Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807008665/hb2272sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807008665/hb2272Isup2.hkl |
CCDC reference: 640338
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.010 Å
- R factor = 0.040
- wR factor = 0.098
- Data-to-parameter ratio = 20.1
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.53 Ratio PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.18 Ratio PLAT410_ALERT_2_B Short Intra H...H Contact H0 .. H50 .. 1.81 Ang.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ......... 2 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ir - P2 .. 5.55 su PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C56 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 10 PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 35.00 A 3 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 1
Alert level G REFLT03_ALERT_4_G 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. From the CIF: _diffrn_reflns_theta_max 27.50 From the CIF: _reflns_number_total 11258 Count of symmetry unique reflns 6084 Completeness (_total/calc) 185.04% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 5174 Fraction of Friedel pairs measured 0.850 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 7 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 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: PROCESS in TEXSAN (Rigaku/MSC, 2004); program(s) used to solve structure: DIRDIF99 (Beurskens et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1999); software used to prepare material for publication: modified SHELXL97.
[Ir2ClH2(C6H5S)2(C48H40P2)2]Cl·2C2H4Cl2 | F(000) = 4480 |
Mr = 2231.02 | Dx = 1.513 Mg m−3 |
Orthorhombic, C2221 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: C 2c 2 | Cell parameters from 253402 reflections |
a = 16.8773 (3) Å | θ = 1.5–32.6° |
b = 21.1322 (4) Å | µ = 3.04 mm−1 |
c = 27.4623 (4) Å | T = 100 K |
V = 9794.5 (3) Å3 | Prism, pale yellow |
Z = 4 | 0.29 × 0.09 × 0.08 mm |
Rigaku RAXIS-RAPID Imaging Plate diffractometer | 11258 independent reflections |
Radiation source: normal-focus sealed tube | 10700 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.085 |
Detector resolution: 10.00 pixels mm-1 | θmax = 27.5°, θmin = 2.5° |
ω scans | h = −21→21 |
Absorption correction: numerical (NUMABS; Higashi, 1998) | k = −27→27 |
Tmin = 0.839, Tmax = 0.957 | l = −34→35 |
103545 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)] = 0.040 | H-atom parameters constrained |
wR(F2) = 0.098 | w = 1/[σ2(Fo2) + (0.0487P)2 + 60.5557P] where P = (Fo2 + 2Fc2)/3 |
S = 1.10 | (Δ/σ)max = 0.002 |
11258 reflections | Δρmax = 1.62 e Å−3 |
559 parameters | Δρmin = −1.24 e Å−3 |
6 restraints | Absolute structure: Flack (1983), 5178 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.007 (6) |
Experimental. Indexing was performed from 2 oscillations which were exposed for 6.8 minunites. The camera radiuswas 127.40 mm. Readout performed in the 0.100 mm pixel mode. #1 Phi=0.0, chi=55.0, omega=60.0 to 240.0 with 2.0deg step #2 Phi=180.0, chi=45.0, omega=0.0 to 180.0 with 2.0deg step #4 Phi=180.0, chi=410.0, omega=0.0 to 180.0 with 2.0deg step A total of 270 images, corresponding to 540.0 °. osillation angles, were collected with 3 different goniometer setting. Exposure time was 130 s per degree. The camera radiuswas 127.40 mm. Readout performed in the 0.100 mm pixel mode. 1H NMR (CD2Cl2, 300 MHz, 303 K): δ 5.97–8.20 (m, 66H, Ph + naphthyl + SPh), 2.12 (s, 6H, CH3), 2.10 (s, 6H, CH3), 1.95 (s, 6H, CH3), 1.78 (s, 6H, CH3), -23.00 (dd, 2JH–P = 13.5, 19.2 Hz, 2H, Ir—H), 31P{1H} NMR (CD2Cl2, 121.49 MHz, 303 K): δ 5.7 (m), -8.8 (m). The simulated 31P{1H} NMR spectrum showed a four spin system of AA'BB' pattern. The simulated chemical shifts and the coupling constants were as follows: δ P1: -8.771, P2: -8.763, P3: 5.698, P4: 5.696; 3J12 = 20.78, 2J13 = 9.74, 3J14 = 16.22, 3J23 = 16.08, 2J24 = -0.49, 3J34 = 20.38 Hz. IR (KBr tablet, cm-1): 2265 (br, m, νIr—H). Λ0 = 102.7 S cm2 mol-1 (CH2Cl2, 298 K). Single crystals of (I) suitable for X-ray analysis were grown from a solution in a 1,2-dichloroethane–hexanes mixture (1:1 v/v). Analysis calculated for C108H92Cl2Ir2P4S2·2C2H4Cl2: C 60.29, H 4.52%; found: C 60.00, H 4.47%. [{IrH{(S)-binap}}2(µ-Cl)(µ-SPh)2]Cl [96% yield, m.p. > 397 K (decomposition in a capillary under argon)]. 