

Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536808021879/kp2179sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S1600536808021879/kp2179Isup2.hkl |
CCDC reference: 705932
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean
(C-C) = 0.007 Å
- R factor = 0.064
- wR factor = 0.214
- Data-to-parameter ratio = 12.4
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.24 Ratio PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.74 Ratio PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C23 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for O1 PLAT231_ALERT_4_B Hirshfeld Test (Solvent) P1 -- F1 .. 16.34 su PLAT231_ALERT_4_B Hirshfeld Test (Solvent) P1 -- F3 .. 13.72 su
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 7 PLAT360_ALERT_2_C Short C(sp3)-C(sp3) Bond C23 - C24 ... 1.36 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact F1 .. O1 .. 2.91 Ang. PLAT231_ALERT_4_C Hirshfeld Test (Solvent) P1 -- F2 .. 8.96 su PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for P1
Alert level G PLAT343_ALERT_2_G Check sp3 Angle Range in Main Residue for .. C23 PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 6 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
A mixture of manganese(III) 2,4-pentanedionate (0.5 mmol), 5,10,15,20-tetraphenyl-calix[4]pyrrole (0.5 mmol), H2O (8 ml) and ethanol (8 mL) in a 25 mL Teflon-lined stainless steel autoclave was kept at 433 K for three days. Red crystals were obtained after cooling to room temperature with a yield of 18%. Anal. Calc. for C48H38MnN4O2F6P: C 66.61, H 3.82, N 6.48%; Found: C 66.65, H 3.78, N 6.52%.
All H atoms were placed in calculated positions with C—H = 0.93Å and refined as riding with Uiso(H) = 1.2Ueq(carrier).
Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
![]() | Fig. 1. The molecular structure of (I) drawn with the 30% probability displacement ellipsoids for the non-hydrogen atoms. Symmetry codes used: - x + 2,-y,-z + 2; - x +1,-y,-z). |
[Mn(C2H5O)2(C44H28N4)]PF6 | F(000) = 928 |
Mr = 902.73 | Dx = 1.462 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 3535 reflections |
a = 10.7487 (8) Å | θ = 2.2–25.0° |
b = 16.8682 (14) Å | µ = 0.44 mm−1 |
c = 11.9913 (19) Å | T = 293 K |
β = 109.412 (9)° | Block, yellow |
V = 2050.6 (4) Å3 | 0.43 × 0.28 × 0.22 mm |
Z = 2 |
Bruker APEXII CCD area-detector diffractometer | 3535 independent reflections |
Radiation source: fine-focus sealed tube | 2142 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.040 |
ϕ and ω scans | θmax = 25.0°, θmin = 2.2° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −1→12 |
