Low-temperature phase of di­aqua(1,5-cyclo­octa­diene)­rhodium(I) tri­fluoro­methane­sulfonate

Crystals of the title compound, [Rh(C₈H₁₂)(H₂O)₂](CF₃SO₃), undergo a reversible phase transition at 215 (2) K. The high-temperature structure is disordered in space group P2₁/m with Z' = ½, while the twinned low-temperature structure is ordered in space group P with Z' = 2.

Key indicators

• Single-crystal X-ray study
• T = 152 K
• Mean [sigma](C-C) = 0.012 Å
• R factor = 0.055
• wR factor = 0.140
• Data-to-parameter ratio = 21.3

checkCIF/PLATON results

No syntax errors found



Alert level C
DIFMX01_ALERT_2_C  The maximum difference density is > 0.1*ZMAX*0.75
            _refine_diff_density_max given =      3.788
            Test value =      3.375
DIFMX02_ALERT_1_C  The minimum difference density is > 0.1*ZMAX*0.75
            The relevant atom site should be identified.
PLAT097_ALERT_2_C Maximum (Positive) Residual Density ............       3.79 e/A   3
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....         S1
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....        C17
PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor ....       2.09
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         12
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          8
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          3
              C F3 O3 S

Alert level G
ABSTM02_ALERT_3_G  The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
            Tmin and Tmax reported:      0.414     0.872
            Tmin' and Tmax expected:      0.471     0.839
            RR' =      0.847
            Please check that your absorption correction is appropriate.

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   9 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   5 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
   2 ALERT type 4 Improvement, methodology, query or suggestion

---

Computing details

Data collection: SMART (Siemens, 1995); cell refinement: SMART; data reduction: SAINT (Siemens, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Sheldrick, 1996); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

diaqua(1,5-cyclooctadiene)rhodium(I) trifluoromethanesulfonate

Crystal data

[Rh(C8H12)(H2O)2](CF3O3S)	Z = 4
Mr = 396.19	F(000) = 792
Triclinic, P1	Dx = 1.939 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 11.9569 (11) Å	Cell parameters from 177 reflections
b = 12.0716 (17) Å	θ = 3–23°
c = 12.1417 (17) Å	µ = 1.46 mm^−1
α = 104.944 (12)°	T = 152 K
β = 105.414 (10)°	Block, orange
γ = 116.683 (10)°	0.50 × 0.48 × 0.12 mm
V = 1357.1 (4) Å^3

Data collection

Siemens SMART 1K CCD diffractometer	7851 independent reflections
Radiation source: normal-focus sealed tube	7426 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.089
ω scans	θmax = 30.2°, θmin = 1.9°
Absorption correction: numerical (SHELXTL; Sheldrick, 1996)	h = −14→17
Tmin = 0.414, Tmax = 0.872	k = −14→17
17620 measured reflections	l = −18→17

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.055	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.140	w = 1/[σ^2(Fo^2) + (0.07P)^2 + 5P] where P = (Fo^2 + 2Fc^2)/3
S = 1.08	(Δ/σ)max = 0.002
7851 reflections	Δρmax = 3.79 e Å^−3
369 parameters	Δρmin = −3.26 e Å^−3
12 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0052 (7)

