Undeca­carbon­yl(pyridine-κN)-tetra­hedro-tetra­iridium(4Ir—Ir)

Pardey, A.J.; Moreno, M.A.; Lutz, M.; Haukka, M.; Atencio, R.

doi:10.1107/S1600536806009780

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Undecacarbonyl(pyridine-κN)-tetrahedro-tetrairidium(4Ir—Ir)

A. J. Pardey, M. A. Moreno, M. Lutz, M. Haukka and R. Atencio

The title compound, [Ir₄(C₅H₅N)(CO)₁₁], shows a tetrahedral Ir₄ core in which each Ir atom is linked to three other Ir atoms and three terminal carbonyl groups, except for one Ir atom, which carries two carbonyl ligands and one N-coordinated pyridine molecule. An intricate set of C—H

π hydrogen bonds stabilizes the crystal packing, where the π-systems are those of the C [triple bond]

O bonds of the carbonyl ligands.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806009780/tk2014sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806009780/tk2014Isup2.hkl Contains datablock I

CCDC reference: 605199

checkCIF report

Key indicators

Single-crystal X-ray study
T = 150 K
Mean (C-C) = 0.018 Å
R factor = 0.037
wR factor = 0.090
Data-to-parameter ratio = 13.4

checkCIF/PLATON results

No syntax errors found



Alert level A
ABSTM02_ALERT_3_A  Crystal and compound unsuitable for non-numerical
               corrections. Product of mu and tmid > 3.0
             Value of mu given =    24.523 tmid =     0.150

Author Response: Face indexation of the crystal could not be done.

PLAT060_ALERT_3_A Ratio Tmax/Tmin (Exp-to-Rep) (too) Large .......       3.58

Author Response: ... This kind of cluster commonly presents this problem. The numerical correction was not possible but a multi-scan correction was applied as an alternative.

PLAT065_ALERT_3_A Crystal Requires Numerical Correction mu*tmid ..       3.68

Author Response: A multi-scan correction was applied.


Alert level B
PLAT432_ALERT_2_B Short Inter X...Y Contact  C12    ..  C31     ..       3.10 Ang.
PLAT432_ALERT_2_B Short Inter X...Y Contact  C21    ..  C41     ..       3.09 Ang.
PLAT432_ALERT_2_B Short Inter X...Y Contact  C32    ..  C42     ..       3.06 Ang.

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.22
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         18
PLAT432_ALERT_2_C Short Inter X...Y Contact  C11    ..  C41     ..       3.18 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  C11    ..  C21     ..       3.19 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  C12    ..  C22     ..       3.15 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  C22    ..  C31     ..       3.13 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  C23    ..  C33     ..       3.12 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  C23    ..  C43     ..       3.19 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  C33    ..  C43     ..       3.14 Ang.
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          9
            O12 -C12 -IR1 -C11    94.00  9.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         10
            O12 -C12 -IR1 -N1   -168.00  9.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         11
            O12 -C12 -IR1 -IR2    -7.00  9.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         12
            O12 -C12 -IR1 -IR3   -68.00  9.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         13
            O12 -C12 -IR1 -IR4   -33.00  9.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         14
            O11 -C11 -IR1 -C12    12.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         15
            O11 -C11 -IR1 -N1     15.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         16
            O11 -C11 -IR1 -IR2     2.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         17
            O11 -C11 -IR1 -IR3     2.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         18
            O11 -C11 -IR1 -IR4     4.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         29
            O21 -C21 -IR2 -C23    17.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         30
            O21 -C21 -IR2 -C22     9.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         31
            O21 -C21 -IR2 -IR1     1.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         32
            O21 -C21 -IR2 -IR3     4.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         33
            O21 -C21 -IR2 -IR4     7.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         34
            O23 -C23 -IR2 -C21    71.00 14.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         35
            O23 -C23 -IR2 -C22   173.00 14.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         36
            O23 -C23 -IR2 -IR1   -58.00 14.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         37
            O23 -C23 -IR2 -IR3   -88.00 14.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         38
            O23 -C23 -IR2 -IR4   -27.00 14.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         39
            O22 -C22 -IR2 -C21     9.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         40
            O22 -C22 -IR2 -C23    17.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         41
            O22 -C22 -IR2 -IR1     1.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         42
            O22 -C22 -IR2 -IR3     7.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         43
            O22 -C22 -IR2 -IR4     4.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         67
            O31 -C31 -IR3 -C32     5.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         68
            O31 -C31 -IR3 -C33    16.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         69
            O31 -C31 -IR3 -IR2    10.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         70
            O31 -C31 -IR3 -IR1     4.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         71
            O31 -C31 -IR3 -IR4     7.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         72
            O32 -C32 -IR3 -C31     3.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         73
            O32 -C32 -IR3 -C33    13.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         74
            O32 -C32 -IR3 -IR2    10.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         75
            O32 -C32 -IR3 -IR1     7.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         76
            O32 -C32 -IR3 -IR4    13.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         77
            O33 -C33 -IR3 -C31    18.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         78
            O33 -C33 -IR3 -C32     7.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         79
            O33 -C33 -IR3 -IR2     8.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         80
            O33 -C33 -IR3 -IR1     6.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         81
            O33 -C33 -IR3 -IR4     2.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        128
            O41 -C41 -IR4 -C42  -165.00 13.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        129
            O41 -C41 -IR4 -C43    89.00 14.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        130
            O41 -C41 -IR4 -IR2   -10.00 14.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        131
            O41 -C41 -IR4 -IR1   -70.00 14.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        132
            O41 -C41 -IR4 -IR3   -37.00 14.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        133
            O42 -C42 -IR4 -C41     7.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        134
            O42 -C42 -IR4 -C43    18.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        135
            O42 -C42 -IR4 -IR2     5.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        136
            O42 -C42 -IR4 -IR1     3.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        137
            O42 -C42 -IR4 -IR3     9.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        138
            O43 -C43 -IR4 -C41    15.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        139
            O43 -C43 -IR4 -C42     4.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        140
            O43 -C43 -IR4 -IR2    12.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        141
            O43 -C43 -IR4 -IR1     8.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        142
            O43 -C43 -IR4 -IR3     6.00  0.00   1.555   1.555   1.555   1.555
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.21 Ratio
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          1
              C7 H5 Ir N O2

