Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805018702/ob6535sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805018702/ob6535Isup2.hkl |
CCDC reference: 277740
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.003 Å
- R factor = 0.018
- wR factor = 0.045
- Data-to-parameter ratio = 16.4
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for P2 PLAT432_ALERT_2_C Short Inter X...Y Contact C13 .. C18 .. 3.15 Ang.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: KENX (Sakai, 2002); software used to prepare material for publication: SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), KENX and ORTEPII (Johnson, 1976).
[IrCl(C10H8N2)(C22H17N3)](PF6)2(C2H3N)2 | F(000) = 2112 |
Mr = 1079.27 | ? # Insert any comments here. |
Monoclinic, P21/c | Dx = 1.873 Mg m−3 |
Hall symbol: -P 2ybc | Mo Kα radiation, λ = 0.71073 Å |
a = 11.3701 (5) Å | Cell parameters from 9226 reflections |
b = 19.4632 (8) Å | θ = 2.2–28.3° |
c = 17.7735 (7) Å | µ = 3.74 mm−1 |
β = 103.338 (1)° | T = 100 K |
V = 3827.2 (3) Å3 | Prism, yellow |
Z = 4 | 0.28 × 0.26 × 0.2 mm |
Bruker SMART APEX CCD-detector diffractometer | 8779 independent reflections |
Radiation source: fine-focus sealed tube | 8138 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
Detector resolution: 8.366 pixels mm-1 | θmax = 27.5°, θmin = 2.4° |
ω scans | h = −14→14 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −25→25 |
Tmin = 0.373, Tmax = 0.473 | l = −23→23 |
47376 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.018 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.045 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0241P)2 + 2.5729P] where P = (Fo2 + 2Fc2)/3 |
8779 reflections | (Δ/σ)max = 0.004 |
535 parameters | Δρmax = 0.88 e Å−3 |
0 restraints | Δρmin = −0.48 e Å−3 |
Experimental. The first 50 frames were rescanned at the end of data collection to evaluate any possible decay phenomenon. Since it was judged to be negligible, no decay correction was applied to the data. |
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. Mean-plane data from final SHELXL refinement run:- Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 8.2627 (0.0040) x + 1.0181 (0.0086) y + 8.8660 (0.0081) z = 10.9958 (0.0029) * 0.0384 (0.0006) Cl1 * -0.0411 (0.0007) N2 * 0.0461 (0.0008) N5 * -0.0433 (0.0007) N4 - 0.0011 (0.0007) Ir1 Rms deviation of fitted atoms = 0.0423 -6.5997 (0.0052) x + 11.6974 (0.0088) y + 11.8820 (0.0076) z = 6.4479 (0.0064) Angle to previous plane (with approximate e.s.d.) = 89.20 (0.04) * 0.0355 (0.0008) N3 * -0.0431 (0.0009) N2 * 0.0367 (0.0008) N1 * -0.0291 (0.0006) N4 0.0004 (0.0008) Ir1 Rms deviation of fitted atoms = 0.0365 -7.4474 (0.0066) x + 11.6179 (0.0125) y + 10.6984 (0.0115) z = 4.9773 (0.0117) Angle to previous plane (with approximate e.s.d.) = 6.53 (0.11) * -0.0006 (0.0013) N3 * 0.0043 (0.0013) C11 * -0.0060 (0.0014) C12 * 0.0042 (0.0014) C13 * -0.0006 (0.0014) C14 * -0.0012 (0.0014) C15 Rms deviation of fitted atoms = 0.0035 -6.7037 (0.0070) x + 10.9914 (0.0116) y + 12.4042 (0.0095) z = 6.3486 (0.0094) Angle to previous plane (with approximate e.s.d.) = 7.77 (0.12) * -0.0222 (0.0012) N2 * 0.0119 (0.0013) C6 * 