Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802013466/cm6013sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802013466/cm6013Isup2.hkl |
CCDC reference: 193724
Data collection: COLLECT (Nonius, 1999); cell refinement: DIRAX (Duisenberg, 1992); data reduction: EVALCCD (Duisenberg, 1998) and DREAD (Blessing, 1987); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976).
[Rh(CH3)(NH3)5]0.73[RhCl(NH3)5]2.27(S2O6)3 | F(000) = 960 |
Mr = 1135.58 | Dx = 2.258 Mg m−3 |
Monoclinic, Im | Mo Kα radiation, λ = 0.71073 Å |
a = 6.271 (2) Å | Cell parameters from 474 reflections |
b = 27.205 (3) Å | θ = 4.4–31.0° |
c = 9.871 (2) Å | µ = 2.11 mm−1 |
β = 97.29 (1)° | T = 122 K |
V = 1670.4 Å3 | Rod, colourless |
Z = 2 | 0.37 × 0.17 × 0.08 mm |
Nonius KappaCCD diffractometer | 7322 independent reflections |
Radiation source: fine-focus sealed tube | 7148 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.057 |
Detector resolution: 9 pixels mm-1 | θmax = 35.0°, θmin = 2.2° |
θ and φ scans | h = −10→10 |
Absorption correction: integration Gaussian integration (Coppens, 1970) | k = −43→43 |
Tmin = 0.542, Tmax = 0.898 | l = −15→15 |
34422 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.036 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.102 | w = 1/[σ2(Fo2) + (0.0598P)2 + 6.9449P] where P = (Fo2 + 2Fc2)/3 |
S = 1.07 | (Δ/σ)max = 0.023 |
7322 reflections | Δρmax = 3.30 e Å−3 |
225 parameters | Δρmin = −1.68 e Å−3 |
4 restraints | Absolute structure: Flack (1983), 0000 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.43 (3) |
Experimental. Gaussian integration (Coppens, 1970) |
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. |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Rh2 | 0.96197 (3) | 0.166778 (9) | 0.62172 (2) | 0.01111 (5) | |
N21 | 0.8546 (6) | 0.11675 (12) | 0.7539 (3) | 0.0144 (6) | |
H21A | 0.9600 | 0.0959 | 0.7826 | 0.022* | |
H21B | 0.7435 | 0.1002 | 0.7111 | 0.022* | |
H21C | 0.8137 | 0.1325 | 0.8253 | 0.022* | |
N22 | 1.2650 (7) | 0.15910 (15) | 0.7268 (4) | 0.0214 (7) | |
H22A | 1.2813 | 0.1801 | 0.7966 | 0.032* | |
H22B | 1.3627 | 0.1654 | 0.6712 | 0.032* | |
H22C | 1.2821 | 0.1285 | 0.7582 | 0.032* | |
N23 | 0.8991 (6) | 0.22508 (13) | 0.7440 (3) | 0.0167 (6) | |
H23A | 0.8660 | 0.2138 | 0.8233 | 0.025* | |
H23B | 0.7893 | 0.2424 | 0.7026 | 0.025* | |
H23C | 1.0149 | 0.2442 | 0.7588 | 0.025* | |
N24 | 1.0663 (6) | 0.21550 (15) | 0.4822 (4) | 0.0188 (6) | |
H24A | 1.1241 | 0.2418 | 0.5261 | 0.028* | |
H24B | 0.9552 | 0.2247 | 0.4224 | 0.028* | |
H24C | 1.1643 | 0.2009 | 0.4382 | 0.028* | |
N25 | 1.0187 (7) | 0.10934 (15) | 0.4902 (4) | 0.0203 (7) | |