   3 ALERT level A = In general: serious problem
   3 ALERT level B = Potentially serious problem
  67 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
  10 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
  58 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: DENZO–SCALEPACK (Otwinowski & Minor, 1997); cell refinement: DENZO–SCALEPACK; data reduction: DENZO–SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXTL (Sheldrick, 2001); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Undecacarbonyl(pyridine-κN)-tetrahedro-tetrairidium(4 Ir—Ir) top

Crystal data top

[Ir₄(C₅H₅N)(CO)₁₁]	F(000) = 2016
M_r = 1156.01	D_x = 3.540 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 6184 reflections
a = 8.5042 (1) Å	θ = 2.1–27.8°
b = 13.1544 (2) Å	µ = 24.52 mm⁻¹
c = 19.8188 (4) Å	T = 150 K
β = 101.9766 (7)°	Irregular block, red
V = 2168.82 (6) Å³	0.30 × 0.15 × 0.10 mm
Z = 4

Data collection top

Nonius KappaCCD diffractometer	3866 independent reflections
Radiation source: normal-focus sealed tube	3422 reflections with I > 2σ(I)
Horizonally mounted graphite crystal monochromator	R_int = 0.092
φ and ω scans	θ_max = 25.1°, θ_min = 2.5°
Absorption correction: multi-scan (SHELXTL; Sheldrick, 2001)	h = −10→10
T_min = 0.271, T_max = 0.385	k = −15→15
18728 measured reflections	l = −23→23

Refinement top

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)] = 0.037	Hydrogen site location: calcd
wR(F²) = 0.090	H-atom parameters constrained
S = 1.10	w = 1/[σ²(F_o²) + (0.0451P)² + 5.447P] where P = (F_o² + 2F_c²)/3
3866 reflections	(Δ/σ)_max = 0.001
289 parameters	Δρ_max = 2.27 e Å⁻³
0 restraints	Δρ_min = −2.42 e Å⁻³

Special details top

Experimental. FT–IR data (cm^-1, CaF₂): 2095 (w), 2068 (sh), 2048 (s), 2032 (s) and 2013 (s).