0.0054 (0.0013) C7 * -0.0126 (0.0013) C8 * 0.0034 (0.0013) C9 * 0.0140 (0.0012) C10 Rms deviation of fitted atoms = 0.0131 -9.8624 (0.0048) x + 7.7717 (0.0146) y + 8.6921 (0.0131) z = 0.4484 (0.0135) Angle to previous plane (with approximate e.s.d.) = 24.72 (0.09) * 0.0099 (0.0014) C16 * -0.0054 (0.0014) C17 * -0.0030 (0.0015) C18 * 0.0070 (0.0015) C19 * -0.0024 (0.0015) C20 * -0.0060 (0.0014) C21 Rms deviation of fitted atoms = 0.0061 -6.7037 (0.0070) x + 10.9914 (0.0116) y + 12.4042 (0.0095) z = 6.3486 (0.0094) Angle to previous plane (with approximate e.s.d.) = 24.72 (0.09) * -0.0222 (0.0012) N2 * 0.0119 (0.0013) C6 * 0.0054 (0.0013) C7 * -0.0126 (0.0013) C8 * 0.0034 (0.0013) C9 * 0.0140 (0.0012) C10 Rms deviation of fitted atoms = 0.0131 -6.0393 (0.0075) x + 11.2386 (0.0127) y + 12.9010 (0.0094) z = 7.1161 (0.0062) Angle to previous plane (with approximate e.s.d.) = 4.21 (0.12) * 0.0119 (0.0013) N1 * -0.0027 (0.0013) C1 * -0.0077 (0.0014) C2 * 0.0088 (0.0014) C3 * 0.0004 (0.0013) C4 * -0.0107 (0.0013) C5 Rms deviation of fitted atoms = 0.0082 -7.4474 (0.0066) x + 11.6179 (0.0125) y + 10.6984 (0.0115) z = 4.9773 (0.0117) Angle to previous plane (with approximate e.s.d.) = 11.52 (0.12) * -0.0006 (0.0013) N3 * 0.0043 (0.0013) C11 * -0.0060 (0.0014) C12 * 0.0042 (0.0014) C13 * -0.0006 (0.0014) C14 * -0.0012 (0.0014) C15 Rms deviation of fitted atoms = 0.0035 7.5873 (0.0074) x - 0.8361 (0.0154) y + 10.1229 (0.0127) z = 10.9204 (0.0055) Angle to previous plane (with approximate e.s.d.) = 83.21 (0.06) * -0.0107 (0.0013) N4 * 0.0023 (0.0014) C23 * 0.0082 (0.0016) C24 * -0.0103 (0.0015) C25 * 0.0020 (0.0014) C26 * 0.0085 (0.0014) C27 Rms deviation of fitted atoms = 0.0078 7.6205 (0.0074) x + 1.6901 (0.0163) y + 9.9988 (0.0129) z = 11.3374 (0.0027) Angle to previous plane (with approximate e.s.d.) = 7.45 (0.13) * 0.0089 (0.0013) N5 * -0.0071 (0.0014) C28 * -0.0007 (0.0015) C29 * 0.0067 (0.0015) C30 * -0.0050 (0.0015) C31 * -0.0028 (0.0014) C32 - 3.2351 (0.0024) N7 - 3.3872 (0.0025) C35 Rms deviation of fitted atoms = 0.0059 -6.0393 (0.0075) x + 11.2386 (0.0127) y + 12.9009 (0.0094) z = 10.9842 (0.0097) Angle to previous plane (with approximate e.s.d.) = 81.31 (0.06) * -0.0119 (0.0013) N1_$3 $3 corresponds to –X+1, –Y+1, –Z+1 * 0.0027 (0.0013) C1_$3 * 0.0077 (0.0014) C2_$3 * -0.0088 (0.0014) C3_$3 * -0.0004 (0.0013) C4_$3 * 0.0107 (0.0013) C5_$3 Rms deviation of fitted atoms = 0.0082 -9.8624 (0.0048) x + 7.7717 (0.0146) y + 8.6921 (0.0131) z = 0.4484 (0.0135) Angle to previous plane (with approximate e.s.d.) = 28.91 (0.09) * 0.0099 (0.0014) C16 * -0.0054 (0.0014) C17 * -0.0030 (0.0015) C18 * 0.0070 (0.0015) C19 * -0.0024 (0.0015) C20 * -0.0060 (0.0014) C21 Rms deviation of fitted atoms = 0.0061 -7.4474 (0.0066) x + 11.6179 (0.0125) y + 10.6984 (0.0115) z = 2.4443 (0.0132) Angle to previous plane (with approximate e.s.d.) = 19.25 (0.10) * 0.0006 (0.0013) N3_$2 $2 corresponds to –X+2, –Y+1, –Z+1 * -0.0043 (0.0013) C11_$2 * 0.0060 (0.0014) C12_$2 * -0.0042 (0.0014) C13_$2 * 0.0006 (0.0014) C14_$2 * 0.0012 (0.0014) C15_$2 Rms deviation of fitted atoms = 0.0035 |
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 | ||