1H NMR (CD2Cl2, 300 MHz, 303 K): δ 6.05–8.25 (m, 74H, Ph + naphthyl + SPh), -22.75 (dd, 2JH–P = 12.9, 18.7 Hz, 2H, Ir—H), 31P{1H} NMR (CD2Cl2, 121 MHz, 303 K): δ 6.8 (m), -6.5 (m). IR (KBr tablet, cm-1): 2261 (br, m, νIr—H). Λ0 = 62.9 S cm2 mol-1 (CH2Cl2, 298 K). [{IrH{(S)-binap}}2(µ-Cl)(µ-SC6H4CH3-p)2]Cl [quantitative yield, m.p. > 404 K (decomposition in a capillary under argon). 1H NMR (CD2Cl2, 300 MHz, 303 K): δ 6.08–8.24 (m, 72H, Ph + naphthyl + SC6H4CH3-p), 2.24 (s, 6H, CH3), -22.75 (dd, 2JH–P = 13.2, 19.2 Hz, 2H, Ir—H), 31P {1H} NMR (CD2Cl2, 121 MHz, 303 K): δ 6.9 (m), -6.7 (m). IR (KBr tablet, cm-1): 2265 (br, m, νIr—H). Λ0 = S cm2 mol-1 (CH2Cl2, 298 K). [{IrH{(S)-tolbinap}}2(µ-Cl)(µ-SC6H4CH3-p)2]Cl [quantitative yield, m.p. > 465 K (decompition in a capillary under argon). 1H NMR (CD2Cl2, 300 MHz, 308 K: δ 5.96–8.20 (m, 64H, Ph + naphthyl + SC6H4CH3-p), 2.23 (s, 6H, SC6H4CH3-p), 2.12 (s, 6H, CH3), 2.10 (s, 6H, CH3), 1.95 (s, 6H, CH3), 1.80 (s, 6H, CH3), -23.08 (dd, 2JH–P = 13.5, 19.0 Hz, 2H, Ir—H), 31P {1H} NMR (CD2Cl2, 121 MHz, 308 K: δ 5.8 (m), -8.6 (m). IR (KBr tablet, cm-1): 2265 (br, m, νIr–H). Λ0 = 99.6 S cm2 mol-1(CH2Cl2, 298 K). Analysis calculated for C110H96Cl2Ir2P4S2C2H4Cl2: C 60.61, H 4.64%; found: C 60.00, H 4.47%. |
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) 15.5622 (0.0046) x + 6.3759 (0.0115) y - 6.6556 (0.0129) z = 8.8090 (0.0059) * 0.0000 (0.0000) Ir * 0.0000 (0.0000) S * 0.0000 (0.0000) S_$1 Rms deviation of fitted atoms = 0.0000 15.5622 (0.0045) x - 6.3760 (0.0114) y + 6.6556 (0.0130) z = 9.0886 (0.0058) Angle to previous plane (with approximate e.s.d.) = 45.54 (0.03) * 0.0000 (0.0000) Ir_$1 * 0.0000 (0.0000) S * 0.0000 (0.0000) S_$1 Rms deviation of fitted atoms = 0.0000 15.4851 (0.0030) x + 7.1768 (0.0082) y - 5.6837 (0.0105) z = 9.6512 (0.0061) Angle to previous plane (with approximate e.s.d.) = 46.10 (0.03) * -0.0770 (0.0006) P1 * 0.0775 (0.0005) P2 * 0.0812 (0.0006) S * -0.0817 (0.0006) S_$1 0.0157 (0.0008) Ir -2.4123 (0.0019) Cl1 Rms deviation of fitted atoms = 0.0793 15.4851 (0.0030) x - 7.1768 (0.0082) y + 5.6837 (0.0105) z = 8.1582 (0.0063) Angle to previous plane (with approximate e.s.d.) = 46.87 (0.02) * -0.0770 (0.0006) P1_$1 * 0.0775 (0.0005) P2_$1 * -0.0817 (0.0006) S * 0.0812 (0.0006) S_$1 Rms deviation of fitted atoms = 0.0793 - 0.3873(0.0300)x + 21.0254(0.0035)y + 2.6846(0.0402)z = 15.3266(0.0133) Angle to previous plane (with approximate e.s.d.) = 70.20 (0.10) * -0.0443 (0.0047) C1 * -0.0052 (0.0049) C2 * 0.0212 (0.0052) C3 * 0.0197 (0.0057) C4 * -0.0080 (0.0058) C5 * -0.0191 (0.0063) C6 * -0.0163 (0.0059) C7 * 0.0153 (0.0055) C8 * 0.0227 (0.0052) C9 * 0.0140 (0.0045) C10 Rms deviation of fitted atoms = 0.0211 8.7714(0.0290)x + 4.0530(0.0256)y + 22.8633(0.0309)z = 15.2551(0.0178) Angle to previous plane (with approximate e.s.d.) = 74.91 (0.12) * 0.0230 (0.0048) C11 * -0.0066 (0.0054) C12 * -0.0203 (0.0055) C13 * -0.0206 (0.0058) C14 * 0.0126 (0.0059) C15 * 0.0280 (0.0059) C16 * 0.0132 (0.0059) C17 * -0.0266 (0.0058) C18 * -0.0257 (0.0052) C19 * 0.0230 (0.0046) C20 Rms deviation of fitted atoms = 0.0210 - 3.1346(0.0443)x + 20.7488(0.0109)y + 1.0509(0.0789)z = 10.4480(0.0325) Angle to previous plane (with approximate e.s.d.) = 82.90 (0.18) * -0.0012 (0.0044) C35 * 0.0063 (0.0050) C36 * -0.0048 (0.0054) C37 * -0.0021 (0.0051) C38 * 0.0073 (0.0048) C39 * -0.0056 (0.0045) C40 Rms deviation of fitted atoms = 0.0050 8.7714(0.0290)x + 4.0530(0.0256)y + 22.8633(0.0309)z = 15.2551(0.0178) Angle to previous plane (with approximate e.s.d.) = 82.90 (0.18) * 0.0230 (0.0048) C11 * -0.0066 (0.0054) C12 * -0.0203 (0.0055) C13 * -0.0206 (0.0058) C14 * 0.0126 (0.0059) C15 * 0.0280 (0.0059) C16 * 0.0132 (0.0059) C17 * -0.0266 (0.0058) C18 * -0.0257 (0.0052) C19 * 0.0230 (0.0046) C20 Rms deviation of fitted atoms = 0.0210 12.6244(0.0324)x - 13.2160(0.0485)y + 6.1010(0.0734)z = 0.2536(0.0659) Angle to previous plane (with approximate e.s.d.) = 63.01 (0.18) * -0.0182 (0.0044) C28 * 0.0011 (0.0050) C29 * 0.0126 (0.0053) C30 * -0.0093 (0.0051) C31 * -0.0080 (0.0048) C32 * 0.0219 (0.0045) C33 Rms deviation of fitted atoms = 0.0137 5.6299 (0.0455) x + 1.3171 (0.0612) y + 25.8327 (0.0266) z = 15.9828 (0.0469) Angle to previous plane (with approximate e.s.d.) = 65.20 (0.24) * -0.0096 (0.0044) C21 * 0.0014 (0.0051) C22 * 0.0059 (0.0056) C23 * -0.0049 (0.0054) C24 * -0.0034 (0.0049) C25 * 0.0105 (0.0044) C26 Rms deviation of fitted atoms = 0.0067 8.7714 (0.0290) x + 4.0530 (0.0256) y + 22.8633 (0.0309) z = 15.2551 (0.0178) Angle to previous plane (with