cis-Di­chlorobis(1,10-phenanthroline)­iridium(III) hexa­fluoro­phosphate

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.

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

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Computing details

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)

Crystal data

[IrCl2(C12H8N2)2]PF6	F(000) = 1472
Mr = 768.51	Dx = 1.949 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.7107 Å
Hall symbol: -C 2yc	Cell parameters from 13893 reflections
a = 16.340 (1) Å	θ = 1.6–27.5°
b = 12.679 (1) Å	µ = 5.44 mm^−1
c = 12.9870 (8) Å	T = 200 K
β = 103.321 (2)°	Prism, yellow
V = 2618.2 (4) Å^3	0.13 × 0.12 × 0.10 mm
Z = 4

Data collection

Rigaku RAXIS-RAPID Imaging Plate diffractometer	2675 reflections with I > 2σ(I)
Detector resolution: 10.00 pixels mm^-1	Rint = 0.061
ω scans	θmax = 27.5°, θmin = 1.6°
Absorption correction: multi-scan ABSCOR (Higashi, 1995)	h = −21→20
Tmin = 0.426, Tmax = 0.580	k = −16→16
11793 measured reflections	l = −14→16
3007 independent reflections

Refinement

Refinement on F^2	H atoms treated by a mixture of independent and constrained refinement
R[F^2 > 2σ(F^2)] = 0.040	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.091	(Δ/σ)max = −0.032
S = 1.20	Δρmax = 0.96 e Å^−3
2675 reflections	Δρmin = −1.37 e Å^−3
206 parameters