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Rh1	0.92523 (4)	0.67499 (4)	0.79963 (4)	0.01578 (10)
Rh2	0.42928 (4)	0.17097 (4)	0.77696 (4)	0.01552 (11)
S1	−0.07044 (14)	−0.32416 (14)	0.37044 (11)	0.0202 (2)
S2	0.42595 (14)	0.18430 (14)	0.36525 (11)	0.0203 (2)
O1	1.0109 (6)	0.6084 (6)	0.6859 (5)	0.0272 (9)
O2	0.8782 (6)	0.7600 (6)	0.6749 (5)	0.0263 (10)
O3	0.5237 (6)	0.1237 (6)	0.6619 (5)	0.0260 (9)
O4	0.3668 (6)	0.2556 (6)	0.6592 (5)	0.0270 (10)
O5	−0.0459 (6)	−0.4088 (6)	0.2864 (5)	0.0366 (11)
O6	−0.1713 (6)	−0.3009 (6)	0.3070 (5)	0.0367 (11)
O7	−0.0879 (6)	−0.3598 (5)	0.4724 (4)	0.0347 (10)
O8	0.3692 (5)	0.1308 (5)	0.2302 (4)	0.0317 (9)
O9	0.4677 (6)	0.1079 (5)	0.4195 (4)	0.0308 (10)
O10	0.3492 (5)	0.2252 (6)	0.4218 (4)	0.0325 (10)
F1	0.1207 (8)	−0.1036 (7)	0.3733 (6)	0.083 (3)
F2	0.1967 (7)	−0.1632 (10)	0.5132 (7)	0.092 (3)
F3	0.0849 (9)	−0.0691 (6)	0.5391 (6)	0.079 (2)
F4	0.6747 (6)	0.3266 (7)	0.3804 (7)	0.0573 (15)
F5	0.5690 (7)	0.4313 (6)	0.3828 (6)	0.0606 (16)
F6	0.6541 (6)	0.4070 (6)	0.5479 (4)	0.0670 (15)
C1	0.9141 (7)	0.5413 (6)	0.8839 (6)	0.0208 (10)
H1	0.8926	0.4779	0.8039	0.025*
C2	1.0451 (7)	0.6634 (7)	0.9511 (6)	0.0225 (11)
H2	1.1088	0.6746	0.9153	0.027*
C3	1.0971 (9)	0.7812 (8)	1.0762 (7)	0.0359 (16)
H3A	1.1128	0.7524	1.1452	0.043*
H3B	1.1879	0.8611	1.0945	0.043*
C4	0.9978 (8)	0.8253 (8)	1.0767 (6)	0.0331 (15)
H4A	1.0515	0.9251	1.1334	0.040*
H4B	0.9357	0.7750	1.1109	0.040*
C5	0.9100 (7)	0.7974 (6)	0.9448 (6)	0.0201 (10)
H5	0.9456	0.8663	0.9163	0.024*
C6	0.7792 (7)	0.6755 (7)	0.8631 (6)	0.0218 (11)
H6	0.7300	0.6703	0.7843	0.026*
C7	0.7086 (7)	0.5513 (8)	0.8876 (8)	0.0334 (14)
H7A	0.6246	0.4748	0.8086	0.040*
H7B	0.6778	0.5741	0.9531	0.040*
C8	0.8032 (7)	0.5036 (7)	0.9316 (7)	0.0305 (13)
H8A	0.8491	0.5462	1.0257	0.037*
H8B	0.7458	0.4023	0.9007	0.037*
C9	0.2898 (7)	−0.0439 (7)	0.8591 (7)	0.0302 (12)