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 (Å²) top

	x	y	z	U_iso*/U_eq
C11	1.1999 (12)	0.4209 (7)	0.6266 (6)	0.027 (3)
C12	0.9749 (12)	0.5347 (7)	0.6833 (6)	0.023 (2)
C21	0.9150 (14)	0.3658 (8)	0.4996 (7)	0.032 (3)
C22	0.6848 (12)	0.4793 (8)	0.5622 (6)	0.025 (2)
C23	0.6227 (13)	0.2643 (8)	0.5236 (6)	0.026 (2)
C31	0.6717 (13)	0.4320 (8)	0.7158 (6)	0.028 (3)
C32	0.8622 (13)	0.2596 (8)	0.7903 (6)	0.027 (3)
C33	0.5855 (13)	0.2160 (8)	0.6735 (6)	0.027 (3)
C41	1.1224 (13)	0.1926 (8)	0.5778 (7)	0.031 (3)
C42	1.1092 (11)	0.1517 (8)	0.7232 (7)	0.025 (3)
C43	0.8335 (12)	0.0896 (8)	0.6106 (7)	0.031 (3)
C50	1.1331 (12)	0.4327 (7)	0.8327 (6)	0.022 (2)
H50	1.0291	0.4625	0.8246	0.026*
C51	1.2230 (13)	0.4355 (8)	0.8980 (6)	0.032 (3)
H51	1.1804	0.4635	0.9346	0.038*
C52	1.3794 (15)	0.3966 (8)	0.9102 (7)	0.041 (3)
H52	1.4488	0.4021	0.9543	0.050*
C53	1.4297 (14)	0.3493 (8)	0.8552 (7)	0.039 (3)
H53	1.5313	0.3164	0.8622	0.046*
C54	1.3332 (12)	0.3507 (8)	0.7924 (7)	0.030 (3)
H54	1.3730	0.3224	0.7551	0.036*
N1	1.1824 (10)	0.3900 (6)	0.7787 (5)	0.023 (2)
O11	1.2984 (9)	0.4331 (6)	0.5960 (5)	0.041 (2)
O12	0.9308 (9)	0.6171 (5)	0.6838 (4)	0.0324 (19)
O21	0.9912 (10)	0.3768 (6)	0.4579 (4)	0.042 (2)
O22	0.6244 (9)	0.5546 (6)	0.5592 (5)	0.040 (2)
O23	0.5260 (9)	0.2087 (6)	0.4964 (5)	0.038 (2)
O31	0.6184 (9)	0.5075 (6)	0.7267 (5)	0.042 (2)
O32	0.9175 (10)	0.2343 (6)	0.8440 (5)	0.043 (2)
O33	0.4786 (9)	0.1625 (6)	0.6585 (5)	0.040 (2)
O41	1.2030 (10)	0.1912 (6)	0.5380 (5)	0.042 (2)
O42	1.1879 (9)	0.1254 (6)	0.7717 (5)	0.038 (2)
O43	0.7482 (10)	0.0232 (6)	0.5951 (5)	0.052 (3)
Ir1	1.03222 (4)	0.39781 (3)	0.67454 (2)	0.01762 (13)
Ir2	0.79552 (4)	0.34982 (3)	0.56961 (2)	0.01881 (13)
Ir3	0.76792 (4)	0.30557 (3)	0.69883 (2)	0.01812 (13)
Ir4	0.97732 (4)	0.20144 (3)	0.63943 (2)	0.01943 (13)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C11	0.030 (6)	0.016 (5)	0.032 (8)	0.000 (4)	−0.003 (5)	−0.001 (5)
C12	0.029 (5)	0.021 (6)	0.017 (7)	−0.012 (4)	0.003 (5)	0.004 (4)
C21	0.037 (6)	0.024 (6)	0.032 (8)	0.004 (5)	0.001 (6)	−0.001 (5)
C22	0.021 (5)	0.023 (6)	0.030 (8)	0.001 (5)	0.001 (5)	−0.001 (5)
C23	0.029 (6)	0.033 (6)	0.019 (7)	0.000 (5)	0.010 (5)	0.006 (5)
C31	0.035 (6)	0.030 (6)	0.021 (7)	−0.004 (5)	0.010 (5)	0.007 (5)
C32	0.031 (6)	0.028 (6)	0.025 (8)	−0.010 (5)	0.013 (6)	0.001 (5)
C33	0.033 (6)	0.025 (5)	0.023 (7)	0.003 (5)	0.009 (5)	0.005 (5)
C41	0.021 (5)	0.027 (6)	0.042 (9)	−0.001 (4)	0.004 (6)	0.007 (5)
C42	0.010 (5)	0.026 (6)	0.040 (8)	0.010 (4)	0.007 (5)	0.007 (5)
C43	0.022 (5)	0.026 (6)	0.039 (9)	−0.002 (5)	−0.006 (5)	0.007 (5)
C50	0.026 (5)	0.014 (5)	0.026 (7)	0.001 (4)	0.004 (5)	0.007 (4)
C51	0.043 (7)	0.025 (6)	0.024 (8)	−0.005 (5)	0.000 (6)	0.003 (5)
C52	0.057 (8)	0.029 (6)	0.031 (9)	−0.004 (6)	−0.009 (6)	0.009 (6)
C53	0.035 (6)	0.033 (6)	0.043 (9)	0.000 (5)	−0.001 (6)	0.005 (6)
C54	0.026 (6)	0.025 (6)	0.043 (9)	0.003 (5)	0.012 (6)	0.002 (5)
N1	0.031 (5)	0.011 (4)	0.028 (6)	−0.004 (3)	0.007 (4)	0.007 (4)
O11	0.024 (4)	0.053 (5)	0.055 (7)	−0.007 (3)	0.026 (4)	0.004 (4)
O12	0.045 (5)	0.018 (4)	0.037 (6)	0.004 (3)	0.016 (4)	0.003 (3)
O21	0.058 (5)	0.044 (5)	0.032 (6)	0.000 (4)	0.026 (5)	0.005 (4)
O22	0.040 (5)	0.035 (5)	0.044 (6)	0.013 (4)	0.005 (4)	−0.001 (4)
O23	0.027 (4)	0.043 (5)	0.039 (6)	−0.012 (4)	−0.002 (4)	−0.006 (4)
O31	0.046 (5)	0.028 (4)	0.056 (7)	0.014 (4)	0.018 (4)	−0.010 (4)
O32	0.053 (5)	0.052 (5)	0.019 (6)	−0.013 (4)	−0.004 (4)	0.019 (4)
O33	0.035 (4)	0.043 (5)	0.037 (6)	−0.021 (4)	−0.004 (4)	0.006 (4)
O41	0.039 (5)	0.063 (6)	0.028 (6)	0.008 (4)	0.016 (4)	−0.003 (4)
O42	0.028 (4)	0.038 (4)	0.043 (6)	0.002 (4)	−0.004 (4)	0.016 (4)
O43	0.036 (5)	0.033 (5)	0.079 (8)	−0.010 (4)	−0.003 (5)	−0.008 (5)
Ir1	0.0161 (2)	0.0166 (2)	0.0207 (3)	−0.00133 (14)	0.00500 (18)	0.00036 (15)
Ir2	0.0184 (2)	0.0189 (2)	0.0192 (3)	0.00063 (15)	0.00405 (18)	0.00150 (16)
Ir3	0.0170 (2)	0.0181 (2)	0.0203 (3)	−0.00043 (14)	0.00644 (19)	0.00108 (16)
Ir4	0.0173 (2)	0.0162 (2)	0.0251 (3)	0.00174 (14)	0.00506 (19)	−0.00012 (16)

