The title compound, bis(μ-benzene-1,2-dithiolato)bis[(2-mercaptobenzenethiolato)triphenylphosphine)rhodium(III)] dichloromethane tetrasolvate, [Rh2(C6H4S2)2(C6H5S2)2(C18H15)2]·4CH2Cl2, isolated from the reaction of Wilkinson's catalyst RhCl(PPh3)3 and benzo[1,3,2]dithiaborole, is a neutral dinuclear species with two bridging benzenedithiolate ligands and two 2-mercaptobenzenethiolate ligands chelating each RhIII ion. This compound is derived from decomposition of the borole derivative after its oxidative addition to RhI. The compound crystallizes as the dichloromethane tetrasolvate. The molecule is centrosymmetric. The Rh—S distances in the Rh2S2 core are inequivalent, measuring 2.383 (1) and 2.409 (1) Å.
Supporting information
CCDC reference: 633996
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.003 Å
- R factor = 0.025
- wR factor = 0.060
- Data-to-parameter ratio = 14.8
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) . 50 Ang.
PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 400 Deg.
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Rh1 - S2 .. 5.82 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Rh1 - S3 .. 5.29 su
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
6 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
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
0 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
Data collection: CrysAlis CCD (Oxford Diffraction, 2005); cell refinement: CrysAlis RED (Oxford Diffraction, 2005); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
bis(µ-benzene-1,2-dithiolato)bis[(2-
mercaptobenzenethiolato)triphenylphosphine)rhodium(III)] dichloromethane
tetrasolvate
top
Crystal data top
[Rh2(C6H4S2)2(C6H5S2)2(C18H15P)2]·4CH2Cl2 | Z = 1 |
Mr = 1632.93 | F(000) = 824 |
Triclinic, P1 | Dx = 1.67 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.8719 (5) Å | Cell parameters from 15065 reflections |
b = 11.0495 (5) Å | θ = 4.4–25.0° |
c = 14.2621 (5) Å | µ = 1.19 mm−1 |
α = 104.781 (4)° | T = 100 K |
β = 97.789 (4)° | Rhomb, red |
γ = 96.089 (4)° | 0.22 × 0.12 × 0.04 mm |
V = 1623.53 (12) Å3 | |
Data collection top
Oxford Xcalibur2 CCD area-detector diffractometer | 5476 reflections with I > 2σ(I) |
ω/2θ scans | Rint = 0.021 |
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2005) | θmax = 25.1°, θmin = 4.4° |
