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In the title compound, [Rh22-CH3COO)4(C15H15N3O2S)2]·2C2H3N, the dirhodium tetra­acetate complex lies on a centre of inversion. The conformation of the complex differs from that in a previously reported 1:2 chloro­form solvate.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806025311/ya2019sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806025311/ya2019Isup2.hkl
Contains datablock I

CCDC reference: 618354

Key indicators

  • Single-crystal X-ray study
  • T = 180 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.028
  • wR factor = 0.061
  • Data-to-parameter ratio = 15.0

checkCIF/PLATON results

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Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT230_ALERT_2_C Hirshfeld Test Diff for O1 - C4_a .. 6.44 su PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C1S PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 3
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: APEX2 (Bruker Nonius, 2004); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Tetra-µ2-acetato-bis{1-[5-(dimethylamino)naphthylsulfonyl]imidazole- κN3]rhodium} (Rh—Rh) acetonitrile disolvate top
Crystal data top
[Rh2(C2H3O2)4(C15H15N3O2S)2]·2C2H3NF(000) = 1148
Mr = 1126.82Dx = 1.617 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 5860 reflections
a = 8.8710 (9) Åθ = 2.5–25.8°
b = 25.256 (3) ŵ = 0.87 mm1
c = 10.9402 (10) ÅT = 180 K
β = 109.195 (4)°Block, red
V = 2314.8 (4) Å30.15 × 0.12 × 0.10 mm
Z = 2
Data collection top
Bruker Nonius X8 APEX-II CCD area-detector
diffractometer
4539 independent reflections
Radiation source: fine-focus sealed tube3604 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
thin–slice ω and φ scansθmax = 26.4°, θmin = 3.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
h = 119
Tmin = 0.807, Tmax = 0.918k = 3130
22091 measured reflectionsl = 1313
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)] = 0.028Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.061H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0274P)2]
where P = (Fo2 + 2Fc2)/3
4539 reflections(Δ/σ)max = 0.002
303 parametersΔρmax = 0.34 e Å3
0 restraintsΔρmin = 0.50 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.

Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane)

5.7173 (0.0070) x + 11.7939 (0.0230) y - 8.5737 (0.0076) z = 4.8492 (0.0184)

* -0.0018 (0.0012) C1 * 0.0000 (0.0013) C2 * -0.0010 (0.0013) C3 * 0.0011 (0.0012) N1 * 0.0017 (0.0013) N2

Rms deviation of fitted atoms = 0.0013

2.7127 (0.0091) x - 2.1030 (0.0541) y + 8.6994 (0.0089) z = 4.6822 (0.0297)

Angle to previous plane (with approximate e.s.d.) = 65.42 (0.09)

* 0.0045 (0.0007) Rh1 * -0.0022 (0.0004) O1 * -0.0026 (0.0004) O2 * 0.0003 (0.0000) C4