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ir1	1.0000	0.18155 (2)	0.2500	0.0231 (1)
Cl1	0.89614 (8)	0.0509 (1)	0.2306 (1)	0.0362 (3)
P1	0.7500	0.2500	0.5000	0.0433 (5)
F1	0.7710 (5)	0.1989 (5)	0.3986 (5)	0.111 (3)
F2	0.6693 (3)	0.1777 (4)	0.4899 (4)	0.081 (2)
F3	0.6974 (4)	0.3376 (6)	0.4298 (7)	0.132 (3)
N1	1.0932 (3)	0.2928 (3)	0.2809 (4)	0.0258 (9)
N2	1.0201 (3)	0.1875 (4)	0.4118 (4)	0.0286 (9)
C1	1.1287 (4)	0.3428 (4)	0.2131 (5)	0.035 (1)
C2	1.1948 (4)	0.4137 (5)	0.2462 (5)	0.045 (1)
C3	1.2251 (4)	0.4338 (5)	0.3515 (5)	0.042 (1)
C4	1.1899 (4)	0.3798 (4)	0.4265 (5)	0.035 (1)
C5	1.1226 (3)	0.3096 (4)	0.3869 (4)	0.028 (1)
C6	1.2177 (4)	0.3902 (5)	0.5384 (5)	0.043 (1)
C7	1.1823 (4)	0.3336 (5)	0.6055 (5)	0.044 (2)
C8	1.1134 (4)	0.2634 (5)	0.5666 (5)	0.035 (1)
C9	1.0845 (3)	0.2522 (4)	0.4571 (4)	0.027 (1)
C10	1.0725 (4)	0.2040 (5)	0.6306 (5)	0.040 (1)
C11	1.0062 (4)	0.1404 (5)	0.5847 (5)	0.039 (1)
C12	0.9812 (4)	0.1348 (5)	0.4744 (4)	0.033 (1)
H1	1.1082	0.3304	0.1393	0.0293 (2)*
H2	1.2189	0.4482	0.1951	0.0849 (3)*
H3	1.2695	0.4831	0.3743	0.0282 (2)*
H4	1.2620	0.4378	0.5666	0.0523 (2)*
H5	1.2038	0.3406	0.6798	0.0657 (3)*
H6	1.0907	0.2073	0.7053	0.0342 (2)*
H7	0.9775	0.1011	0.6274	0.0502 (2)*
H8	0.9344	0.0915	0.4432	0.0332 (2)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ir1	0.0230 (2)	0.0221 (2)	0.0245 (2)	0.0000	0.0063 (1)	0.0000
Cl1	0.0317 (7)	0.0341 (7)	0.0404 (8)	−0.0047 (6)	0.0039 (6)	0.0020 (6)
P1	0.048 (1)	0.041 (1)	0.048 (1)	0.003 (1)	0.024 (1)	0.004 (1)
F1	0.158 (7)	0.096 (4)	0.115 (5)	−0.052 (4)	0.105 (5)	−0.044 (4)
F2	0.078 (4)	0.099 (4)	0.077 (4)	−0.041 (3)	0.041 (3)	−0.014 (3)
F3	0.081 (4)	0.141 (6)	0.184 (8)	0.038 (4)	0.050 (5)	0.108 (6)
N1	0.025 (2)	0.027 (2)	0.027 (2)	−0.001 (2)	0.007 (2)	−0.004 (2)
N2	0.030 (2)	0.026 (2)	0.031 (2)	0.000 (2)	0.008 (2)	−0.001 (2)
C1	0.040 (3)	0.033 (3)	0.039 (3)	−0.003 (2)	0.019 (3)	−0.004 (2)
C2	0.057 (4)	0.034 (3)	0.050 (4)	−0.010 (3)	0.023 (3)	−0.003 (3)
C3	0.037 (3)	0.030 (3)	0.061 (4)	−0.012 (3)	0.017 (3)	−0.008 (3)
C4	0.032 (3)	0.026 (3)	0.046 (3)	−0.004 (2)	0.009 (3)	−0.007 (2)
C5	0.027 (3)	0.025 (3)	0.031 (3)	−0.004 (2)	0.007 (2)	−0.004 (2)
C6	0.042 (4)	0.038 (3)	0.046 (4)	−0.007 (3)	0.003 (3)	−0.012 (3)
C7	0.046 (4)	0.039 (4)	0.041 (4)	−0.004 (3)	−0.005 (3)	−0.012 (3)
C8	0.041 (3)	0.031 (3)	0.034 (3)	0.003 (3)	0.008 (3)	−0.001 (2)
C9	0.034 (3)	0.026 (3)	0.019 (2)	0.001 (2)	0.005 (2)	−0.005 (2)
C10	0.053 (4)	0.042 (4)	0.026 (3)	0.006 (3)	0.010 (3)	0.000 (3)
C11	0.045 (4)	0.037 (3)	0.037 (3)	0.000 (3)	0.014 (3)	0.004 (3)
C12	0.035 (3)	0.034 (3)	0.035 (3)	−0.003 (2)	0.018 (2)	0.000 (2)

Geometric parameters (Å, º)