Tmin = 0.835, Tmax = 0.910 | k = −1→20 |
4407 measured reflections | l = −14→13 |
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)] = 0.063 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.214 | H-atom parameters constrained |
S = 1.00 | w = 1/[σ2(Fo2) + (0.135P)2] where P = (Fo2 + 2Fc2)/3 |
3535 reflections | (Δ/σ)max < 0.001 |
284 parameters | Δρmax = 0.33 e Å−3 |
0 restraints | Δρmin = −0.42 e Å−3 |
[Mn(C2H5O)2(C44H28N4)]PF6 | V = 2050.6 (4) Å3 |
Mr = 902.73 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 10.7487 (8) Å | µ = 0.44 mm−1 |
b = 16.8682 (14) Å | T = 293 K |
c = 11.9913 (19) Å | 0.43 × 0.28 × 0.22 mm |
β = 109.412 (9)° |
Bruker APEXII CCD area-detector diffractometer | 3535 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | 2142 reflections with I > 2σ(I) |
Tmin = 0.835, Tmax = 0.910 | Rint = 0.040 |
4407 measured reflections |
R[F2 > 2σ(F2)] = 0.063 | 0 restraints |
wR(F2) = 0.214 | H-atom parameters constrained |
S = 1.00 | Δρmax = 0.33 e Å−3 |
3535 reflections | Δρmin = −0.42 e Å−3 |
284 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Mn1 | 1.0000 | 0.0000 | 1.0000 | 0.0507 (3) | |
C1 | 0.8291 (4) | 0.0451 (2) | 0.7085 (3) | 0.0579 (10) | |
C2 | 0.8243 (4) | 0.0985 (2) | 0.7966 (4) | 0.0572 (10) | |
C3 | 0.7590 (4) | 0.1738 (3) | 0.7732 (4) | 0.0670 (12) | |
H3A | 0.7183 | 0.1961 | 0.6991 | 0.080* | |
C4 | 0.7671 (5) | 0.2059 (3) | 0.8768 (4) | 0.0680 (12) | |
H4A | 0.7311 | 0.2541 | 0.8881 | 0.082* | |
C5 | 0.8417 (4) | 0.1524 (2) | 0.9685 (4) | 0.0572 (10) | |
C6 | 0.8735 (4) | 0.1665 (2) | 1.0892 (4) | 0.0570 (10) | |
C7 | 0.9596 (4) | 0.1198 (2) | 1.1763 (4) | 0.0551 (9) | |
C8 | 1.0066 (4) | 0.1385 (3) | 1.2992 (4) | 0.0617 (10) | |
H8A | 0.9820 | 0.1821 | 1.3345 | 0.074* | |
C9 | 1.0931 (4) | 0.0817 (3) | 1.3555 (4) | 0.0598 (10) | |
H9A | 1.1410 | 0.0798 | 1.4358 | 0.072* | |
C10 | 1.0973 (4) | 0.0248 (2) | 1.2677 (3) | 0.0542 (9) | |
C11 | 0.7496 (4) | 0.0648 (2) | 0.5827 (4) | 0.0594 (10) | |
C12 | 0.8044 (5) | 0.0722 (3) | 0.4937 (4) | 0.0697 (12) | |
H12A | 0.8948 | 0.0654 | 0.5115 | 0.084* | |
C13 | 0.7273 (6) | 0.0893 (3) | 0.3793 (5) | 0.0814 (14) | |
H13A | 0.7655 | 0.0920 | 0.3202 | 0.098* | |
C14 | 0.5958 (6) | 0.1024 (3) | 0.3521 (5) | 0.0864 (16) | |
H14A | 0.5448 | 0.1156 | 0.2752 | 0.104* | |
C15 | 0.5383 (5) | 0.0959 (3) | 0.4383 (5) | 0.0862 (15) | |
H15A | 0.4481 | 0.1041 | 0.4193 | 0.103* | |
C16 | 0.6152 (5) | 0.0771 (3) | 0.5547 (4) | 0.0701 (12) | |
H16A | 0.5761 | 0.0728 | 0.6129 | 0.084* | |
C17 | 0.8100 (4) | 0.2373 (2) | 1.1233 (4) | 0.0560 (10) | |
C18 | 0.6787 (5) | 0.2366 (3) | 1.1115 (4) | 0.0735 (12) | |