Tmin = 0.808, Tmax = 0.880 | h = −12→12 |
15977 measured reflections | k = −13→13 |
5650 independent reflections | l = −16→16 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.025 | w = 1/[σ2(Fo2) + (0.025P)2 + 2.3569P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.06 | (Δ/σ)max = 0.001 |
S = 1.08 | Δρmax = 0.49 e Å−3 |
5650 reflections | Δρmin = −0.38 e Å−3 |
383 parameters | |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
C1 | 0.4359 (2) | 0.4129 (2) | 0.79067 (16) | 0.0118 (4) | |
C2 | 0.4398 (2) | 0.3692 (2) | 0.87469 (18) | 0.0182 (5) | |
H2 | 0.5185 | 0.3705 | 0.9134 | 0.022* | |
C3 | 0.3304 (2) | 0.3240 (2) | 0.90211 (18) | 0.0207 (5) | |
H3 | 0.3349 | 0.2946 | 0.9593 | 0.025* | |
C4 | 0.2135 (2) | 0.3214 (2) | 0.84656 (18) | 0.0183 (5) | |
H4 | 0.1387 | 0.2886 | 0.8648 | 0.022* | |
C5 | 0.2080 (2) | 0.3672 (2) | 0.76435 (17) | 0.0152 (5) | |
H5 | 0.129 | 0.369 | 0.7273 | 0.018* | |
C6 | 0.3187 (2) | 0.4107 (2) | 0.73610 (16) | 0.0112 (4) | |
C21 | 0.7793 (2) | 0.4692 (2) | 0.57917 (15) | 0.0096 (4) | |
C22 | 0.9081 (2) | 0.4609 (2) | 0.58625 (16) | 0.0131 (4) | |
H22 | 0.9679 | 0.5345 | 0.6164 | 0.016* | |
C23 | 0.9486 (2) | 0.3454 (2) | 0.54935 (17) | 0.0152 (5) | |
H23 | 1.0359 | 0.3412 | 0.5532 | 0.018* | |
C24 | 0.8624 (2) | 0.2361 (2) | 0.50680 (16) | 0.0135 (5) | |
H24 | 0.8907 | 0.157 | 0.4838 | 0.016* | |
C31 | 0.4901 (2) | 0.8854 (2) | 0.70877 (16) | 0.0111 (4) | |
C32 | 0.4060 (2) | 0.9702 (2) | 0.73617 (17) | 0.0147 (5) | |
H32 | 0.3494 | 0.9548 | 0.7785 | 0.018* | |
C33 | 0.4053 (2) | 1.0768 (2) | 0.70146 (18) | 0.0190 (5) | |
H33 | 0.3465 | 1.1329 | 0.7188 | 0.023* | |
C34 | 0.4893 (2) | 1.1018 (2) | 0.64192 (18) | 0.0198 (5) | |
H34 | 0.4886 | 1.175 | 0.6186 | 0.024* | |
C35 | 0.5752 (2) | 1.0191 (2) | 0.61627 (17) | 0.0167 (5) | |
H35 | 0.6343 | 1.037 | 0.5766 | 0.02* | |
C36 | 0.5746 (2) | 0.9111 (2) | 0.64840 (16) | 0.0132 (5) | |
H36 | 0.632 | 0.8541 | 0.6293 | 0.016* | |
C41 | 0.3702 (2) | 0.72549 (19) | 0.81345 (16) | 0.0101 (4) | |
C42 | 0.2489 (2) | 0.7282 (2) | 0.76618 (17) | 0.0132 (5) | |
H42 | 0.2376 | 0.7474 | 0.7046 | 0.016* | |
C43 | 0.1450 (2) | 0.7029 (2) | 0.80924 (17) | 0.0157 (5) | |
H43 | 0.0633 | 0.7068 | 0.7777 | 0.019* | |
C44 | 0.1606 (2) | 0.6720 (2) | 0.89803 (18) | 0.0172 (5) | |