Rms deviation of fitted atoms = 0.0028

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*/Ueq
Rh10.47076 (2)0.544476 (7)0.523569 (16)0.01554 (7)
S10.09853 (7)0.73740 (2)0.51757 (5)0.01902 (15)
O10.65992 (19)0.56821 (6)0.46955 (14)0.0206 (4)
O20.28461 (18)0.51541 (6)0.57378 (14)0.0222 (4)
O30.3251 (2)0.55113 (6)0.33604 (14)0.0228 (4)
O40.61765 (19)0.53225 (6)0.70848 (14)0.0198 (4)
O50.02361 (19)0.70686 (7)0.42744 (14)0.0247 (4)
O60.14766 (19)0.78571 (6)0.47560 (14)0.0242 (4)
N10.2579 (2)0.69612 (7)0.56388 (16)0.0157 (4)
N20.4089 (2)0.62632 (7)0.56846 (17)0.0176 (4)
N30.0212 (2)0.68135 (8)1.07099 (18)0.0236 (5)
C10.2725 (3)0.64850 (9)0.5084 (2)0.0180 (5)
H1A0.19310.63370.43560.022*
C20.3972 (3)0.70353 (9)0.6671 (2)0.0191 (5)
H2A0.42330.73280.72470.023*
C30.4884 (3)0.66046 (9)0.6688 (2)0.0199 (6)
H3A0.59160.65440.72950.024*
C40.2623 (3)0.46587 (10)0.5691 (2)0.0212 (6)
C50.1271 (3)0.44573 (10)0.6120 (3)0.0326 (7)
H5A0.14310.40800.63320.049*
H5B0.02560.45070.54190.049*
H5C0.12510.46550.68850.049*
C60.3139 (3)0.51219 (10)0.2609 (2)0.0201 (5)
C70.2045 (3)0.51824 (10)0.1234 (2)0.0291 (6)
H7A0.23790.49390.06730.044*
H7B0.20960.55470.09460.044*
H7C0.09480.51000.11870.044*
C80.0675 (3)0.74735 (9)0.6668 (2)0.0173 (5)
C90.0978 (3)0.79692 (9)0.7174 (2)0.0217 (6)
H9A0.12550.82450.66960.026*
C100.0879 (3)0.80713 (10)0.8406 (2)0.0252 (6)
H10A0.10200.84210.87430.030*
C110.0579 (3)0.76654 (9)0.9116 (2)0.0219 (6)
H11A0.05540.77360.99620.026*
C120.0305 (3)0.71431 (9)0.8634 (2)0.0182 (5)
C130.0014 (3)0.67173 (10)0.9391 (2)0.0209 (6)
C140.0587 (3)0.62473 (10)0.8790 (2)0.0249 (6)
H14A0.08830.59740.92630.030*
C150.0743 (3)0.61657 (10)0.7482 (2)0.0281 (6)
H15A0.11680.58400.70820.034*
C160.0301 (3)0.65412 (10)0.6773 (2)0.0246 (6)
H16A0.03550.64680.59080.030*
C170.0240 (3)0.70419 (9)0.7333 (2)0.0173 (5)
C180.0549 (3)0.64434 (10)1.1342 (2)0.0276 (6)
H18A0.16610.63891.07980.041*
H18B0.05190.65881.21820.041*
H18C0.00210.61051.14730.041*
C190.1852 (3)0.69225 (11)1.1522 (2)0.0345 (7)
H19A0.23650.71511.10500.052*
H19B0.24430.65891.17440.052*
H19C0.18490.71011.23160.052*
N1S0.5885 (4)0.56774 (13)1.0778 (3)0.0827 (11)
C1S0.4868 (4)0.57100 (13)0.9847 (3)0.0474 (8)
C2S0.3547 (4)0.57480 (14)0.8656 (3)0.0610 (10)
H2S10.26720.55220.87070.091*
H2S20.38900.56320.79340.091*