H18A | 0.6285 | 0.1915 | 1.0830 | 0.088* | |
C19 | 0.6202 (5) | 0.3030 (3) | 1.1418 (5) | 0.0822 (14) | |
H19A | 0.5314 | 0.3019 | 1.1346 | 0.099* | |
C20 | 0.6936 (6) | 0.3702 (3) | 1.1824 (4) | 0.0824 (15) | |
H20A | 0.6543 | 0.4145 | 1.2027 | 0.099* | |
C21 | 0.8222 (6) | 0.3720 (3) | 1.1929 (5) | 0.0829 (14) | |
H21A | 0.8712 | 0.4178 | 1.2197 | 0.099* | |
C22 | 0.8817 (5) | 0.3065 (3) | 1.1642 (5) | 0.0742 (13) | |
H22A | 0.9707 | 0.3084 | 1.1723 | 0.089* | |
C23 | 1.2032 (10) | 0.1503 (5) | 1.0298 (13) | 0.204 (6) | |
H23A | 1.1197 | 0.1743 | 1.0256 | 0.245* | |
H23B | 1.2537 | 0.1461 | 1.1133 | 0.245* | |
C24 | 1.2665 (15) | 0.2060 (6) | 0.9868 (11) | 0.227 (6) | |
H24A | 1.2841 | 0.2517 | 1.0374 | 0.341* | |
H24B | 1.2119 | 0.2210 | 0.9086 | 0.341* | |
H24C | 1.3481 | 0.1846 | 0.9839 | 0.341* | |
P1 | 0.5000 | 0.0000 | 0.0000 | 0.1018 (9) | |
N1 | 0.8781 (3) | 0.0872 (2) | 0.9162 (3) | 0.0541 (8) | |
N2 | 1.0169 (3) | 0.05011 (19) | 1.1572 (3) | 0.0552 (8) | |
F1 | 0.6259 (11) | 0.0076 (5) | 0.0792 (8) | 0.217 (3) | |
F2 | 0.4786 (14) | 0.0803 (9) | −0.0209 (16) | 0.350 (8) | |
F3 | 0.460 (2) | 0.0081 (15) | 0.0848 (14) | 0.387 (10) | |
O1 | 1.1729 (3) | 0.07288 (19) | 0.9912 (3) | 0.0787 (10) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.0513 (5) | 0.0471 (5) | 0.0521 (5) | 0.0032 (3) | 0.0152 (4) | −0.0035 (3) |
C1 | 0.062 (2) | 0.057 (2) | 0.052 (2) | 0.0003 (19) | 0.0165 (19) | −0.0015 (18) |
C2 | 0.056 (2) | 0.058 (2) | 0.055 (2) | 0.0046 (19) | 0.0136 (18) | 0.0003 (18) |
C3 | 0.077 (3) | 0.055 (2) | 0.059 (2) | 0.014 (2) | 0.010 (2) | 0.0028 (19) |
C4 | 0.076 (3) | 0.056 (2) | 0.069 (3) | 0.017 (2) | 0.021 (2) | 0.000 (2) |
C5 | 0.057 (2) | 0.054 (2) | 0.060 (2) | 0.0050 (18) | 0.0173 (19) | −0.0075 (18) |
C6 | 0.058 (2) | 0.049 (2) | 0.064 (2) | −0.0013 (18) | 0.0195 (19) | −0.0075 (18) |
C7 | 0.057 (2) | 0.052 (2) | 0.059 (2) | 0.0011 (18) | 0.0225 (19) | −0.0026 (18) |
C8 | 0.073 (3) | 0.054 (2) | 0.060 (2) | 0.003 (2) | 0.024 (2) | −0.0111 (19) |
C9 | 0.066 (3) | 0.057 (2) | 0.053 (2) | 0.004 (2) | 0.0163 (19) | −0.0026 (19) |
C10 | 0.058 (2) | 0.051 (2) | 0.053 (2) | −0.0007 (19) | 0.0185 (19) | −0.0005 (17) |
C11 | 0.068 (3) | 0.050 (2) | 0.057 (2) | −0.0011 (19) | 0.016 (2) | −0.0018 (18) |
C12 | 0.071 (3) | 0.071 (3) | 0.065 (3) | −0.001 (2) | 0.019 (2) | 0.005 (2) |
C13 | 0.098 (4) | 0.078 (3) | 0.066 (3) | 0.001 (3) | 0.026 (3) | 0.010 (2) |
C14 | 0.095 (4) | 0.089 (4) | 0.060 (3) | −0.005 (3) | 0.005 (3) | 0.008 (3) |
C15 | 0.071 (3) | 0.086 (4) | 0.083 (3) | 0.008 (3) | 0.002 (3) | 0.004 (3) |
C16 | 0.062 (3) | 0.078 (3) | 0.065 (3) | 0.003 (2) | 0.014 (2) | 0.002 (2) |