H44 | 0.0896 | 0.6545 | 0.9272 | 0.021* | |
C45 | 0.2802 (2) | 0.6666 (2) | 0.94422 (17) | 0.0172 (5) | |
H45 | 0.2908 | 0.6445 | 1.0047 | 0.021* | |
C46 | 0.3838 (2) | 0.6933 (2) | 0.90239 (16) | 0.0130 (5) | |
H46 | 0.4652 | 0.6898 | 0.9346 | 0.016* | |
P1 | 0.50557 (5) | 0.74546 (5) | 0.75307 (4) | 0.00798 (12) | |
Rh1 | 0.516868 (15) | 0.559012 (15) | 0.631842 (11) | 0.00660 (6) | |
S1 | 0.57820 (5) | 0.47043 (5) | 0.76088 (4) | 0.01074 (11) | |
S2 | 0.30796 (5) | 0.47635 (5) | 0.63334 (4) | 0.00959 (11) | |
S3 | 0.72913 (5) | 0.61691 (5) | 0.62473 (4) | 0.00973 (11) | |
S4 | 0.52994 (5) | 0.36774 (5) | 0.51249 (4) | 0.00713 (11) | |
Cl3 | 0.85112 (6) | 0.89997 (6) | 0.53038 (5) | 0.02969 (15) | |
Cl2 | 0.90066 (7) | 0.41800 (7) | 0.85316 (6) | 0.03787 (18) | |
C26 | 0.6934 (2) | 0.3598 (2) | 0.53249 (15) | 0.0093 (4) | |
C25 | 0.7350 (2) | 0.2432 (2) | 0.49825 (16) | 0.0118 (4) | |
H25 | 0.6758 | 0.1689 | 0.4691 | 0.014* | |
C51 | 0.6359 (2) | 0.8126 (2) | 0.85671 (16) | 0.0106 (4) | |
C52 | 0.6236 (2) | 0.9252 (2) | 0.92502 (16) | 0.0141 (5) | |
H52 | 0.5483 | 0.961 | 0.9181 | 0.017* | |
C56 | 0.7476 (2) | 0.7613 (2) | 0.86780 (16) | 0.0136 (5) | |
H56 | 0.7572 | 0.6844 | 0.823 | 0.016* | |
C53 | 0.7201 (2) | 0.9850 (2) | 1.00256 (17) | 0.0174 (5) | |
H53 | 0.7101 | 1.0605 | 1.049 | 0.021* | |
C55 | 0.8447 (2) | 0.8238 (2) | 0.94497 (17) | 0.0175 (5) | |
H55 | 0.9211 | 0.7898 | 0.9514 | 0.021* | |
C54 | 0.8315 (2) | 0.9346 (2) | 1.01233 (17) | 0.0182 (5) | |
H54 | 0.8981 | 0.9759 | 1.0649 | 0.022* | |
Cl1 | 0.81361 (8) | 0.15369 (7) | 0.83715 (5) | 0.03757 (18) | |
Cl4 | 1.05266 (7) | 1.02331 (7) | 0.69693 (6) | 0.0434 (2) | |
C1S | 0.8249 (3) | 0.2712 (3) | 0.7737 (2) | 0.0297 (6) | |
H1S1 | 0.7397 | 0.2808 | 0.7447 | 0.036* | |
H1S2 | 0.8725 | 0.2445 | 0.7194 | 0.036* | |
C2S | 0.9222 (3) | 0.9025 (3) | 0.6506 (2) | 0.0332 (7) | |
H2S1 | 0.8596 | 0.9159 | 0.6952 | 0.04* | |
H2S2 | 0.9498 | 0.8196 | 0.6492 | 0.04* | |
H100 | 0.293 (3) | 0.367 (3) | 0.568 (2) | 0.022 (7)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.0141 (11) | 0.0095 (10) | 0.0125 (11) | 0.0015 (9) | 0.0049 (9) | 0.0030 (9) |
C2 | 0.0176 (12) | 0.0232 (13) | 0.0168 (12) | 0.0038 (10) | 0.0015 (9) | 0.0109 (10) |
C3 | 0.0235 (13) | 0.0269 (13) | 0.0175 (12) | 0.0040 (11) | 0.0051 (10) | 0.0153 (11) |