approximate e.s.d.) = 14.43 (0.26) * 0.0230 (0.0048) C11 * -0.0066 (0.0054) C12 * -0.0203 (0.0055) C13 * -0.0206 (0.0058) C14 * 0.0126 (0.0059) C15 * 0.0280 (0.0059) C16 * 0.0132 (0.0059) C17 * -0.0266 (0.0058) C18 * -0.0257 (0.0052) C19 * 0.0230 (0.0046) C20 Rms deviation of fitted atoms = 0.0210 5.6299 (0.0455) x + 1.3171 (0.0612) y + 25.8327 (0.0266) z = 15.9828 (0.0469) Angle to previous plane (with approximate e.s.d.) = 14.43 (0.26) * -0.0096 (0.0044) C21 * 0.0014 (0.0051) C22 * 0.0059 (0.0056) C23 * -0.0049 (0.0054) C24 * -0.0034 (0.0049) C25 * 0.0105 (0.0044) C26 Rms deviation of fitted atoms = 0.0067 8.7714 (0.0290) x + 4.0530 (0.0256) y + 22.8633 (0.0309) z = 15.2551 (0.0178) Angle to previous plane (with approximate e.s.d.) = 14.43 (0.26) * 0.0230 (0.0048) C11 * -0.0066 (0.0054) C12 * -0.0203 (0.0055) C13 * -0.0206 (0.0058) C14 * 0.0126 (0.0059) C15 * 0.0280 (0.0059) C16 * 0.0132 (0.0059) C17 * -0.0266 (0.0058) C18 * -0.0257 (0.0052) C19 * 0.0230 (0.0046) C20 Rms deviation of fitted atoms = 0.0210 0.2358(0.0499)x - 9.3835 (0.0550)y + 24.6034(0.0353)z = 3.8888(0.0507) Angle to previous plane (with approximate e.s.d.) = 48.09 (0.16) * -0.0039 (0.0046) C42 * -0.0091 (0.0048) C43 * 0.0134 (0.0052) C44 * -0.0048 (0.0052) C45 * -0.0082 (0.0052) C46 * 0.0126 (0.0051) C47 Rms deviation of fitted atoms = 0.0094 - 3.1346(0.0443)x + 20.7488 (0.0109)y + 1.0509(0.0789)z = 10.4480(0.0325) Angle to previous plane (with approximate e.s.d.) = 66.15 (0.23) * -0.0012 (0.0044) C35 * 0.0063 (0.0050) C36 * -0.0048 (0.0054) C37 * -0.0021 (0.0051) C38 * 0.0073 (0.0048) C39 * -0.0056 (0.0045) C40 Rms deviation of fitted atoms = 0.0050 0.2358(0.0499)x - 9.3835(0.0550)y + 24.6034(0.0353)z = 3.8888(0.0507) Angle to previous plane (with approximate e.s.d.) = 66.15 (0.23) * -0.0039 (0.0046) C42 * -0.0091 (0.0048) C43 * 0.0134 (0.0052) C44 * -0.0048 (0.0052) C45 * -0.0082 (0.0052) C46 * 0.0126 (0.0051) C47 Rms deviation of fitted atoms = 0.0094 -1.3203(0.0546)x + 0.6045(0.0726)y + 27.3669(0.0074)z = 14.4383(0.0613) Angle to previous plane (with approximate e.s.d.) = 28.48 (1/5) * -0.0090 (0.0049) C49 * -0.0053 (0.0051) C50 * 0.0130 (0.0060) C51 * -0.0060 (0.0067) C52 * -0.0086 (0.0068) C53 * 0.0159 (0.0060) C54 Rms deviation of fitted atoms = 0.0103 0.2358 (0.0499) x - 9.3835 (0.0550) y + 24.6034 (0.0353) z = 3.8888 (0.0507) Angle to previous plane (with approximate e.s.d.) = 28.48 (1/5) * -0.0039 (0.0046) C42 * -0.0091 (0.0048) C43 * 0.0134 (0.0052) C44 * -0.0048 (0.0052) C45 * -0.0082 (0.0052) C46 * 0.0126 (0.0051) C47 Rms deviation of fitted atoms = 0.0094 |
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. The Friedel pairs reflections were included in the refinements. Six restraints were applied to the solvate molecules (CH2CH2Cl). |
x | y | z | Uiso*/Ueq | ||
Ir | 0.533307 (12) | 0.562118 (10) | 0.461944 (7) | 0.01859 (6) | |
H0 | 0.6262 | 0.5644 | 0.4501 | 0.022* | |
S | 0.57503 (8) | 0.54702 (6) | 0.54504 (5) | 0.0207 (3) | |
Cl1 | 0.41927 (11) | 0.5000 | 0.5000 | 0.0207 (4) | |
Cl2 | 1.0000 | 0.6482 (2) | 0.2500 | 0.0898 (14) | |
P1 | 0.48675 (8) | 0.66185 (7) | 0.47733 (5) | 0.0193 (3) | |
P2 | 0.50500 (9) | 0.56718 (8) | 0.38035 (5) | 0.0223 (3) | |
C1 | 0.3942 (3) | 0.6774 (3) | 0.4444 (2) | 0.0207 (11) | |
C2 | 0.3209 (3) | 0.6747 (3) | 0.4697 (2) | 0.0252 (12) | |
H2 | 0.3209 | 0.6706 | 0.5041 | 0.030* | |
C3 | 0.2506 (3) | 0.6777 (3) | 0.4456 (2) | 0.0277 (13) | |
H3 | 0.2025 | 0.6754 | 0.4636 | 0.033* | |
C4 | 0.2477 (3) | 0.6841 (3) | 0.3946 (2) | 0.0244 (12) | |
C5 | 0.1741 (4) | 0.6847 (3) | 0.3685 (2) | 0.0310 (14) | |
H5 | 0.1257 | 0.6811 | 0.3859 | 0.037* | |
C6 | 0.1727 (4) | 0.6905 (4) | 0.3187 (3) | 0.0371 (15) | |
H6 | 0.1235 | 0.6913 | 0.3018 | 0.045* | |
C7 | 0.2441 (4) | 0.6953 (4) | 0.2929 (2) | 0.0341 (15) | |
H7 | 0.2428 | 0.6987 | 0.2584 | 0.041* | |
C8 | 0.3161 (4) | 0.6951 (3) | 0.3165 (2) | 0.0287 (13) | |
H8 | 0.3637 | 0.6991 | 0.2983 | 0.034* | |
C9 | 0.3192 (4) | 0.6889 (3) | 0.3685 (2) | 0.0223 (11) | |
C10 | 0.3948 (3) | 0.6866 (2) | 0.3938 (2) | 0.0174 (10) | |
C11 | 0.4685 (4) | 0.6962 (3) | 0.36509 (19) | 0.0223 (10) | |
C12 | 0.4841 (4) | 0.7583 (3) | 0.3468 (2) | 0.0261 (13) | |
C13 | 0.4338 (4) | 0.8101 (3) | 0.3563 (3) | 0.0310 (14) | |
H13 | 0.3870 | 0.8038 | 0.3750 | 0.037* | |
C14 | 0.4511 (4) | 0.8689 (3) | 0.3392 (3) | 0.0405 (17) | |
H14 | 0.4156 | 0.9027 | 0.3458 | 0.049* | |
C15 | 0.5202 (5) | 0.8811 (4) | 0.3120 (3) | 0.045 (2) | |