H9A	0.3067	−0.0795	0.9224	0.036*
H9B	0.2119	−0.1236	0.7781	0.036*
C10	0.4190 (7)	0.0228 (6)	0.8392 (6)	0.0211 (10)
H10	0.4154	−0.0258	0.7617	0.025*
C11	0.5433 (6)	0.1495 (7)	0.9245 (6)	0.0201 (11)
H11	0.6166	0.1836	0.9001	0.024*
C12	0.5670 (7)	0.2361 (7)	1.0553 (6)	0.0250 (12)
H12A	0.6663	0.2857	1.1160	0.030*
H12B	0.5099	0.1743	1.0859	0.030*
C13	0.5285 (7)	0.3404 (7)	1.0518 (6)	0.0248 (11)
H13A	0.4959	0.3569	1.1174	0.030*
H13B	0.6129	0.4290	1.0728	0.030*
C14	0.4161 (6)	0.2922 (6)	0.9236 (5)	0.0176 (10)
H14	0.4326	0.3547	0.8863	0.021*
C15	0.2906 (6)	0.1639 (6)	0.8561 (5)	0.0193 (10)
H15	0.2283	0.1433	0.7751	0.023*
C16	0.2469 (7)	0.0539 (7)	0.9046 (6)	0.0248 (11)
H16A	0.2910	0.0989	0.9987	0.030*
H16B	0.1445	0.0008	0.8740	0.030*
C17	0.0929 (9)	−0.1548 (9)	0.4534 (7)	0.0474 (18)
C18	0.5904 (8)	0.3459 (8)	0.4224 (6)	0.0368 (13)
H01A	0.998 (11)	0.613 (9)	0.612 (5)	0.045*
H01B	1.014 (10)	0.536 (7)	0.683 (8)	0.045*
H02A	0.874 (10)	0.729 (10)	0.597 (5)	0.045*
H02B	0.815 (9)	0.782 (11)	0.668 (8)	0.045*
H03A	0.525 (10)	0.147 (9)	0.599 (6)	0.045*
H03B	0.528 (11)	0.049 (7)	0.647 (8)	0.045*
H04A	0.343 (9)	0.219 (9)	0.577 (3)	0.045*
H04B	0.314 (9)	0.286 (10)	0.674 (8)	0.045*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rh1	0.0208 (2)	0.0200 (2)	0.01717 (18)	0.01521 (15)	0.01167 (15)	0.01173 (14)
Rh2	0.0221 (2)	0.0210 (2)	0.01520 (17)	0.01651 (16)	0.01177 (15)	0.01160 (14)
S1	0.0298 (6)	0.0287 (6)	0.0179 (5)	0.0230 (5)	0.0143 (5)	0.0147 (5)
S2	0.0281 (6)	0.0272 (6)	0.0164 (5)	0.0196 (5)	0.0126 (5)	0.0131 (4)
O1	0.044 (3)	0.037 (3)	0.027 (2)	0.033 (2)	0.025 (2)	0.020 (2)
O2	0.039 (3)	0.041 (3)	0.025 (2)	0.032 (2)	0.021 (2)	0.025 (2)
O3	0.041 (3)	0.037 (2)	0.024 (2)	0.032 (2)	0.023 (2)	0.0186 (19)
O4	0.040 (3)	0.046 (3)	0.023 (2)	0.035 (2)	0.019 (2)	0.025 (2)
O5	0.065 (3)	0.050 (3)	0.031 (2)	0.049 (3)	0.032 (2)	0.024 (2)
