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The crystal structure of the title compound, [IrCl2(C12H8N2)2]PF6, contains a monomeric [IrCl2(phen)2]+ cation (phen is 1,10-phenanthroline) and a hexa­fluoro­phosphate anion. The iridium(III) ion is coordinated by four N atoms from two phen ligands [mean Ir-N distance 2.050 (5) Å] and two Cl atoms [Ir-Cl = 2.343 (1) Å], forming a distorted octahedral environment.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803021755/ww6123sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803021755/ww6123Isup2.hkl
Contains datablock I

CCDC reference: 226640

Key indicators

  • Single-crystal X-ray study
  • T = 200 K
  • Mean [sigma](C-C) = 0.009 Å
  • R factor = 0.040
  • wR factor = 0.091
  • Data-to-parameter ratio = 13.0

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 171.00 A   3
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.426 0.580 Tmin' and Tmax expected: 0.482 0.580 RR' = 0.884 Please check that your absorption correction is appropriate. PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.86 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.01 Ratio PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ir1 - Cl1 = 7.27 su PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... P1 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9 PLAT703_ALERT_1_C Torsion Calc 1.2(10), Rep 0.0(10), Dev.. 1.20 Sigma N2 -C12 -C11 -C10 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 13 CL1 -IR1 -N1 -C1 167.00 1.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 14 CL1 -IR1 -N1 -C5 -9.00 1.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 36 N2 -IR1 -N2 -C9 -50.10 0.40 1.555 1.555 2.755 2.755 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 37 N2 -IR1 -N2 -C12 132.50 0.50 1.555 1.555 2.755 2.755
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 5 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: TEXSAN (Molecular Structure Corporation/Rigaku, 2000); program(s) used to solve structure: SIR92 (Altomare et al., 1992); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII; software used to prepare material for publication: TEXSAN.

(I) top
Crystal data top
[IrCl2(C12H8N2)2]PF6F(000) = 1472
Mr = 768.51Dx = 1.949 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.7107 Å
Hall symbol: -C 2ycCell parameters from 13893 reflections
a = 16.340 (1) Åθ = 1.6–27.5°
b = 12.679 (1) ŵ = 5.44 mm1
c = 12.9870 (8) ÅT = 200 K
β = 103.321 (2)°Prism, yellow
V = 2618.2 (4) Å30.13 × 0.12 × 0.10 mm
Z = 4
Data collection top
Rigaku RAXIS-RAPID Imaging Plate
diffractometer
2675 reflections with I > 2σ(I)
Detector resolution: 10.00 pixels mm-1Rint = 0.061
ω scansθmax = 27.5°, θmin = 1.6°
Absorption correction: multi-scan
ABSCOR (Higashi, 1995)
h = 2120
Tmin = 0.426, Tmax = 0.580k = 1616
11793 measured reflectionsl = 1416
3007 independent reflections
Refinement top
Refinement on F2H atoms treated by a mixture of independent and constrained refinement
R[F2 > 2σ(F2)] = 0.040 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.091(Δ/σ)max = 0.032
S = 1.20Δρmax = 0.96 e Å3
2675 reflectionsΔρmin = 1.37 e Å3
206 parameters
Special details top

