Tris(1,10-phenanthroline)manganese(II) bis­(hexa­fluoro­phosphate)

In the title complex, [Mn(C₁₂H₈N₂)₃](PF₆)₂, the Mn²⁺ ion is coordinated by three 1,10-phenanthroline mol­ecules that define a distorted octa­hedral geometry. Each cation and anion lies on a twofold axis. In the crystal structure, there are inter­molecular π–π inter­actions between adjacent phenanthroline ligands.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.008 Å
• Disorder in solvent or counterion
• R factor = 0.077
• wR factor = 0.185
• Data-to-parameter ratio = 15.0

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.14
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature .        293 K
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors for       F22A
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors for       F23A
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for         P2
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for         P1
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      22.00 Perc.
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          8

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
  10 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   3 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
   1 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: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

Tris(1,10-phenanthroline)manganese(II) bis(hexafluorophosphate)

Crystal data

[Mn(C12H8N2)3](PF6)2	F(000) = 890
Mr = 885.49	Dx = 1.619 Mg m^−3
Monoclinic, P2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yc	Cell parameters from 48 reflections
a = 9.3133 (7) Å	θ = 2.1–28.3°
b = 15.2753 (11) Å	µ = 0.55 mm^−1
c = 12.8037 (9) Å	T = 293 K
β = 94.263 (1)°	Needle, yellow
V = 1816.5 (2) Å^3	0.2 × 0.1 × 0.1 mm
Z = 2

Data collection

Bruker SMART 1000 area-detector CCD diffractometer	2469 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.040
Graphite monochromator	θmax = 28.3°, θmin = 2.1°
φ and ω scans	h = −12→12
11432 measured reflections	k = −19→17
4178 independent reflections	l = −14→16