C4 | 0.0161 (12) | 0.0201 (12) | 0.0216 (13) | 0.0001 (10) | 0.0079 (10) | 0.0095 (10) |
C5 | 0.0140 (12) | 0.0159 (11) | 0.0164 (12) | 0.0027 (9) | 0.0022 (9) | 0.0055 (9) |
C6 | 0.0151 (11) | 0.0087 (10) | 0.0102 (10) | 0.0015 (9) | 0.0035 (8) | 0.0027 (8) |
C21 | 0.0130 (11) | 0.0098 (10) | 0.0064 (10) | 0.0016 (8) | 0.0024 (8) | 0.0026 (8) |
C22 | 0.0125 (11) | 0.0158 (11) | 0.0092 (10) | 0.0001 (9) | 0.0008 (8) | 0.0016 (9) |
C23 | 0.0115 (11) | 0.0228 (12) | 0.0130 (11) | 0.0072 (9) | 0.0034 (9) | 0.0056 (10) |
C24 | 0.0181 (12) | 0.0137 (11) | 0.0099 (11) | 0.0067 (9) | 0.0030 (9) | 0.0031 (9) |
C31 | 0.0150 (11) | 0.0074 (10) | 0.0088 (10) | −0.0002 (9) | −0.0010 (8) | 0.0003 (8) |
C32 | 0.0184 (12) | 0.0116 (11) | 0.0144 (11) | 0.0028 (9) | 0.0047 (9) | 0.0026 (9) |
C33 | 0.0235 (13) | 0.0105 (11) | 0.0228 (13) | 0.0068 (10) | 0.0053 (10) | 0.0020 (10) |
C34 | 0.0282 (14) | 0.0109 (11) | 0.0217 (13) | 0.0023 (10) | 0.0038 (10) | 0.0074 (10) |
C35 | 0.0212 (13) | 0.0141 (11) | 0.0152 (12) | −0.0010 (10) | 0.0041 (10) | 0.0053 (9) |
C36 | 0.0147 (11) | 0.0117 (11) | 0.0113 (11) | 0.0011 (9) | 0.0009 (9) | 0.0005 (9) |
C41 | 0.0137 (11) | 0.0063 (10) | 0.0088 (10) | 0.0012 (8) | 0.0040 (8) | −0.0017 (8) |
C42 | 0.0174 (12) | 0.0094 (10) | 0.0120 (11) | 0.0032 (9) | 0.0032 (9) | 0.0005 (9) |
C43 | 0.0118 (11) | 0.0156 (11) | 0.0168 (12) | 0.0034 (9) | 0.0018 (9) | −0.0009 (9) |
C44 | 0.0159 (12) | 0.0156 (12) | 0.0194 (12) | 0.0021 (9) | 0.0094 (9) | 0.0003 (10) |
C45 | 0.0225 (13) | 0.0183 (12) | 0.0122 (11) | 0.0041 (10) | 0.0050 (9) | 0.0054 (9) |
C46 | 0.0133 (11) | 0.0132 (11) | 0.0120 (11) | 0.0029 (9) | 0.0018 (9) | 0.0024 (9) |
P1 | 0.0095 (3) | 0.0074 (3) | 0.0067 (3) | 0.0017 (2) | 0.0019 (2) | 0.0009 (2) |
Rh1 | 0.00805 (9) | 0.00616 (9) | 0.00563 (9) | 0.00127 (6) | 0.00194 (6) | 0.00117 (6) |
S1 | 0.0100 (3) | 0.0131 (3) | 0.0109 (3) | 0.0019 (2) | 0.0018 (2) | 0.0062 (2) |
S2 | 0.0098 (3) | 0.0119 (3) | 0.0068 (2) | 0.0008 (2) | 0.00188 (19) | 0.0022 (2) |
S3 | 0.0103 (3) | 0.0082 (2) | 0.0097 (3) | 0.0003 (2) | 0.0032 (2) | 0.0003 (2) |
S4 | 0.0085 (3) | 0.0058 (2) | 0.0070 (2) | 0.00107 (19) | 0.00163 (19) | 0.00136 (19) |
Cl3 | 0.0257 (3) | 0.0272 (3) | 0.0426 (4) | 0.0082 (3) | 0.0131 (3) | 0.0155 (3) |