Refinement. Refinement using reflections with F2 > -10.0 σ(F2). The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ir11.00000.18155 (2)0.25000.0231 (1)
Cl10.89614 (8)0.0509 (1)0.2306 (1)0.0362 (3)
P10.75000.25000.50000.0433 (5)
F10.7710 (5)0.1989 (5)0.3986 (5)0.111 (3)
F20.6693 (3)0.1777 (4)0.4899 (4)0.081 (2)
F30.6974 (4)0.3376 (6)0.4298 (7)0.132 (3)
N11.0932 (3)0.2928 (3)0.2809 (4)0.0258 (9)
N21.0201 (3)0.1875 (4)0.4118 (4)0.0286 (9)
C11.1287 (4)0.3428 (4)0.2131 (5)0.035 (1)
C21.1948 (4)0.4137 (5)0.2462 (5)0.045 (1)
C31.2251 (4)0.4338 (5)0.3515 (5)0.042 (1)
C41.1899 (4)0.3798 (4)0.4265 (5)0.035 (1)
C51.1226 (3)0.3096 (4)0.3869 (4)0.028 (1)
C61.2177 (4)0.3902 (5)0.5384 (5)0.043 (1)
C71.1823 (4)0.3336 (5)0.6055 (5)0.044 (2)
C81.1134 (4)0.2634 (5)0.5666 (5)0.035 (1)
C91.0845 (3)0.2522 (4)0.4571 (4)0.027 (1)
C101.0725 (4)0.2040 (5)0.6306 (5)0.040 (1)
C111.0062 (4)0.1404 (5)0.5847 (5)0.039 (1)
C120.9812 (4)0.1348 (5)0.4744 (4)0.033 (1)
H11.10820.33040.13930.0293 (2)*
H21.21890.44820.19510.0849 (3)*
H31.26950.48310.37430.0282 (2)*
H41.26200.43780.56660.0523 (2)*
H51.20380.34060.67980.0657 (3)*
H61.09070.20730.70530.0342 (2)*
H70.97750.10110.62740.0502 (2)*
H80.93440.09150.44320.0332 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ir10.0230 (2)0.0221 (2)0.0245 (2)0.00000.0063 (1)0.0000
Cl10.0317 (7)0.0341 (7)0.0404 (8)0.0047 (6)0.0039 (6)0.0020 (6)
P10.048 (1)0.041 (1)0.048 (1)0.003 (1)0.024 (1)0.004 (1)
F10.158 (7)0.096 (4)0.115 (5)0.052 (4)0.105 (5)0.044 (4)
F20.078 (4)0.099 (4)0.077 (4)0.041 (3)0.041 (3)0.014 (3)
F30.081 (4)0.141 (6)0.184 (8)0.038 (4)0.050 (5)0.108 (6)
N10.025 (2)0.027 (2)0.027 (2)0.001 (2)0.007 (2)0.004 (2)
N20.030 (2)0.026 (2)0.031 (2)0.000 (2)0.008 (2)0.001 (2)
C10.040 (3)0.033 (3)0.039 (3)0.003 (2)0.019 (3)0.004 (2)
C20.057 (4)0.034 (3)0.050 (4)0.010 (3)0.023 (3)0.003 (3)
C30.037 (3)0.030 (3)0.061 (4)0.012 (3)0.017 (3)0.008 (3)
C40.032 (3)0.026 (3)0.046 (3)0.004 (2)0.009 (3)0.007 (2)
C50.027 (3)0.025 (3)0.031 (3)0.004 (2)0.007 (2)0.004 (2)
C60.042 (4)0.038 (3)0.046 (4)0.007 (3)0.003 (3)0.012 (3)
C70.046 (4)0.039 (4)0.041 (4)0.004 (3)0.005 (3)0.012 (3)
C80.041 (3)0.031 (3)0.034 (3)0.003 (3)0.008 (3)0.001 (2)
C90.034 (3)0.026 (3)0.019 (2)0.001 (2)0.005 (2)0.005 (2)
C100.053 (4)0.042 (4)0.026 (3)0.006 (3)0.010 (3)0.000 (3)
C110.045 (4)0.037 (3)0.037 (3)0.000 (3)0.014 (3)0.004 (3)
C120.035 (3)0.034 (3)0.035 (3)0.003 (2)0.018 (2)0.000 (2)
Geometric parameters (Å, º) top
Ir1—Cl12.343 (1)C2—C31.367 (9)
Ir1—Cl1i2.343 (1)C2—H20.952
Ir1—N12.046 (4)C3—C41.416 (10)
Ir1—N1i2.046 (4)C3—H30.952
Ir1—N22.053 (5)C4—C51.416 (7)
Ir1—N2i2.053 (5)C4—C61.426 (9)
P1—F11.575 (7)C5—C91.418 (8)
P1—F1ii1.575 (7)C6—C71.36 (1)
P1—F21.586 (6)C6—H40.950
P1—F2ii1.586 (6)C7—C81.433 (9)
P1—F31.562 (7)C7—H50.951
P1—F3ii1.562 (7)C8—C91.398 (7)
N1—C11.324 (8)C8—C101.400 (9)
N1—C51.365 (7)C10—C111.372 (9)
N2—C91.356 (7)C10—H60.949
N2—C121.322 (8)C11—C121.399 (8)
C1—C21.395 (9)C11—H70.946
C1—H10.952C12—H80.952
Cl1···C6iii3.455 (6)F2···C2vii3.455 (9)