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.077	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.185	H-atom parameters constrained
S = 1.06	w = 1/[σ^2(Fo^2) + (0.0752P)^2] where P = (Fo^2 + 2Fc^2)/3
4178 reflections	(Δ/σ)max < 0.001
279 parameters	Δρmax = 0.47 e Å^−3
0 restraints	Δρmin = −0.22 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Mn	0.5	0.28106 (5)	0.75	0.0493 (3)
N1	0.4343 (4)	0.1887 (2)	0.6194 (3)	0.0621 (9)
N2	0.6928 (4)	0.2693 (2)	0.6553 (3)	0.0565 (9)
N3	0.4178 (3)	0.3978 (2)	0.6578 (2)	0.0491 (8)
C1	0.3053 (6)	0.1523 (3)	0.5998 (4)	0.0783 (14)
H1	0.2357	0.1623	0.6468	0.094*
C2	0.2691 (7)	0.1001 (4)	0.5130 (5)	0.1014 (19)
H2	0.1778	0.0757	0.5021	0.122*
C3	0.3715 (8)	0.0860 (4)	0.4447 (4)	0.104 (2)
H3	0.3499	0.0511	0.3861	0.125*
C4	0.5085 (7)	0.1229 (3)	0.4607 (4)	0.0823 (15)
C5	0.6248 (8)	0.1112 (4)	0.3924 (4)	0.104 (2)
H5	0.6105	0.0745	0.3346	0.124*
C6	0.7511 (8)	0.1512 (4)	0.4096 (4)	0.0977 (19)
H6	0.8221	0.1428	0.3632	0.117*
C7	0.7790 (6)	0.2066 (3)	0.4974 (4)	0.0733 (14)
C8	0.9080 (6)	0.2547 (4)	0.5175 (5)	0.0855 (16)
H8	0.9822	0.2484	0.4733	0.103*
C9	0.9244 (5)	0.3096 (4)	0.6003 (4)	0.0873 (17)
H9	1.0067	0.3438	0.6116	0.105*
C10	0.8147 (5)	0.3134 (3)	0.6681 (4)	0.0726 (13)
H10	0.8282	0.3495	0.7266	0.087*
C11	0.6731 (5)	0.2168 (3)	0.5691 (3)	0.0569 (10)
C12	0.5359 (5)	0.1748 (3)	0.5502 (3)	0.0609 (11)
C13	0.3401 (4)	0.3996 (3)	0.5659 (3)	0.0688 (12)
H13	0.3136	0.3465	0.5347	0.083*
C14	0.2969 (5)	0.4754 (4)	0.5147 (4)	0.0834 (16)
H14	0.2421	0.4731	0.4510	0.100*
C15	0.3354 (6)	0.5530 (4)	0.5584 (5)	0.0881 (17)
H15	0.3066	0.6046	0.5246	0.106*
C16	0.4181 (5)	0.5567 (3)	0.6540 (4)	0.0664 (12)
C17	0.4611 (6)	0.6353 (3)	0.7044 (5)	0.0927 (19)
H17	0.4345	0.6884	0.6732	0.111*
C18	0.4578 (4)	0.4761 (3)	0.7015 (3)	0.0497 (10)
P1	0	0.02571 (12)	0.75	0.0774 (6)
F11	0.0006 (4)	0.0267 (3)	0.8722 (3)	0.1401 (14)
F12	0.1697 (3)	0.0246 (2)	0.7557 (3)	0.1216 (13)
F13	0	−0.0762 (3)	0.75	0.187 (3)
F14	0	0.1280 (3)	0.75	0.1140 (16)
P2	0	0.41737 (17)	0.25	0.0933 (7)
F21	−0.1230 (5)	0.4845 (3)	0.2365 (3)	0.1563 (16)
F22A	0.0112 (16)	0.3973 (13)	0.1415 (13)	0.155 (6)	0.58 (3)
F23A	0.1090 (14)	0.3396 (8)	0.2287 (17)	0.160 (6)	0.58 (3)
F22B	0.0128 (16)	0.455 (2)	0.1281 (14)	0.167 (9)	0.42 (3)