H15 | 0.5320 | 0.9225 | 0.3007 | 0.055* | |
C16 | 0.5700 (5) | 0.8312 (4) | 0.3024 (3) | 0.0415 (18) | |
H16 | 0.6168 | 0.8386 | 0.2841 | 0.050* | |
C17 | 0.5534 (4) | 0.7692 (3) | 0.3191 (2) | 0.0304 (14) | |
C18 | 0.6030 (4) | 0.7178 (4) | 0.3075 (3) | 0.0366 (16) | |
H18 | 0.6483 | 0.7247 | 0.2877 | 0.044* | |
C19 | 0.5874 (4) | 0.6580 (3) | 0.3241 (2) | 0.0284 (13) | |
H19 | 0.6218 | 0.6243 | 0.3154 | 0.034* | |
C20 | 0.5207 (4) | 0.6456 (3) | 0.35404 (19) | 0.0245 (12) | |
C21 | 0.5483 (3) | 0.7301 (3) | 0.4616 (2) | 0.0234 (11) | |
C22 | 0.5159 (3) | 0.7907 (3) | 0.4660 (3) | 0.0329 (14) | |
H22 | 0.4631 | 0.7954 | 0.4774 | 0.039* | |
C23 | 0.5590 (4) | 0.8434 (3) | 0.4541 (3) | 0.0402 (17) | |
H23 | 0.5356 | 0.8840 | 0.4575 | 0.048* | |
C24 | 0.6357 (4) | 0.8386 (4) | 0.4372 (3) | 0.0387 (17) | |
C25 | 0.6688 (4) | 0.7782 (3) | 0.4331 (2) | 0.0325 (15) | |
H25 | 0.7215 | 0.7739 | 0.4215 | 0.039* | |
C26 | 0.6262 (3) | 0.7243 (3) | 0.4457 (2) | 0.0254 (12) | |
H26 | 0.6502 | 0.6838 | 0.4434 | 0.031* | |
C27 | 0.6809 (5) | 0.8958 (4) | 0.4230 (4) | 0.059 (3) | |
H27A | 0.7333 | 0.8833 | 0.4111 | 0.089* | |
H27B | 0.6868 | 0.9236 | 0.4513 | 0.089* | |
H27C | 0.6523 | 0.9183 | 0.3972 | 0.089* | |
C28 | 0.4637 (4) | 0.6754 (2) | 0.5420 (2) | 0.0240 (10) | |
C29 | 0.5009 (4) | 0.7220 (3) | 0.5694 (2) | 0.0301 (13) | |
H29 | 0.5376 | 0.7496 | 0.5540 | 0.036* | |
C30 | 0.4853 (4) | 0.7293 (4) | 0.6192 (3) | 0.0376 (16) | |
H30 | 0.5120 | 0.7613 | 0.6371 | 0.045* | |
C31 | 0.4315 (4) | 0.6904 (4) | 0.6425 (2) | 0.0311 (14) | |
C32 | 0.3953 (4) | 0.6433 (3) | 0.6158 (2) | 0.0301 (13) | |
H32 | 0.3579 | 0.6161 | 0.6311 | 0.036* | |
C33 | 0.4130 (4) | 0.6351 (3) | 0.5664 (2) | 0.0263 (13) | |
H33 | 0.3895 | 0.6010 | 0.5491 | 0.032* | |
C34 | 0.4112 (5) | 0.6996 (5) | 0.6955 (3) | 0.050 (2) | |
H34A | 0.4427 | 0.7345 | 0.7089 | 0.075* | |
H34B | 0.4229 | 0.6607 | 0.7136 | 0.075* | |
H34C | 0.3547 | 0.7096 | 0.6986 | 0.075* | |
C35 | 0.4081 (4) | 0.5471 (3) | 0.3566 (2) | 0.0239 (12) | |
C36 | 0.3966 (4) | 0.5483 (3) | 0.3056 (2) | 0.0337 (15) | |
H36 | 0.4399 | 0.5565 | 0.2844 | 0.040* | |
C37 | 0.3216 (5) | 0.5374 (4) | 0.2870 (3) | 0.0408 (17) | |
H37 | 0.3143 | 0.5375 | 0.2527 | 0.049* | |
C38 | 0.2580 (4) | 0.5264 (3) | 0.3163 (3) | 0.0357 (16) | |
C39 | 0.2692 (4) | 0.5260 (3) | 0.3666 (3) | 0.0319 (15) | |
H39 | 0.2250 | 0.5190 | 0.3874 | 0.038* | |
C40 | 0.3429 (4) | 0.5355 (3) | 0.3867 (2) | 0.0268 (12) | |
H40 | 0.3495 | 0.5342 | 0.4210 | 0.032* | |
C41 | 0.1743 (5) | 0.5188 (4) | 0.2960 (4) | 0.055 (2) | |
H41A | 0.1761 | 0.5191 | 0.2604 | 0.083* | |
H41B | 0.1411 | 0.5539 | 0.3074 | 0.083* | |
H41C | 0.1518 | 0.4787 | 0.3073 | 0.083* | |
C42 | 0.5717 (4) | 0.5132 (3) | 0.3482 (2) | 0.0263 (12) | |
C43 | 0.5442 (4) | 0.4581 (3) | 0.3272 (2) | 0.0308 (14) | |
H43 | 0.4886 | 0.4518 | 0.3245 | 0.037* | |
C44 | 0.5951 (5) | 0.4117 (4) | 0.3099 (3) | 0.0394 (17) | |
H44 | 0.5742 | 0.3736 | 0.2967 | 0.047* | |
C45 | 0.6764 (5) | 0.4208 (4) | 0.3119 (3) | 0.0397 (17) | |
C46 | 0.7038 (4) | 0.4760 (4) | 0.3325 (3) | 0.0380 (16) | |
H46 | 0.7593 | 0.4833 | 0.3341 | 0.046* | |
C47 | 0.6531 (4) | 0.5209 (3) | 0.3510 (3) | 0.0332 (15) | |
H47 | 0.6742 | 0.5578 | 0.3659 | 0.040* | |
C48 | 0.7323 (6) | 0.3706 (5) | 0.2924 (4) | 0.061 (3) | |
H48A | 0.7014 | 0.3356 | 0.2786 | 0.092* | |
H48B | 0.7654 | 0.3546 | 0.3190 | 0.092* | |
H48C | 0.7660 | 0.3890 | 0.2671 | 0.092* | |
C49 | 0.6787 (3) | 0.5619 (3) | 0.5476 (2) | 0.0292 (12) | |
C50 | 0.7371 (4) | 0.5161 (3) | 0.5515 (3) | 0.0339 (15) | |
H50 | 0.7227 | 0.4726 | 0.5514 | 0.041* | |
C51 | 0.8151 (4) | 0.5327 (4) | 0.5556 (3) | 0.0389 (16) | |
H51 | 0.8542 | 0.5007 | 0.5592 | 0.047* | |
C52 | 0.8374 (5) | 0.5951 (4) | 0.5546 (3) | 0.051 (2) | |
H52 | 0.8918 | 0.6062 | 0.5566 | 0.061* | |
C53 | 0.7797 (5) | 0.6423 (4) | 0.5507 (4) | 0.053 (2) | |
H53 | 0.7953 | 0.6855 | 0.5498 | 0.064* | |
C54 | 0.7010 (5) | 0.6268 (3) | 0.5481 (3) | 0.0417 (18) | |
H54 | 0.6618 | 0.6590 | 0.5467 | 0.050* | |
Cl3 | 0.4932 (4) | 0.9211 (4) | 0.5859 (4) | 0.280 (6) | |
Cl4 | 0.2866 (4) | 0.8362 (4) | 0.6344 (4) | 0.340 (8) | |
C55 | 0.4013 (13) | 0.8769 (14) | 0.5843 (8) | 0.228 (13)* | |
H55A | 0.3617 | 0.8977 | 0.5630 | 0.274* | |
H55B | 0.4099 | 0.8330 | 0.5730 | 0.274* | |
C56 | 0.3742 (11) | 0.8788 (11) | 0.6409 (7) | 0.174 (9)* | |
H56A | 0.3648 | 0.9224 | 0.6526 | 0.209* | |
H56B | 0.4126 | 0.8572 | 0.6625 | 0.209* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ir | 0.01902 (9) | 0.02020 (9) | 0.01654 (8) | 0.00008 (9) | 0.00126 (8) | 0.00000 (8) |