Cl2 | 0.0235 (4) | 0.0339 (4) | 0.0538 (5) | −0.0003 (3) | 0.0021 (3) | 0.0118 (3) |
C26 | 0.0108 (11) | 0.0124 (11) | 0.0064 (10) | 0.0031 (8) | 0.0019 (8) | 0.0050 (8) |
C25 | 0.0155 (11) | 0.0108 (11) | 0.0092 (10) | 0.0024 (9) | 0.0024 (8) | 0.0023 (9) |
C51 | 0.0107 (11) | 0.0109 (10) | 0.0094 (10) | −0.0027 (8) | 0.0022 (8) | 0.0027 (8) |
C52 | 0.0159 (12) | 0.0132 (11) | 0.0133 (11) | 0.0033 (9) | 0.0042 (9) | 0.0028 (9) |
C56 | 0.0146 (11) | 0.0149 (11) | 0.0117 (11) | 0.0012 (9) | 0.0059 (9) | 0.0026 (9) |
C53 | 0.0240 (13) | 0.0121 (11) | 0.0133 (11) | −0.0009 (10) | 0.0035 (10) | −0.0003 (9) |
C55 | 0.0130 (12) | 0.0233 (13) | 0.0153 (12) | 0.0024 (10) | 0.0020 (9) | 0.0043 (10) |
C54 | 0.0167 (12) | 0.0209 (12) | 0.0129 (11) | −0.0051 (10) | −0.0009 (9) | 0.0024 (10) |
Cl1 | 0.0584 (5) | 0.0301 (4) | 0.0244 (4) | 0.0054 (3) | 0.0137 (3) | 0.0049 (3) |
Cl4 | 0.0315 (4) | 0.0366 (4) | 0.0496 (5) | −0.0099 (3) | 0.0153 (3) | −0.0090 (4) |
C1S | 0.0322 (16) | 0.0323 (15) | 0.0263 (14) | 0.0117 (12) | 0.0065 (12) | 0.0073 (12) |
C2S | 0.0317 (16) | 0.0274 (15) | 0.0359 (16) | −0.0066 (12) | 0.0098 (13) | 0.0031 (13) |
Geometric parameters (Å, º) top
C1—C6 | 1.394 (3) | C43—C44 | 1.387 (3) |
C1—C2 | 1.399 (3) | C43—H43 | 0.95 |
C1—S1 | 1.757 (2) | C44—C45 | 1.390 (3) |
C2—C3 | 1.384 (3) | C44—H44 | 0.95 |
C2—H2 | 0.95 | C45—C46 | 1.383 (3) |
C3—C4 | 1.397 (4) | C45—H45 | 0.95 |
C3—H3 | 0.95 | C46—H46 | 0.95 |
C4—C5 | 1.387 (3) | P1—C51 | 1.842 (2) |
C4—H4 | 0.95 | P1—Rh1 | 2.3542 (5) |
C5—C6 | 1.396 (3) | Rh1—S1 | 2.3483 (5) |
C5—H5 | 0.95 | Rh1—S3 | 2.3512 (6) |
C6—S2 | 1.789 (2) | Rh1—S2 | 2.3614 (6) |
C21—C26 | 1.400 (3) | Rh1—S4 | 2.3829 (5) |
C21—C22 | 1.404 (3) | Rh1—S4i | 2.4093 (5) |
C21—S3 | 1.769 (2) | S2—H100 | 1.31 (3) |
C22—C23 | 1.392 (3) | S4—C26 | 1.777 (2) |
C22—H22 | 0.95 | S4—Rh1i | 2.4093 (5) |
C23—C24 | 1.392 (3) | Cl3—C2S | 1.775 (3) |
C23—H23 | 0.95 | Cl2—C1S | 1.766 (3) |
C24—C25 | 1.386 (3) | C26—C25 | 1.402 (3) |
C24—H24 | 0.95 | C25—H25 | 0.95 |
C31—C36 | 1.396 (3) | C51—C56 | 1.400 (3) |
C31—C32 | 1.399 (3) | C51—C52 | 1.402 (3) |
C31—P1 | 1.829 (2) | C52—C53 | 1.388 (3) |
C32—C33 | 1.390 (3) | C52—H52 | 0.95 |
C32—H32 | 0.95 | C56—C55 | 1.395 (3) |
C33—C34 | 1.381 (4) | C56—H56 | 0.95 |
C33—H33 | 0.95 | C53—C54 | 1.390 (4) |