H25A | 1.1585 | 0.1078 | 0.4828 | 0.030* | |
H25B | 0.9455 | 0.1147 | 0.4083 | 0.030* | |
H25C | 0.9762 | 0.0811 | 0.5235 | 0.030* | |
Cl | 0.61140 (19) | 0.17248 (4) | 0.50636 (11) | 0.02194 (19) | |
Rh1 | 0.48747 (5) | 0.0000 | 0.15369 (3) | 0.01348 (8) | |
N13 | 0.5745 (7) | 0.05419 (14) | 0.0245 (4) | 0.0195 (7) | |
H13A | 0.6521 | 0.0410 | −0.0357 | 0.029* | |
H13B | 0.6522 | 0.0770 | 0.0731 | 0.029* | |
H13C | 0.4568 | 0.0679 | −0.0196 | 0.029* | |
N12 | 0.4006 (8) | 0.05356 (17) | 0.2846 (4) | 0.0249 (8) | |
H12A | 0.3951 | 0.0826 | 0.2427 | 0.037* | |
H12B | 0.4972 | 0.0547 | 0.3588 | 0.037* | |
H12C | 0.2720 | 0.0465 | 0.3086 | 0.037* | |
Cl1 | 0.8391 (8) | 0.0000 | 0.2738 (5) | 0.0126 (12)* | 0.27 (1) |
C11 | 0.782 (3) | 0.0000 | 0.2567 (17) | 0.041 (3)* | 0.73 (2) |
N11 | 0.1657 (10) | 0.0000 | 0.0412 (6) | 0.0221 (10) | |
H11A | 0.1179 | 0.0308 | 0.0312 | 0.033* | 0.50 |
H11B | 0.0780 | −0.0173 | 0.0869 | 0.033* | 0.50 |
H11C | 0.1695 | −0.0134 | −0.0407 | 0.033* | 0.50 |
S3 | 0.5967 (3) | 0.0000 | 0.64904 (13) | 0.0166 (2) | |
S4 | 0.2697 (3) | 0.0000 | 0.68079 (18) | 0.0222 (3) | |
O32 | 0.6211 (6) | −0.04480 (10) | 0.5726 (3) | 0.0252 (7) | |
O31 | 0.7225 (8) | 0.0000 | 0.7845 (4) | 0.0180 (8) | |
O42 | 0.2457 (6) | 0.04457 (11) | 0.7579 (4) | 0.0270 (7) | |
O41 | 0.1538 (10) | 0.0000 | 0.5435 (6) | 0.0352 (14) | |
S1 | 0.82960 (19) | 0.17203 (3) | 0.12449 (10) | 0.01545 (17) | |
S2 | 1.15676 (19) | 0.16083 (3) | 0.09385 (12) | 0.01922 (19) | |
O11 | 0.7843 (6) | 0.13023 (11) | 0.2063 (3) | 0.0240 (6) | |
O12 | 0.8273 (5) | 0.21944 (10) | 0.1934 (3) | 0.0216 (5) | |
O13 | 0.7098 (6) | 0.17221 (11) | −0.0127 (3) | 0.0173 (6) | |
O21 | 1.2712 (8) | 0.16123 (12) | 0.2308 (4) | 0.0313 (9) | |
O22 | 1.2068 (5) | 0.20179 (11) | 0.0079 (4) | 0.0266 (6) | |
O23 | 1.1573 (5) | 0.11329 (11) | 0.0254 (4) | 0.0251 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Rh2 | 0.01615 (10) | 0.00997 (9) | 0.00688 (8) | 0.00083 (7) | 0.00018 (6) | 0.00031 (7) |
N21 | 0.0199 (13) | 0.0112 (11) | 0.0112 (12) | 0.0006 (10) | −0.0023 (10) | 0.0003 (9) |
N22 | 0.0223 (17) | 0.0257 (13) | 0.0162 (15) | −0.0033 (13) | 0.0020 (12) | −0.0041 (12) |
N23 | 0.0243 (15) | 0.0134 (12) | 0.0120 (13) | 0.0025 (10) | 0.0012 (10) | −0.0011 (10) |
N24 | 0.0219 (14) | 0.0225 (15) | 0.0122 (13) | −0.0033 (11) | 0.0024 (11) | 0.0009 (11) |
N25 | 0.0288 (17) | 0.0186 (14) | 0.0124 (13) | 0.0050 (12) | −0.0015 (11) | −0.0038 (10) |
Cl | 0.0217 (4) | 0.0251 (4) | 0.0188 (4) | 0.0006 (3) | 0.0016 (3) | 0.0014 (3) |
Rh1 | 0.02122 (18) | 0.01070 (14) | 0.00788 (13) | 0.000 | −0.00064 (12) | 0.000 |