Geometric parameters (Å, º) top

C11—O11	1.143 (12)	C43—O43	1.136 (12)
C11—Ir1	1.895 (11)	C43—Ir4	1.923 (11)
C12—O12	1.148 (11)	C50—N1	1.349 (13)
C12—Ir1	1.883 (10)	C50—C51	1.360 (15)
C21—O21	1.160 (13)	C50—H50	0.9500
C21—Ir2	1.894 (12)	C51—C52	1.398 (16)
C22—O22	1.112 (12)	C51—H51	0.9500
C22—Ir2	1.937 (10)	C52—C53	1.397 (17)
C23—O23	1.147 (13)	C52—H52	0.9500
C23—Ir2	1.924 (12)	C53—C54	1.341 (18)
C31—O31	1.131 (12)	C53—H53	0.9500
C31—Ir3	1.914 (11)	C54—N1	1.358 (13)
C32—O32	1.122 (13)	C54—H54	0.9500
C32—Ir3	1.921 (13)	Ir1—Ir2	2.6529 (6)
C33—O33	1.139 (13)	Ir1—Ir3	2.6842 (5)
C33—Ir3	1.930 (11)	Ir1—Ir4	2.6906 (5)
C41—O41	1.147 (13)	Ir1—N1	2.193 (10)
C41—Ir4	1.911 (12)	Ir2—Ir3	2.6836 (6)
C42—O42	1.106 (13)	Ir2—Ir4	2.6883 (5)
C42—Ir4	1.915 (12)	Ir3—Ir4	2.7024 (5)