Ir1 | 0.657900 (6) | 0.323296 (3) | 0.589845 (4) | 0.01299 (3) | |
Cl1 | 0.57592 (4) | 0.40302 (2) | 0.66155 (3) | 0.02155 (10) | |
P1 | 0.89970 (5) | 0.12826 (3) | 0.81247 (3) | 0.01949 (10) | |
P2 | 0.25051 (5) | 0.09065 (3) | 0.46921 (3) | 0.02187 (11) | |
F1 | 0.97777 (12) | 0.19409 (6) | 0.85015 (8) | 0.0279 (3) | |
F2 | 1.02366 (11) | 0.08827 (6) | 0.81391 (8) | 0.0297 (3) | |
F3 | 0.90231 (12) | 0.09989 (7) | 0.89776 (8) | 0.0337 (3) | |
F4 | 0.82443 (12) | 0.06233 (7) | 0.77601 (8) | 0.0326 (3) | |
F5 | 0.77844 (12) | 0.16958 (7) | 0.81207 (8) | 0.0304 (3) | |
F6 | 0.89804 (13) | 0.15656 (7) | 0.72771 (7) | 0.0298 (3) | |
F7 | 0.39321 (14) | 0.08746 (13) | 0.48916 (10) | 0.0717 (7) | |
F8 | 0.24581 (17) | 0.03238 (8) | 0.53106 (9) | 0.0488 (4) | |
F9 | 0.24481 (14) | 0.03308 (7) | 0.40338 (8) | 0.0356 (3) | |
F10 | 0.10653 (13) | 0.09444 (9) | 0.44775 (9) | 0.0463 (4) | |
F11 | 0.25260 (17) | 0.14770 (8) | 0.40475 (9) | 0.0466 (4) | |
F12 | 0.25496 (17) | 0.14789 (9) | 0.53353 (9) | 0.0505 (4) | |
N1 | 0.50573 (15) | 0.32992 (8) | 0.50186 (10) | 0.0158 (3) | |
N2 | 0.70344 (14) | 0.40216 (8) | 0.53383 (9) | 0.0141 (3) | |
N3 | 0.82225 (14) | 0.34688 (8) | 0.66087 (9) | 0.0151 (3) | |
N4 | 0.60644 (14) | 0.23791 (8) | 0.64284 (9) | 0.0156 (3) | |
N5 | 0.73059 (14) | 0.24736 (8) | 0.53614 (9) | 0.0152 (3) | |
N6 | 0.2687 (2) | 0.03871 (11) | 0.72617 (12) | 0.0363 (5) | |
N7 | 0.5313 (2) | 0.20600 (12) | 0.37058 (12) | 0.0350 (5) | |
C1 | 0.40672 (18) | 0.29036 (10) | 0.48883 (12) | 0.0187 (4) | |
H1 | 0.4051 | 0.2525 | 0.5205 | 0.022* | |
C2 | 0.30661 (18) | 0.30399 (11) | 0.42970 (12) | 0.0198 (4) | |
H2 | 0.2392 | 0.2755 | 0.4218 | 0.024* | |
C3 | 0.30781 (18) | 0.36029 (10) | 0.38251 (12) | 0.0199 (4) | |
H3 | 0.2406 | 0.3707 | 0.3433 | 0.024* | |
C4 | 0.41093 (18) | 0.40129 (10) | 0.39441 (11) | 0.0185 (4) | |
H4 | 0.4138 | 0.4391 | 0.3629 | 0.022* | |
C5 | 0.50900 (17) | 0.38494 (10) | 0.45370 (11) | 0.0161 (4) | |
C6 | 0.62201 (17) | 0.42561 (10) | 0.47180 (11) | 0.0156 (4) | |
C7 | 0.64815 (17) | 0.48362 (10) | 0.43400 (11) | 0.0166 (4) | |
H7 | 0.5929 | 0.4996 | 0.3905 | 0.020* | |
C8 | 0.75789 (17) | 0.51851 (9) | 0.46093 (11) | 0.0156 (4) | |
C9 | 0.83795 (17) | 0.49349 (9) | 0.52766 (11) | 0.0154 (4) | |
H9 | 0.9107 | 0.5159 | 0.5474 | 0.018* | |
C10 | 0.80783 (16) | 0.43524 (9) | 0.56386 (11) | 0.0146 (3) | |
C11 | 0.87543 (17) | 0.40364 (9) | 0.63671 (11) | 0.0150 (3) | |
C12 | 0.98179 (17) | 0.43030 (10) | 0.68083 (11) | 0.0174 (4) | |
H12 | 1.0177 | 0.4682 | 0.6634 | 0.021* | |
C13 | 1.03456 (18) | 0.40020 (10) | 0.75121 (11) | 0.0196 (4) | |
H13 | 1.1053 | 0.4181 | 0.7819 | 0.023* | |
C14 | 0.98060 (19) | 0.34321 (11) | 0.77508 (12) | 0.0208 (4) | |
H14 | 1.0152 | 0.3221 | 0.8219 | 0.025* | |
C15 | 0.87431 (19) | 0.31771 (10) | 0.72872 (12) | 0.0190 (4) | |
H15 | 0.8382 | 0.2794 | 0.7452 | 0.023* | |
C16 | 0.78352 (17) | 0.58190 (10) | 0.42145 (11) | 0.0165 (4) | |
C17 | 0.72651 (18) | 0.59409 (11) | 0.34411 (12) | 0.0204 (4) | |
H17 | 0.6766 | 0.5606 | 0.3161 | 0.024* | |
C18 | 0.74361 (19) | 0.65565 (11) | 0.30873 (13) | 0.0239 (4) | |
H18 | 0.7046 | 0.6629 | 0.2573 | 0.029* | |