Ir1—Cl1	2.343 (1)	C2—C3	1.367 (9)
Ir1—Cl1^i	2.343 (1)	C2—H2	0.952
Ir1—N1	2.046 (4)	C3—C4	1.416 (10)
Ir1—N1^i	2.046 (4)	C3—H3	0.952
Ir1—N2	2.053 (5)	C4—C5	1.416 (7)
Ir1—N2^i	2.053 (5)	C4—C6	1.426 (9)
P1—F1	1.575 (7)	C5—C9	1.418 (8)
P1—F1^ii	1.575 (7)	C6—C7	1.36 (1)
P1—F2	1.586 (6)	C6—H4	0.950
P1—F2^ii	1.586 (6)	C7—C8	1.433 (9)
P1—F3	1.562 (7)	C7—H5	0.951
P1—F3^ii	1.562 (7)	C8—C9	1.398 (7)
N1—C1	1.324 (8)	C8—C10	1.400 (9)
N1—C5	1.365 (7)	C10—C11	1.372 (9)
N2—C9	1.356 (7)	C10—H6	0.949
N2—C12	1.322 (8)	C11—C12	1.399 (8)
C1—C2	1.395 (9)	C11—H7	0.946
C1—H1	0.952	C12—H8	0.952
Cl1···C6^iii	3.455 (6)	F2···C2^vii	3.455 (9)
Cl1···C11^iv	3.528 (7)	C4···C7^viii	3.498 (9)
Cl1···F3^v	3.539 (8)	C11···C12^iv	3.592 (9)
F1···C3^vi	3.469 (9)	C12···C12^iv	3.51 (1)
F2···C1^vii	3.128 (10)
Cl1—Ir1—Cl1^i	90.02 (7)	N1—C1—C2	122.1 (6)
Cl1—Ir1—N1	174.9 (1)	N1—C1—H1	118.9
Cl1—Ir1—N1^i	88.7 (1)	C2—C1—H1	119.0
Cl1—Ir1—N2	94.4 (1)	C1—C2—C3	120.3 (7)
Cl1—Ir1—N2^i	88.5 (1)	C1—C2—H2	119.7
Cl1^i—Ir1—N1	88.7 (1)	C3—C2—H2	120.0
Cl1^i—Ir1—N1^i	174.9 (1)	C2—C3—C4	119.2 (6)
Cl1^i—Ir1—N2	88.5 (1)	C2—C3—H3	120.4
Cl1^i—Ir1—N2^i	94.4 (1)	C4—C3—H3	120.4
N1—Ir1—N1^i	92.9 (2)	C3—C4—C5	117.3 (5)
N1—Ir1—N2	80.6 (2)	C3—C4—C6	124.9 (5)
N1—Ir1—N2^i	96.4 (2)	C5—C4—C6	117.8 (6)
N1^i—Ir1—N2	96.4 (2)	N1—C5—C4	121.9 (5)
N1^i—Ir1—N2^i	80.6 (2)	N1—C5—C9	117.6 (4)
N2—Ir1—N2^i	175.8 (2)	C4—C5—C9	120.6 (5)
F1—P1—F1^ii	180.0000 (1)	C4—C6—C7	121.6 (6)
F1—P1—F2	91.7 (3)	C4—C6—H4	119.2
F1—P1—F2^ii	88.3 (3)	C7—C6—H4	119.2
F1—P1—F3	90.0 (4)	C6—C7—C8	121.2 (6)
F1—P1—F3^ii	90.0 (4)	C6—C7—H5	119.3
F1^ii—P1—F2	88.3 (3)	C8—C7—H5	119.5
F1^ii—P1—F2^ii	91.7 (3)	C7—C8—C9	118.5 (6)
F1^ii—P1—F3	90.0 (4)	C7—C8—C10	124.6 (5)
F1^ii—P1—F3^ii	90.0 (4)	C9—C8—C10	116.9 (5)
F2—P1—F2^ii	180.0	N2—C9—C5	116.3 (4)
F2—P1—F3	91.6 (3)	N2—C9—C8	123.3 (5)
F2—P1—F3^ii	88.4 (3)	C5—C9—C8	120.4 (5)
F2^ii—P1—F3	88.4 (3)	C8—C10—C11	119.7 (5)
F2^ii—P1—F3^ii	91.6 (3)	C8—C10—H6	120.2
F3—P1—F3^ii	180.0	C11—C10—H6	120.0