C34—C35 | 1.394 (4) | C53—H53 | 0.95 |
C34—H34 | 0.95 | C55—C54 | 1.385 (3) |
C35—C36 | 1.383 (3) | C55—H55 | 0.95 |
C35—H35 | 0.95 | C54—H54 | 0.95 |
C36—H36 | 0.95 | Cl1—C1S | 1.765 (3) |
C41—C46 | 1.396 (3) | Cl4—C2S | 1.768 (3) |
C41—C42 | 1.405 (3) | C1S—H1S1 | 0.99 |
C41—P1 | 1.824 (2) | C1S—H1S2 | 0.99 |
C42—C43 | 1.393 (3) | C2S—H2S1 | 0.99 |
C42—H42 | 0.95 | C2S—H2S2 | 0.99 |
| | | |
C6—C1—C2 | 118.0 (2) | C41—P1—C31 | 105.35 (10) |
C6—C1—S1 | 123.53 (17) | C41—P1—C51 | 103.38 (10) |
C2—C1—S1 | 118.41 (18) | C31—P1—C51 | 99.43 (10) |
C3—C2—C1 | 120.8 (2) | C41—P1—Rh1 | 110.98 (7) |
C3—C2—H2 | 119.6 | C31—P1—Rh1 | 115.45 (7) |
C1—C2—H2 | 119.6 | C51—P1—Rh1 | 120.47 (7) |
C2—C3—C4 | 120.7 (2) | S1—Rh1—S3 | 89.708 (19) |
C2—C3—H3 | 119.7 | S1—Rh1—P1 | 87.264 (19) |
C4—C3—H3 | 119.7 | S3—Rh1—P1 | 94.227 (19) |
C5—C4—C3 | 119.1 (2) | S1—Rh1—S2 | 87.451 (19) |
C5—C4—H4 | 120.4 | S3—Rh1—S2 | 173.370 (19) |
C3—C4—H4 | 120.4 | P1—Rh1—S2 | 91.621 (19) |
C4—C5—C6 | 119.9 (2) | S1—Rh1—S4 | 91.223 (19) |
C4—C5—H5 | 120 | S3—Rh1—S4 | 85.765 (18) |
C6—C5—H5 | 120 | P1—Rh1—S4 | 178.486 (19) |
C1—C6—C5 | 121.4 (2) | S2—Rh1—S4 | 88.307 (19) |
C1—C6—S2 | 119.78 (17) | S1—Rh1—S4i | 172.623 (19) |
C5—C6—S2 | 118.66 (17) | S3—Rh1—S4i | 86.131 (19) |
C26—C21—C22 | 118.52 (19) | P1—Rh1—S4i | 99.105 (19) |
C26—C21—S3 | 121.51 (16) | S2—Rh1—S4i | 96.034 (19) |
C22—C21—S3 | 119.93 (17) | S4—Rh1—S4i | 82.405 (19) |
C23—C22—C21 | 120.4 (2) | C1—S1—Rh1 | 104.14 (8) |
C23—C22—H22 | 119.8 | C6—S2—Rh1 | 104.54 (8) |
C21—C22—H22 | 119.8 | C6—S2—H100 | 94.3 (12) |
C22—C23—C24 | 120.6 (2) | Rh1—S2—H100 | 102.1 (12) |
C22—C23—H23 | 119.7 | C21—S3—Rh1 | 102.76 (7) |
C24—C23—H23 | 119.7 | C26—S4—Rh1 | 101.90 (7) |
C25—C24—C23 | 119.6 (2) | C26—S4—Rh1i | 107.82 (7) |
C25—C24—H24 | 120.2 | Rh1—S4—Rh1i | 97.595 (19) |
C23—C24—H24 | 120.2 | C21—C26—C25 | 120.6 (2) |
C36—C31—C32 | 119.2 (2) | C21—C26—S4 | 120.31 (16) |
C36—C31—P1 | 116.22 (16) | C25—C26—S4 | 119.02 (17) |
C32—C31—P1 | 124.47 (17) | C24—C25—C26 | 120.2 (2) |
C33—C32—C31 | 120.0 (2) | C24—C25—H25 | 119.9 |
C33—C32—H32 | 120 | C26—C25—H25 | 119.9 |
C31—C32—H32 | 120 | C56—C51—C52 | 118.9 (2) |
C34—C33—C32 | 120.5 (2) | C56—C51—P1 | 123.77 (17) |
C34—C33—H33 | 119.7 | C52—C51—P1 | 117.27 (17) |
C32—C33—H33 | 119.7 | C53—C52—C51 | 120.8 (2) |