C19 | 0.81818 (19) | 0.70669 (11) | 0.34886 (13) | 0.0236 (4) | |
C20 | 0.8766 (2) | 0.69398 (11) | 0.42546 (13) | 0.0223 (4) | |
H20 | 0.9276 | 0.7273 | 0.4531 | 0.027* | |
C21 | 0.86021 (18) | 0.63254 (10) | 0.46137 (12) | 0.0194 (4) | |
H21 | 0.9007 | 0.6250 | 0.5125 | 0.023* | |
C22 | 0.8356 (2) | 0.77405 (12) | 0.31078 (15) | 0.0328 (5) | |
H22A | 0.8087 | 0.7695 | 0.2557 | 0.049* | |
H22B | 0.9196 | 0.7863 | 0.3238 | 0.049* | |
H22C | 0.7894 | 0.8092 | 0.3286 | 0.049* | |
C23 | 0.53831 (18) | 0.23835 (11) | 0.69522 (12) | 0.0204 (4) | |
H23 | 0.5182 | 0.2802 | 0.7142 | 0.024* | |
C24 | 0.4971 (2) | 0.17803 (11) | 0.72168 (13) | 0.0244 (4) | |
H24 | 0.4506 | 0.1795 | 0.7583 | 0.029* | |
C25 | 0.5256 (2) | 0.11595 (11) | 0.69338 (13) | 0.0250 (4) | |
H25 | 0.4967 | 0.0752 | 0.7096 | 0.030* | |
C26 | 0.59800 (19) | 0.11485 (10) | 0.64025 (12) | 0.0220 (4) | |
H26 | 0.6194 | 0.0734 | 0.6211 | 0.026* | |
C27 | 0.63775 (18) | 0.17659 (9) | 0.61620 (11) | 0.0163 (4) | |
C28 | 0.71282 (18) | 0.18207 (9) | 0.55912 (11) | 0.0165 (4) | |
C29 | 0.76399 (19) | 0.12637 (11) | 0.53018 (12) | 0.0223 (4) | |
H29 | 0.7521 | 0.0821 | 0.5467 | 0.027* | |
C30 | 0.8332 (2) | 0.13708 (11) | 0.47633 (13) | 0.0264 (5) | |
H30 | 0.8688 | 0.1002 | 0.4567 | 0.032* | |
C31 | 0.8486 (2) | 0.20341 (12) | 0.45227 (13) | 0.0255 (4) | |
H31 | 0.8936 | 0.2116 | 0.4156 | 0.031* | |
C32 | 0.79635 (18) | 0.25742 (11) | 0.48315 (12) | 0.0205 (4) | |
H32 | 0.8070 | 0.3019 | 0.4669 | 0.025* | |
C33 | 0.1741 (2) | 0.04024 (12) | 0.68685 (13) | 0.0281 (5) | |
C34 | 0.0544 (2) | 0.04416 (13) | 0.63618 (14) | 0.0327 (5) | |
H34A | 0.0010 | 0.0677 | 0.6622 | 0.049* | |
H34B | 0.0245 | −0.0014 | 0.6227 | 0.049* | |
H34C | 0.0585 | 0.0688 | 0.5901 | 0.049* | |
C35 | 0.5309 (2) | 0.14744 (13) | 0.36556 (13) | 0.0286 (5) | |
C36 | 0.5298 (2) | 0.07291 (13) | 0.35768 (14) | 0.0350 (5) | |
H36A | 0.4485 | 0.0575 | 0.3373 | 0.053* | |
H36B | 0.5608 | 0.0523 | 0.4074 | 0.053* | |
H36C | 0.5794 | 0.0598 | 0.3231 | 0.053* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ir1 | 0.01342 (4) | 0.01063 (4) | 0.01489 (4) | −0.00068 (2) | 0.00320 (3) | 0.00123 (2) |
Cl1 | 0.0239 (2) | 0.0170 (2) | 0.0250 (2) | 0.00375 (18) | 0.00815 (19) | −0.00008 (18) |
P1 | 0.0190 (2) | 0.0168 (2) | 0.0214 (3) | 0.00117 (19) | 0.00196 (19) | 0.00291 (19) |
P2 | 0.0240 (3) | 0.0208 (3) | 0.0201 (3) | −0.0007 (2) | 0.0038 (2) | −0.0015 (2) |
F1 | 0.0301 (7) | 0.0203 (6) | 0.0308 (7) | −0.0041 (5) | 0.0019 (5) | −0.0016 (5) |
F2 | 0.0217 (6) | 0.0223 (6) | 0.0437 (8) | 0.0048 (5) | 0.0046 (6) | 0.0012 (6) |
F3 | 0.0308 (7) | 0.0419 (8) | 0.0266 (7) | −0.0056 (6) | 0.0026 (5) | 0.0140 (6) |
F4 | 0.0270 (7) | 0.0219 (6) | 0.0432 (8) | −0.0043 (5) | −0.0032 (6) | −0.0011 (6) |
F5 | 0.0236 (7) | 0.0351 (8) | 0.0316 (7) | 0.0093 (5) | 0.0043 (5) | −0.0017 (6) |
F6 | 0.0389 (8) | 0.0280 (7) | 0.0229 (6) | 0.0029 (6) | 0.0080 (6) | 0.0042 (5) |
F7 | 0.0254 (8) | 0.150 (2) | 0.0361 (9) | 0.0017 (10) | 0.0004 (7) | −0.0112 (11) |
F8 | 0.0861 (13) | 0.0346 (8) | 0.0308 (8) | 0.0147 (8) | 0.0236 (8) | 0.0111 (6) |
F9 | 0.0586 (9) | 0.0235 (7) | 0.0255 (7) | 0.0069 (6) | 0.0115 (6) | −0.0031 (5) |