S | 0.0217 (6) | 0.0208 (7) | 0.0197 (7) | −0.0011 (5) | −0.0003 (5) | −0.0006 (5) |
Cl1 | 0.0193 (8) | 0.0225 (9) | 0.0202 (9) | 0.000 | 0.000 | 0.0019 (7) |
Cl2 | 0.067 (2) | 0.080 (3) | 0.123 (4) | 0.000 | −0.056 (2) | 0.000 |
P1 | 0.0187 (7) | 0.0211 (7) | 0.0182 (6) | −0.0018 (5) | 0.0020 (5) | 0.0011 (5) |
P2 | 0.0235 (6) | 0.0245 (7) | 0.0190 (6) | −0.0010 (6) | 0.0028 (5) | −0.0014 (6) |
C1 | 0.018 (2) | 0.018 (3) | 0.027 (3) | 0.003 (2) | 0.002 (2) | −0.001 (2) |
C2 | 0.026 (3) | 0.026 (3) | 0.023 (3) | −0.003 (2) | 0.006 (2) | 0.001 (2) |
C3 | 0.017 (3) | 0.033 (3) | 0.033 (3) | −0.001 (2) | 0.007 (2) | 0.003 (3) |
C4 | 0.019 (3) | 0.023 (3) | 0.031 (3) | 0.002 (2) | 0.004 (2) | −0.001 (2) |
C5 | 0.024 (3) | 0.035 (3) | 0.034 (3) | 0.006 (3) | 0.008 (3) | 0.004 (3) |
C6 | 0.028 (3) | 0.050 (4) | 0.034 (4) | 0.004 (3) | −0.007 (3) | 0.000 (3) |
C7 | 0.032 (3) | 0.046 (4) | 0.024 (3) | −0.004 (3) | −0.002 (3) | 0.000 (3) |
C8 | 0.028 (3) | 0.032 (3) | 0.026 (3) | −0.003 (3) | 0.003 (2) | 0.003 (3) |
C9 | 0.032 (3) | 0.013 (2) | 0.021 (3) | 0.006 (2) | 0.007 (2) | 0.002 (2) |
C10 | 0.016 (2) | 0.011 (2) | 0.025 (3) | −0.003 (2) | 0.001 (2) | 0.002 (2) |
C11 | 0.019 (2) | 0.027 (3) | 0.021 (2) | 0.000 (3) | 0.002 (2) | 0.002 (2) |
C12 | 0.028 (3) | 0.025 (3) | 0.025 (3) | −0.007 (2) | −0.007 (2) | 0.006 (2) |
C13 | 0.026 (3) | 0.031 (3) | 0.036 (4) | −0.003 (3) | −0.004 (3) | 0.007 (3) |
C14 | 0.038 (4) | 0.031 (3) | 0.053 (4) | −0.003 (3) | −0.015 (3) | 0.009 (3) |
C15 | 0.045 (5) | 0.046 (4) | 0.046 (4) | −0.022 (4) | −0.012 (3) | 0.022 (3) |
C16 | 0.040 (4) | 0.049 (4) | 0.035 (4) | −0.024 (4) | −0.002 (3) | 0.020 (3) |
C17 | 0.031 (3) | 0.035 (3) | 0.026 (3) | −0.011 (3) | −0.004 (2) | 0.007 (3) |
C18 | 0.034 (4) | 0.051 (4) | 0.025 (3) | −0.015 (3) | 0.007 (3) | 0.007 (3) |
C19 | 0.021 (3) | 0.039 (4) | 0.025 (3) | −0.007 (3) | 0.005 (2) | −0.003 (3) |
C20 | 0.023 (3) | 0.034 (3) | 0.016 (2) | −0.001 (2) | −0.002 (2) | 0.003 (2) |
C21 | 0.024 (3) | 0.029 (3) | 0.018 (2) | −0.005 (2) | −0.005 (2) | 0.001 (2) |
C22 | 0.024 (3) | 0.032 (3) | 0.042 (4) | 0.003 (2) | −0.005 (3) | 0.006 (3) |
C23 | 0.032 (3) | 0.029 (3) | 0.060 (5) | −0.003 (3) | −0.006 (3) | 0.017 (3) |
C24 | 0.029 (3) | 0.035 (4) | 0.052 (4) | −0.011 (3) | −0.009 (3) | 0.019 (3) |
C25 | 0.023 (3) | 0.039 (4) | 0.035 (4) | −0.010 (3) | 0.000 (3) | 0.009 (3) |
C26 | 0.022 (3) | 0.032 (3) | 0.022 (3) | −0.006 (2) | −0.003 (2) | 0.001 (2) |
C27 | 0.037 (4) | 0.046 (5) | 0.095 (7) | −0.017 (4) | −0.012 (4) | 0.030 (5) |
C28 | 0.027 (3) | 0.024 (2) | 0.021 (2) | 0.003 (2) | 0.006 (3) | 0.001 (2) |
C29 | 0.028 (3) | 0.033 (3) | 0.029 (3) | −0.006 (3) | 0.005 (2) | −0.008 (3) |
C30 | 0.035 (4) | 0.048 (4) | 0.030 (3) | −0.010 (3) | 0.002 (3) | −0.014 (3) |
C31 | 0.030 (3) | 0.042 (4) | 0.021 (3) | 0.002 (3) | 0.004 (2) | −0.002 (3) |
C32 | 0.033 (3) | 0.036 (3) | 0.022 (3) | 0.000 (3) | 0.006 (3) | 0.005 (3) |
C33 | 0.025 (3) | 0.030 (3) | 0.024 (3) | 0.000 (2) | 0.003 (2) | −0.001 (2) |
C34 | 0.052 (5) | 0.074 (6) | 0.023 (3) | −0.012 (4) | 0.008 (3) | −0.016 (4) |
C35 | 0.029 (3) | 0.020 (3) | 0.023 (3) | 0.002 (2) | −0.001 (2) | −0.003 (2) |
C36 | 0.037 (3) | 0.043 (4) | 0.022 (3) | −0.006 (3) | −0.001 (3) | −0.003 (3) |
C37 | 0.044 (4) | 0.048 (4) | 0.031 (4) | −0.005 (3) | −0.012 (3) | −0.005 (3) |
C38 | 0.035 (4) | 0.024 (3) | 0.048 (4) | −0.010 (3) | −0.012 (3) | 0.001 (3) |
C39 | 0.029 (3) | 0.026 (3) | 0.041 (4) | −0.009 (3) | −0.001 (3) | 0.009 (3) |
C40 | 0.030 (3) | 0.021 (3) | 0.029 (3) | −0.001 (2) | −0.001 (3) | 0.003 (2) |
C41 | 0.047 (5) | 0.050 (5) | 0.068 (6) | −0.017 (4) | −0.027 (4) | 0.005 (4) |
C42 | 0.027 (3) | 0.030 (3) | 0.021 (3) | 0.007 (3) | 0.003 (2) | −0.001 (2) |
C43 | 0.030 (3) | 0.038 (3) | 0.025 (3) | 0.005 (3) | 0.006 (3) | −0.001 (2) |
C44 | 0.047 (4) | 0.034 (4) | 0.038 (4) | 0.007 (3) | 0.009 (3) | −0.010 (3) |
C45 | 0.042 (4) | 0.044 (4) | 0.033 (4) | 0.016 (3) | 0.006 (3) | 0.003 (3) |
C46 | 0.033 (4) | 0.049 (4) | 0.032 (4) | 0.012 (3) | 0.001 (3) | −0.008 (3) |
C47 | 0.036 (4) | 0.033 (4) | 0.031 (4) | 0.004 (3) | −0.002 (3) | −0.003 (3) |
C48 | 0.057 (5) | 0.059 (6) | 0.067 (6) | 0.031 (5) | 0.007 (5) | −0.021 (5) |
C49 | 0.026 (3) | 0.032 (3) | 0.030 (3) | −0.003 (3) | 0.000 (2) | 0.002 (3) |
C50 | 0.037 (3) | 0.029 (3) | 0.035 (4) | −0.002 (3) | −0.002 (3) | −0.001 (3) |