O6	0.047 (3)	0.056 (3)	0.036 (2)	0.043 (3)	0.023 (2)	0.028 (2)
O7	0.057 (3)	0.047 (3)	0.029 (2)	0.038 (2)	0.030 (2)	0.028 (2)
O8	0.042 (2)	0.035 (2)	0.0152 (15)	0.0198 (19)	0.0120 (16)	0.0114 (15)
O9	0.051 (3)	0.043 (3)	0.030 (2)	0.038 (2)	0.027 (2)	0.027 (2)
O10	0.046 (3)	0.054 (3)	0.028 (2)	0.041 (3)	0.025 (2)	0.027 (2)
F1	0.084 (5)	0.060 (4)	0.055 (3)	0.000 (3)	0.034 (3)	0.030 (3)
F2	0.036 (3)	0.125 (7)	0.066 (4)	0.030 (4)	−0.001 (3)	0.028 (4)
F3	0.113 (6)	0.040 (3)	0.042 (3)	0.026 (3)	0.028 (3)	0.000 (2)
F4	0.034 (3)	0.062 (3)	0.075 (4)	0.022 (3)	0.030 (3)	0.032 (3)
F5	0.066 (4)	0.036 (3)	0.075 (4)	0.022 (3)	0.027 (3)	0.033 (3)
F6	0.057 (4)	0.060 (4)	0.031 (2)	0.017 (2)	−0.004 (2)	−0.001 (2)
C1	0.029 (3)	0.022 (2)	0.023 (2)	0.019 (2)	0.014 (2)	0.015 (2)
C2	0.028 (3)	0.032 (3)	0.022 (3)	0.023 (3)	0.014 (2)	0.016 (2)
C3	0.044 (4)	0.038 (4)	0.024 (3)	0.029 (3)	0.008 (3)	0.008 (3)
C4	0.041 (4)	0.042 (4)	0.018 (3)	0.032 (3)	0.009 (2)	0.007 (2)
C5	0.026 (3)	0.021 (2)	0.020 (2)	0.016 (2)	0.014 (2)	0.010 (2)
C6	0.026 (3)	0.029 (3)	0.030 (3)	0.022 (2)	0.020 (2)	0.018 (2)
C7	0.031 (3)	0.035 (3)	0.056 (4)	0.021 (3)	0.031 (3)	0.031 (3)
C8	0.035 (3)	0.036 (3)	0.044 (4)	0.024 (3)	0.028 (3)	0.029 (3)
C9	0.037 (3)	0.028 (3)	0.041 (3)	0.021 (3)	0.023 (3)	0.023 (3)
C10	0.031 (3)	0.024 (2)	0.023 (2)	0.020 (2)	0.017 (2)	0.016 (2)
C11	0.024 (3)	0.034 (3)	0.020 (2)	0.024 (3)	0.014 (2)	0.018 (2)
C12	0.031 (3)	0.033 (3)	0.021 (2)	0.023 (3)	0.011 (2)	0.015 (2)
C13	0.036 (3)	0.028 (3)	0.019 (2)	0.023 (3)	0.013 (2)	0.009 (2)
C14	0.026 (2)	0.023 (2)	0.017 (2)	0.020 (2)	0.014 (2)	0.0110 (19)
C15	0.023 (2)	0.027 (3)	0.018 (2)	0.019 (2)	0.0124 (19)	0.0105 (19)
C16	0.028 (3)	0.032 (3)	0.031 (3)	0.020 (2)	0.021 (2)	0.023 (2)
C17	0.044 (4)	0.045 (4)	0.030 (3)	0.011 (3)	0.015 (3)	0.014 (3)
C18	0.035 (3)	0.036 (3)	0.032 (3)	0.018 (3)	0.009 (3)	0.013 (3)