F23B	0.1271 (16)	0.3657 (16)	0.299 (3)	0.189 (10)	0.42 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mn	0.0595 (6)	0.0502 (5)	0.0393 (5)	0	0.0094 (4)	0
N1	0.077 (3)	0.057 (2)	0.055 (2)	−0.0168 (19)	0.0229 (18)	−0.0077 (16)
N2	0.053 (2)	0.063 (2)	0.054 (2)	0.0049 (17)	0.0051 (16)	0.0121 (17)
N3	0.0446 (18)	0.062 (2)	0.0395 (18)	0.0009 (16)	−0.0022 (14)	0.0012 (15)
C1	0.095 (4)	0.069 (3)	0.074 (3)	−0.028 (3)	0.027 (3)	−0.017 (2)
C2	0.123 (5)	0.095 (4)	0.088 (4)	−0.051 (4)	0.019 (4)	−0.020 (3)
C3	0.158 (6)	0.079 (4)	0.077 (4)	−0.039 (4)	0.019 (4)	−0.033 (3)
C4	0.124 (5)	0.059 (3)	0.067 (3)	−0.006 (3)	0.027 (3)	−0.014 (2)
C5	0.162 (6)	0.086 (4)	0.068 (4)	0.006 (4)	0.040 (4)	−0.026 (3)
C6	0.133 (6)	0.093 (4)	0.073 (4)	0.030 (4)	0.046 (4)	−0.002 (3)
C7	0.077 (3)	0.078 (3)	0.068 (3)	0.027 (3)	0.026 (3)	0.023 (3)
C8	0.061 (3)	0.119 (4)	0.079 (4)	0.032 (3)	0.026 (3)	0.038 (3)
C9	0.052 (3)	0.130 (5)	0.080 (4)	0.003 (3)	0.001 (3)	0.031 (4)
C10	0.056 (3)	0.097 (4)	0.063 (3)	0.005 (3)	−0.005 (2)	0.014 (3)
C11	0.066 (3)	0.051 (2)	0.055 (2)	0.016 (2)	0.013 (2)	0.012 (2)
C12	0.083 (3)	0.044 (2)	0.058 (3)	0.002 (2)	0.022 (2)	0.0012 (19)
C13	0.055 (3)	0.098 (4)	0.052 (3)	0.005 (3)	−0.005 (2)	−0.004 (3)
C14	0.063 (3)	0.129 (5)	0.056 (3)	0.016 (3)	−0.011 (2)	0.024 (3)
C15	0.072 (3)	0.102 (4)	0.091 (4)	0.030 (3)	0.010 (3)	0.042 (3)
C16	0.055 (3)	0.066 (3)	0.079 (3)	0.008 (2)	0.012 (2)	0.017 (2)
C17	0.085 (4)	0.057 (3)	0.137 (6)	0.007 (3)	0.012 (3)	0.013 (3)
C18	0.036 (2)	0.060 (3)	0.054 (2)	0.0038 (18)	0.0102 (17)	0.0070 (18)
P1	0.0940 (15)	0.0669 (12)	0.0756 (13)	0	0.0356 (11)	0
F11	0.154 (3)	0.190 (4)	0.081 (2)	0.029 (3)	0.043 (2)	0.020 (2)
F12	0.094 (2)	0.153 (3)	0.122 (3)	0.025 (2)	0.036 (2)	0.042 (2)
F13	0.245 (7)	0.066 (3)	0.276 (8)	0	0.182 (6)	0
F14	0.128 (4)	0.068 (3)	0.146 (4)	0	0.012 (3)	0
P2	0.0684 (14)	0.1033 (17)	0.110 (2)	0	0.0200 (12)	0
F21	0.163 (4)	0.166 (4)	0.145 (4)	0.071 (3)	0.038 (3)	0.032 (3)
F22A	0.185 (10)	0.181 (12)	0.107 (9)	0.004 (10)	0.054 (8)	−0.074 (8)
F23A	0.105 (7)	0.120 (7)	0.251 (16)	0.041 (5)	−0.004 (8)	−0.066 (8)
F22B	0.092 (8)	0.29 (2)	0.114 (9)	0.022 (12)	0.002 (7)	0.095 (12)
F23B	0.094 (8)	0.174 (16)	0.29 (3)	0.028 (9)	−0.030 (12)	−0.063 (15)