C51 | 0.034 (4) | 0.038 (4) | 0.045 (4) | 0.000 (3) | 0.000 (3) | −0.006 (3) |
C52 | 0.027 (4) | 0.057 (5) | 0.069 (6) | −0.008 (3) | −0.001 (4) | 0.001 (4) |
C53 | 0.049 (5) | 0.036 (4) | 0.075 (7) | −0.019 (3) | −0.017 (4) | 0.005 (4) |
C54 | 0.038 (4) | 0.026 (3) | 0.061 (5) | −0.003 (3) | −0.010 (4) | 0.000 (3) |
Cl3 | 0.124 (4) | 0.320 (11) | 0.397 (13) | 0.127 (6) | 0.076 (6) | 0.193 (10) |
Cl4 | 0.200 (7) | 0.306 (11) | 0.514 (18) | 0.179 (8) | −0.215 (10) | −0.232 (12) |
Ir—P1 | 2.2885 (15) | C27—H27B | 0.9800 |
Ir—P2 | 2.2937 (14) | C27—H27C | 0.9800 |
Ir—S | 2.4094 (14) | C28—C33 | 1.380 (8) |
Ir—Si | 2.4190 (13) | C28—C29 | 1.389 (9) |
Ir—Cl1 | 2.5534 (14) | C29—C30 | 1.400 (9) |
Ir—Iri | 3.3558 (4) | C29—H29 | 0.9500 |
Ir—H0 | 1.603 | C30—C31 | 1.382 (10) |
S—C49 | 1.779 (6) | C30—H30 | 0.9500 |
S—Iri | 2.4190 (13) | C31—C32 | 1.380 (10) |
Cl1—Iri | 2.5534 (14) | C31—C34 | 1.508 (9) |
P1—C21 | 1.829 (6) | C32—C33 | 1.401 (9) |
P1—C1 | 1.834 (6) | C32—H32 | 0.9500 |
P1—C28 | 1.841 (6) | C33—H33 | 0.9500 |
P2—C35 | 1.811 (6) | C34—H34A | 0.9800 |
P2—C20 | 1.827 (6) | C34—H34B | 0.9800 |
P2—C42 | 1.830 (6) | C34—H34C | 0.9800 |
C1—C10 | 1.404 (8) | C35—C40 | 1.398 (9) |
C1—C2 | 1.421 (8) | C35—C36 | 1.413 (8) |
C2—C3 | 1.359 (9) | C36—C37 | 1.386 (10) |
C2—H2 | 0.9500 | C36—H36 | 0.9500 |
C3—C4 | 1.409 (9) | C37—C38 | 1.361 (11) |
C3—H3 | 0.9500 | C37—H37 | 0.9500 |
C4—C9 | 1.408 (8) | C38—C39 | 1.394 (10) |
C4—C5 | 1.434 (9) | C38—C41 | 1.528 (10) |
C5—C6 | 1.375 (10) | C39—C40 | 1.376 (9) |
C5—H5 | 0.9500 | C39—H39 | 0.9500 |
C6—C7 | 1.402 (10) | C40—H40 | 0.9500 |
C6—H6 | 0.9500 | C41—H41A | 0.9800 |
C7—C8 | 1.377 (9) | C41—H41B | 0.9800 |
C7—H7 | 0.9500 | C41—H41C | 0.9800 |
C8—C9 | 1.436 (8) | C42—C43 | 1.378 (9) |
C8—H8 | 0.9500 | C42—C47 | 1.386 (10) |
C9—C10 | 1.453 (8) | C43—C44 | 1.388 (9) |
C10—C11 | 1.486 (8) | C43—H43 | 0.9500 |
C11—C20 | 1.417 (8) | C44—C45 | 1.387 (11) |
C11—C12 | 1.430 (8) | C44—H44 | 0.9500 |
C12—C13 | 1.410 (9) | C45—C46 | 1.377 (11) |
C12—C17 | 1.414 (9) | C45—C48 | 1.517 (10) |
C13—C14 | 1.360 (10) | C46—C47 | 1.375 (10) |
C13—H13 | 0.9500 | C46—H46 | 0.9500 |
C14—C15 | 1.408 (11) | C47—H47 | 0.9500 |
C14—H14 | 0.9500 | C48—H48A | 0.9800 |
C15—C16 | 1.372 (12) | C48—H48B | 0.9800 |
C15—H15 | 0.9500 | C48—H48C | 0.9800 |
C16—C17 | 1.416 (9) | C49—C50 | 1.385 (9) |
C16—H16 | 0.9500 | C49—C54 | 1.422 (10) |
C17—C18 | 1.409 (11) | C50—C51 | 1.367 (10) |
C18—C19 | 1.367 (10) | C50—H50 | 0.9500 |
C18—H18 | 0.9500 | C51—C52 | 1.372 (11) |
C19—C20 | 1.419 (8) | C51—H51 | 0.9500 |
C19—H19 | 0.9500 | C52—C53 | 1.397 (12) |
C21—C26 | 1.391 (8) | C52—H52 | 0.9500 |
C21—C22 | 1.397 (8) | C53—C54 | 1.371 (11) |
C22—C23 | 1.371 (9) | C53—H53 | 0.9500 |
C22—H22 | 0.9500 | C54—H54 | 0.9500 |
C23—C24 | 1.379 (10) | Cl3—C55 | 1.811 (16) |
C23—H23 | 0.9500 | Cl4—C56 | 1.740 (15) |
C24—C25 | 1.398 (11) | C55—C56 | 1.621 (17) |
C24—C27 | 1.480 (10) | C55—H55A | 0.9900 |
C25—C26 | 1.390 (9) | C55—H55B | 0.9900 |
C25—H25 | 0.9500 | C56—H56A | 0.9900 |
C26—H26 | 0.9500 | C56—H56B | 0.9900 |
C27—H27A | 0.9800 | ||
P1—Ir—P2 | 93.78 (6) | C25—C26—C21 | 119.7 (6) |
P1—Ir—S | 92.72 (5) | C25—C26—H26 | 120.2 |
P2—Ir—S | 172.91 (5) | C21—C26—H26 | 120.2 |
P1—Ir—Si | 173.00 (5) | C24—C27—H27A | 109.5 |
P2—Ir—Si | 91.58 (5) | C24—C27—H27B | 109.5 |
S—Ir—Si | 82.17 (5) | H27A—C27—H27B | 109.5 |
P1—Ir—Cl1 | 97.99 (4) | C24—C27—H27C | 109.5 |
P2—Ir—Cl1 | 105.48 (4) | H27A—C27—H27C | 109.5 |
S—Ir—Cl1 | 76.38 (4) | H27B—C27—H27C | 109.5 |
Si—Ir—Cl1 | 76.22 (4) | C33—C28—C29 | 117.1 (6) |
P1—Ir—Iri | 127.26 (4) | C33—C28—P1 | 120.1 (4) |
P2—Ir—Iri | 130.16 (4) | C29—C28—P1 | 122.5 (5) |
S—Ir—Iri | 46.09 (3) | C28—C29—C30 | 121.5 (6) |
Si—Ir—Iri | 45.85 (3) | C28—C29—H29 | 119.3 |
Cl1—Ir—Iri | 48.92 (3) | C30—C29—H29 | 119.3 |
P1—Ir—H0 | 110.2 | C31—C30—C29 | 120.7 (6) |
P2—Ir—H0 | 90.2 | C31—C30—H30 | 119.7 |
S—Ir—H0 | 84.9 | C29—C30—H30 | 119.7 |
Si—Ir—H0 | 74.2 | C32—C31—C30 | 118.3 (6) |
Cl1—Ir—H0 | 146.8 | C32—C31—C34 | 120.4 (7) |
Iri—Ir—H0 | 98.7 | C30—C31—C34 | 121.3 (7) |
C49—S—Ir | 107.5 (2) | C31—C32—C33 | 120.7 (6) |
C49—S—Iri | 117.3 (2) | C31—C32—H32 | 119.7 |
Ir—S—Iri | 88.06 (4) | C33—C32—H32 | 119.7 |
Ir—Cl1—Iri | 82.16 (5) | C28—C33—C32 | 121.7 (6) |
C21—P1—C1 | 103.1 (3) | C28—C33—H33 | 119.2 |
C21—P1—C28 | 103.0 (3) | C32—C33—H33 | 119.2 |
C1—P1—C28 | 105.6 (3) | C31—C34—H34A | 109.5 |
C21—P1—Ir | 119.18 (19) | C31—C34—H34B | 109.5 |
C1—P1—Ir | 111.47 (19) | H34A—C34—H34B | 109.5 |