Geometric parameters (Å, º)

Rh1—C6	2.088 (5)	C2—C3	1.518 (9)
Rh1—C2	2.090 (6)	C2—H2	0.9500
Rh1—C5	2.096 (6)	C3—C4	1.504 (9)
Rh1—C1	2.098 (6)	C3—H3A	0.9900
Rh1—O1	2.126 (4)	C3—H3B	0.9900
Rh1—O2	2.128 (4)	C4—C5	1.513 (9)
Rh2—C10	2.082 (5)	C4—H4A	0.9900
Rh2—C14	2.086 (5)	C4—H4B	0.9900
Rh2—C11	2.096 (6)	C5—C6	1.396 (9)
Rh2—C15	2.108 (5)	C5—H5	0.9500
Rh2—O4	2.125 (4)	C6—C7	1.508 (9)
Rh2—O3	2.135 (4)	C6—H6	0.9500
S1—O6	1.431 (5)	C7—C8	1.522 (9)
S1—O5	1.436 (4)	C7—H7A	0.9900
S1—O7	1.447 (4)	C7—H7B	0.9900
S1—C17	1.820 (8)	C8—H8A	0.9900
S2—O8	1.426 (4)	C8—H8B	0.9900
S2—O9	1.444 (5)	C9—C10	1.508 (9)
S2—O10	1.457 (5)	C9—C16	1.523 (9)
S2—C18	1.812 (7)	C9—H9A	0.9900
O1—H01A	0.89 (7)	C9—H9B	0.9900
O1—H01B	0.88 (10)	C10—C11	1.394 (9)
O2—H02A	0.90 (7)	C10—H10	0.9500
O2—H02B	0.90 (13)	C11—C12	1.528 (8)
O3—H03A	0.88 (8)	C11—H11	0.9500
O3—H03B	0.90 (11)	C12—C13	1.528 (8)
O4—H04A	0.89 (4)	C12—H12A	0.9900
O4—H04B	0.89 (12)	C12—H12B	0.9900
F1—C17	1.318 (9)	C13—C14	1.513 (8)
F2—C17	1.323 (14)	C13—H13A	0.9900
F3—C17	1.323 (12)	C13—H13B	0.9900
F4—C18	1.325 (10)	C14—C15	1.388 (8)
F5—C18	1.336 (10)	C14—H14	0.9500
F6—C18	1.321 (8)	C15—C16	1.525 (8)
C1—C2	1.385 (9)	C15—H15	0.9500
C1—C8	1.518 (8)	C16—H16A	0.9900
C1—H1	0.9500	C16—H16B	0.9900
C6—Rh1—C2	98.1 (2)	C6—C5—H5	118.3
C6—Rh1—C5	39.0 (3)	C4—C5—H5	118.3
C2—Rh1—C5	82.2 (2)	Rh1—C5—H5	86.0
C6—Rh1—C1	82.6 (2)	C5—C6—C7	126.4 (6)
C2—Rh1—C1	38.6 (2)	C5—C6—Rh1	70.8 (3)
C5—Rh1—C1	91.9 (2)	C7—C6—Rh1	111.0 (4)
C6—Rh1—O1	160.2 (3)	C5—C6—H6	116.8
C2—Rh1—O1	90.3 (2)	C7—C6—H6	116.8
C5—Rh1—O1	160.8 (3)	Rh1—C6—H6	88.1
C1—Rh1—O1	93.2 (2)	C6—C7—C8	112.9 (5)
C6—Rh1—O2	92.1 (2)	C6—C7—H7A	109.0
C2—Rh1—O2	157.9 (3)	C8—C7—H7A	109.0
C5—Rh1—O2	93.8 (2)	C6—C7—H7B	109.0
C1—Rh1—O2	163.4 (3)	C8—C7—H7B	109.0
O1—Rh1—O2	86.58 (17)	H7A—C7—H7B	107.8
C10—Rh2—C14	98.9 (2)	C1—C8—C7	112.3 (5)
C10—Rh2—C11	39.0 (2)	C1—C8—H8A	109.1
C14—Rh2—C11	82.74 (19)	C7—C8—H8A	109.1
C10—Rh2—C15	82.5 (2)	C1—C8—H8B	109.1
C14—Rh2—C15	38.7 (2)	C7—C8—H8B	109.1