Geometric parameters (Å, º)

Mn—N1^i	2.239 (3)	C10—H10	0.9300
Mn—N1	2.239 (3)	C11—C12	1.434 (6)
Mn—N3^i	2.242 (3)	C13—C14	1.376 (7)
Mn—N3	2.242 (3)	C13—H13	0.9300
Mn—N2^i	2.247 (3)	C14—C15	1.347 (7)
Mn—N2	2.247 (3)	C14—H14	0.9300
N1—C1	1.330 (5)	C15—C16	1.398 (7)
N1—C12	1.360 (5)	C15—H15	0.9300
N2—C10	1.320 (5)	C16—C17	1.408 (6)
N2—C11	1.366 (5)	C16—C18	1.410 (5)
N3—C13	1.335 (5)	C17—C17^i	1.327 (10)
N3—C18	1.361 (5)	C17—H17	0.9300
C1—C2	1.388 (6)	C18—C18^i	1.419 (7)
C1—H1	0.9300	P1—F13	1.556 (5)
C2—C3	1.359 (8)	P1—F14	1.562 (4)
C2—H2	0.9300	P1—F11	1.564 (3)
C3—C4	1.396 (8)	P1—F11^ii	1.564 (3)
C3—H3	0.9300	P1—F12^ii	1.577 (3)
C4—C12	1.401 (6)	P1—F12	1.577 (3)
C4—C5	1.454 (8)	P2—F22A^iii	1.435 (13)
C5—C6	1.328 (8)	P2—F22A	1.435 (13)
C5—H5	0.9300	P2—F23B^iii	1.518 (16)
C6—C7	1.416 (7)	P2—F23B	1.518 (16)
C6—H6	0.9300	P2—F21^iii	1.537 (4)
C7—C11	1.405 (6)	P2—F21	1.537 (4)
C7—C8	1.415 (7)	P2—F23A^iii	1.600 (10)
C8—C9	1.352 (7)	P2—F23A	1.600 (10)
C8—H8	0.9300	P2—F22B^iii	1.677 (13)
C9—C10	1.391 (6)	P2—F22B	1.677 (13)
C9—H9	0.9300	F22A—F23A	1.64 (3)
N1^i—Mn—N1	101.85 (18)	C16—C15—H15	119.6
N1^i—Mn—N3^i	92.56 (12)	C15—C16—C17	123.8 (5)
N1—Mn—N3^i	163.43 (12)	C15—C16—C18	116.9 (5)
N1^i—Mn—N3	163.43 (12)	C17—C16—C18	119.3 (4)
N1—Mn—N3	92.56 (12)	C17^i—C17—C16	121.4 (3)
N3^i—Mn—N3	74.57 (16)	C17^i—C17—H17	119.3
N1^i—Mn—N2^i	74.42 (13)	C16—C17—H17	119.3
N1—Mn—N2^i	99.66 (12)	N3—C18—C16	122.3 (4)
N3^i—Mn—N2^i	92.01 (11)	N3—C18—C18^i	118.5 (2)
N3—Mn—N2^i	95.29 (12)	C16—C18—C18^i	119.2 (3)
N1^i—Mn—N2	99.66 (12)	F13—P1—F14	180.000 (1)
N1—Mn—N2	74.42 (13)	F13—P1—F11	90.56 (17)
N3^i—Mn—N2	95.29 (12)	F14—P1—F11	89.44 (17)
N3—Mn—N2	92.01 (11)	F13—P1—F11^ii	90.56 (17)
N2^i—Mn—N2	170.82 (18)	F14—P1—F11^ii	89.44 (17)
C1—N1—C12	118.3 (4)	F11—P1—F11^ii	178.9 (3)
C1—N1—Mn	126.7 (3)	F13—P1—F12^ii	89.37 (15)
C12—N1—Mn	114.8 (3)	F14—P1—F12^ii	90.63 (15)
C10—N2—C11	117.6 (4)	F11—P1—F12^ii	88.61 (19)
C10—N2—Mn	127.3 (3)	F11^ii—P1—F12^ii	91.41 (19)
C11—N2—Mn	114.7 (3)	F13—P1—F12	89.37 (15)
C13—N3—C18	117.3 (4)	F14—P1—F12	90.63 (15)
C13—N3—Mn	128.4 (3)	F11—P1—F12	91.41 (19)
C18—N3—Mn	114.2 (2)	F11^ii—P1—F12	88.61 (19)
N1—C1—C2	123.6 (5)	F12^ii—P1—F12	178.7 (3)
N1—C1—H1	118.2	F22A^iii—P2—F22A	155.3 (18)
C2—C1—H1	118.2	F22A^iii—P2—F23B^iii	100.2 (19)
C3—C2—C1	117.8 (5)	F22A—P2—F23B^iii	66.5 (12)