H2S30.31810.61160.85170.091*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.01835 (12)0.01179 (12)0.01602 (10)0.00092 (9)0.00504 (8)0.00012 (7)
S10.0196 (3)0.0207 (4)0.0165 (3)0.0038 (3)0.0056 (3)0.0012 (2)
O10.0253 (10)0.0151 (9)0.0232 (8)0.0005 (8)0.0106 (8)0.0002 (7)
O20.0221 (10)0.0188 (10)0.0281 (9)0.0002 (8)0.0116 (8)0.0003 (7)
O30.0259 (10)0.0176 (10)0.0199 (8)0.0048 (8)0.0008 (8)0.0012 (7)
O40.0243 (10)0.0152 (10)0.0182 (8)0.0003 (8)0.0047 (8)0.0011 (7)
O50.0205 (10)0.0323 (11)0.0181 (8)0.0016 (8)0.0020 (7)0.0022 (7)
O60.0313 (11)0.0192 (10)0.0233 (9)0.0039 (8)0.0104 (8)0.0061 (7)
N10.0147 (11)0.0166 (11)0.0150 (9)0.0029 (9)0.0039 (9)0.0021 (8)
N20.0221 (12)0.0149 (11)0.0159 (9)0.0007 (10)0.0066 (9)0.0002 (8)
N30.0228 (12)0.0303 (13)0.0194 (10)0.0050 (10)0.0090 (9)0.0015 (9)
C10.0221 (15)0.0153 (14)0.0183 (11)0.0024 (11)0.0091 (11)0.0019 (10)
C20.0220 (15)0.0182 (14)0.0152 (11)0.0020 (12)0.0037 (11)0.0043 (10)
C30.0198 (14)0.0202 (15)0.0179 (12)0.0020 (12)0.0039 (11)0.0005 (10)
C40.0210 (15)0.0242 (16)0.0150 (11)0.0044 (12)0.0014 (11)0.0009 (10)
C50.0306 (17)0.0318 (17)0.0397 (15)0.0064 (13)0.0173 (14)0.0009 (12)
C60.0177 (14)0.0203 (15)0.0230 (12)0.0037 (12)0.0076 (11)0.0022 (11)
C70.0350 (17)0.0273 (16)0.0185 (12)0.0031 (13)0.0000 (12)0.0003 (11)
C80.0144 (13)0.0185 (14)0.0192 (12)0.0042 (11)0.0060 (10)0.0023 (10)
C90.0193 (14)0.0203 (15)0.0277 (13)0.0006 (11)0.0106 (11)0.0001 (11)
C100.0237 (15)0.0215 (15)0.0323 (14)0.0009 (12)0.0116 (12)0.0091 (11)
C110.0194 (14)0.0252 (15)0.0241 (12)0.0028 (12)0.0112 (11)0.0076 (11)
C120.0124 (13)0.0208 (14)0.0227 (12)0.0020 (11)0.0075 (11)0.0025 (10)
C130.0159 (14)0.0261 (15)0.0217 (12)0.0020 (11)0.0073 (11)0.0010 (11)
C140.0273 (15)0.0218 (15)0.0264 (13)0.0041 (12)0.0099 (12)0.0020 (11)
C150.0349 (17)0.0195 (15)0.0282 (14)0.0092 (13)0.0079 (13)0.0063 (11)
C160.0300 (16)0.0236 (15)0.0213 (12)0.0042 (12)0.0097 (12)0.0053 (11)
C170.0138 (13)0.0190 (14)0.0186 (11)0.0009 (11)0.0048 (10)0.0024 (10)
C180.0322 (16)0.0281 (16)0.0256 (13)0.0035 (13)0.0136 (12)0.0024 (11)
C190.0281 (17)0.0463 (19)0.0266 (14)0.0050 (14)0.0056 (13)0.0027 (12)
N1S0.070 (3)0.065 (2)0.095 (3)0.018 (2)0.003 (2)0.010 (2)
C1S0.049 (2)0.035 (2)0.060 (2)0.0073 (18)0.021 (2)0.0056 (17)
C2S0.068 (3)0.075 (3)0.048 (2)0.002 (2)0.030 (2)0.0084 (18)
Geometric parameters (Å, º) top
Rh1—Rh1i2.3997 (4)C7—H7A0.980
Rh1—O12.0436 (16)C7—H7B0.980