C33—C34—C35 | 119.7 (2) | C53—C52—H52 | 119.6 |
C33—C34—H34 | 120.2 | C51—C52—H52 | 119.6 |
C35—C34—H34 | 120.2 | C55—C56—C51 | 119.7 (2) |
C36—C35—C34 | 120.3 (2) | C55—C56—H56 | 120.2 |
C36—C35—H35 | 119.9 | C51—C56—H56 | 120.2 |
C34—C35—H35 | 119.9 | C52—C53—C54 | 120.0 (2) |
C35—C36—C31 | 120.4 (2) | C52—C53—H53 | 120 |
C35—C36—H36 | 119.8 | C54—C53—H53 | 120 |
C31—C36—H36 | 119.8 | C54—C55—C56 | 121.0 (2) |
C46—C41—C42 | 118.7 (2) | C54—C55—H55 | 119.5 |
C46—C41—P1 | 120.38 (17) | C56—C55—H55 | 119.5 |
C42—C41—P1 | 120.57 (17) | C55—C54—C53 | 119.6 (2) |
C43—C42—C41 | 120.3 (2) | C55—C54—H54 | 120.2 |
C43—C42—H42 | 119.9 | C53—C54—H54 | 120.2 |
C41—C42—H42 | 119.9 | Cl1—C1S—Cl2 | 111.25 (16) |
C44—C43—C42 | 120.1 (2) | Cl1—C1S—H1S1 | 109.4 |
C44—C43—H43 | 119.9 | Cl2—C1S—H1S1 | 109.4 |
C42—C43—H43 | 119.9 | Cl1—C1S—H1S2 | 109.4 |
C43—C44—C45 | 119.9 (2) | Cl2—C1S—H1S2 | 109.4 |
C43—C44—H44 | 120 | H1S1—C1S—H1S2 | 108 |
C45—C44—H44 | 120 | Cl4—C2S—Cl3 | 111.79 (16) |
C46—C45—C44 | 120.2 (2) | Cl4—C2S—H2S1 | 109.3 |
C46—C45—H45 | 119.9 | Cl3—C2S—H2S1 | 109.3 |
C44—C45—H45 | 119.9 | Cl4—C2S—H2S2 | 109.3 |
C45—C46—C41 | 120.8 (2) | Cl3—C2S—H2S2 | 109.3 |
C45—C46—H46 | 119.6 | H2S1—C2S—H2S2 | 107.9 |
C41—C46—H46 | 119.6 | | |
| | | |
C6—C1—C2—C3 | 0.6 (3) | C31—P1—Rh1—S4i | −8.28 (8) |
S1—C1—C2—C3 | 179.37 (19) | C51—P1—Rh1—S4i | −127.64 (8) |
C1—C2—C3—C4 | −0.1 (4) | C6—C1—S1—Rh1 | 7.4 (2) |
C2—C3—C4—C5 | −1.4 (4) | C2—C1—S1—Rh1 | −171.39 (17) |
C3—C4—C5—C6 | 2.4 (4) | S3—Rh1—S1—C1 | 179.61 (8) |
C2—C1—C6—C5 | 0.5 (3) | P1—Rh1—S1—C1 | 85.36 (8) |
S1—C1—C6—C5 | −178.22 (17) | S2—Rh1—S1—C1 | −6.39 (8) |
C2—C1—C6—S2 | 175.37 (17) | S4—Rh1—S1—C1 | −94.64 (8) |
S1—C1—C6—S2 | −3.4 (3) | C1—C6—S2—Rh1 | −2.59 (19) |
C4—C5—C6—C1 | −2.0 (3) | C5—C6—S2—Rh1 | 172.40 (16) |
C4—C5—C6—S2 | −176.94 (18) | S1—Rh1—S2—C6 | 5.17 (7) |
C26—C21—C22—C23 | −1.4 (3) | P1—Rh1—S2—C6 | −82.02 (7) |
S3—C21—C22—C23 | −179.06 (17) | S4—Rh1—S2—C6 | 96.47 (7) |
C21—C22—C23—C24 | −1.4 (3) | S4i—Rh1—S2—C6 | 178.65 (7) |
C22—C23—C24—C25 | 2.2 (3) | C26—C21—S3—Rh1 | 17.52 (19) |
C36—C31—C32—C33 | 1.5 (3) | C22—C21—S3—Rh1 | −164.84 (16) |
P1—C31—C32—C33 | 177.30 (18) | S1—Rh1—S3—C21 | 68.87 (7) |
C31—C32—C33—C34 | −1.6 (4) | P1—Rh1—S3—C21 | 156.11 (7) |
C32—C33—C34—C35 | 0.2 (4) | S4—Rh1—S3—C21 | −22.37 (7) |