C3—C2—H2	121.1	F22A^iii—P2—F23B	66.5 (12)
C1—C2—H2	121.1	F22A—P2—F23B	100.2 (19)
C2—C3—C4	121.2 (5)	F23B^iii—P2—F23B	117.3 (19)
C2—C3—H3	119.4	F22A^iii—P2—F21^iii	98.1 (9)
C4—C3—H3	119.4	F22A—P2—F21^iii	98.3 (6)
C3—C4—C12	117.2 (5)	F23B^iii—P2—F21^iii	160.9 (14)
C3—C4—C5	125.2 (5)	F23B—P2—F21^iii	75.5 (9)
C12—C4—C5	117.6 (5)	F22A^iii—P2—F21	98.3 (6)
C6—C5—C4	122.3 (5)	F22A—P2—F21	98.1 (9)
C6—C5—H5	118.9	F23B^iii—P2—F21	75.5 (8)
C4—C5—H5	118.9	F23B—P2—F21	160.9 (14)
C5—C6—C7	121.0 (5)	F21^iii—P2—F21	96.4 (4)
C5—C6—H6	119.5	F22A^iii—P2—F23A^iii	65.4 (14)
C7—C6—H6	119.5	F22A—P2—F23A^iii	95.7 (8)
C11—C7—C8	116.9 (5)	F23B—P2—F23A^iii	91.6 (10)
C11—C7—C6	119.3 (5)	F21^iii—P2—F23A^iii	162.4 (8)
C8—C7—C6	123.9 (5)	F21—P2—F23A^iii	92.2 (6)
C9—C8—C7	120.6 (5)	F22A^iii—P2—F23A	95.7 (8)
C9—C8—H8	119.7	F22A—P2—F23A	65.4 (14)
C7—C8—H8	119.7	F23B^iii—P2—F23A	91.6 (10)
C8—C9—C10	118.0 (5)	F21^iii—P2—F23A	92.2 (6)
C8—C9—H9	121.0	F21—P2—F23A	162.4 (8)
C10—C9—H9	121.0	F23A^iii—P2—F23A	84.0 (10)
N2—C10—C9	124.5 (5)	F22A—P2—F22B^iii	172 (2)
N2—C10—H10	117.8	F23B^iii—P2—F22B^iii	117.1 (15)
C9—C10—H10	117.8	F23B—P2—F22B^iii	84.5 (10)
N2—C11—C7	122.3 (4)	F21^iii—P2—F22B^iii	76.6 (9)
N2—C11—C12	117.6 (4)	F21—P2—F22B^iii	76.7 (10)
C7—C11—C12	120.0 (4)	F23A^iii—P2—F22B^iii	90.5 (15)
N1—C12—C4	121.8 (4)	F23A—P2—F22B^iii	120.4 (9)
N1—C12—C11	118.3 (4)	F22A^iii—P2—F22B	172 (2)
C4—C12—C11	119.8 (4)	F23B^iii—P2—F22B	84.5 (10)
N3—C13—C14	123.8 (5)	F23B—P2—F22B	117.1 (15)
N3—C13—H13	118.1	F21^iii—P2—F22B	76.7 (10)
C14—C13—H13	118.1	F21—P2—F22B	76.6 (9)
C15—C14—C13	118.9 (5)	F23A^iii—P2—F22B	120.4 (9)
C15—C14—H14	120.6	F23A—P2—F22B	90.5 (15)
C13—C14—H14	120.6	F22B^iii—P2—F22B	140 (3)
C14—C15—C16	120.7 (5)	P2—F22A—F23A	62.2 (12)
C14—C15—H15	119.6	P2—F23A—F22A	52.5 (5)
N1^i—Mn—N1—C1	86.2 (4)	N3^i—Mn—N2—C11	−165.1 (3)
N3^i—Mn—N1—C1	−123.9 (5)	N3—Mn—N2—C11	−90.4 (3)
N3—Mn—N1—C1	−85.6 (4)	N1—Mn—N3—C13	8.7 (4)
N2^i—Mn—N1—C1	10.2 (4)	N2^i—Mn—N3—C13	−91.3 (3)
N1^i—Mn—N1—C12	−98.9 (3)	N2—Mn—N3—C13	83.1 (3)
N3^i—Mn—N1—C12	51.0 (6)	N1^i—Mn—N3—C18	40.4 (6)
N3—Mn—N1—C12	89.4 (3)	N1—Mn—N3—C18	−169.0 (3)
N3^i—Mn—N2—C10	7.8 (3)	N2^i—Mn—N3—C18	91.0 (3)
N3—Mn—N2—C10	82.4 (3)	N2—Mn—N3—C18	−94.5 (3)

Symmetry codes: (i) −x+1, y, −z+3/2; (ii) −x, y, −z+3/2; (iii) −x, y, −z+1/2.