C11—Rh2—C15	91.4 (2)	H8A—C8—H8B	107.9
C10—Rh2—O4	158.4 (3)	C10—C9—C16	113.3 (5)
C14—Rh2—O4	90.0 (2)	C10—C9—H9A	108.9
C11—Rh2—O4	162.6 (3)	C16—C9—H9A	108.9
C15—Rh2—O4	92.8 (2)	C10—C9—H9B	108.9
C10—Rh2—O3	91.3 (2)	C16—C9—H9B	108.9
C14—Rh2—O3	156.6 (2)	H9A—C9—H9B	107.7
C11—Rh2—O3	92.50 (19)	C11—C10—C9	125.8 (5)
C15—Rh2—O3	164.7 (3)	C11—C10—Rh2	71.0 (3)
O4—Rh2—O3	87.86 (15)	C9—C10—Rh2	110.8 (4)
O6—S1—O5	114.2 (3)	C11—C10—H10	117.1
O6—S1—O7	114.2 (3)	C9—C10—H10	117.1
O5—S1—O7	114.6 (3)	Rh2—C10—H10	88.1
O6—S1—C17	104.2 (5)	C10—C11—C12	123.0 (5)
O5—S1—C17	104.7 (4)	C10—C11—Rh2	70.0 (3)
O7—S1—C17	103.1 (3)	C12—C11—Rh2	113.3 (4)
O8—S2—O9	116.0 (3)	C10—C11—H11	118.5
O8—S2—O10	115.4 (3)	C12—C11—H11	118.5
O9—S2—O10	112.4 (2)	Rh2—C11—H11	86.8
O8—S2—C18	104.4 (3)	C11—C12—C13	111.8 (5)
O9—S2—C18	102.9 (3)	C11—C12—H12A	109.3
O10—S2—C18	103.6 (4)	C13—C12—H12A	109.3
Rh1—O1—H01A	121 (6)	C11—C12—H12B	109.3
Rh1—O1—H01B	119 (5)	C13—C12—H12B	109.3
H01A—O1—H01B	111 (5)	H12A—C12—H12B	107.9
Rh1—O2—H02A	120 (6)	C14—C13—C12	112.6 (5)
Rh1—O2—H02B	123 (6)	C14—C13—H13A	109.1
H02A—O2—H02B	107 (9)	C12—C13—H13A	109.1
Rh2—O3—H03A	123 (5)	C14—C13—H13B	109.1
Rh2—O3—H03B	122 (5)	C12—C13—H13B	109.1
H03A—O3—H03B	109 (9)	H13A—C13—H13B	107.8
Rh2—O4—H04A	121 (6)	C15—C14—C13	125.1 (5)
Rh2—O4—H04B	118 (6)	C15—C14—Rh2	71.5 (3)
H04A—O4—H04B	110 (5)	C13—C14—Rh2	111.2 (4)
C2—C1—C8	123.3 (6)	C15—C14—H14	117.5
C2—C1—Rh1	70.4 (3)	C13—C14—H14	117.5
C8—C1—Rh1	113.2 (4)	Rh2—C14—H14	87.2
C2—C1—H1	118.3	C14—C15—C16	123.8 (5)
C8—C1—H1	118.3	C14—C15—Rh2	69.8 (3)
Rh1—C1—H1	86.4	C16—C15—Rh2	113.3 (4)
C1—C2—C3	126.6 (6)	C14—C15—H15	118.1
C1—C2—Rh1	71.0 (3)	C16—C15—H15	118.1
C3—C2—Rh1	110.5 (4)	Rh2—C15—H15	86.9
C1—C2—H2	116.7	C9—C16—C15	111.1 (5)
C3—C2—H2	116.7	C9—C16—H16A	109.4
Rh1—C2—H2	88.5	C15—C16—H16A	109.4
C4—C3—C2	113.3 (6)	C9—C16—H16B	109.4
C4—C3—H3A	108.9	C15—C16—H16B	109.4
C2—C3—H3A	108.9	H16A—C16—H16B	108.0
C4—C3—H3B	108.9	F1—C17—F3	108.6 (10)