F10 | 0.0258 (8) | 0.0691 (11) | 0.0433 (9) | 0.0029 (7) | 0.0067 (6) | −0.0041 (8) |
F11 | 0.0790 (12) | 0.0259 (7) | 0.0368 (8) | −0.0158 (8) | 0.0171 (8) | 0.0021 (6) |
F12 | 0.0731 (12) | 0.0410 (9) | 0.0379 (9) | −0.0106 (8) | 0.0139 (8) | −0.0198 (7) |
N1 | 0.0151 (8) | 0.0139 (8) | 0.0184 (8) | −0.0009 (6) | 0.0038 (6) | −0.0008 (6) |
N2 | 0.0164 (8) | 0.0109 (7) | 0.0145 (7) | −0.0004 (6) | 0.0023 (6) | 0.0011 (6) |
N3 | 0.0156 (8) | 0.0130 (7) | 0.0163 (8) | 0.0007 (6) | 0.0029 (6) | 0.0014 (6) |
N4 | 0.0150 (8) | 0.0138 (7) | 0.0171 (8) | −0.0006 (6) | 0.0018 (6) | 0.0023 (6) |
N5 | 0.0138 (7) | 0.0137 (7) | 0.0173 (8) | −0.0007 (6) | 0.0018 (6) | −0.0004 (6) |
N6 | 0.0381 (12) | 0.0396 (12) | 0.0292 (10) | 0.0040 (9) | 0.0036 (9) | −0.0002 (9) |
N7 | 0.0382 (12) | 0.0375 (12) | 0.0302 (11) | 0.0005 (9) | 0.0093 (9) | 0.0011 (9) |
C1 | 0.0190 (9) | 0.0149 (9) | 0.0229 (10) | −0.0025 (7) | 0.0061 (8) | −0.0014 (7) |
C2 | 0.0159 (9) | 0.0194 (9) | 0.0242 (10) | −0.0038 (7) | 0.0046 (8) | −0.0049 (8) |
C3 | 0.0162 (9) | 0.0222 (10) | 0.0196 (9) | 0.0007 (8) | 0.0007 (7) | −0.0048 (8) |
C4 | 0.0202 (10) | 0.0178 (9) | 0.0175 (9) | 0.0004 (7) | 0.0040 (7) | 0.0002 (7) |
C5 | 0.0174 (9) | 0.0142 (8) | 0.0177 (9) | −0.0016 (7) | 0.0057 (7) | −0.0018 (7) |
C6 | 0.0144 (9) | 0.0155 (9) | 0.0165 (9) | 0.0005 (7) | 0.0030 (7) | 0.0000 (7) |
C7 | 0.0158 (9) | 0.0170 (9) | 0.0162 (9) | 0.0009 (7) | 0.0022 (7) | 0.0031 (7) |
C8 | 0.0173 (9) | 0.0144 (9) | 0.0158 (9) | 0.0008 (7) | 0.0052 (7) | 0.0001 (7) |
C9 | 0.0156 (9) | 0.0136 (8) | 0.0166 (9) | −0.0009 (7) | 0.0031 (7) | −0.0009 (7) |
C10 | 0.0143 (9) | 0.0133 (8) | 0.0164 (9) | 0.0009 (7) | 0.0036 (7) | −0.0008 (7) |
C11 | 0.0166 (9) | 0.0124 (8) | 0.0164 (9) | 0.0010 (7) | 0.0046 (7) | 0.0007 (7) |
C12 | 0.0186 (9) | 0.0148 (9) | 0.0183 (9) | −0.0007 (7) | 0.0035 (7) | 0.0006 (7) |
C13 | 0.0179 (9) | 0.0210 (10) | 0.0183 (9) | −0.0021 (7) | 0.0011 (7) | −0.0019 (7) |
C14 | 0.0222 (10) | 0.0225 (10) | 0.0161 (9) | 0.0021 (8) | 0.0010 (8) | 0.0037 (8) |
C15 | 0.0225 (10) | 0.0151 (9) | 0.0189 (10) | 0.0001 (7) | 0.0040 (8) | 0.0034 (7) |
C16 | 0.0155 (9) | 0.0159 (9) | 0.0187 (9) | 0.0012 (7) | 0.0053 (7) | 0.0034 (7) |
C17 | 0.0161 (9) | 0.0225 (10) | 0.0215 (10) | −0.0023 (7) | 0.0023 (7) | 0.0041 (8) |
C18 | 0.0192 (10) | 0.0284 (11) | 0.0242 (10) | 0.0015 (8) | 0.0052 (8) | 0.0106 (9) |
C19 | 0.0217 (10) | 0.0186 (10) | 0.0333 (12) | 0.0026 (8) | 0.0123 (9) | 0.0088 (9) |
C20 | 0.0237 (10) | 0.0158 (9) | 0.0283 (11) | −0.0023 (8) | 0.0079 (8) | 0.0006 (8) |
C21 | 0.0191 (9) | 0.0173 (9) | 0.0213 (10) | 0.0008 (7) | 0.0036 (8) | 0.0011 (7) |
C22 | 0.0348 (13) | 0.0238 (11) | 0.0428 (14) | 0.0023 (9) | 0.0153 (11) | 0.0150 (10) |
C23 | 0.0206 (10) | 0.0194 (10) | 0.0220 (10) | 0.0008 (8) | 0.0066 (8) | 0.0026 (8) |
C24 | 0.0228 (11) | 0.0279 (11) | 0.0243 (11) | −0.0020 (8) | 0.0092 (9) | 0.0072 (8) |
C25 | 0.0273 (11) | 0.0206 (10) | 0.0272 (11) | −0.0067 (8) | 0.0067 (9) | 0.0071 (8) |
C26 | 0.0263 (11) | 0.0148 (9) | 0.0240 (10) | −0.0021 (8) | 0.0040 (8) | 0.0005 (8) |
C27 | 0.0150 (9) | 0.0163 (9) | 0.0157 (9) | −0.0002 (7) | −0.0002 (7) | 0.0013 (7) |