N13 | 0.0298 (17) | 0.0141 (12) | 0.0137 (14) | −0.0009 (11) | −0.0004 (12) | 0.0003 (10) |
N12 | 0.036 (2) | 0.0239 (17) | 0.0136 (15) | 0.0077 (14) | 0.0006 (13) | −0.0024 (12) |
N11 | 0.026 (2) | 0.022 (2) | 0.018 (2) | 0.000 | 0.0019 (17) | 0.000 |
S3 | 0.0307 (6) | 0.0090 (4) | 0.0081 (4) | 0.000 | −0.0050 (4) | 0.000 |
S4 | 0.0227 (6) | 0.0124 (5) | 0.0282 (7) | 0.000 | −0.0102 (5) | 0.000 |
O32 | 0.0491 (19) | 0.0120 (11) | 0.0131 (11) | 0.0067 (11) | −0.0011 (11) | −0.0030 (8) |
O31 | 0.0231 (19) | 0.0192 (16) | 0.0101 (15) | 0.000 | −0.0048 (13) | 0.000 |
O42 | 0.0258 (14) | 0.0196 (13) | 0.0342 (17) | 0.0064 (10) | −0.0019 (12) | −0.0045 (11) |
O41 | 0.038 (3) | 0.0211 (19) | 0.039 (3) | 0.000 | −0.026 (2) | 0.000 |
S1 | 0.0246 (4) | 0.0104 (3) | 0.0101 (3) | 0.0018 (3) | −0.0026 (3) | −0.0004 (3) |
S2 | 0.0227 (4) | 0.0132 (3) | 0.0191 (4) | 0.0037 (3) | −0.0079 (3) | −0.0040 (3) |
O11 | 0.0409 (17) | 0.0160 (11) | 0.0141 (11) | −0.0033 (11) | −0.0001 (10) | −0.0007 (9) |
O12 | 0.0354 (15) | 0.0123 (10) | 0.0155 (11) | 0.0035 (9) | −0.0028 (10) | −0.0047 (8) |
O13 | 0.0215 (14) | 0.0201 (11) | 0.0085 (11) | 0.0034 (9) | −0.0051 (9) | −0.0011 (9) |
O21 | 0.038 (2) | 0.0246 (14) | 0.0260 (18) | 0.0045 (13) | −0.0175 (15) | −0.0053 (12) |
O22 | 0.0271 (14) | 0.0191 (12) | 0.0326 (16) | −0.0005 (10) | 0.0001 (12) | −0.0021 (11) |
O23 | 0.0262 (14) | 0.0160 (11) | 0.0302 (16) | 0.0074 (10) | −0.0074 (11) | −0.0073 (11) |
Rh2—N22 | 2.057 (4) | Rh1—N11 | 2.177 (6) |
Rh2—N21 | 2.057 (4) | Rh1—Cl1 | 2.368 (5) |
Rh2—N23 | 2.061 (4) | N13—H13A | 0.8900 |
Rh2—N24 | 2.076 (4) | N13—H13B | 0.8900 |
Rh2—N25 | 2.091 (4) | N13—H13C | 0.8900 |
Rh2—Cl | 2.3492 (12) | N12—H12A | 0.8900 |
N21—H21A | 0.8900 | N12—H12B | 0.8900 |
N21—H21B | 0.8900 | N12—H12C | 0.8900 |
N21—H21C | 0.8900 | N11—H11A | 0.8900 |
N22—H22A | 0.8900 | N11—H11B | 0.8900 |
N22—H22B | 0.8900 | N11—H11C | 0.8900 |
N22—H22C | 0.8900 | S3—O32 | 1.451 (3) |
N23—H23A | 0.8900 | S3—O31 | 1.463 (5) |
N23—H23B | 0.8900 | S3—S4 | 2.113 (3) |
N23—H23C | 0.8900 | S4—O42 | 1.450 (3) |
N24—H24A | 0.8900 | S4—O41 | 1.454 (5) |
N24—H24B | 0.8900 | S1—O11 | 1.444 (3) |
N24—H24C | 0.8900 | S1—O12 | 1.459 (3) |
N25—H25A | 0.8900 | S1—O13 | 1.463 (3) |
N25—H25B | 0.8900 | S1—S2 | 2.133 (2) |
N25—H25C | 0.8900 | S2—O21 | 1.448 (4) |
Rh1—C11 | 1.99 (2) | S2—O22 | 1.458 (4) |
Rh1—N12 | 2.066 (4) | S2—O23 | 1.460 (3) |
Rh1—N13 | 2.068 (4) | ||
N22—Rh2—N21 | 88.21 (15) | N12—Rh1—N13i | 179.34 (18) |
N22—Rh2—N23 | 90.91 (15) | N12—Rh1—N13 | 89.67 (16) |
N21—Rh2—N23 | 92.04 (14) | N13i—Rh1—N13 | 91.0 (2) |