C2—C3—H3B	108.9	F1—C17—F2	109.1 (9)
H3A—C3—H3B	107.7	F3—C17—F2	108.0 (7)
C3—C4—C5	111.8 (6)	F1—C17—S1	110.9 (5)
C3—C4—H4A	109.3	F3—C17—S1	110.1 (7)
C5—C4—H4A	109.3	F2—C17—S1	110.2 (8)
C3—C4—H4B	109.3	F6—C18—F4	108.3 (7)
C5—C4—H4B	109.3	F6—C18—F5	108.0 (7)
H4A—C4—H4B	107.9	F4—C18—F5	108.0 (6)
C6—C5—C4	123.3 (6)	F6—C18—S2	110.5 (5)
C6—C5—Rh1	70.2 (3)	F4—C18—S2	111.4 (6)
C4—C5—Rh1	113.8 (4)	F5—C18—S2	110.4 (5)
C6—Rh1—C1—C2	−113.0 (4)	O4—Rh2—C10—C9	−58.0 (8)
C5—Rh1—C1—C2	−75.0 (4)	O3—Rh2—C10—C9	−145.6 (5)
O1—Rh1—C1—C2	86.4 (4)	C9—C10—C11—C12	3.0 (9)
O2—Rh1—C1—C2	175.1 (6)	Rh2—C10—C11—C12	105.4 (5)
C6—Rh1—C1—C8	5.8 (5)	C9—C10—C11—Rh2	−102.4 (6)
C2—Rh1—C1—C8	118.8 (6)	C14—Rh2—C11—C10	113.9 (4)
C5—Rh1—C1—C8	43.8 (5)	C15—Rh2—C11—C10	76.2 (3)
O1—Rh1—C1—C8	−154.7 (5)	O4—Rh2—C11—C10	−179.8 (6)
O2—Rh1—C1—C8	−66.0 (9)	O3—Rh2—C11—C10	−89.0 (3)
C8—C1—C2—C3	−3.7 (10)	C10—Rh2—C11—C12	−118.3 (6)
Rh1—C1—C2—C3	101.8 (6)	C14—Rh2—C11—C12	−4.4 (4)
C8—C1—C2—Rh1	−105.5 (5)	C15—Rh2—C11—C12	−42.1 (5)
C6—Rh1—C2—C1	67.2 (4)	O4—Rh2—C11—C12	61.8 (9)
C5—Rh1—C2—C1	102.9 (4)	O3—Rh2—C11—C12	152.6 (5)
O1—Rh1—C2—C1	−94.8 (4)	C10—C11—C12—C13	−92.3 (7)
O2—Rh1—C2—C1	−176.3 (4)	Rh2—C11—C12—C13	−11.8 (7)
C6—Rh1—C2—C3	−55.8 (5)	C11—C12—C13—C14	28.5 (7)
C5—Rh1—C2—C3	−20.1 (5)	C12—C13—C14—C15	49.8 (7)
C1—Rh1—C2—C3	−123.0 (6)	C12—C13—C14—Rh2	−32.0 (6)
O1—Rh1—C2—C3	142.3 (5)	C10—Rh2—C14—C15	−65.9 (4)
O2—Rh1—C2—C3	60.7 (8)	C11—Rh2—C14—C15	−101.5 (4)
C1—C2—C3—C4	−48.9 (10)	O4—Rh2—C14—C15	94.4 (4)
Rh1—C2—C3—C4	32.1 (9)	O3—Rh2—C14—C15	179.1 (4)
C2—C3—C4—C5	−28.0 (10)	C10—Rh2—C14—C13	55.4 (4)
C3—C4—C5—C6	91.9 (8)	C11—Rh2—C14—C13	19.8 (4)
C3—C4—C5—Rh1	10.7 (8)	C15—Rh2—C14—C13	121.4 (6)
C2—Rh1—C5—C6	−113.3 (4)	O4—Rh2—C14—C13	−144.3 (4)
C1—Rh1—C5—C6	−75.8 (4)	O3—Rh2—C14—C13	−59.6 (7)
O1—Rh1—C5—C6	179.0 (5)	C13—C14—C15—C16	1.7 (9)
O2—Rh1—C5—C6	88.6 (4)	Rh2—C14—C15—C16	105.1 (5)
C6—Rh1—C5—C4	118.6 (6)	C13—C14—C15—Rh2	−103.4 (5)
C2—Rh1—C5—C4	5.4 (5)	C10—Rh2—C15—C14	114.5 (4)