Rh1—O22.0406 (15)C7—H7C0.980
Rh1—O32.0406 (15)C8—C91.360 (3)
Rh1—O42.0378 (15)C8—C171.432 (3)
Rh1—N22.2343 (18)C9—C101.403 (3)
S1—O61.4217 (16)C9—H9A0.950
S1—O51.4277 (17)C10—C111.365 (3)
S1—N11.6948 (19)C10—H10A0.950
S1—C81.761 (2)C11—C121.412 (3)
O1—C4i1.260 (3)C11—H11A0.950
O2—C41.265 (3)C12—C171.429 (3)
O3—C61.265 (3)C12—C131.441 (3)
O4—C6i1.267 (3)C13—C141.371 (3)
N1—C11.372 (3)C14—C151.408 (3)
N1—C21.385 (3)C14—H14A0.950
N2—C11.299 (3)C15—C161.362 (3)
N2—C31.391 (3)C15—H15A0.950
N3—C131.411 (3)C16—C171.418 (3)
N3—C181.454 (3)C16—H16A0.950
N3—C191.460 (3)C18—H18A0.980
C1—H1A0.950C18—H18B0.980
C2—C31.352 (3)C18—H18C0.980
C2—H2A0.950C19—H19A0.980
C3—H3A0.950C19—H19B0.980
C4—O1i1.260 (3)C19—H19C0.980
C4—C51.512 (3)N1S—C1S1.119 (4)
C5—H5A0.980C1S—C2S1.441 (4)
C5—H5B0.980C2S—H2S10.980
C5—H5C0.980C2S—H2S20.980
C6—O4i1.268 (3)C2S—H2S30.980
C6—C71.506 (3)
O4—Rh1—O289.32 (6)C6—C7—H7A109.5
O4—Rh1—O3175.93 (6)C6—C7—H7B109.5
O2—Rh1—O389.95 (6)H7A—C7—H7B109.5
O4—Rh1—O190.79 (6)C6—C7—H7C109.5
O2—Rh1—O1175.91 (6)H7A—C7—H7C109.5
O3—Rh1—O189.65 (6)H7B—C7—H7C109.5
O4—Rh1—N292.58 (6)C9—C8—C17123.0 (2)
O2—Rh1—N289.70 (7)C9—C8—S1116.03 (17)
O3—Rh1—N291.41 (6)C17—C8—S1120.84 (17)
O1—Rh1—N294.39 (7)C8—C9—C10119.6 (2)
O4—Rh1—Rh1i87.63 (4)C8—C9—H9A120.2
O2—Rh1—Rh1i88.41 (5)C10—C9—H9A120.2
O3—Rh1—Rh1i88.35 (4)C11—C10—C9119.6 (2)
O1—Rh1—Rh1i87.50 (5)C11—C10—H10A120.2
N2—Rh1—Rh1i178.10 (5)C9—C10—H10A120.2
O6—S1—O5118.96 (10)C10—C11—C12122.1 (2)
O6—S1—N1108.07 (10)C10—C11—H11A119.0
O5—S1—N1104.09 (10)C12—C11—H11A119.0
O6—S1—C8109.57 (10)C11—C12—C17119.0 (2)
O5—S1—C8113.76 (10)C11—C12—C13121.6 (2)
N1—S1—C8100.38 (10)C17—C12—C13119.2 (2)
C4i—O1—Rh1119.28 (15)C14—C13—N3123.0 (2)
C4—O2—Rh1118.34 (15)C14—C13—C12118.9 (2)
C6—O3—Rh1118.54 (15)N3—C13—C12118.1 (2)
C6i—O4—Rh1119.40 (14)C13—C14—C15120.7 (2)
C1—N1—C2106.88 (19)C13—C14—H14A119.6
C1—N1—S1126.70 (16)C15—C14—H14A119.6
C2—N1—S1126.41 (15)C16—C15—C14121.8 (2)
C1—N2—C3106.15 (19)C16—C15—H15A119.1
C1—N2—Rh1122.89 (15)C14—C15—H15A119.1
C3—N2—Rh1130.48 (16)C15—C16—C17119.7 (2)
C13—N3—C18116.35 (19)C15—C16—H16A120.2
C13—N3—C19115.62 (18)C17—C16—H16A120.2
C18—N3—C19110.94 (19)C16—C17—C12119.1 (2)
N2—C1—N1111.2 (2)C16—C17—C8124.67 (19)
N2—C1—H1A124.4C12—C17—C8116.1 (2)
N1—C1—H1A124.4N3—C18—H18A109.5
C3—C2—N1105.8 (2)N3—C18—H18B109.5
C3—C2—H2A127.1H18A—C18—H18B109.5
N1—C2—H2A127.1N3—C18—H18C109.5