O11—C11—Ir1	177.8 (10)	C21—Ir2—C22	100.0 (4)
O12—C12—Ir1	174.5 (10)	C23—Ir2—C22	99.6 (4)
O21—C21—Ir2	178.2 (11)	C21—Ir2—Ir1	96.5 (4)
O22—C22—Ir2	178.2 (10)	C23—Ir2—Ir1	153.1 (3)
O23—C23—Ir2	176.0 (9)	C22—Ir2—Ir1	97.4 (3)
O31—C31—Ir3	178.3 (11)	C21—Ir2—Ir3	152.8 (4)
O32—C32—Ir3	178.8 (10)	C23—Ir2—Ir3	96.7 (3)
O33—C33—Ir3	179.5 (10)	C22—Ir2—Ir3	97.2 (3)
O41—C41—Ir4	175.7 (10)	Ir1—Ir2—Ir3	60.393 (14)
O42—C42—Ir4	178.0 (9)	C21—Ir2—Ir4	96.9 (3)
O43—C43—Ir4	178.4 (12)	C23—Ir2—Ir4	96.9 (3)
N1—C50—C51	124.0 (10)	C22—Ir2—Ir4	153.6 (3)
N1—C50—H50	118.0	Ir1—Ir2—Ir4	60.492 (14)
C51—C50—H50	118.0	Ir3—Ir2—Ir4	60.406 (14)
C50—C51—C52	118.8 (11)	C31—Ir3—C32	102.6 (5)
C50—C51—H51	120.6	C31—Ir3—C33	103.1 (4)
C52—C51—H51	120.6	C32—Ir3—C33	102.0 (4)
C53—C52—C51	117.6 (12)	C31—Ir3—Ir2	96.0 (3)
C53—C52—H52	121.2	C32—Ir3—Ir2	150.0 (3)
C51—C52—H52	121.2	C33—Ir3—Ir2	96.3 (3)
C54—C53—C52	119.3 (11)	C31—Ir3—Ir1	92.5 (3)
C54—C53—H53	120.3	C32—Ir3—Ir1	96.3 (3)
C52—C53—H53	120.3	C33—Ir3—Ir1	152.5 (3)
C53—C54—N1	124.1 (11)	Ir2—Ir3—Ir1	59.236 (14)
C53—C54—H54	117.9	C31—Ir3—Ir4	149.5 (3)
N1—C54—H54	117.9	C32—Ir3—Ir4	93.9 (3)
C50—N1—C54	115.9 (10)	C33—Ir3—Ir4	98.3 (3)
C50—N1—Ir1	120.7 (7)	Ir2—Ir3—Ir4	59.882 (14)
C54—N1—Ir1	123.2 (8)	Ir1—Ir3—Ir4	59.932 (13)
C12—Ir1—C11	97.4 (4)	C41—Ir4—C42	101.2 (4)
C12—Ir1—N1	94.0 (4)	C41—Ir4—C43	102.7 (5)
C11—Ir1—N1	97.3 (4)	C42—Ir4—C43	102.6 (5)
C12—Ir1—Ir2	97.5 (3)	C41—Ir4—Ir2	95.4 (3)
C11—Ir1—Ir2	100.0 (3)	C42—Ir4—Ir2	149.9 (3)
N1—Ir1—Ir2	157.78 (19)	C43—Ir4—Ir2	98.1 (3)
C12—Ir1—Ir3	100.0 (3)	C41—Ir4—Ir1	97.1 (3)
C11—Ir1—Ir3	155.2 (3)	C42—Ir4—Ir1	93.7 (3)
N1—Ir1—Ir3	99.0 (2)	C43—Ir4—Ir1	151.3 (3)
Ir2—Ir1—Ir3	60.371 (14)	Ir2—Ir4—Ir1	59.102 (14)
C12—Ir1—Ir4	155.2 (3)	C41—Ir4—Ir3	151.7 (3)
C11—Ir1—Ir4	97.6 (3)	C42—Ir4—Ir3	96.6 (3)
N1—Ir1—Ir4	103.57 (19)	C43—Ir4—Ir3	94.7 (3)
Ir2—Ir1—Ir4	60.406 (14)	Ir2—Ir4—Ir3	59.712 (14)
Ir3—Ir1—Ir4	60.370 (13)	Ir1—Ir4—Ir3	59.698 (13)
C21—Ir2—C23	101.0 (5)