C1—Rh1—C5—C4	42.9 (5)	C11—Rh2—C15—C14	76.5 (4)
O1—Rh1—C5—C4	−62.4 (8)	O4—Rh2—C15—C14	−86.6 (4)
O2—Rh1—C5—C4	−152.8 (5)	O3—Rh2—C15—C14	−178.6 (6)
C4—C5—C6—C7	−3.7 (9)	C10—Rh2—C15—C16	−4.6 (4)
Rh1—C5—C6—C7	102.4 (6)	C14—Rh2—C15—C16	−119.1 (6)
C4—C5—C6—Rh1	−106.1 (6)	C11—Rh2—C15—C16	−42.6 (5)
C2—Rh1—C6—C5	66.8 (4)	O4—Rh2—C15—C16	154.3 (4)
C1—Rh1—C6—C5	102.3 (4)	O3—Rh2—C15—C16	62.3 (9)
O1—Rh1—C6—C5	−179.0 (5)	C10—C9—C16—C15	29.4 (8)
O2—Rh1—C6—C5	−93.4 (4)	C14—C15—C16—C9	−92.5 (7)
C2—Rh1—C6—C7	−55.8 (5)	Rh2—C15—C16—C9	−12.0 (6)
C5—Rh1—C6—C7	−122.6 (6)	O6—S1—C17—F1	−57.1 (10)
C1—Rh1—C6—C7	−20.3 (5)	O5—S1—C17—F1	63.1 (10)
O1—Rh1—C6—C7	58.3 (8)	O7—S1—C17—F1	−176.7 (9)
O2—Rh1—C6—C7	144.0 (5)	O6—S1—C17—F3	63.1 (7)
C5—C6—C7—C8	−49.6 (9)	O5—S1—C17—F3	−176.7 (7)
Rh1—C6—C7—C8	31.5 (8)	O7—S1—C17—F3	−56.5 (8)
C2—C1—C8—C7	90.9 (8)	O6—S1—C17—F2	−177.9 (6)
Rh1—C1—C8—C7	9.8 (8)	O5—S1—C17—F2	−57.7 (6)
C6—C7—C8—C1	−27.0 (9)	O7—S1—C17—F2	62.5 (7)
C16—C9—C10—C11	47.9 (8)	O8—S2—C18—F6	179.8 (7)
C16—C9—C10—Rh2	−33.2 (7)	O9—S2—C18—F6	−58.7 (7)
C14—Rh2—C10—C11	−66.6 (3)	O10—S2—C18—F6	58.6 (7)
C15—Rh2—C10—C11	−101.7 (4)	O8—S2—C18—F4	−59.7 (6)
O4—Rh2—C10—C11	179.9 (5)	O9—S2—C18—F4	61.8 (6)
O3—Rh2—C10—C11	92.3 (3)	O10—S2—C18—F4	179.1 (5)
C14—Rh2—C10—C9	55.5 (5)	O8—S2—C18—F5	60.3 (6)
C11—Rh2—C10—C9	122.1 (6)	O9—S2—C18—F5	−178.2 (5)
C15—Rh2—C10—C9	20.4 (4)	O10—S2—C18—F5	−60.9 (6)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H01A···O7^i	0.89 (7)	1.92 (9)	2.749 (8)	153 (13)
O1—H01B···O5^ii	0.88 (10)	1.84 (10)	2.710 (10)	168 (8)
O2—H02A···O7^i	0.90 (7)	1.90 (10)	2.743 (9)	155 (11)
O2—H02B···O10^iii	0.90 (13)	1.93 (12)	2.766 (10)	155 (8)
O3—H03A···O9	0.88 (8)	1.96 (7)	2.774 (7)	154 (8)
O3—H03B···O9^ii	0.90 (11)	1.89 (11)	2.773 (10)	167 (8)
O4—H04A···O10	0.88 (4)	1.92 (6)	2.748 (7)	154 (9)
O4—H04B···O6^iv	0.89 (12)	1.86 (12)	2.732 (11)	165 (11)

Symmetry codes: (i) x+1, y+1, z; (ii) −x+1, −y, −z+1; (iii) −x+1, −y+1, −z+1; (iv) −x, −y, −z+1.