C2—C3—N2110.0 (2)H18A—C18—H18C109.5
C2—C3—H3A125.0H18B—C18—H18C109.5
N2—C3—H3A125.0N3—C19—H19A109.5
O1i—C4—O2126.4 (2)N3—C19—H19B109.5
O1i—C4—C5116.9 (2)H19A—C19—H19B109.5
O2—C4—C5116.7 (2)N3—C19—H19C109.5
C4—C5—H5A109.5H19A—C19—H19C109.5
C4—C5—H5B109.5H19B—C19—H19C109.5
H5A—C5—H5B109.5N1S—C1S—C2S179.3 (4)
C4—C5—H5C109.5C1S—C2S—H2S1109.5
H5A—C5—H5C109.5C1S—C2S—H2S2109.5
H5B—C5—H5C109.5H2S1—C2S—H2S2109.5
O3—C6—O4i126.0 (2)C1S—C2S—H2S3109.5
O3—C6—C7117.2 (2)H2S1—C2S—H2S3109.5
O4i—C6—C7116.7 (2)H2S2—C2S—H2S3109.5
O4—Rh1—O1—C4i88.74 (16)Rh1—O2—C4—O1i3.4 (3)
O3—Rh1—O1—C4i87.22 (16)Rh1—O2—C4—C5177.71 (16)
N2—Rh1—O1—C4i178.61 (16)Rh1—O3—C6—O4i2.1 (3)
Rh1i—Rh1—O1—C4i1.15 (16)Rh1—O3—C6—C7179.56 (15)
O4—Rh1—O2—C485.86 (16)O6—S1—C8—C91.5 (2)
O3—Rh1—O2—C490.14 (16)O5—S1—C8—C9137.40 (18)
N2—Rh1—O2—C4178.45 (16)N1—S1—C8—C9112.04 (19)
Rh1i—Rh1—O2—C41.79 (16)O6—S1—C8—C17177.23 (18)
O2—Rh1—O3—C689.91 (16)O5—S1—C8—C1746.9 (2)
O1—Rh1—O3—C686.01 (16)N1—S1—C8—C1763.7 (2)
N2—Rh1—O3—C6179.61 (16)C17—C8—C9—C100.5 (4)
Rh1i—Rh1—O3—C61.50 (16)S1—C8—C9—C10175.12 (18)
O2—Rh1—O4—C6i88.39 (16)C8—C9—C10—C114.1 (4)
O1—Rh1—O4—C6i87.52 (16)C9—C10—C11—C122.3 (4)
N2—Rh1—O4—C6i178.06 (16)C10—C11—C12—C174.0 (4)
Rh1i—Rh1—O4—C6i0.05 (16)C10—C11—C12—C13179.9 (2)
O6—S1—N1—C1116.54 (18)C18—N3—C13—C1414.6 (3)
O5—S1—N1—C110.8 (2)C19—N3—C13—C14118.2 (3)
C8—S1—N1—C1128.75 (19)C18—N3—C13—C12162.4 (2)
O6—S1—N1—C265.04 (19)C19—N3—C13—C1264.8 (3)
O5—S1—N1—C2167.59 (17)C11—C12—C13—C14166.8 (2)
C8—S1—N1—C249.7 (2)C17—C12—C13—C149.0 (3)
O4—Rh1—N2—C1150.26 (16)C11—C12—C13—N310.3 (3)
O2—Rh1—N2—C160.95 (16)C17—C12—C13—N3173.8 (2)
O3—Rh1—N2—C128.99 (16)N3—C13—C14—C15178.0 (2)
O1—Rh1—N2—C1118.75 (16)C12—C13—C14—C155.0 (4)
O4—Rh1—N2—C320.62 (19)C13—C14—C15—C161.5 (4)
O2—Rh1—N2—C3109.93 (19)C14—C15—C16—C174.0 (4)
O3—Rh1—N2—C3160.12 (19)C15—C16—C17—C120.2 (4)
O1—Rh1—N2—C370.36 (19)C15—C16—C17—C8177.4 (2)
C3—N2—C1—N10.3 (2)C11—C12—C17—C16169.3 (2)
Rh1—N2—C1—N1173.14 (13)C13—C12—C17—C166.6 (3)
C2—N1—C1—N20.3 (2)C11—C12—C17—C88.1 (3)
S1—N1—C1—N2178.96 (14)C13—C12—C17—C8175.9 (2)
C1—N1—C2—C30.1 (2)C9—C8—C17—C16170.7 (2)
S1—N1—C2—C3178.77 (16)S1—C8—C17—C1613.9 (3)
N1—C2—C3—N20.1 (2)C9—C8—C17—C126.6 (3)
C1—N2—C3—C20.3 (2)S1—C8—C17—C12168.83 (17)
Rh1—N2—C3—C2172.32 (14)
Symmetry code: (i) x+1, y+1, z+1.
 

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