C17 | 0.056 (2) | 0.054 (2) | 0.057 (2) | 0.0087 (19) | 0.0183 (18) | −0.0007 (18) |
C18 | 0.067 (3) | 0.061 (3) | 0.092 (3) | 0.004 (2) | 0.026 (2) | −0.009 (2) |
C19 | 0.073 (3) | 0.083 (3) | 0.098 (4) | 0.019 (3) | 0.038 (3) | 0.000 (3) |
C20 | 0.115 (5) | 0.065 (3) | 0.070 (3) | 0.031 (3) | 0.035 (3) | −0.004 (2) |
C21 | 0.095 (4) | 0.062 (3) | 0.093 (4) | 0.006 (3) | 0.031 (3) | −0.015 (3) |
C22 | 0.074 (3) | 0.057 (3) | 0.093 (3) | −0.004 (2) | 0.030 (3) | −0.015 (2) |
C23 | 0.187 (9) | 0.105 (6) | 0.404 (18) | −0.072 (6) | 0.210 (11) | −0.095 (9) |
C24 | 0.39 (2) | 0.111 (7) | 0.234 (13) | −0.052 (10) | 0.170 (13) | −0.041 (7) |
P1 | 0.0807 (16) | 0.1047 (19) | 0.1054 (19) | 0.0316 (13) | 0.0113 (14) | −0.0304 (15) |
N1 | 0.0532 (18) | 0.0542 (18) | 0.0538 (18) | 0.0027 (15) | 0.0164 (15) | −0.0062 (14) |
N2 | 0.0538 (19) | 0.0549 (19) | 0.0559 (18) | 0.0009 (15) | 0.0171 (15) | −0.0046 (15) |
F1 | 0.216 (9) | 0.238 (8) | 0.206 (8) | −0.015 (6) | 0.080 (7) | −0.014 (5) |
F2 | 0.338 (16) | 0.247 (13) | 0.40 (2) | 0.005 (12) | 0.030 (15) | −0.013 (13) |
F3 | 0.346 (19) | 0.47 (2) | 0.288 (18) | 0.205 (16) | 0.030 (14) | 0.022 (15) |
O1 | 0.0648 (19) | 0.0609 (19) | 0.116 (3) | −0.0143 (15) | 0.0377 (19) | −0.0146 (18) |
Mn1—N1 | 2.004 (3) | C13—C14 | 1.358 (8) |
Mn1—N1i | 2.004 (3) | C13—H13A | 0.9300 |
Mn1—N2 | 2.018 (3) | C14—C15 | 1.373 (8) |
Mn1—N2i | 2.018 (3) | C14—H14A | 0.9300 |
Mn1—O1i | 2.260 (3) | C15—C16 | 1.402 (7) |
Mn1—O1 | 2.260 (3) | C15—H15A | 0.9300 |
C1—C10i | 1.395 (6) | C16—H16A | 0.9300 |
C1—C2 | 1.403 (6) | C17—C18 | 1.371 (6) |
C1—C11 | 1.504 (6) | C17—C22 | 1.394 (6) |
C2—N1 | 1.369 (5) | C18—C19 | 1.390 (7) |
C2—C3 | 1.432 (6) | C18—H18A | 0.9300 |
C3—C4 | 1.331 (6) | C19—C20 | 1.375 (8) |
C3—H3A | 0.9300 | C19—H19A | 0.9300 |
C4—C5 | 1.442 (6) | C20—C21 | 1.346 (8) |
C4—H4A | 0.9300 | C20—H20A | 0.9300 |
C5—N1 | 1.386 (5) | C21—C22 | 1.377 (7) |
C5—C6 | 1.393 (6) | C21—H21A | 0.9300 |
C6—C7 | 1.388 (6) | C22—H22A | 0.9300 |
C6—C17 | 1.497 (5) | C23—C24 | 1.358 (11) |
C7—N2 | 1.381 (5) | C23—O1 | 1.388 (8) |
C7—C8 | 1.425 (6) | C23—H23A | 0.9700 |
C8—C9 | 1.348 (6) | C23—H23B | 0.9700 |
C8—H8A | 0.9300 | C24—H24A | 0.9600 |
C9—C10 | 1.436 (6) | C24—H24B | 0.9600 |
C9—H9A | 0.9300 | C24—H24C | 0.9600 |
C10—N2 | 1.387 (5) | P1—F3 | 1.23 (2) |
C10—C1i | 1.395 (6) | P1—F3ii | 1.23 (2) |
C11—C12 | 1.385 (6) | P1—F1ii | 1.376 (11) |
C11—C16 | 1.385 (6) | P1—F1 | 1.376 (11) |
C12—C13 | 1.378 (7) | P1—F2 | 1.382 (15) |
C12—H12A | 0.9300 | P1—F2ii | 1.382 (15) |
N1—Mn1—N1i | 180.000 (1) | C14—C15—H15A | 119.9 |