N1—C50—C51—C52	3.2 (15)	N1—Ir1—Ir3—C31	93.2 (4)
C50—C51—C52—C53	−5.1 (16)	Ir2—Ir1—Ir3—C31	−95.5 (4)
C51—C52—C53—C54	5.7 (16)	Ir4—Ir1—Ir3—C31	−166.2 (4)
C52—C53—C54—N1	−4.5 (17)	C12—Ir1—Ir3—C32	−105.5 (5)
C51—C50—N1—C54	−1.6 (13)	C11—Ir1—Ir3—C32	120.7 (8)
C51—C50—N1—Ir1	−176.4 (7)	N1—Ir1—Ir3—C32	−9.8 (4)
C53—C54—N1—C50	2.3 (14)	Ir2—Ir1—Ir3—C32	161.5 (3)
C53—C54—N1—Ir1	176.9 (8)	Ir4—Ir1—Ir3—C32	90.8 (3)
O12—C12—Ir1—C11	94 (9)	C12—Ir1—Ir3—C33	122.6 (8)
O12—C12—Ir1—N1	−168 (9)	C11—Ir1—Ir3—C33	−11.3 (10)
O12—C12—Ir1—Ir2	−7 (9)	N1—Ir1—Ir3—C33	−141.7 (7)
O12—C12—Ir1—Ir3	−68 (9)	Ir2—Ir1—Ir3—C33	29.6 (7)
O12—C12—Ir1—Ir4	−33 (9)	Ir4—Ir1—Ir3—C33	−41.1 (7)
O11—C11—Ir1—C12	−117 (26)	C12—Ir1—Ir3—Ir2	93.0 (3)
O11—C11—Ir1—N1	148 (26)	C11—Ir1—Ir3—Ir2	−40.9 (8)
O11—C11—Ir1—Ir2	−18 (26)	N1—Ir1—Ir3—Ir2	−171.3 (2)
O11—C11—Ir1—Ir3	17 (26)	Ir4—Ir1—Ir3—Ir2	−70.723 (16)
O11—C11—Ir1—Ir4	43 (26)	C12—Ir1—Ir3—Ir4	163.7 (3)
C50—N1—Ir1—C12	42.3 (7)	C11—Ir1—Ir3—Ir4	29.9 (8)
C54—N1—Ir1—C12	−132.1 (7)	N1—Ir1—Ir3—Ir4	−100.6 (2)
C50—N1—Ir1—C11	140.3 (7)	Ir2—Ir1—Ir3—Ir4	70.723 (16)
C54—N1—Ir1—C11	−34.1 (8)	O41—C41—Ir4—C42	−165 (13)
C50—N1—Ir1—Ir2	−78.8 (9)	O41—C41—Ir4—C43	89 (14)
C54—N1—Ir1—Ir2	106.8 (8)	O41—C41—Ir4—Ir2	−10 (14)
C50—N1—Ir1—Ir3	−58.5 (7)	O41—C41—Ir4—Ir1	−70 (14)
C54—N1—Ir1—Ir3	127.1 (7)	O41—C41—Ir4—Ir3	−37 (14)
C50—N1—Ir1—Ir4	−120.0 (6)	O42—C42—Ir4—C41	69 (28)
C54—N1—Ir1—Ir4	65.6 (7)	O42—C42—Ir4—C43	175 (100)
O21—C21—Ir2—C23	−171 (32)	O42—C42—Ir4—Ir2	−53 (28)
O21—C21—Ir2—C22	87 (32)	O42—C42—Ir4—Ir1	−29 (28)
O21—C21—Ir2—Ir1	−11 (32)	O42—C42—Ir4—Ir3	−89 (28)
O21—C21—Ir2—Ir3	−41 (33)	O43—C43—Ir4—C41	146 (34)
O21—C21—Ir2—Ir4	−72 (32)	O43—C43—Ir4—C42	41 (34)
O23—C23—Ir2—C21	71 (14)	O43—C43—Ir4—Ir2	−117 (34)
O23—C23—Ir2—C22	173 (14)	O43—C43—Ir4—Ir1	−82 (34)
O23—C23—Ir2—Ir1	−58 (14)	O43—C43—Ir4—Ir3	−57 (34)