Ir1—N1—C1	128.3 (4)	C10—C11—C12	119.3 (6)
Ir1—N1—C5	112.3 (4)	C10—C11—H7	120.3
C1—N1—C5	119.3 (4)	C12—C11—H7	120.5
Ir1—N2—C9	113.0 (4)	N2—C12—C11	122.4 (5)
Ir1—N2—C12	128.6 (4)	N2—C12—H8	118.9
C9—N2—C12	118.3 (5)	C11—C12—H8	118.7
Ir1—N1—C1—C2	−176.8 (5)	N2—Ir1—N1—C5	3.0 (4)
Ir1—N1—C5—C4	177.0 (4)	N2—Ir1—N1^i—C1^i	−3.8 (5)
Ir1—N1—C5—C9	−1.7 (6)	N2—Ir1—N1^i—C5^i	180.0 (4)
Ir1—N1^i—C1^i—C2^i	−176.8 (5)	N2—Ir1—N2^i—C9^i	−50.1 (4)
Ir1—N1^i—C5^i—C4^i	177.0 (4)	N2—Ir1—N2^i—C12^i	132.5 (5)
Ir1—N1^i—C5^i—C9^i	−1.7 (6)	N2—C9—C5—C4	179.6 (5)
Ir1—N2—C9—C5	4.2 (6)	N2—C9—C8—C7	179.5 (6)
Ir1—N2—C9—C8	−175.6 (5)	N2—C9—C8—C10	−0.1 (9)
Ir1—N2—C12—C11	174.7 (5)	N2—C12—C11—C10	0 (1)
Ir1—N2^i—C9^i—C5^i	4.2 (6)	C1—N1—C5—C4	0.4 (8)
Ir1—N2^i—C9^i—C8^i	−175.6 (5)	C1—N1—C5—C9	−178.3 (5)
Ir1—N2^i—C12^i—C11^i	174.7 (5)	C1—C2—C3—C4	1 (1)
Cl1—Ir1—N1—C1	167 (1)	C2—C1—N1—C5	−0.8 (9)
Cl1—Ir1—N1—C5	−9 (1)	C2—C3—C4—C5	−1.8 (9)
Cl1—Ir1—N1^i—C1^i	90.5 (5)	C2—C3—C4—C6	177.6 (6)
Cl1—Ir1—N1^i—C5^i	−85.7 (4)	C3—C4—C5—C9	179.6 (5)
Cl1—Ir1—N2—C9	175.0 (4)	C3—C4—C6—C7	−178.1 (7)
Cl1—Ir1—N2—C12	−2.4 (5)	C4—C5—C9—C8	−0.6 (8)
Cl1—Ir1—N2^i—C9^i	85.1 (4)	C4—C6—C7—C8	−2 (1)
Cl1—Ir1—N2^i—C12^i	−92.4 (5)	C5—C4—C6—C7	1.3 (10)
N1—Ir1—N1^i—C1^i	−84.7 (5)	C5—C9—N2—C12	−178.1 (5)
N1—Ir1—N1^i—C5^i	99.0 (4)	C5—C9—C8—C7	−0.3 (9)
N1—Ir1—N2—C9	−3.9 (4)	C5—C9—C8—C10	−179.9 (6)
N1—Ir1—N2—C12	178.6 (5)	C6—C4—C5—C9	0.2 (8)
N1—Ir1—N2^i—C9^i	−95.7 (4)	C6—C7—C8—C9	1.7 (10)
N1—Ir1—N2^i—C12^i	86.8 (5)	C6—C7—C8—C10	−178.7 (7)
N1—C1—C2—C3	0 (1)	C7—C8—C10—C11	178.9 (7)
N1—C5—C4—C3	0.9 (8)	C8—C9—N2—C12	2.2 (8)
N1—C5—C4—C6	−178.5 (5)	C8—C10—C11—C12	1 (1)
N1—C5—C9—N2	−1.7 (8)	C9—N2—C12—C11	−2.6 (9)
N1—C5—C9—C8	178.1 (5)	C9—C8—C10—C11	−1.6 (10)
N2—Ir1—N1—C1	179.3 (5)	C9—C8—C10—C11	−1.6 (10)

Symmetry codes: (i) −x+2, y, −z+1/2; (ii) −x+3/2, −y+1/2, −z+1; (iii) x−1/2, −y+1/2, z−1/2; (iv) −x+2, −y, −z+1; (v) −x+3/2, y−1/2, −z+1/2; (vi) x−1/2, y−1/2, z; (vii) x−1/2, −y+1/2, z+1/2; (viii) −x+5/2, −y+1/2, −z+1.