N1—Mn1—N2 | 90.13 (13) | C16—C15—H15A | 119.9 |
N1i—Mn1—N2 | 89.87 (13) | C11—C16—C15 | 119.8 (5) |
N1—Mn1—N2i | 89.87 (13) | C11—C16—H16A | 120.1 |
N1i—Mn1—N2i | 90.13 (13) | C15—C16—H16A | 120.1 |
N2—Mn1—N2i | 180.000 (1) | C18—C17—C22 | 118.2 (4) |
N1—Mn1—O1i | 90.70 (13) | C18—C17—C6 | 120.8 (4) |
N1i—Mn1—O1i | 89.30 (13) | C22—C17—C6 | 121.0 (4) |
N2—Mn1—O1i | 90.25 (13) | C17—C18—C19 | 120.4 (5) |
N2i—Mn1—O1i | 89.75 (13) | C17—C18—H18A | 119.8 |
N1—Mn1—O1 | 89.30 (13) | C19—C18—H18A | 119.8 |
N1i—Mn1—O1 | 90.70 (13) | C20—C19—C18 | 120.0 (5) |
N2—Mn1—O1 | 89.75 (13) | C20—C19—H19A | 120.0 |
N2i—Mn1—O1 | 90.25 (13) | C18—C19—H19A | 120.0 |
O1i—Mn1—O1 | 180.0 | C21—C20—C19 | 120.2 (5) |
C10i—C1—C2 | 123.3 (4) | C21—C20—H20A | 119.9 |
C10i—C1—C11 | 119.2 (4) | C19—C20—H20A | 119.9 |
C2—C1—C11 | 117.5 (4) | C20—C21—C22 | 120.4 (5) |
N1—C2—C1 | 126.2 (4) | C20—C21—H21A | 119.8 |
N1—C2—C3 | 109.7 (4) | C22—C21—H21A | 119.8 |
C1—C2—C3 | 124.1 (4) | C21—C22—C17 | 120.8 (5) |
C4—C3—C2 | 107.6 (4) | C21—C22—H22A | 119.6 |
C4—C3—H3A | 126.2 | C17—C22—H22A | 119.6 |
C2—C3—H3A | 126.2 | C24—C23—O1 | 128.0 (9) |
C3—C4—C5 | 107.7 (4) | C24—C23—H23A | 105.3 |
C3—C4—H4A | 126.1 | O1—C23—H23A | 105.3 |
C5—C4—H4A | 126.1 | C24—C23—H23B | 105.3 |
N1—C5—C6 | 126.7 (4) | O1—C23—H23B | 105.3 |
N1—C5—C4 | 108.7 (3) | H23A—C23—H23B | 106.0 |
C6—C5—C4 | 124.6 (4) | C23—C24—H24A | 109.5 |
C7—C6—C5 | 123.8 (4) | C23—C24—H24B | 109.5 |
C7—C6—C17 | 119.9 (4) | H24A—C24—H24B | 109.5 |
C5—C6—C17 | 116.3 (4) | C23—C24—H24C | 109.5 |
N2—C7—C6 | 125.6 (4) | H24A—C24—H24C | 109.5 |
N2—C7—C8 | 109.6 (3) | H24B—C24—H24C | 109.5 |
C6—C7—C8 | 124.8 (4) | F3—P1—F3ii | 180 (2) |
C9—C8—C7 | 108.0 (4) | F3—P1—F1ii | 92.8 (9) |
C9—C8—H8A | 126.0 | F3ii—P1—F1ii | 87.2 (9) |
C7—C8—H8A | 126.0 | F3—P1—F1 | 87.2 (9) |
C8—C9—C10 | 107.0 (4) | F3ii—P1—F1 | 92.8 (9) |
C8—C9—H9A | 126.5 | F1ii—P1—F1 | 180.0 (13) |
C10—C9—H9A | 126.5 | F3—P1—F2 | 87.6 (9) |
N2—C10—C1i | 125.9 (4) | F3ii—P1—F2 | 92.4 (9) |
N2—C10—C9 | 109.4 (4) | F1ii—P1—F2 | 84.2 (6) |
C1i—C10—C9 | 124.7 (4) | F1—P1—F2 | 95.8 (6) |
C12—C11—C16 | 118.4 (4) | F3—P1—F2ii | 92.4 (9) |
C12—C11—C1 | 123.1 (4) | F3ii—P1—F2ii | 87.6 (9) |
C16—C11—C1 | 118.4 (4) | F1ii—P1—F2ii | 95.8 (6) |
C13—C12—C11 | 121.1 (5) | F1—P1—F2ii | 84.2 (6) |
C13—C12—H12A | 119.4 | F2—P1—F2ii | 180.0 (3) |
C11—C12—H12A | 119.4 | C2—N1—C5 | 106.2 (3) |
C14—C13—C12 | 120.4 (5) | C2—N1—Mn1 | 127.3 (3) |
C14—C13—H13A | 119.8 | C5—N1—Mn1 | 126.3 (3) |
C12—C13—H13A | 119.8 | C7—N2—C10 | 105.9 (3) |
C13—C14—C15 | 120.0 (5) | C7—N2—Mn1 | 127.2 (3) |
C13—C14—H14A | 120.0 | C10—N2—Mn1 | 126.7 (3) |