C28 | 0.0169 (9) | 0.0138 (9) | 0.0173 (9) | −0.0015 (7) | 0.0012 (7) | 0.0011 (7) |
C29 | 0.0263 (11) | 0.0159 (9) | 0.0247 (10) | 0.0019 (8) | 0.0056 (8) | −0.0003 (8) |
C30 | 0.0282 (11) | 0.0234 (11) | 0.0288 (11) | 0.0056 (9) | 0.0094 (9) | −0.0046 (9) |
C31 | 0.0260 (11) | 0.0280 (11) | 0.0259 (11) | 0.0007 (9) | 0.0129 (9) | −0.0021 (9) |
C32 | 0.0206 (10) | 0.0188 (9) | 0.0231 (10) | −0.0033 (8) | 0.0070 (8) | 0.0009 (8) |
C33 | 0.0351 (13) | 0.0256 (11) | 0.0252 (11) | 0.0014 (9) | 0.0105 (10) | −0.0023 (9) |
C34 | 0.0298 (12) | 0.0401 (14) | 0.0288 (12) | −0.0019 (10) | 0.0077 (9) | −0.0057 (10) |
C35 | 0.0252 (11) | 0.0393 (14) | 0.0210 (10) | 0.0006 (10) | 0.0048 (8) | 0.0008 (9) |
C36 | 0.0407 (14) | 0.0346 (13) | 0.0313 (13) | 0.0011 (11) | 0.0114 (11) | −0.0025 (10) |
Ir1—N2 | 1.9629 (15) | C11—C12 | 1.382 (3) |
Ir1—N5 | 2.0354 (16) | C12—C13 | 1.386 (3) |
Ir1—N1 | 2.0512 (17) | C12—H12 | 0.9300 |
Ir1—N3 | 2.0513 (16) | C13—C14 | 1.381 (3) |
Ir1—N4 | 2.0605 (16) | C13—H13 | 0.9300 |
Ir1—Cl1 | 2.3343 (5) | C14—C15 | 1.388 (3) |
P1—F4 | 1.5947 (14) | C14—H14 | 0.9300 |
P1—F5 | 1.5947 (14) | C15—H15 | 0.9300 |
P1—F6 | 1.6001 (13) | C16—C21 | 1.396 (3) |
P1—F2 | 1.6052 (13) | C16—C17 | 1.398 (3) |
P1—F3 | 1.6071 (14) | C17—C18 | 1.388 (3) |
P1—F1 | 1.6137 (13) | C17—H17 | 0.9300 |
P2—F7 | 1.5800 (17) | C18—C19 | 1.391 (3) |
P2—F12 | 1.5886 (15) | C18—H18 | 0.9300 |
P2—F8 | 1.5889 (15) | C19—C20 | 1.392 (3) |
P2—F10 | 1.5946 (15) | C19—C22 | 1.509 (3) |
P2—F11 | 1.5996 (15) | C20—C21 | 1.388 (3) |
P2—F9 | 1.6106 (14) | C20—H20 | 0.9300 |
N1—C1 | 1.339 (2) | C21—H21 | 0.9300 |
N1—C5 | 1.377 (2) | C22—H22A | 0.9600 |
N2—C6 | 1.345 (2) | C22—H22B | 0.9600 |
N2—C10 | 1.348 (2) | C22—H22C | 0.9600 |
N3—C15 | 1.341 (2) | C23—C24 | 1.386 (3) |
N3—C11 | 1.375 (2) | C23—H23 | 0.9300 |
N4—C23 | 1.341 (2) | C24—C25 | 1.376 (3) |
N4—C27 | 1.361 (2) | C24—H24 | 0.9300 |
N5—C32 | 1.345 (2) | C25—C26 | 1.388 (3) |
N5—C28 | 1.364 (2) | C25—H25 | 0.9300 |
N6—C33 | 1.140 (3) | C26—C27 | 1.386 (3) |
N7—C35 | 1.143 (3) | C26—H26 | 0.9300 |
N7—C32 | 3.362 (3) | C27—C28 | 1.473 (3) |
C1—C2 | 1.385 (3) | C28—C29 | 1.384 (3) |
C1—H1 | 0.9300 | C29—C30 | 1.388 (3) |
C2—C3 | 1.382 (3) | C29—H29 | 0.9300 |
C2—H2 | 0.9300 | C30—C31 | 1.384 (3) |
C3—C4 | 1.394 (3) | C30—H30 | 0.9300 |
C3—H3 | 0.9300 | C31—C32 | 1.382 (3) |
C4—C5 | 1.383 (3) | C31—H31 | 0.9300 |
C4—H4 | 0.9300 | C32—H32 | 0.9300 |
C5—C6 | 1.480 (3) | C33—C34 | 1.450 (3) |
C6—C7 | 1.381 (3) | C34—H34A | 0.9600 |
C7—C8 | 1.404 (3) | C34—H34B | 0.9600 |
C7—H7 | 0.9300 | C34—H34C | 0.9600 |
C8—C9 | 1.405 (3) | C35—C36 | 1.457 (3) |
C8—C16 | 1.481 (3) | C36—H36A | 0.9600 |
C9—C10 | 1.385 (3) | C36—H36B | 0.9600 |
C9—H9 | 0.9300 | C36—H36C | 0.9600 |
C10—C11 | 1.479 (3) | ||
C32···N7 | 3.362 (3) | C18···C13i | 3.149 (3) |
C29···C35 | 3.489 (3) | C21···C2ii | 3.251 (3) |
C30···C35 | 3.551 (3) | ||
N2—Ir1—N5 | 98.44 (7) | N3—C11—C12 | 120.99 (17) |
N2—Ir1—N1 | 80.74 (6) | N3—C11—C10 | 115.50 (16) |
N5—Ir1—N1 | 92.89 (6) | C12—C11—C10 | 123.42 (17) |
N2—Ir1—N3 | 80.08 (6) | C11—C12—C13 | 119.55 (18) |
N5—Ir1—N3 | 92.31 (6) | C11—C12—H12 | 120.2 |
N1—Ir1—N3 | 160.66 (6) | C13—C12—H12 | 120.2 |