C28—P1—Ir | 113.20 (18) | C31—C34—H34C | 109.5 |
C35—P2—C20 | 101.6 (3) | H34A—C34—H34C | 109.5 |
C35—P2—C42 | 103.6 (3) | H34B—C34—H34C | 109.5 |
C20—P2—C42 | 106.6 (3) | C40—C35—C36 | 118.7 (6) |
C35—P2—Ir | 122.0 (2) | C40—C35—P2 | 122.6 (5) |
C20—P2—Ir | 113.48 (19) | C36—C35—P2 | 118.5 (5) |
C42—P2—Ir | 108.4 (2) | C37—C36—C35 | 119.3 (6) |
C10—C1—C2 | 119.7 (5) | C37—C36—H36 | 120.4 |
C10—C1—P1 | 120.5 (4) | C35—C36—H36 | 120.4 |
C2—C1—P1 | 119.6 (4) | C38—C37—C36 | 122.0 (7) |
C3—C2—C1 | 121.4 (6) | C38—C37—H37 | 119.0 |
C3—C2—H2 | 119.3 | C36—C37—H37 | 119.0 |
C1—C2—H2 | 119.3 | C37—C38—C39 | 118.8 (6) |
C2—C3—C4 | 121.2 (5) | C37—C38—C41 | 122.1 (7) |
C2—C3—H3 | 119.4 | C39—C38—C41 | 119.0 (7) |
C4—C3—H3 | 119.4 | C40—C39—C38 | 121.2 (7) |
C9—C4—C3 | 118.9 (5) | C40—C39—H39 | 119.4 |
C9—C4—C5 | 119.2 (6) | C38—C39—H39 | 119.4 |
C3—C4—C5 | 121.9 (5) | C39—C40—C35 | 120.1 (6) |
C6—C5—C4 | 120.9 (6) | C39—C40—H40 | 120.0 |
C6—C5—H5 | 119.5 | C35—C40—H40 | 120.0 |
C4—C5—H5 | 119.5 | C38—C41—H41A | 109.5 |
C5—C6—C7 | 119.6 (6) | C38—C41—H41B | 109.5 |
C5—C6—H6 | 120.2 | H41A—C41—H41B | 109.5 |
C7—C6—H6 | 120.2 | C38—C41—H41C | 109.5 |
C8—C7—C6 | 121.4 (6) | H41A—C41—H41C | 109.5 |
C8—C7—H7 | 119.3 | H41B—C41—H41C | 109.5 |
C6—C7—H7 | 119.3 | C43—C42—C47 | 117.1 (6) |
C7—C8—C9 | 120.1 (6) | C43—C42—P2 | 121.4 (5) |
C7—C8—H8 | 119.9 | C47—C42—P2 | 120.6 (5) |
C9—C8—H8 | 119.9 | C42—C43—C44 | 122.0 (7) |
C4—C9—C8 | 118.8 (6) | C42—C43—H43 | 119.0 |
C4—C9—C10 | 120.5 (5) | C44—C43—H43 | 119.0 |
C8—C9—C10 | 120.7 (5) | C45—C44—C43 | 120.1 (7) |
C1—C10—C9 | 118.1 (5) | C45—C44—H44 | 119.9 |
C1—C10—C11 | 123.3 (5) | C43—C44—H44 | 119.9 |
C9—C10—C11 | 118.5 (5) | C46—C45—C44 | 117.7 (7) |
C20—C11—C12 | 120.2 (6) | C46—C45—C48 | 122.0 (8) |
C20—C11—C10 | 122.1 (5) | C44—C45—C48 | 120.3 (8) |
C12—C11—C10 | 117.7 (5) | C47—C46—C45 | 121.8 (7) |
C13—C12—C17 | 118.1 (6) | C47—C46—H46 | 119.1 |
C13—C12—C11 | 122.5 (6) | C45—C46—H46 | 119.1 |
C17—C12—C11 | 119.4 (6) | C46—C47—C42 | 121.1 (7) |
C14—C13—C12 | 121.1 (7) | C46—C47—H47 | 119.5 |
C14—C13—H13 | 119.5 | C42—C47—H47 | 119.5 |
C12—C13—H13 | 119.5 | C45—C48—H48A | 109.5 |
C13—C14—C15 | 121.9 (7) | C45—C48—H48B | 109.5 |
C13—C14—H14 | 119.1 | H48A—C48—H48B | 109.5 |
C15—C14—H14 | 119.1 | C45—C48—H48C | 109.5 |
C16—C15—C14 | 117.9 (6) | H48A—C48—H48C | 109.5 |
C16—C15—H15 | 121.0 | H48B—C48—H48C | 109.5 |
C14—C15—H15 | 121.0 | C50—C49—C54 | 119.0 (6) |
C15—C16—C17 | 121.8 (7) | C50—C49—S | 125.4 (5) |
C15—C16—H16 | 119.1 | C54—C49—S | 115.5 (5) |
C17—C16—H16 | 119.1 | C51—C50—C49 | 120.8 (7) |
C18—C17—C12 | 119.1 (6) | C51—C50—H50 | 119.6 |
C18—C17—C16 | 121.6 (6) | C49—C50—H50 | 119.6 |
C12—C17—C16 | 119.3 (7) | C50—C51—C52 | 120.6 (7) |
C19—C18—C17 | 121.5 (6) | C50—C51—H51 | 119.7 |
C19—C18—H18 | 119.2 | C52—C51—H51 | 119.7 |
C17—C18—H18 | 119.2 | C51—C52—C53 | 119.8 (7) |
C18—C19—C20 | 121.1 (6) | C51—C52—H52 | 120.1 |
C18—C19—H19 | 119.4 | C53—C52—H52 | 120.1 |
C20—C19—H19 | 119.4 | C54—C53—C52 | 120.5 (7) |
C11—C20—C19 | 118.5 (6) | C54—C53—H53 | 119.7 |
C11—C20—P2 | 120.6 (4) | C52—C53—H53 | 119.7 |
C19—C20—P2 | 120.8 (5) | C53—C54—C49 | 119.2 (7) |
C26—C21—C22 | 118.5 (5) | C53—C54—H54 | 120.4 |
C26—C21—P1 | 122.8 (5) | C49—C54—H54 | 120.4 |
C22—C21—P1 | 118.7 (4) | C56—C55—Cl3 | 101.9 (12) |
C23—C22—C21 | 121.1 (6) | C56—C55—H55A | 111.4 |
C23—C22—H22 | 119.4 | Cl3—C55—H55A | 111.4 |
C21—C22—H22 | 119.4 | C56—C55—H55B | 111.4 |
C22—C23—C24 | 121.3 (7) | Cl3—C55—H55B | 111.4 |
C22—C23—H23 | 119.3 | H55A—C55—H55B | 109.3 |
C24—C23—H23 | 119.3 | C55—C56—Cl4 | 97.4 (11) |
C23—C24—C25 | 117.9 (6) | C55—C56—H56A | 112.3 |
C23—C24—C27 | 120.8 (8) | Cl4—C56—H56A | 112.3 |
C25—C24—C27 | 121.3 (7) | C55—C56—H56B | 112.3 |
C26—C25—C24 | 121.5 (6) | Cl4—C56—H56B | 112.3 |
C26—C25—H25 | 119.3 | H56A—C56—H56B | 109.9 |
C24—C25—H25 | 119.3 | ||
P1—Ir—S—C49 | −99.3 (3) | C10—C11—C20—C19 | 176.4 (5) |
Si—Ir—S—C49 | 85.5 (2) | C12—C11—C20—P2 | 176.0 (4) |
Cl1—Ir—S—C49 | 163.2 (3) | C10—C11—C20—P2 | −6.7 (8) |
Iri—Ir—S—C49 | 118.0 (3) | C18—C19—C20—C11 | 2.2 (9) |
P1—Ir—S—Iri | 142.71 (4) | C18—C19—C20—P2 | −174.7 (5) |
Si—Ir—S—Iri | −32.49 (6) | C35—P2—C20—C11 | 61.0 (5) |
Cl1—Ir—S—Iri | 45.14 (3) | C42—P2—C20—C11 | 169.1 (5) |
P1—Ir—Cl1—Iri | −133.52 (4) | Ir—P2—C20—C11 | −71.7 (5) |
P2—Ir—Cl1—Iri | 130.28 (4) | C35—P2—C20—C19 | −122.2 (5) |
S—Ir—Cl1—Iri | −42.65 (3) | C42—P2—C20—C19 | −14.1 (6) |
Si—Ir—Cl1—Iri | 42.48 (3) | Ir—P2—C20—C19 | 105.1 (5) |