C33—C34—C35—C36 | 1.4 (4) | S4i—Rh1—S3—C21 | −105.03 (7) |
C34—C35—C36—C31 | −1.6 (4) | S1—Rh1—S4—C26 | −66.17 (7) |
C32—C31—C36—C35 | 0.1 (3) | S3—Rh1—S4—C26 | 23.45 (7) |
P1—C31—C36—C35 | −176.03 (18) | S2—Rh1—S4—C26 | −153.58 (7) |
C46—C41—C42—C43 | 1.9 (3) | S4i—Rh1—S4—C26 | 110.10 (7) |
P1—C41—C42—C43 | 174.86 (17) | S1—Rh1—S4—Rh1i | −176.27 (2) |
C41—C42—C43—C44 | −1.5 (3) | S3—Rh1—S4—Rh1i | −86.65 (2) |
C42—C43—C44—C45 | 0.2 (3) | S2—Rh1—S4—Rh1i | 96.32 (2) |
C43—C44—C45—C46 | 0.7 (3) | S4i—Rh1—S4—Rh1i | 0 |
C44—C45—C46—C41 | −0.3 (3) | C22—C21—C26—C25 | 3.3 (3) |
C42—C41—C46—C45 | −1.0 (3) | S3—C21—C26—C25 | −179.01 (16) |
P1—C41—C46—C45 | −174.01 (17) | C22—C21—C26—S4 | −174.76 (16) |
C46—C41—P1—C31 | −138.13 (18) | S3—C21—C26—S4 | 2.9 (3) |
C42—C41—P1—C31 | 49.01 (19) | Rh1—S4—C26—C21 | −21.29 (18) |
C46—C41—P1—C51 | −34.2 (2) | Rh1i—S4—C26—C21 | 80.81 (17) |
C42—C41—P1—C51 | 152.89 (17) | Rh1—S4—C26—C25 | 160.60 (15) |
C46—C41—P1—Rh1 | 96.25 (17) | Rh1i—S4—C26—C25 | −97.30 (17) |
C42—C41—P1—Rh1 | −76.61 (18) | C23—C24—C25—C26 | −0.2 (3) |
C36—C31—P1—C41 | −171.99 (17) | C21—C26—C25—C24 | −2.6 (3) |
C32—C31—P1—C41 | 12.1 (2) | S4—C26—C25—C24 | 175.52 (17) |
C36—C31—P1—C51 | 81.22 (18) | C41—P1—C51—C56 | 126.69 (19) |
C32—C31—P1—C51 | −94.7 (2) | C31—P1—C51—C56 | −124.93 (19) |
C36—C31—P1—Rh1 | −49.19 (19) | Rh1—P1—C51—C56 | 2.2 (2) |
C32—C31—P1—Rh1 | 134.87 (18) | C41—P1—C51—C52 | −56.69 (19) |
C41—P1—Rh1—S1 | −72.26 (8) | C31—P1—C51—C52 | 51.68 (19) |
C31—P1—Rh1—S1 | 167.97 (8) | Rh1—P1—C51—C52 | 178.77 (14) |
C51—P1—Rh1—S1 | 48.61 (8) | C56—C51—C52—C53 | −0.1 (3) |
C41—P1—Rh1—S3 | −161.77 (8) | P1—C51—C52—C53 | −176.93 (18) |
C31—P1—Rh1—S3 | 78.47 (8) | C52—C51—C56—C55 | −1.1 (3) |
C51—P1—Rh1—S3 | −40.89 (8) | P1—C51—C56—C55 | 175.48 (17) |
C41—P1—Rh1—S2 | 15.11 (8) | C51—C52—C53—C54 | 1.1 (3) |
C31—P1—Rh1—S2 | −104.66 (8) | C51—C56—C55—C54 | 1.4 (3) |
C51—P1—Rh1—S2 | 135.98 (8) | C56—C55—C54—C53 | −0.5 (4) |
C41—P1—Rh1—S4i | 111.48 (8) | C52—C53—C54—C55 | −0.8 (4) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
S2—H100···S3i | 1.31 (3) | 2.78 (3) | 3.5137 (8) | 113.8 (18) |
C1S—H1S1···S1 | 0.99 | 2.86 | 3.660 (3) | 139 |
C56—H56···S1 | 0.95 | 2.77 | 3.396 (2) | 125 |
C56—H56···S3 | 0.95 | 2.70 | 3.395 (2) | 131 |
Symmetry code: (i) −x+1, −y+1, −z+1. |