O23—C23—Ir2—Ir3	−88 (14)	C21—Ir2—Ir4—C41	−1.4 (5)
O23—C23—Ir2—Ir4	−27 (14)	C23—Ir2—Ir4—C41	100.6 (5)
O22—C22—Ir2—C21	−90 (34)	C22—Ir2—Ir4—C41	−130.9 (7)
O22—C22—Ir2—C23	167 (34)	Ir1—Ir2—Ir4—C41	−95.0 (3)
O22—C22—Ir2—Ir1	8 (34)	Ir3—Ir2—Ir4—C41	−165.7 (3)
O22—C22—Ir2—Ir3	69 (34)	C21—Ir2—Ir4—C42	121.9 (6)
O22—C22—Ir2—Ir4	39 (34)	C23—Ir2—Ir4—C42	−136.1 (6)
C12—Ir1—Ir2—C21	97.9 (4)	C22—Ir2—Ir4—C42	−7.5 (8)
C11—Ir1—Ir2—C21	−1.1 (4)	Ir1—Ir2—Ir4—C42	28.3 (5)
N1—Ir1—Ir2—C21	−141.6 (6)	Ir3—Ir2—Ir4—C42	−42.3 (5)
Ir3—Ir1—Ir2—C21	−164.9 (3)	C21—Ir2—Ir4—C43	−105.1 (5)
Ir4—Ir1—Ir2—C21	−94.2 (3)	C23—Ir2—Ir4—C43	−3.1 (5)
C12—Ir1—Ir2—C23	−131.8 (7)	C22—Ir2—Ir4—C43	125.5 (7)
C11—Ir1—Ir2—C23	129.3 (7)	Ir1—Ir2—Ir4—C43	161.3 (4)
N1—Ir1—Ir2—C23	−11.3 (9)	Ir3—Ir2—Ir4—C43	90.7 (4)
Ir3—Ir1—Ir2—C23	−34.6 (7)	C21—Ir2—Ir4—Ir1	93.6 (3)
Ir4—Ir1—Ir2—C23	36.1 (7)	C23—Ir2—Ir4—Ir1	−164.4 (3)
C12—Ir1—Ir2—C22	−3.1 (4)	C22—Ir2—Ir4—Ir1	−35.8 (6)
C11—Ir1—Ir2—C22	−102.0 (4)	Ir3—Ir2—Ir4—Ir1	−70.645 (15)
N1—Ir1—Ir2—C22	117.4 (6)	C21—Ir2—Ir4—Ir3	164.2 (3)
Ir3—Ir1—Ir2—C22	94.1 (3)	C23—Ir2—Ir4—Ir3	−93.8 (3)
Ir4—Ir1—Ir2—C22	164.8 (3)	C22—Ir2—Ir4—Ir3	34.8 (6)
C12—Ir1—Ir2—Ir3	−97.3 (3)	Ir1—Ir2—Ir4—Ir3	70.645 (15)
C11—Ir1—Ir2—Ir3	163.8 (3)	C12—Ir1—Ir4—C41	121.7 (8)
N1—Ir1—Ir2—Ir3	23.3 (5)	C11—Ir1—Ir4—C41	−5.1 (5)
Ir4—Ir1—Ir2—Ir3	70.666 (14)	N1—Ir1—Ir4—C41	−104.6 (4)
C12—Ir1—Ir2—Ir4	−167.9 (3)	Ir2—Ir1—Ir4—C41	92.1 (4)
C11—Ir1—Ir2—Ir4	93.2 (3)	Ir3—Ir1—Ir4—C41	162.7 (4)
N1—Ir1—Ir2—Ir4	−47.4 (5)	C12—Ir1—Ir4—C42	−136.6 (8)
Ir3—Ir1—Ir2—Ir4	−70.666 (14)	C11—Ir1—Ir4—C42	96.6 (4)
O31—C31—Ir3—C32	54 (34)	N1—Ir1—Ir4—C42	−2.8 (3)
O31—C31—Ir3—C33	160 (34)	Ir2—Ir1—Ir4—C42	−166.2 (3)
O31—C31—Ir3—Ir2	−103 (34)	Ir3—Ir1—Ir4—C42	−95.5 (3)
O31—C31—Ir3—Ir1	−43 (34)	C12—Ir1—Ir4—C43	−11.6 (11)
O31—C31—Ir3—Ir4	−67 (34)	C11—Ir1—Ir4—C43	−138.4 (8)
O32—C32—Ir3—C31	−25 (44)	N1—Ir1—Ir4—C43	122.1 (8)