P2—Ir—P1—C21 | −78.0 (2) | C1—P1—C21—C26 | −131.6 (5) |
S—Ir—P1—C21 | 99.2 (2) | C28—P1—C21—C26 | 118.8 (5) |
Cl1—Ir—P1—C21 | 175.8 (2) | Ir—P1—C21—C26 | −7.5 (6) |
Iri—Ir—P1—C21 | 132.4 (2) | C1—P1—C21—C22 | 48.8 (6) |
P2—Ir—P1—C1 | 41.9 (2) | C28—P1—C21—C22 | −60.9 (6) |
S—Ir—P1—C1 | −141.0 (2) | Ir—P1—C21—C22 | 172.9 (4) |
Cl1—Ir—P1—C1 | −64.4 (2) | C26—C21—C22—C23 | 1.2 (10) |
Iri—Ir—P1—C1 | −107.7 (2) | P1—C21—C22—C23 | −179.1 (6) |
P2—Ir—P1—C28 | 160.7 (2) | C21—C22—C23—C24 | 0.2 (12) |
S—Ir—P1—C28 | −22.1 (2) | C22—C23—C24—C25 | −0.8 (12) |
Cl1—Ir—P1—C28 | 54.5 (2) | C22—C23—C24—C27 | 178.1 (8) |
Iri—Ir—P1—C28 | 11.1 (2) | C23—C24—C25—C26 | −0.1 (11) |
P1—Ir—P2—C35 | −85.8 (2) | C27—C24—C25—C26 | −179.0 (7) |
Si—Ir—P2—C35 | 89.7 (2) | C24—C25—C26—C21 | 1.6 (10) |
Cl1—Ir—P2—C35 | 13.6 (2) | C22—C21—C26—C25 | −2.1 (9) |
Iri—Ir—P2—C35 | 62.4 (2) | P1—C21—C26—C25 | 178.3 (5) |
P1—Ir—P2—C20 | 36.2 (2) | C21—P1—C28—C33 | 175.6 (5) |
Si—Ir—P2—C20 | −148.3 (2) | C1—P1—C28—C33 | 67.8 (5) |
Cl1—Ir—P2—C20 | 135.5 (2) | Ir—P1—C28—C33 | −54.4 (5) |
Iri—Ir—P2—C20 | −175.7 (2) | C21—P1—C28—C29 | −10.1 (6) |
P1—Ir—P2—C42 | 154.3 (2) | C1—P1—C28—C29 | −117.9 (6) |
Si—Ir—P2—C42 | −30.2 (2) | Ir—P1—C28—C29 | 119.9 (5) |
Cl1—Ir—P2—C42 | −106.3 (2) | C33—C28—C29—C30 | −2.2 (10) |
Iri—Ir—P2—C42 | −57.5 (2) | P1—C28—C29—C30 | −176.7 (6) |
C21—P1—C1—C10 | 56.6 (5) | C28—C29—C30—C31 | −0.7 (11) |
C28—P1—C1—C10 | 164.3 (4) | C29—C30—C31—C32 | 1.6 (11) |
Ir—P1—C1—C10 | −72.4 (5) | C29—C30—C31—C34 | −177.0 (7) |
C21—P1—C1—C2 | −128.8 (5) | C30—C31—C32—C33 | 0.3 (11) |
C28—P1—C1—C2 | −21.1 (5) | C34—C31—C32—C33 | 179.0 (7) |
Ir—P1—C1—C2 | 102.2 (4) | C29—C28—C33—C32 | 4.2 (9) |
C10—C1—C2—C3 | 3.3 (9) | P1—C28—C33—C32 | 178.8 (5) |
P1—C1—C2—C3 | −171.4 (5) | C31—C32—C33—C28 | −3.4 (10) |
C1—C2—C3—C4 | −0.4 (9) | C20—P2—C35—C40 | −118.8 (5) |
C2—C3—C4—C9 | −1.5 (9) | C42—P2—C35—C40 | 130.7 (5) |
C2—C3—C4—C5 | 177.4 (6) | Ir—P2—C35—C40 | 8.5 (6) |
C9—C4—C5—C6 | −0.6 (10) | C20—P2—C35—C36 | 55.8 (5) |
C3—C4—C5—C6 | −179.5 (7) | C42—P2—C35—C36 | −54.6 (5) |
C4—C5—C6—C7 | 0.6 (11) | Ir—P2—C35—C36 | −176.8 (4) |
C5—C6—C7—C8 | −0.9 (12) | C40—C35—C36—C37 | −0.7 (10) |
C6—C7—C8—C9 | 1.1 (11) | P2—C35—C36—C37 | −175.5 (6) |
C3—C4—C9—C8 | 179.7 (6) | C35—C36—C37—C38 | 1.0 (11) |
C5—C4—C9—C8 | 0.8 (9) | C36—C37—C38—C39 | −0.2 (11) |
C3—C4—C9—C10 | 0.6 (9) | C36—C37—C38—C41 | 175.7 (7) |
C5—C4—C9—C10 | −178.3 (6) | C37—C38—C39—C40 | −0.9 (11) |
C7—C8—C9—C4 | −1.1 (10) | C41—C38—C39—C40 | −177.0 (7) |
C7—C8—C9—C10 | 178.1 (6) | C38—C39—C40—C35 | 1.3 (10) |
C2—C1—C10—C9 | −4.1 (8) | C36—C35—C40—C39 | −0.5 (9) |
P1—C1—C10—C9 | 170.5 (4) | P2—C35—C40—C39 | 174.2 (5) |
C2—C1—C10—C11 | 174.0 (5) | C35—P2—C42—C43 | −21.0 (6) |
P1—C1—C10—C11 | −11.4 (8) | C20—P2—C42—C43 | −127.7 (5) |
C4—C9—C10—C1 | 2.2 (8) | Ir—P2—C42—C43 | 109.8 (5) |
C8—C9—C10—C1 | −176.9 (5) | C35—P2—C42—C47 | 169.8 (6) |
C4—C9—C10—C11 | −176.0 (5) | C20—P2—C42—C47 | 63.1 (6) |
C8—C9—C10—C11 | 4.9 (8) | Ir—P2—C42—C47 | −59.4 (6) |
C1—C10—C11—C20 | 75.2 (7) | C47—C42—C43—C44 | 0.6 (10) |
C9—C10—C11—C20 | −106.7 (6) | P2—C42—C43—C44 | −169.0 (5) |
C1—C10—C11—C12 | −107.4 (6) | C42—C43—C44—C45 | −2.3 (11) |
C9—C10—C11—C12 | 70.6 (7) | C43—C44—C45—C46 | 1.8 (11) |
C20—C11—C12—C13 | 179.4 (6) | C43—C44—C45—C48 | −179.2 (8) |
C10—C11—C12—C13 | 2.0 (9) | C44—C45—C46—C47 | 0.3 (11) |
C20—C11—C12—C17 | −2.3 (8) | C48—C45—C46—C47 | −178.7 (8) |
C10—C11—C12—C17 | −179.7 (5) | C45—C46—C47—C42 | −2.0 (11) |
C17—C12—C13—C14 | 0.3 (10) | C43—C42—C47—C46 | 1.5 (10) |
C11—C12—C13—C14 | 178.6 (6) | P2—C42—C47—C46 | 171.1 (6) |
C12—C13—C14—C15 | −1.0 (11) | Ir—S—C49—C50 | −104.9 (5) |
C13—C14—C15—C16 | 0.8 (11) | Iri—S—C49—C50 | −7.9 (6) |
C14—C15—C16—C17 | −0.1 (11) | Ir—S—C49—C54 | 78.6 (5) |
C13—C12—C17—C18 | −177.5 (6) | Iri—S—C49—C54 | 175.6 (5) |
C11—C12—C17—C18 | 4.1 (9) | C54—C49—C50—C51 | −0.4 (10) |
C13—C12—C17—C16 | 0.4 (9) | S—C49—C50—C51 | −176.8 (6) |
C11—C12—C17—C16 | −177.9 (6) | C49—C50—C51—C52 | −1.7 (12) |
C15—C16—C17—C18 | 177.3 (7) | C50—C51—C52—C53 | 1.7 (14) |
C15—C16—C17—C12 | −0.6 (10) | C51—C52—C53—C54 | 0.4 (15) |
C12—C17—C18—C19 | −2.9 (10) | C52—C53—C54—C49 | −2.4 (14) |
C16—C17—C18—C19 | 179.2 (7) | C50—C49—C54—C53 | 2.5 (11) |
C17—C18—C19—C20 | −0.3 (10) | S—C49—C54—C53 | 179.2 (7) |
C12—C11—C20—C19 | −0.9 (8) | Cl3—C55—C56—Cl4 | 179.6 (14) |
Symmetry code: (i) x, −y+1, −z+1. |
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