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
Key indicators
- Single-crystal X-ray study
- T = 122 K
- Mean (S-O) = 0.004 Å
- H-atom completeness 96%
- Disorder in solvent or counterion
- R factor = 0.036
- wR factor = 0.102
- Data-to-parameter ratio = 32.5
checkCIF results
No syntax errors found
Alert Level B:
PLAT_111 Alert B ADDSYM detects (pseudo) centre of symmetry ... 92 Perc Fit
Author response: Structure solution and refinement has been attempted in several space groups. In P-1 this leads to disorder, unrealistic thermal parameters and an R1-factor of 0.1408 (for anisotropic thermal parameters, but without hydrogen atoms included). In P1 the solution is identical to the solution in Im and R1=0.0499 (for anisotropic thermal parameters, but without hydrogen atoms included). |
PLAT_111 Alert B ADDSYM detects (pseudo) centre of symmetry ... 92 Perc Fit
Author response: Structure solution and refinement has been attempted in several space groups. In P-1 this leads to disorder, unrealistic thermal parameters and an R1-factor of 0.1408 (for anisotropic thermal parameters, but without hydrogen atoms included). In P1 the solution is identical to the solution in Im and R1=0.0499 (for anisotropic thermal parameters, but without hydrogen atoms included). |
Alert Level C:
STRVAL_01 From the CIF: _refine_ls_abs_structure_Flack 0.430 From the CIF: _refine_ls_abs_structure_Flack_su 0.030 Alert C Flack test results are ambiguous. PLAT_202 Alert C Isotropic non-H Atoms in Anion/Solvent = 1 PLAT_302 Alert C Anion/Solvent Disorder ....................... 4.00 Perc. PLAT_420 Alert C D-H Without Acceptor N(11) - *H(11B) ? PLAT_420 Alert C D-H Without Acceptor N(12) - H(12C) ? PLAT_420 Alert C D-H Without Acceptor N(21) - H(21B) ? PLAT_420 Alert C D-H Without Acceptor N(23) - H(23B) ? PLAT_420 Alert C D-H Without Acceptor N(23) - H(23C) ? General Notes
FORMU_01 There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C0.73 H47.19 Cl2.27 N15 O18 Rh3 Atom count from the _atom_site data: C0.73 H45 Cl2.27 N15 O18 Rh3 S6 CELLZ_01 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C0.73 H47.19 Cl2.27 N15 O18 Rh3 S TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 1.46 1.46 0.00 H 94.38 90.00 4.38 Cl 4.54 4.54 0.00 N 30.00 30.00 0.00 O 36.00 36.00 0.00 Rh 6.00 6.00 0.00 S 12.00 12.00 0.00 Difference between formula and atom_site contents detected. WARNING: H atoms missing from atom site list. Is this intentional? REFLT_03 From the CIF: _diffrn_reflns_theta_max 35.02 From the CIF: _reflns_number_total 7322 Count of symmetry unique reflns 3751 Completeness (_total/calc) 195.20% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 3571 Fraction of Friedel pairs measured 0.952 Are heavy atom types Z>Si present yes Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF.
0 Alert Level A = Potentially serious problem
2 Alert Level B = Potential problem
8 Alert Level C = Please check
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. |
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