N22—Rh2—N24 | 92.90 (16) | C11—Rh1—N11 | 180.0 (5) |
N21—Rh2—N24 | 177.83 (15) | N12—Rh1—N11 | 91.04 (17) |
N23—Rh2—N24 | 89.81 (15) | N13—Rh1—N11 | 89.17 (15) |
N22—Rh2—N25 | 91.04 (15) | N12—Rh1—Cl1 | 89.40 (15) |
N21—Rh2—N25 | 89.69 (14) | N13—Rh1—Cl1 | 90.40 (14) |
N23—Rh2—N25 | 177.43 (15) | N11—Rh1—Cl1 | 179.4 (2) |
N24—Rh2—N25 | 88.42 (16) | Rh1—N13—H13A | 109.5 |
N22—Rh2—Cl | 177.54 (13) | Rh1—N13—H13B | 109.5 |
N21—Rh2—Cl | 89.40 (10) | H13A—N13—H13B | 109.5 |
N23—Rh2—Cl | 89.79 (11) | Rh1—N13—H13C | 109.5 |
N24—Rh2—Cl | 89.46 (11) | H13A—N13—H13C | 109.5 |
N25—Rh2—Cl | 88.33 (11) | H13B—N13—H13C | 109.5 |
Rh2—N21—H21A | 109.5 | Rh1—N12—H12A | 109.5 |
Rh2—N21—H21B | 109.5 | Rh1—N12—H12B | 109.5 |
H21A—N21—H21B | 109.5 | H12A—N12—H12B | 109.5 |
Rh2—N21—H21C | 109.5 | Rh1—N12—H12C | 109.5 |
H21A—N21—H21C | 109.5 | H12A—N12—H12C | 109.5 |
H21B—N21—H21C | 109.5 | H12B—N12—H12C | 109.5 |
Rh2—N22—H22A | 109.5 | Rh1—N11—H11A | 109.5 |
Rh2—N22—H22B | 109.5 | Rh1—N11—H11B | 109.5 |
H22A—N22—H22B | 109.5 | H11A—N11—H11B | 109.5 |
Rh2—N22—H22C | 109.5 | Rh1—N11—H11C | 109.5 |
H22A—N22—H22C | 109.5 | H11A—N11—H11C | 109.5 |
H22B—N22—H22C | 109.5 | H11B—N11—H11C | 109.5 |
Rh2—N23—H23A | 109.5 | O32—S3—O32i | 114.2 (3) |
Rh2—N23—H23B | 109.5 | O32—S3—O31 | 113.23 (16) |
H23A—N23—H23B | 109.5 | O32—S3—S4 | 104.19 (18) |
Rh2—N23—H23C | 109.5 | O31—S3—S4 | 106.6 (2) |
H23A—N23—H23C | 109.5 | O42—S4—O42i | 113.5 (3) |
H23B—N23—H23C | 109.5 | O42—S4—O41 | 114.60 (19) |
Rh2—N24—H24A | 109.5 | O42—S4—S3 | 104.20 (15) |
Rh2—N24—H24B | 109.5 | O41—S4—S3 | 104.0 (3) |
H24A—N24—H24B | 109.5 | O11—S1—O12 | 114.93 (18) |
Rh2—N24—H24C | 109.5 | O11—S1—O13 | 113.95 (19) |
H24A—N24—H24C | 109.5 | O12—S1—O13 | 113.22 (17) |
H24B—N24—H24C | 109.5 | O11—S1—S2 | 103.18 (16) |
Rh2—N25—H25A | 109.5 | O12—S1—S2 | 105.00 (15) |
Rh2—N25—H25B | 109.5 | O13—S1—S2 | 105.03 (16) |
H25A—N25—H25B | 109.5 | O21—S2—O22 | 114.8 (2) |
Rh2—N25—H25C | 109.5 | O21—S2—O23 | 114.1 (2) |
H25A—N25—H25C | 109.5 | O22—S2—O23 | 113.2 (2) |
H25B—N25—H25C | 109.5 | O21—S2—S1 | 103.8 (2) |
C11—Rh1—N12 | 89.0 (3) | O22—S2—S1 | 104.77 (14) |
N12—Rh1—N12i | 89.7 (3) | O23—S2—S1 | 104.55 (15) |
C11—Rh1—N13i | 90.8 (3) | ||
O32—S3—S4—O42 | 179.6 (2) | O13—S1—S2—O21 | 179.5 (2) |
O31—S3—S4—O42 | 59.64 (17) | O11—S1—S2—O22 | 178.43 (19) |
O32—S3—S4—O42i | 60.3 (2) | O12—S1—S2—O22 | −60.8 (2) |
O32i—S3—S4—O41 | 60.01 (14) | O13—S1—S2—O22 | 58.8 (2) |
O31—S3—S4—O41 | 180.0 | O11—S1—S2—O23 | 59.1 (2) |
O11—S1—S2—O21 | −60.8 (2) | O12—S1—S2—O23 | 179.8 (2) |
O12—S1—S2—O21 | 59.9 (2) | O13—S1—S2—O23 | −60.5 (2) |
Symmetry code: (i) x, −y, z. |