C15—C14—H14A | 120.0 | C23—O1—Mn1 | 127.0 (4) |
C14—C15—C16 | 120.2 (5) |
Symmetry codes: (i) −x+2, −y, −z+2; (ii) −x+1, −y, −z. |
Experimental details
Crystal data | |
Chemical formula | [Mn(C2H5O)2(C44H28N4)]PF6 |
Mr | 902.73 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 10.7487 (8), 16.8682 (14), 11.9913 (19) |
β (°) | 109.412 (9) |
V (Å3) | 2050.6 (4) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.44 |
Crystal size (mm) | 0.43 × 0.28 × 0.22 |
Data collection | |
Diffractometer | Bruker APEXII CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2001) |
Tmin, Tmax | 0.835, 0.910 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 4407, 3535, 2142 |
Rint | 0.040 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.063, 0.214, 1.00 |
No. of reflections | 3535 |
No. of parameters | 284 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.33, −0.42 |
Computer programs: APEX2 (Bruker, 2004), SAINT-Plus (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
Mn1—N1 | 2.004 (3) | Mn1—O1 | 2.260 (3) |
Mn1—N2 | 2.018 (3) | ||
N1—Mn1—N2 | 90.13 (13) | N2—Mn1—O1i | 90.25 (13) |
N1—Mn1—O1i | 90.70 (13) | N2—Mn1—O1 | 89.75 (13) |
Symmetry code: (i) −x+2, −y, −z+2. |
In recent years, nitrogen-containing organics have been widely used as polydentate ligands, which can coordinate to transition or rare earth ions yielding complexes with interesting properties that are useful in materials science (Church & Halvorson, 1959; Chung et al., 1971) and in biological systems (Okabe & Oya, 2000; Serre et al., 2005; Pocker & Fong, 1980; Scapin et al., 1997). Herein, we report the synthesis and X-ray crystal structure analysis of the title compound, {[5,10,15,20-tetraphenyl-calix[4]pyrrole]manganese(III) bis-ethanol} hexafluorophosphate.
The MnIII ion is hexa-coordinated with four N atoms from one 5,10,15,20-tetraphenyl-calix[4]pyrrole ligand and two O atoms from two ethanol molecules (Fig. 1). One hexafluorophosphate anion acts as charge balance. MnIII is located at the inversion centre and the asymmetric unit comprises one-half molecule. The MnIII ion is hexa-coordinated with four N atoms from one 5,10,15,20-tetraphenyl-calix[4]pyrrole ligand and two O atoms from two ethanol molecules. The equatorially located atoms Mn(1), N(1), N(2), N(1 A), and N(2 A) are planar. The dihedral angles between the planes of Ph rings [C(11), C(12), C(13), C(14), C(15), C(16)] and [C(17), C(18), C(19), C(20), C(21), C(22)] and quatorial plane are 53.3 (2) and 81.8 (2) Å, respectively. The Mn—N and Mn—O bond lengths are in the range of 2.004 (3)–2.018 (3) and 2.260 (3) Å, respectively (Table 1).