N2—Ir1—N4 | 176.84 (6) | C14—C13—C12 | 119.10 (18) |
N5—Ir1—N4 | 79.49 (7) | C14—C13—H13 | 120.4 |
N1—Ir1—N4 | 96.93 (6) | C12—C13—H13 | 120.4 |
N3—Ir1—N4 | 102.33 (6) | C13—C14—C15 | 119.51 (18) |
N2—Ir1—Cl1 | 86.69 (5) | C13—C14—H14 | 120.2 |
N5—Ir1—Cl1 | 174.41 (5) | C15—C14—H14 | 120.2 |
N1—Ir1—Cl1 | 90.09 (5) | N3—C15—C14 | 121.72 (18) |
N3—Ir1—Cl1 | 86.39 (5) | N3—C15—H15 | 119.1 |
N4—Ir1—Cl1 | 95.47 (5) | C14—C15—H15 | 119.1 |
F4—P1—F5 | 91.24 (7) | C21—C16—C17 | 118.25 (18) |
F4—P1—F6 | 90.33 (8) | C21—C16—C8 | 121.02 (17) |
F5—P1—F6 | 89.99 (7) | C17—C16—C8 | 120.65 (17) |
F4—P1—F2 | 90.19 (7) | C18—C17—C16 | 120.69 (19) |
F5—P1—F2 | 178.57 (8) | C18—C17—H17 | 119.7 |
F6—P1—F2 | 90.09 (7) | C16—C17—H17 | 119.7 |
F4—P1—F3 | 89.90 (8) | C17—C18—C19 | 121.1 (2) |
F5—P1—F3 | 90.30 (8) | C17—C18—C13i | 93.56 (14) |
F6—P1—F3 | 179.62 (8) | C19—C18—C13i | 88.79 (13) |
F2—P1—F3 | 89.62 (8) | C17—C18—H18 | 119.4 |
F4—P1—F1 | 178.98 (8) | C19—C18—H18 | 119.4 |
F5—P1—F1 | 89.64 (7) | C13i—C18—H18 | 87.6 |
F6—P1—F1 | 90.18 (7) | C18—C19—C20 | 118.12 (19) |
F2—P1—F1 | 88.94 (7) | C18—C19—C22 | 121.2 (2) |
F3—P1—F1 | 89.58 (7) | C20—C19—C22 | 120.7 (2) |
F7—P2—F12 | 90.32 (11) | C21—C20—C19 | 121.2 (2) |
F7—P2—F8 | 90.77 (11) | C21—C20—H20 | 119.4 |
F12—P2—F8 | 90.19 (9) | C19—C20—H20 | 119.4 |
F7—P2—F10 | 179.06 (11) | C20—C21—C16 | 120.59 (19) |
F12—P2—F10 | 90.01 (9) | C20—C21—C2ii | 96.04 (13) |
F8—P2—F10 | 90.11 (10) | C16—C21—C2ii | 100.90 (12) |
F7—P2—F11 | 90.22 (11) | C20—C21—H21 | 119.7 |
F12—P2—F11 | 91.46 (9) | C16—C21—H21 | 119.7 |
F8—P2—F11 | 178.08 (9) | C2ii—C21—H21 | 72.7 |
F10—P2—F11 | 88.89 (9) | C19—C22—H22A | 109.5 |
F7—P2—F9 | 90.16 (10) | C19—C22—H22B | 109.5 |
F12—P2—F9 | 179.37 (10) | H22A—C22—H22B | 109.5 |
F8—P2—F9 | 90.22 (8) | C19—C22—H22C | 109.5 |
F10—P2—F9 | 89.50 (9) | H22A—C22—H22C | 109.5 |
F11—P2—F9 | 88.13 (8) | H22B—C22—H22C | 109.5 |
C1—N1—C5 | 118.81 (17) | N4—C23—C24 | 121.63 (19) |
C1—N1—Ir1 | 128.56 (14) | N4—C23—H23 | 119.2 |
C5—N1—Ir1 | 112.57 (12) | C24—C23—H23 | 119.2 |
C6—N2—C10 | 122.63 (16) | C25—C24—C23 | 119.6 (2) |
C6—N2—Ir1 | 117.95 (13) | C25—C24—H24 | 120.2 |
C10—N2—Ir1 | 118.95 (12) | C23—C24—H24 | 120.2 |
C15—N3—C11 | 119.11 (17) | C24—C25—C26 | 119.26 (19) |
C15—N3—Ir1 | 127.53 (13) | C24—C25—H25 | 120.4 |
C11—N3—Ir1 | 113.05 (12) | C26—C25—H25 | 120.4 |
C23—N4—C27 | 119.09 (17) | C27—C26—C25 | 118.88 (19) |
C23—N4—Ir1 | 125.62 (13) | C27—C26—H26 | 120.6 |
C27—N4—Ir1 | 115.06 (13) | C25—C26—H26 | 120.6 |
C32—N5—C28 | 119.34 (17) | N4—C27—C26 | 121.53 (19) |
C32—N5—Ir1 | 125.03 (13) | N4—C27—C28 | 114.57 (16) |
C28—N5—Ir1 | 115.59 (13) | C26—C27—C28 | 123.88 (18) |
N1—C1—C2 | 122.14 (19) | N5—C28—C29 | 120.95 (19) |
N1—C1—H1 | 118.9 | N5—C28—C27 | 115.03 (16) |
C2—C1—H1 | 118.9 | C29—C28—C27 | 124.01 (17) |
C3—C2—C1 | 119.40 (18) | C28—C29—C30 | 119.51 (19) |
C3—C2—H2 | 120.3 | C28—C29—H29 | 120.2 |
C1—C2—H2 | 120.3 | C30—C29—H29 | 120.2 |
C2—C3—C4 | 119.19 (18) | C31—C30—C29 | 119.01 (19) |
C2—C3—H3 | 120.4 | C31—C30—H30 | 120.5 |
C4—C3—H3 | 120.4 | C29—C30—H30 | 120.5 |
C5—C4—C3 | 119.08 (18) | C32—C31—C30 | 119.41 (19) |
C5—C4—H4 | 120.5 | C32—C31—H31 | 120.3 |
C3—C4—H4 | 120.5 | C30—C31—H31 | 120.3 |