Cl1···C11iv3.528 (7)C4···C7viii3.498 (9)
Cl1···F3v3.539 (8)C11···C12iv3.592 (9)
F1···C3vi3.469 (9)C12···C12iv3.51 (1)
F2···C1vii3.128 (10)
Cl1—Ir1—Cl1i90.02 (7)N1—C1—C2122.1 (6)
Cl1—Ir1—N1174.9 (1)N1—C1—H1118.9
Cl1—Ir1—N1i88.7 (1)C2—C1—H1119.0
Cl1—Ir1—N294.4 (1)C1—C2—C3120.3 (7)
Cl1—Ir1—N2i88.5 (1)C1—C2—H2119.7
Cl1i—Ir1—N188.7 (1)C3—C2—H2120.0
Cl1i—Ir1—N1i174.9 (1)C2—C3—C4119.2 (6)
Cl1i—Ir1—N288.5 (1)C2—C3—H3120.4
Cl1i—Ir1—N2i94.4 (1)C4—C3—H3120.4
N1—Ir1—N1i92.9 (2)C3—C4—C5117.3 (5)
N1—Ir1—N280.6 (2)C3—C4—C6124.9 (5)
N1—Ir1—N2i96.4 (2)C5—C4—C6117.8 (6)
N1i—Ir1—N296.4 (2)N1—C5—C4121.9 (5)
N1i—Ir1—N2i80.6 (2)N1—C5—C9117.6 (4)
N2—Ir1—N2i175.8 (2)C4—C5—C9120.6 (5)
F1—P1—F1ii180.0000 (1)C4—C6—C7121.6 (6)
F1—P1—F291.7 (3)C4—C6—H4119.2
F1—P1—F2ii88.3 (3)C7—C6—H4119.2
F1—P1—F390.0 (4)C6—C7—C8121.2 (6)
F1—P1—F3ii90.0 (4)C6—C7—H5119.3
F1ii—P1—F288.3 (3)C8—C7—H5119.5
F1ii—P1—F2ii91.7 (3)C7—C8—C9118.5 (6)
F1ii—P1—F390.0 (4)C7—C8—C10124.6 (5)
F1ii—P1—F3ii90.0 (4)C9—C8—C10116.9 (5)
F2—P1—F2ii180.0N2—C9—C5116.3 (4)
F2—P1—F391.6 (3)N2—C9—C8123.3 (5)
F2—P1—F3ii88.4 (3)C5—C9—C8120.4 (5)
F2ii—P1—F388.4 (3)C8—C10—C11119.7 (5)
F2ii—P1—F3ii91.6 (3)C8—C10—H6120.2
F3—P1—F3ii180.0C11—C10—H6120.0
Ir1—N1—C1128.3 (4)C10—C11—C12119.3 (6)
Ir1—N1—C5112.3 (4)C10—C11—H7120.3
C1—N1—C5119.3 (4)C12—C11—H7120.5
Ir1—N2—C9113.0 (4)N2—C12—C11122.4 (5)
Ir1—N2—C12128.6 (4)N2—C12—H8118.9
C9—N2—C12118.3 (5)C11—C12—H8118.7
Ir1—N1—C1—C2176.8 (5)N2—Ir1—N1—C53.0 (4)
Ir1—N1—C5—C4177.0 (4)N2—Ir1—N1i—C1i3.8 (5)
Ir1—N1—C5—C91.7 (6)N2—Ir1—N1i—C5i180.0 (4)
Ir1—N1i—C1i—C2i176.8 (5)N2—Ir1—N2i—C9i50.1 (4)
Ir1—N1i—C5i—C4i177.0 (4)N2—Ir1—N2i—C12i132.5 (5)
Ir1—N1i—C5i—C9i1.7 (6)N2—C9—C5—C4179.6 (5)
Ir1—N2—C9—C54.2 (6)N2—C9—C8—C7179.5 (6)
Ir1—N2—C9—C8175.6 (5)N2—C9—C8—C100.1 (9)
Ir1—N2—C12—C11174.7 (5)N2—C12—C11—C100 (1)
Ir1—N2i—C9i—C5i4.2 (6)C1—N1—C5—C40.4 (8)
Ir1—N2i—C9i—C8i175.6 (5)C1—N1—C5—C9178.3 (5)
Ir1—N2i—C12i—C11i174.7 (5)C1—C2—C3—C41 (1)
Cl1—Ir1—N1—C1167 (1)C2—C1—N1—C50.8 (9)
Cl1—Ir1—N1—C59 (1)C2—C3—C4—C51.8 (9)
Cl1—Ir1—N1i—C1i90.5 (5)C2—C3—C4—C6177.6 (6)
Cl1—Ir1—N1i—C5i85.7 (4)C3—C4—C5—C9179.6 (5)
Cl1—Ir1—N2—C9175.0 (4)C3—C4—C6—C7178.1 (7)
Cl1—Ir1—N2—C122.4 (5)C4—C5—C9—C80.6 (8)
Cl1—Ir1—N2i—C9i85.1 (4)C4—C6—C7—C82 (1)
Cl1—Ir1—N2i—C12i92.4 (5)C5—C4—C6—C71.3 (10)
N1—Ir1—N1i—C1i84.7 (5)C5—C9—N2—C12178.1 (5)
N1—Ir1—N1i—C5i99.0 (4)C5—C9—C8—C70.3 (9)
N1—Ir1—N2—C93.9 (4)C5—C9—C8—C10179.9 (6)
N1—Ir1—N2—C12178.6 (5)C6—C4—C5—C90.2 (8)
N1—Ir1—N2i—C9i95.7 (4)C6—C7—C8—C91.7 (10)
N1—Ir1—N2i—C12i86.8 (5)C6—C7—C8—C10178.7 (7)
N1—C1—C2—C30 (1)C7—C8—C10—C11178.9 (7)
N1—C5—C4—C30.9 (8)C8—C9—N2—C122.2 (8)
N1—C5—C4—C6178.5 (5)C8—C10—C11—C121 (1)
N1—C5—C9—N21.7 (8)C9—N2—C12—C112.6 (9)
N1—C5—C9—C8178.1 (5)C9—C8—C10—C111.6 (10)
N2—Ir1—N1—C1179.3 (5)C9—C8—C10—C111.6 (10)
Symmetry codes: (i) x+2, y, z+1/2; (ii) x+3/2, y+1/2, z+1; (iii) x1/2, y+1/2, z1/2; (iv) x+2, y, z+1; (v) x+3/2, y1/2, z+1/2; (vi) x1/2, y1/2, z; (vii) x1/2, y+1/2, z+1/2; (viii) x+5/2, y+1/2, z+1.
 

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