O32—C32—Ir3—C33	−132 (44)	Ir2—Ir1—Ir4—C43	−41.2 (8)
O32—C32—Ir3—Ir2	102 (44)	Ir3—Ir1—Ir4—C43	29.4 (8)
O32—C32—Ir3—Ir1	69 (44)	C12—Ir1—Ir4—Ir2	29.6 (7)
O32—C32—Ir3—Ir4	129 (44)	C11—Ir1—Ir4—Ir2	−97.2 (3)
O33—C33—Ir3—C31	−178 (100)	N1—Ir1—Ir4—Ir2	163.4 (2)
O33—C33—Ir3—C32	−72 (100)	Ir3—Ir1—Ir4—Ir2	70.668 (15)
O33—C33—Ir3—Ir2	84 (100)	C12—Ir1—Ir4—Ir3	−41.1 (7)
O33—C33—Ir3—Ir1	59 (100)	C11—Ir1—Ir4—Ir3	−167.8 (3)
O33—C33—Ir3—Ir4	24 (100)	N1—Ir1—Ir4—Ir3	92.7 (2)
C21—Ir2—Ir3—C31	123.9 (8)	Ir2—Ir1—Ir4—Ir3	−70.668 (15)
C23—Ir2—Ir3—C31	−105.7 (5)	C31—Ir3—Ir4—C41	−10.5 (11)
C22—Ir2—Ir3—C31	−5.1 (4)	C32—Ir3—Ir4—C41	−133.5 (8)
Ir1—Ir2—Ir3—C31	89.3 (3)	C33—Ir3—Ir4—C41	123.8 (8)
Ir4—Ir2—Ir3—C31	160.1 (3)	Ir2—Ir3—Ir4—C41	31.3 (8)
C21—Ir2—Ir3—C32	−4.5 (9)	Ir1—Ir3—Ir4—C41	−38.4 (8)
C23—Ir2—Ir3—C32	125.9 (7)	C31—Ir3—Ir4—C42	118.4 (8)
C22—Ir2—Ir3—C32	−133.5 (7)	C32—Ir3—Ir4—C42	−4.7 (4)
Ir1—Ir2—Ir3—C32	−39.1 (6)	C33—Ir3—Ir4—C42	−107.4 (4)
Ir4—Ir2—Ir3—C32	31.7 (6)	Ir2—Ir3—Ir4—C42	160.1 (3)
C21—Ir2—Ir3—C33	−132.2 (7)	Ir1—Ir3—Ir4—C42	90.4 (3)
C23—Ir2—Ir3—C33	−1.8 (4)	C31—Ir3—Ir4—C43	−138.4 (8)
C22—Ir2—Ir3—C33	98.9 (4)	C32—Ir3—Ir4—C43	98.6 (5)
Ir1—Ir2—Ir3—C33	−166.8 (3)	C33—Ir3—Ir4—C43	−4.1 (5)
Ir4—Ir2—Ir3—C33	−96.0 (3)	Ir2—Ir3—Ir4—C43	−96.6 (4)
C21—Ir2—Ir3—Ir1	34.6 (7)	Ir1—Ir3—Ir4—C43	−166.3 (4)
C23—Ir2—Ir3—Ir1	165.0 (3)	C31—Ir3—Ir4—Ir2	−41.7 (7)
C22—Ir2—Ir3—Ir1	−94.4 (3)	C32—Ir3—Ir4—Ir2	−164.8 (3)
Ir4—Ir2—Ir3—Ir1	70.806 (14)	C33—Ir3—Ir4—Ir2	92.5 (3)
C21—Ir2—Ir3—Ir4	−36.2 (7)	Ir1—Ir3—Ir4—Ir2	−69.668 (15)
C23—Ir2—Ir3—Ir4	94.2 (3)	C31—Ir3—Ir4—Ir1	27.9 (7)
C22—Ir2—Ir3—Ir4	−165.2 (3)	C32—Ir3—Ir4—Ir1	−95.1 (3)
Ir1—Ir2—Ir3—Ir4	−70.806 (14)	C33—Ir3—Ir4—Ir1	162.1 (3)
C12—Ir1—Ir3—C31	−2.5 (5)	Ir2—Ir3—Ir4—Ir1	69.668 (15)
C11—Ir1—Ir3—C31	−136.4 (8)

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