004 (2)
C40.032 (3)0.022 (2)0.023 (2)0.0001 (19)0.0030 (19)0.0015 (19)
C50.033 (3)0.021 (2)0.019 (2)0.001 (2)0.0093 (19)0.0014 (19)
C60.019 (2)0.019 (2)0.022 (2)0.0040 (17)0.0069 (17)0.0012 (18)
C70.021 (2)0.024 (2)0.026 (2)0.0016 (18)0.0056 (18)0.0011 (19)
C80.028 (2)0.020 (2)0.024 (2)0.0007 (18)0.0052 (18)0.0011 (18)
C90.026 (2)0.023 (2)0.013 (2)0.0013 (18)0.0045 (17)0.0008 (18)
C100.023 (2)0.025 (2)0.018 (2)0.0030 (18)0.0099 (17)0.0014 (18)
C110.027 (2)0.025 (2)0.023 (2)0.0018 (19)0.0065 (18)0.0073 (19)
C120.029 (2)0.018 (2)0.022 (2)0.0015 (18)0.0003 (18)0.0016 (18)
C130.029 (2)0.017 (2)0.021 (2)0.0051 (18)0.0001 (18)0.0013 (18)
C140.024 (2)0.017 (2)0.022 (2)0.0081 (18)0.0060 (18)0.0019 (18)
C150.024 (2)0.020 (2)0.028 (2)0.0031 (18)0.0020 (19)0.0023 (19)
C160.026 (2)0.023 (2)0.019 (2)0.0014 (18)0.0011 (18)0.0002 (18)
Geometric parameters (Å, º) top
I1—Rh12.6998 (4)C2—C31.509 (6)
I1—Rh22.7061 (4)C3—C41.531 (6)
I2—Rh12.6833 (4)C4—C51.516 (6)
I2—Rh22.6738 (4)C5—C61.398 (6)
Rh1—C12.120 (4)C6—C71.516 (6)
Rh1—C22.117 (4)C7—C81.526 (5)
Rh1—C52.131 (4)C9—C101.404 (6)
Rh1—C62.120 (4)C9—C161.496 (6)
Rh2—C92.120 (4)C10—C111.514 (6)
Rh2—C102.137 (4)C11—C121.547 (6)
Rh2—C132.117 (4)C12—C131.501 (6)
Rh2—C142.142 (4)C13—C141.405 (6)
C1—C21.400 (6)C14—C151.514 (6)
C1—C81.514 (6)C15—C161.538 (6)
Rh1—I1—Rh288.274 (12)C2—C1—Rh170.6 (2)
Rh2—I2—Rh189.290 (12)C2—C1—C8122.2 (4)
I2—Rh1—I185.839 (12)C8—C1—Rh1113.4 (3)
C1—Rh1—I1159.56 (12)C1—C2—Rh170.8 (2)
C1—Rh1—I293.80 (11)C1—C2—C3124.9 (4)
C1—Rh1—C590.54 (16)C3—C2—Rh1111.4 (3)
C2—Rh1—I1161.67 (12)C2—C3—C4113.4 (3)
C2—Rh1—I290.72 (11)C5—C4—C3112.2 (3)
C2—Rh1—C138.60 (16)C4—C5—Rh1113.8 (3)
C2—Rh1—C581.67 (16)C6—C5—Rh170.4 (2)
C2—Rh1—C697.81 (16)C6—C5—C4123.8 (4)
C5—Rh1—I196.17 (12)C5—C6—Rh171.2 (2)
C5—Rh1—I2161.76 (12)C5—C6—C7124.8 (4)
C6—Rh1—I191.38 (11)C7—C6—Rh1110.9 (3)
C6—Rh1—I2159.83 (11)C6—C7—C8112.4 (3)
C6—Rh1—C181.93 (16)C1—C8—C7112.6 (3)
C6—Rh1—C538.41 (16)C10—C9—Rh271.4 (2)
I2—Rh2—I185.902 (12)C10—C9—C16125.0 (4)
C9—Rh2—I1157.60 (12)C16—C9—Rh2111.8 (3)
C9—Rh2—I292.63 (12)C9—C10—Rh270.1 (2)
C9—Rh2—C1038.52 (16)C9—C10—C11123.0 (4)
C9—Rh2—C1481.27 (16)C11—C10—Rh2113.4 (3)
C10—Rh2—I1163.81 (12)C10—C11—C12111.3 (3)
C10—Rh2—I292.82 (11)C13—C12—C11112.8 (3)
C10—Rh2—C1489.99 (16)C12—C13—Rh2110.5 (3)
C13—Rh2—I192.62 (12)C14—C13—Rh271.7 (2)
C13—Rh2—I2155.19 (12)C14—C13—C12125.6 (4)
C13—Rh2—C997.80 (16)C13—C14—Rh269.8 (2)
C13—Rh2—C1081.78 (16)C13—C14—C15123.3 (4)
C13—Rh2—C1438.53 (16)C15—C14—Rh2113.5 (3)
C14—Rh2—I195.06 (11)C14—C15—C16112.1 (3)
C14—Rh2—I2166.28 (11)C9—C16—C15112.7 (3)
 

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