N1—C5—C4 | 121.33 (17) | N5—C32—C31 | 121.76 (19) |
N1—C5—C6 | 115.32 (17) | N5—C32—N7 | 78.85 (11) |
C4—C5—C6 | 123.32 (17) | N5—C32—H32 | 119.1 |
N2—C6—C7 | 119.44 (17) | C31—C32—H32 | 119.1 |
N2—C6—C5 | 113.29 (16) | N6—C33—C34 | 178.4 (3) |
C7—C6—C5 | 127.24 (17) | C33—C34—H34A | 109.5 |
C6—C7—C8 | 120.25 (17) | C33—C34—H34B | 109.5 |
C6—C7—H7 | 119.9 | H34A—C34—H34B | 109.5 |
C8—C7—H7 | 119.9 | C33—C34—H34C | 109.5 |
C7—C8—C9 | 118.15 (17) | H34A—C34—H34C | 109.5 |
C7—C8—C16 | 119.86 (17) | H34B—C34—H34C | 109.5 |
C9—C8—C16 | 121.91 (17) | N7—C35—C36 | 179.0 (3) |
C10—C9—C8 | 119.63 (17) | C35—C36—H36A | 109.5 |
C10—C9—H9 | 120.2 | C35—C36—H36B | 109.5 |
C8—C9—H9 | 120.2 | H36A—C36—H36B | 109.5 |
N2—C10—C9 | 119.79 (17) | C35—C36—H36C | 109.5 |
N2—C10—C11 | 112.36 (16) | H36A—C36—H36C | 109.5 |
C9—C10—C11 | 127.81 (17) | H36B—C36—H36C | 109.5 |
C5—N1—C1—C2 | −1.6 (3) | C7—C8—C16—C17 | −24.1 (3) |
N1—C1—C2—C3 | −0.3 (3) | C9—C8—C16—C17 | 159.12 (18) |
C1—C2—C3—C4 | 1.4 (3) | C21—C16—C17—C18 | −1.6 (3) |
C2—C3—C4—C5 | −0.6 (3) | C8—C16—C17—C18 | 175.23 (18) |
C1—N1—C5—C4 | 2.3 (3) | C16—C17—C18—C19 | 0.4 (3) |
C1—N1—C5—C6 | −179.56 (16) | C16—C17—C18—C13i | 91.10 (19) |
C3—C4—C5—N1 | −1.2 (3) | C17—C18—C19—C20 | 0.8 (3) |
C3—C4—C5—C6 | −179.19 (17) | C13i—C18—C19—C20 | −92.64 (18) |
C10—N2—C6—C7 | 3.9 (3) | C17—C18—C19—C22 | −179.2 (2) |
C10—N2—C6—C5 | −174.24 (16) | C13i—C18—C19—C22 | 87.39 (19) |
N1—C5—C6—N2 | −0.8 (2) | C18—C19—C20—C21 | −0.7 (3) |
C4—C5—C6—N2 | 177.29 (18) | C22—C19—C20—C21 | 179.2 (2) |
N1—C5—C6—C7 | −178.71 (18) | C19—C20—C21—C16 | −0.5 (3) |
C4—C5—C6—C7 | −0.7 (3) | C19—C20—C21—C2ii | −106.94 (19) |
N2—C6—C7—C8 | −1.1 (3) | C17—C16—C21—C20 | 1.6 (3) |
C5—C6—C7—C8 | 176.71 (18) | C8—C16—C21—C20 | −175.16 (18) |
C6—C7—C8—C9 | −1.3 (3) | C17—C16—C21—C2ii | 105.40 (17) |
C6—C7—C8—C16 | −178.13 (17) | C8—C16—C21—C2ii | −71.38 (18) |
C7—C8—C9—C10 | 1.0 (3) | C27—N4—C23—C24 | −1.3 (3) |
C16—C8—C9—C10 | 177.86 (17) | N4—C23—C24—C25 | −0.5 (3) |
C6—N2—C10—C9 | −4.1 (3) | C23—C24—C25—C26 | 1.7 (3) |
C6—N2—C10—C11 | 173.60 (16) | C24—C25—C26—C27 | −1.1 (3) |
C8—C9—C10—N2 | 1.5 (3) | C23—N4—C27—C26 | 1.9 (3) |
C8—C9—C10—C11 | −175.78 (18) | C23—N4—C27—C28 | −179.84 (17) |
C15—N3—C11—C12 | 0.7 (3) | C25—C26—C27—N4 | −0.7 (3) |
C15—N3—C11—C10 | −176.10 (16) | C25—C26—C27—C28 | −178.79 (19) |
N2—C10—C11—N3 | 0.4 (2) | C32—N5—C28—C29 | 1.7 (3) |
C9—C10—C11—N3 | 177.86 (18) | C32—N5—C28—C27 | −178.91 (17) |
N2—C10—C11—C12 | −176.32 (17) | N4—C27—C28—N5 | −5.7 (3) |
C9—C10—C11—C12 | 1.2 (3) | C26—C27—C28—N5 | 172.49 (18) |
N3—C11—C12—C13 | −1.2 (3) | N4—C27—C28—C29 | 173.67 (18) |
C10—C11—C12—C13 | 175.31 (18) | C26—C27—C28—C29 | −8.1 (3) |
C11—C12—C13—C14 | 1.2 (3) | N5—C28—C29—C30 | −0.7 (3) |
C12—C13—C14—C15 | −0.7 (3) | C27—C28—C29—C30 | 179.9 (2) |
C11—N3—C15—C14 | −0.2 (3) | C28—C29—C30—C31 | −0.6 (3) |
C13—C14—C15—N3 | 0.2 (3) | C29—C30—C31—C32 | 1.0 (3) |
C7—C8—C16—C21 | 152.58 (18) | C28—N5—C32—C31 | −1.2 (3) |
C9—C8—C16—C21 | −24.2 (3) | C30—C31—C32—N5 | −0.1 (3) |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+1, −y+1, −z+1. |
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